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Commercial Report List

Office contact information:

Telephone: +44 (0) 1234 750 422 The Fluid Engineering Centre Facsimile: +44 (0) 1234 750 074 Cranfield, Bedfordshire Email: [email protected] MK43 0AJ Website: www.bhrgroup.com United Kingdom

Registered in England No 2420351 Global Experts in Fluid Engineering

DOM01 March 2008

DOMINO Workplans for 2007-2008 (Draft Workplans released in December 2007)

Gűl N. Őzcan

DOM02 February 2008

Dispersion of Nanoparticle Clusters in Liquids

Gűl N. Őzcan

Executive Summary

This report is prepared for DOMINO members to provide background on the break up of nanoparticle clusters in a liquid. Following on from a description of the process, the incorporation of nanoparticles in a liquid and break up of these are presented. Information on the different types of equipment widely used in industry is also given. DOM03 March 2008 Rheology of Fine Particle Suspensions Neil J Alderman DOM04 April 2008 Draft Design Procedures for the Dispersion of Nanoparticle Clusters V2 September 2013 DOM05 November 2008 Effect of Rotor-stator Geometry on Power and Flow Characteristics of Three in-line Rotor-Stators Gűl N. Őzcan, Dominik Kubicki, Gustavo A Padron Executive Summary

This report details the results of a study undertaken within DOMINO on the power and flow characteristics of three in-line rotor-stators. These devices were also used to investigate the break up process of nanoparticle clusters within DOMINO.

The overall objective of the single phase study has been to: highlight the differences in the power and flow characteristics of three different mixer heads which would contribute towards the explanation of the results from break-up studies and ultimately on the discussions related to the choice of mixer head for this application.



Telephone: +44 (0) 1234 750 422 BHR Group Facsimile: +44 (0) 1234 750 074 The Fluid Engineering Centre Email: [email protected] Cranfield, Bedfordshire Website: www.bhrgroup.com MK43 0AJ

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BHR Group is a trading name of VirtualPiE Limited A company registered in England No 07274578

Global Experts in Fluid Engineering

The three devices studied were:

inner General Purpose Disintegrating Head (GPDH) and an outer Square Hole Screen (SQHS),

dual Emulsor screen (EMSC) from Silverson and

Z unit from Ytron.

DOM06 May 2009

Effect of rotor-stator geometry on break up of silica nanoparticle clusters

Gűl N. Őzcan, Gustavo A Padron Executive Summary

In-line rotor-stator mixers are used in a wide range of energy intensive applications in the chemicals, food, personal, health care and applications numerous other applications for foam generation, chemical reactions, break up of liquid droplets or particle clusters. However there is limited published work on their performance and often process design and equipment selection must be done on a trial-and-error basis. This report presents the results of our study on the comparative performance of three different rotor-stator geometries for the break-up of nanoscale fumed silica clusters:

Silverson/GPDH-SQHS,

Silverson/EMSC and

Ytron Z.

DOM07 December 2008

DOMINO Workplans for 2008-2009

Gűl N. Őzcan Executive Summary

This document provides the details of the work programme of DOMINO 2008-09 proposed for voting to the consortium members. Following on from a description of the project, the outlines of the proposed Work Packages are given in Section 3. The document will be finalised after the votes are received and work programme finalised based on this.




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DOM08 December 2008

Results from preliminary experiments with two nanoclays

Neil J Alderman, Ainee Cheah, N. Gűl N. Őzcan, Gustavo A Padron Executive Summary

In this report, findings from an initial study with two nanoclays are presented.

Either an ultrasonic device or a stirred vessel equipped with a sawtooth impeller was used to prepare the dispersions. Samples taken at regular intervals under different operating conditions have been analysed through particle size measurements, X-Ray diffraction, rheology measurements and electron microscopy to monitor the dispersion process.

DOM09 June 2009

Particle-liquid affinity- DOMINO Results from 2007-08

Neil J Alderman, Ainee Cheah, Gűl N. Őzcan, Gustavo A Padron Executive Summary

In this report, findings from the first year programme of DOMINO are presented on particle-liquid affinity. The study was carried out using two types of nanoscale fumed silica particles:

Aerosil 200V (hydrophilic)

Aerosil R816 in two liquids, both of a similar viscosity of about 10 mPa s:

glycerol solution and

silicone oil Findings on incorporation of particles in a stirred tank using a narrow blade hydrofoil, rheology of dispersions from break up experiments and break up kinetics obtained using a large scale in-line rotor-stator and a small scale ultrasonic disperser are reported.




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DOM10 June 2009 Results from preliminary experiments on break up of nanoscale silica particles using the Microfluidics M-110P Dominik Kubicki Executive Summary This report details the preliminary results on the breakage of nanoscale silica particle clusters in a microfluidizer, Microfluidics M-110P. The objectives of this work have been to:

- determine the range of operating conditions - identify any difficulties that may be encountered during equipment operation and - make an initial assessment of the performance of this device.

DOM11 June 2009 Results of a preliminary study on particle incorporation using the Ytron Y Jet Mixer Gűl N. Őzcan Executive Summary Findings from a preliminary study on the incorporation of nanoscale silica particles using the Ytron Y Jet mixer are presented in this report. The study was carried out within the work package C1 of DOMINO 2008-09 programme at a low solids concentration of 1% (w:w) and within B.2- Effect of solids concentration for higher concentrations of up to 10%. Ytron Y Jet device consists of an axial flow impeller mounted in a draft tube (or stator) positioned off-centre, close to the base of an unbaffled tank. A feed tube connected to a funnel (or hopper as referred to by manufacturers) is intended to introduce the particles into the impeller region. A small scale vessel of 0.29 m diameter was used for the study. Experimental work included determining:

power characteristics for different configurations;

surface aeration conditions;

drawdown rate over a range of power input values;

effect of vessel and mixer unit configuration and

effect of solids concentration. Results and overall trends are also compared with the published data from another project, PROFORM.




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DOM12 December 2009 DOMINO Final Workplans for 2009-2010 Gűl N. Őzcan Executive Summary

This document details the work programme of DOMINO for 2009-10. DOM13 January 2010 Effect of dispersion methods on the delamination of two types of nanoclay (Cloisite 30B in Daltocel and Cloisite Na+ in water) Neil J Alderman, Ainee Cheah, Gűl N. Őzcan, Gustavo A Padron Executive Summary In this report, findings from a study on the importance of different dispersion technologies are presented for two types of nanoclay dispersions. The dispersion devices used were:

1. Hielscher UP200S 24kHz ultrasound disperser in a tank fitted with a PBT

covering a specific power input range of about 40-80 Wkg-1;

2. Lightnin A310 impeller in a tank at a specific power input of about 0.1 Wkg-1; 3. saw tooth high shear impeller in a tank at a specific power input of about 5 Wkg-1; 4. Hielscher UP200S 24kHz ultrasound disperser within a flow cell in the circulation loop of a stirred tank equipped with the large ICI impeller covering a specific power input range of about 40-80 Wkg-1. Samples taken at regular intervals under different operating conditions have been analysed through particle size measurements, X-Ray diffraction, rheology measurements and electron microscopy to monitor the dispersion process. DOM14 March 2010 Literature review on break up of nanoparticle clusters with high pressure jets and valve homogenisers Gűl N. Őzcan Executive Summary This report provides a review of literature on the break up of nanoparticle clusters using high pressure jets and valve homogenisers.




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DOM15 February 2010 Literature review on break up of nanoparticle clusters using stirred bead mills Emmanuela Gavi Executive Summary This report is prepared for DOMINO members to provide background on stirred bead mills and on their application for efficient nanoparticle dispersion. Following on from a description of the equipment, its working principles and operating conditions, some recent advances on nanomilling and modelling of the grinding process in the bead mill are discussed. Information on the different types of equipment widely used in industry is also given. DOM16 April 2010 Effect of residence time in an in-line rotor-stator on break up of silica nanoparticle clusters Gustavo A Padron Executive Summary In-line rotor-stator mixers are used in a wide range of energy intensive applications in the chemicals, food, personal, health care applications and numerous other applications for example, foam generation, chemical reactions, break up of liquid droplets or particle clusters. However, there is limited published work on their performance and often process design and equipment selection must be done on a trial-and-error basis. This report evaluates the effect of residence time within the rotor-stator on the de-agglomeration of fumed silica clusters. The rotor-stator used was a Silverson 150/250MS with a dual EMSC stator. Residence time was varied by either changing the batch size or flow rate. DOM17 May 2010 Preliminary experiments with hydrophilic and hydrophobic zinc oxides Gustavo A Padron Executive Summary Zinc oxide has many industrial applications such as cosmetic UV protection and the production of UV-protected coatings and polymers. It has also potential uses in areas such as cross-linking, chemical catalysis and corrosion protection. It is therefore of interest to determine the best ways to finely disperse ZnO particles in order to take full advantage of their potential. This document reports the findings from the studies undertaken within DOMINO in 2007-08 and 2008-09 using different types of zinc oxide.




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Work has been carried out with three zinc oxides: two naturally hydrophilic manufactured by different processes and one whose surface has been treated to become hydrophobic (VP AdNano Z 805). Also, three different dispersing agents have been tested. The dispersions were produced using an ultrasound disperser. Results for particle size, viscosity, zeta potential and SEM imaging will be shown. An optimised PSD measurement procedure was developed for ZnO dispersions due to their tendency to dissolve and/or settle during analysis. This was done to ensure the reliability of the results. DOM18 May 2010 Population Balance Modelling of the break up of nanoscale silica agglomerates using an in-line rotor-stator: effect of power input, flow rate and particle concentration Dominik Kubicki Executive Summary This report presents the results of numerical modelling of the nanoparticle breakage process. The breakage of Aerosil 200V nanoparticle clusters processed in an in-line rotor-stator device is modelled. The numerical model assumes a simple 1D flow pattern in the system. The evolution of particle size distribution is modelled using the discrete form of population balance equations. The results of numerical simulations are compared with experimental data. Four different breakage mechanisms are studied: erosion, shattering, rupture and binary breakage. Effects of three parameters are investigated: power input, flow rate and particle concentration. DOM19 May 2010 Effect of Particle Concentration on the Performance of Microfluidizer for Breaking up Silica Particles Emmanuela Gavi Executive Summary

Microfluidics M110-P was used within DOMINO in a preliminary study on the break up of a 1% silica dispersion (DOM10). Those first results raised sufficient interest to investigate further the performance of this device at higher particle concentrations. This has been the motivation of the study documented in this report.




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DOM20 May 2010 Effect of Continuous Phase Viscosity on Break Up of Silica Nanoparticles using Microfluidics M-110P Emmanuela Gavi Executive Summary Microfluidics M110-P was used within DOMINO in a preliminary study on the break up of a 1% silica dispersion and this study carried on the investigation and is aimed at testing the effectiveness of operation of the Microfluidizer with increasing continuous phase viscosity. The results are compared with previous results from Rotor-Stator and Ultrasonic devices. DOM21 August 2010 Break up of Zinc Oxide Nanoparticle Clusters Using Surfactants and Microfluidics M-110P Emmanuela Gavi, Gustavo A Padron Executive Summary This document reports the findings from the studies on the dispersion of zinc oxide clusters within DOMINO in 2009-10. Work carried out has two strands: The first set of experiments was aimed at verifying if a polymeric surfactant with a high molecular weight, used in the early work during 2008-09, prevented zinc oxide agglomerates from breaking up by binding particles together. With this objective the stabilising agent Tergitol NP-9, was chosen because of its low molecular weight. The second set of experiments aimed at verifying if a higher energy intensive device may achieve a higher fines volume fraction than the ultrasonic processor. DOM22 October 2010 Effect of Solids Concentration on Break Up of Silica Nanoparticle Clusters with an In-Line Rotor-Stator and an Ultrasound Disperser Neil J Alderman, Dominik Kubicki, Gustavo A Padron Executive Summary Within DOMINO, in-line rotor-stators and ultrasound processors have been used to investigate the break up of nanoparticle clusters. Many nanoparticle break up applications require the processing of dispersions with high solids loadings. Therefore, it is important to understand how solids concentration affects the performance of the process equipment used.




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In this report, results on the effect of solids concentrations up to 15%wt in an in-line rotor-stator mixer (Silverson 150/250MS) and an ultrasound disperser (Hielscher UP200S) on the de-agglomeration rate of fumed silica particle clusters are presented. The effect of solids concentration on dispersion rheology was also investigated and used in the interpretation of the break up results. DOM23 September 2010 Particle-Liquid Affinity - DOMINO results from 2008-2010 Ainee Cheah, Gustavo A Padron, Gűl N. Őzcan

Executive Summary

Findings from 2008 - 2010 programme of DOMINO on particle-liquid affinity are summarised in this report. These studies have been undertaken with a different continuous phase (Dipropylene glycol dimethylether) and a different type of hydrophobic nanoscale fumed silica (Aerosil® R202) particles. DOM24 September 2010 CFD model of flow generated by an ultrasonic disperser Dominik Kubicki Executive Summary This report presents the results of numerical modelling using Computational Fluid Dynamics (CFD) of the flow field generated using an ultrasonic disperser.

The model consists of two parts. First, the acoustic pressure distribution is solved using finite element solver Elmer, then acoustic pressure distribution is used to model cavitation in Fluent. DOM25 December 2010 DOMINO Final Workplans for 2010 – 2011 Gűl N. Őzcan, Gustavo A Padron, Neil J Alderman, Ainee Cheah, Emmanuela Gavi, Dominik Kubicki Executive Summary In this report the workprogramme of DOMINO for 2010 – 2011 is presented. For completeness, first a description of the project is given in Sections 2 and 3, proposed workpackages are presented in Section 4 and Section 5 contains the WorkPackages that will be undertaken in this period based on the votes received from members.




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DOM26 January 2011 Effect of Continuous Phase Viscosity on Break Up of Silica Nanoparticle Clusters with an In-Line Rotor-Stator Gustavo A Padron Executive Summary Within DOMINO, in-line rotor-stators have been used to investigate the break up of nanoparticle clusters. In this report, results on the effect of continuous phase viscosity on the mechanisms and rate of de-agglomeration of fumed silica particle clusters in an in-line rotor-stator mixer are presented. The viscosity of the continuous phase was varied from 1 to 100 mPa·s by using aqueous glycerol solutions of different concentrations. The rotor-stator evaluated was the Silverson 150/250MS equipped with a dual Emulsor screen (EMSC). Results are compared to those previously obtained using the same particle/fluid systems with a batch ultrasound disperser and a high pressure microfluidiser. DOM27 January 2011 Particle incorporation using the large scale Ytron Y Jet (T= 0.61 m) Gűl N. Őzcan Executive Summary Ytron Y Jet, is a commercially available mixing unit, designed for the incorporation of fine powders into liquids. It consists of an axial flow impeller (operated in down pumping mode) placed in a short draft tube (or stator) and is recommended to be used in an unbaffled tank at an off-centre position as close to the vessel base/corner as practicably possible. A feed tube, which is part of the unit, allows the addition to be made into the impeller region from a funnel (or hopper at industrial scale). Following on from the preliminary studies carried out within DOMINO in 2008-09 using a small tank (T= 0.29 m), further work with Ytron Y Jet has been undertaken in a T= 0.61 m diameter vessel to assess the performance of this device. Findings from this large scale vessel are presented in this report. DOM28 February 2011 Particle incorporation using an in-line rotor-stator Ytron ZC1 Gűl N. Őzcan Executive Summary Ytron ZC1 is a commercially available in-line rotor-stator, designed for the incorporation of fine powders into liquids.




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Exploratory work has been undertaken with this unit within DOMINO for an initial assessment of its performance with a view to undertake more detailed work in the future. DOM29 July 2011 Break up of Aerosil200V nanoparticles in the WAB Stirred Bead Mill (Multilab Mill) Emmanuela Gavi Executive Summary The report presents the results of an experimental programme carried out in 2010-2011 to evaluate the performance of Willy A. Bachofen Multilab Mill, a device recently made available within DOMINO in comparison to other process devices studied within DOMINO. Test media used were dispersions of nanoscale silica particles (Aerosil 200V) in water. DOM30 July 2011 Effect of manufacturing process on the break-up of silica nanoparticle clusters: wet synthesis (precipitation) and flame pyrolysis Emmanuela Gavi, Gustavo A Padron Executive Summary This document reports the outcome of the first stage of an investigation on the breakup of silica particles produced through different manufacturing processes. DOMINO used nanoparticles manufactured through flame hydrolysis as this is a technique commonly used for the manufacture of large quantities of particles. In this set of experiments, particles manufactured through a different route, namely wet precipitation, are used to study the break up process in water. DOM31 October 2011 Milling zinc oxide with the WAB Multilab Mill Emmanuela Gavi Executive Summary The present study explores the break-up process of a type of zinc oxide using the Willy A. Bachofen Multilab Mill. The experimental work was carried out within the DOMINO work programme of 2010-2011. Results are analysed and compared with other process devices used in the past within DOMINO to deagglomerate zincoxide: the Microfluidizer and the ultrasound processor.




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DOM32 October 2011 Importance of rheology on break up of nanoscale silica particles using an in-line rotor-stator Gustavo A Padron, Olga Narducci, Emmanuela Gavi, Gűl N. Őzcan Executive Summary Within DOMINO, in-line rotor-stators have been used to investigate the break-up of nanoparticle clusters. This study follows on from the work carried out with Aerosil 200V in water and viscous Newtonian fluids of 10 and 100 mPa s glycerol solutions presented in DOM26 (Padron, 2011). It extends the previous work to an additional Newtonian viscosity and pseudoplastic fluids:

Newtonian glycerol solution at a viscosity of ~ 40 mPa·s,

CMC solutions with K= 0.095 Pa sn, n = 0.92,

Carbopol solution with K= 0.157 Pa sn, n = 0.74. The rotor-stator used was the Silverson 150/250MS equipped with a dual Emulsor screen (EMSC). DOM33 October 2011 Particle incorporation using the large scale Ytron Y Jet (T= 0.61m)- effect of liquid height and increased particle concentration Gűl N. Őzcan Executive Summary Ytron Y Jet, is a commercially available mixing unit, designed for the incorporation of fine powders into liquids. It consists of an axial flow impeller (operated in down pumping mode) placed in a short draft tube (or stator) which has baffles attached. It is recommended to be used in an unbaffled tank at an off-centre position as close to the vessel base/corner as practicably as possible. A feed tube, which is part of the unit, allows the addition to be made into the impeller region from a funnel (or a hopper with industrial scale mixer units). Following on from the preliminary studies carried out within DOMINO in 2008-09 using a small tank (T= 0.29 m), a series of experiments have been conducted using Ytron Y Jet in a tank of T= 0.61 m to assess the performance of this device at a larger scale. Findings obtained in 2009-10 on the rate of drawdown of silica nanoparticles at different power input values and the effect of increasing concentration up to 10% by weight were reported in DOM27. The study included different addition methods (using a hose attached to feed tube or a funnel) and importance of configuration (centrally mounted impeller in a baffled tank). Comparisons were also shown with previous findings from DOMINO and PROFORM. More recent work concentrated on the effect of liquid height and increasing concentration above




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10%. Related results detailed in this report have shown that drawdown rate with the liquid height lowered to H=0.6T is comparable to that at H=T. DOM34 September 2011 Numerical Modelling of the Flow Field Generated by an Ultrasonic Processor Dominik Kubicki Executive Summary This report presents the results of numerical modelling using Computational Fluid Dynamics (CFD) of the flows generated using an ultrasonic disperser. Two configurations were considered: i) Ultrasonic probe placed in a flow cell in the recirculation loop of a stirred tank and ii) Ultrasonic probe placed in a stirred tank along with an impeller and operated as a batch system (both equipment positioned off-centre). Different modelling approaches were used for these two systems. “Flow cell case” was modelled in Fluent making assumptions of the distribution of acoustic pressure. “Stirred tank case” was modelled in OpenFOAM and acoustic pressure was calculated using Elmer, allowing damping effects due to presence of gas phase to be taken into account. DOM35 October 2011 Delamination of Cloisite Na+ at large scale (with an in-line rotor-stator) Emmanuela Gavi, Gustavo A Padron Executive Summary Until 2010-11, the work within DOMINO on the delamination of nanoclays has been conducted using an ultrasonic disperser in either a small scale stirred tank or in a flow cell used in the circulation loop of a stirred tank. In this more recent work, one of the nanoclays studied in small scale, Closite Na+, was chosen to disperse in water using a large scale equipment, the in-line rotor-stator, Silverson 150/250MS. This was equipped with the dual Emulsor screen (EMSC) and used in the circulation loop of a 100 l tank. Cloisite Na+-in-water was selected as the model system because of its convenience to work with at a large scale in an open laboratory using a Perspex vessel. This dispersion does not require temperature control and the cost associated with the experimental work is more reasonable with water being used as the continuous phase rather than a polyol.




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DOM36 October 2011 DOMINO- Proposed workplans for 2011-2012 Gűl N. Őzcan, Neil J Alderman, Gustavo A Padron, Emmanuela Gavi, Dominik Kubicki Executive Summary

In this report the proposed workprogramme of DOMINO for 2011 – 2012 is presented. For completeness, first a description of the project is given in Sections 2 and 3, proposed workpackages are presented in Section 4. DOM37 October 2011 Population balance simulations for break up of nanoparticle clusters using an inline rotor-stator. Dominik Kubicki Executive Summary

This report summarises the latest simulations of the evolution of particle size distributions calculated using a simple 1D model. The model used in this work is described in detail in report DOM18 (Kubicki, 2010). Further changes were made to the model to obtain better predictions in comparison to experimental data. The distribution of turbulent energy dissipation rate was refined in order to take into account the number of screens of the inline rotor-stator. Also a bypass was introduced that takes into account some complexity of the flow field within inline rotor-stator. The breakage mechanism for very large clusters at the start of the process (agglomerates in the hand-prepared pre-dispersion which have very loose bonds) is different from agglomerates achieved shortly after the process has started and this was taken into account by introducing a rupture breakage mechanism for particles larger than 30 μm. Effects of geometry, viscosity and residence time were modelled. DOM39 February 2013 Effect of continuous phase viscosity on the break-up of silica nanoparticle clusters using the ultrasound Dr Olga Narducci, Dr Gustavo Padron, Dr Gul Ozcan-Taskin Executive Summary

Ultrasonic cavitation has been used for break-up and dispersion purposes of silica nanoparticle cluster within DOMINO. This report presents the results on the effect of continuous phase viscosity on the mechanism and rate of de-agglomeration of fumed silica clusters under continuous insonation in a 2 l stirred vessel. The investigation focuses on both Newtonian and Non-Newtonian




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shear thinning liquids. Six continuous phases were used: • Distilled water (1 mPa•s) • 2 Newtonian glycerol aqueous solution at 10 and 100 mPa•s; • 3 shear-thinning CMC solutions in distilled water, with n = 0.5-0.95 Following on from experimental details and procedures, results on dispersion rheology and break up agglomerates are presented. DOM40v2 January 2012 DOMINO-Work plans for 2012-2013 Dr Gűl N. Őzcan, Dr Neil Alderman, Dr Gustavo Padron, Dr Adi Utomo, Dr Tim Addison Executive Summary

In this report, DOMINO workplans for 2012 – 2013 are presented. For completeness, first a description of the project is given in Sections 2 and 3, proposed work packages are presented in Section 4. Workprogramme determined based on the votes from members are presented in Section 5. DOM41 November 2012 A Feasibility study on the use of the WAB Mill for the exfoliation of nanoclays Dr Adi Utomo, Dr Emmanuela Gavi and Dr Gűl N. Őzcan Executive Summary

In this initial feasibility study, WAB Multilab mill has been used for the exfoliation of two test systems: 3% Cloisite 10A in Daltocel F456 and 3% Cloisite 30B in Daltocel F435. Initially encountered problems relating to rapid temperature rise could be overcome. The effect of ageing on the rheology of the dispersion was also investigated. DOM42 November 2012 DOMINO-CFD Simulation of break-up of nanoparticle clusters using an ultrasonic processor Greg Konan, Dr Ying Wang, Dr Dominik Kubicki Executive Summary

This report summarises the findings from the continuation of a work carried out previously and summarized in report DOM34. The flow field generated by ultrasound device in presence of three




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phases (liquid, vapour and Aerosil 200V) was investigated and then evolution of particle size distributions as a result of breakage of nanoparticles clusters was calculated using the population balance model solver available in ANSYS FLUENT 13.0. DOM43 December 2012 Delamination of Nanoclays: Importance of Affinity with Different Nanoclay/Polyol Combinations Dr Adi Utomo and Dr Gustavo Padron Executive Summary

The effect of affinity on the delamination of nanoclays is studied using different test systems: Cloisite 10A and 30B, in different polyols: Daltocel F456 and F555. Wettability was determined using the immersion test, X-ray diffraction to determine the inter-gallery spacing and rheology and particle size distribution changes were used to monitor the process. The intercalation process was carried out in a stirred tank at 50oC for 180 minutes while the exfoliation process was also performed by using an ultrasonic disperser, also at 50oC for 180 minutes. DOM44 January 2013 Break up of fumed silica particles manufactured under different process conditions Dr Gul Ozcan-Taskin, Dr Gustavo Padron, Dr Tim Addison Executive Summary

This document reports the outcome of the second stage of an investigation into the breakup of silica particles produced through different manufacturing conditions. DOMINO has extensively used nanoparticles manufactured through flame hydrolysis, as this is a technique commonly used for the manufacture of large quantities of particles. Aerosil 200V, which is a hydrophilic silica, has been used as a reference test system within DOMINO. In addition, Aerosil R816 and R202, which are surface treated and are hydrophobic, were studied and break up mechanism and kinetics of hydrophilic silica nanoparticle clusters was further investigated with particles produced through precipitation and comparing results with those for Aerosil 200V (reported in DOM30). In this set of experiments, silica particles produced from flame pyrolysis under different process conditions (reagent/O2 flow rates, flame temperature and residence time) are investigated. These particles have different primary particle sizes depending on the conditions at which they were manufactured.




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DOM45 CFD Modelling of the WAB Stirred Bead Mill Dr Greg Konan, Dr Ying Wang Executive Summary

This report summarises the findings from the modelling work carried out on the WAB stirred bead mill. A 3D Computational Fluid Dynamics model is employed to investigate the mill with beads and liquid phase. Using the energy dissipation rate calculated from this approach, a simplified 1D Population Balance Model (PBM) was used to estimate the Particle Size Distributions (PSD). The effects of operation mode (batch or re-circulation) and flow rate are studied. Example results for each case are also presented with PSD predictions compared to experimental data. DOM46 Liquid-liquid dispersions using a Nanoclay (Laponite RD) Dr Adi Utomo, Dr Gul Ozcan-Taskin Executive Summary

Ultrasonic disperser has been used to prepare silicone oil-in-water emulsions stabilised by using a conventional non-ionic surfactant (Tergitol TMN6) and a nanoclay (Laponite RD). This initial study aimed at investigating the size range of droplets produced using the energy intensive ultrasonic disperser and the possibility of using nanoclay as a stabilising agent. DOM47 Break up of clusters of nanoscale silica using the large scale Ytron Z130 in-line rotor-stator Dr Adi Utomo, Dr Gustavo Padron Executive Summary

Power characteristics of Ytron Z130 in single phase and its performance in de-agglomerating nanoparticle clusters have been investigated. This device is a larger version of the Ytron Z (Z-Lab) that was previously used within DOMINO and reported in Özcan-Taşkin and Padron (2009). The power draw characteristics of Z130 were first determined using the calorimetry technique in water. Deagglomeration of nanoscale silica particles was then studied with 1%wt fumed Aerosil 200V dispersion in water.




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DOM48 Power input of a batch rotor-stator and an ultrasonicator Dr Adi Utomo Executive Summary

The power input from a batch rotor-stator mixer (Silverson L5M) and an ultrasonic disperser (Hielscher UP200S) was determined in water and glycerol solutions by using the calorimetry method. DOM49 Importance of nanoclay-polyol affinity with Cloisite 15B Daltocel F456 Dr Adi Utomo, Dr Gul Ozcan-Taskin Executive Summary

Intercalation and exfoliation of nanoclays have been investigated in DOMINO since 2008, with emphasis in the recent years on the importance of affinity between the nanoclay- liquid pair. This study aimed at building on previous results through the study of the most hydrophobic nanoclay (Cloisite 15A) and most hydrophobic polyol (Daltocel F456). DOM50 Characterisation of dispersion processes Dr Tim Addison, Dr Neil Alderman, Dr Emmanuela Gavi, Adi Utomo, Dr Gustavo Padron, Dr Gul Ozcan-Taskin Executive Summary

This document provides a review of experimental techniques for characterising nanoparticles, continuous phase and dispersions with emphasis on those commonly used within DOMINO. It includes experimental procedures followed and where appropriate, recommendations are given to avoid any potential errors. Aside from being a stand-alone document which can be useful to anyone performing measurements; it is produced as a reference document to the Design Procedures of DOMINO, DOM04.




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DOM51 Importance of rheology on break up of nanoscale silica particle clusters using an in-line rotor-stator: further results Dr Gustavo Padron Executive Summary Within DOMINO, in-line rotor-stators have been used to investigate mainly the break-up of nanoparticle clusters and to some extent for the incorporation of particles into the liquid phase. This study follows on from the work carried out with Aerosil 200V in water and viscous Newtonian and non-Newtonian fluids with viscosities or apparent viscosities up to 100 mPa·s. The rotor-stator used was the Silverson 150/250MS equipped with a dual Emulsor screen (EMSC).

DOM53 Modelling of Ytron Z130 device: CFD modelling of flows and PBM for break up Dr Carlos Fonte Executive Summary This report details the results of a study undertaken within DOMINO on the modelling of the Ytron Z130 in-line rotor stator device, used for the break up of silica nanoparticle clusters. A 3D Computational Fluid Dynamics (CFD) model was developed to gain insight into this rotor-stator device and help analyse and interpret break up results. The simulation results were analysed in terms of:

velocity contours and velocity vectors to assess zones with high velocity gradients and formation of high velocity jets;

turbulent energy dissipation rate to identify zones where particle break up is more likely to occur;

particle tracking to observe the average residence time of particles and existence of by-passing and to perceive the amount of turbulent energy dissipation rate a particle experiences as it flows throughout the device.

Computational results are also compared with two other in-line rotor stator devices to explain the comparative performance of the Ytron Z130 in-line rotor stator. Furthermore, a simplified 1D Population Balance Model (PBM) was developed to estimate the Particle Size Distributions (PSD).




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DOM54 October 2013 DOMINO-Work plans for 2013-2014 Dr Gűl N. Őzcan, Dr Neil Alderman, Dr Gustavo Padron, Dr Adi Utomo, Dr Tim Addison, Dr Carlos Fonte Executive Summary This report contains a description of the project presented in Sections 2 and 3, followed by the proposed work programme of DOMINO for 2013 – 2014 in Section 4. Final workplans after voting are presented in Section 5. DOM55 October 2013 Effect of Solids Concentration on the Milling of Aerosil 200V and Initial Mill Optimisation Dr Tim Addison, Dr Gűl N. Őzcan, Dr Neil Alderman, Executive Summary This report presents the results of an experimental study carried out within the DOMINO 2012-2013 programme to evaluate the effects of both grinding media size and tip-speed on breakup kinetics using the WAB stirred bead mill. It follows on from the study undertaken in 2010-2011 (DOM29) with 9% w:w Aerosil 200V concentration to 15% w:w. Dispersion rheology was also studied and could be related to the degree of fineness of the dispersion. DOM56 November 2013 Simultaneous Incorporation and Break Up of Silica Particle Clusters using the Ytron ZC1 Dr Gustavo Padron Executive Summary Several applications in industry (food and personal care products, fermentation processes, polymerisation reactions, minerals processing and wastewater treatment) require the incorporation of floating particles into liquids. In previous DOMINO work, a proprietary design stirred tank, Ytron Y Jet, and an in-line rotor-stator, Ytron ZC1, have been studied for the incorporation of nanoparticle clusters into liquids. The main objective of the study presented herein was to assess the performance of the Ytron ZC1, for the purpose of de-agglomerating nanoparticle clusters and compare with previously used in-line rotor-stators. The study included the identifying effects of the rotor-stator geometry by using both the standard 3.0 mm and 1.5 mm gap rotor-stator and flow rate. A limited amount of incorporation experiments were also undertaken.




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DOM57 July 2014

Combined effect of continuous phase viscosity and particle concentration on deagglomeration of silica particle clusters using the ultrasonicator Dr Gul Ozcan-Taskin, Dr Adi Utomo Executive Summary

Break up of hydrophilic fumed silica nanoparticle cluster (Aerosil 200V) in 100 cP glycerol solution using an ultrasonic disperser has been investigated at solid concentrations of 1, 10 and 15 wt.%. In the previous work (DOM 52), the break up was investigated in water and 10 cP glycerol solution at the same solid concentrations. In addition to analysing the results on the effect of particle concentration at this viscosity, data have been compared with those at 1 and 10 cp to evaluate the combined effects of solid concentration and continuous phase viscosity on the de-agglomeration of hydrophilic fumed silica nanoparticle clusters (Aerosil 200V) using an ultrasonic disperser.

DOM58 July 2014

The effect of flowrate on the break up of silica particle clusters using the stirred bead mill

Dr Adi Utomo Executive Summary In this study, the effect of re-circulation flow rate, and hence the residence time, in a stirred bead mill (WAB Dyno-mill Multi Lab) on the de-agglomeration of 15 wt.% Aerosil 200V in water has been investigated.

DOM59 July 2014

Importance of flowrate using Ytron ZC1

Dr Adi Utomo

Executive Summary The air velocity at the powder inlet of Ytron ZC1 has been measured as an alternative to suction pressure measurements to characterise the performance of Ytron ZC1 for powder incorporation. Experiments were carried out with 1.5 and 3 mm slot heads and with water as the working fluid. The liquid flow rate was varied between 0.5 and 3.2 l/s.




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DOM62 October 2014 Modelling of WAB Stirred Bead Mill device: Effect of particle concentration, tip speed and bead size Dr Carlos Fonte Executive Summary This report details the results of a study undertaken within DOMINO on the modelling of the of a stirred bead mill device, used for deagglomeration of nanoparticle clusters. A 3D Computational Fluid Dynamics (CFD) model was developed to investigate this device and assist with the analysis and interpretation of breakup results. The simulation results were analysed in terms of:

velocity contours to assess zones with higher velocity gradients;

turbulent energy dissipation rate to identify zones where particles break up is more likely to occur;

distribution of beads throughout the chamber to infer about the performance of the device. Furthermore, a simplified 1D Population Balance Model (PBM) was developed to evaluate the evolution of Particle Size Distributions (PSD). The breakage of Aerosil 200V nanoparticle clusters processed in the mill was modelled. The numerical model assumes a simplified 1D flow pattern in the system and the evolution of particle size distribution is modelled using the discrete form of population balance equations.

DOM63 September 2014 Liquid - liquid dispersions using a surfactant or a nanoclay as stabiliser: Effect of dispersed phase concentration Dr Adi Utomo Executive Summary This work is continues from a previous DOMINO study reported on DOM46, investigating the effect of dispersed phase concentration on droplet size using an energy intensive device, namely the ultrasonic disperser. The dispersed phase concentrations used in the current work were 20 and 50 vol.% and the emulsions were stabilised using surfactant (Tergitol TMN6) and nanoclay (Laponite RD). The results obtained in this work were compared with those obtained previously at a dispersed phase volume fraction of 10%.




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DOM64 October 2014

Incorporation of clusters of nanoscale silica into shear thinning CMC using the in-line rotor-stator Ytron ZC1

Dr Gul Ozcan-Taskin Executive Summary The performance of the in-line rotor-stator Ytron ZC1 for the incorporation of Aerosil 200V into a shear thinning CMC solution was studied. This continues from previous DOMINO work during which use water and 100 cp glycerol were used as the continuous phase. The evolution of the rheology with increasing particle concentration was studied. The study also included the determination of air velocity which is related to the suction pressure at the powder inlet and hence the incorporation rate. These measurements were taken at the start of the experiment to compare with values obtained in water and assess the effect of continuous phase rheology and also at increasing particle concentrations to both evaluate the effect of increasing particle concentration and hence rheology and also to maintain it constant with the aim of maintaining incorporation rate constant. The report contains results on rheology, suction performance and incorporation rate at increasing particle concentrations incorporated into a shear thinning CMC solution.

DOM65 November 2014

Results from scouting experiments with the WAB Stirred Bead Mill (MultiLab Mill): effect of fill ratio, continuous phase viscosity and bead size

Dr Timothy Addison, Dr Gul Ozcan-Taskin Executive Summary This report details findings from scouting experiments that have been performed with the WAB stirred bead mill in order to determine the influence of • bead size (0.8 mm and 1.0 mm beads) • fill volume of the mill chamber (50% and 65%) • continuous phase viscosity (10cP glycerol/water and water) • using bi-modal grinding media size (1.0 mm and 0.3 mm beads) on breakup kinetics and mechanism using 15 w:w% Aerosil® 200V.




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DOM66 November 2014 Modelling of ZC1 inline rotor-stator device Dr Carlos Fonte Executive Summary This report details the results of a study undertaken within DOMINO on the modelling of an inline rotor-stator, Ytron ZC1, used for the incorporation and the deagglomeration of nanoparticle clusters. A 3D Computational Fluid Dynamics (CFD) model was developed to investigate this device and assist with the analysis and interpretation of breakup results. The simulation results were analysed in terms of:

velocity magnitude contours and velocity vectors to assess zones with higher velocity gradients;

turbulent energy dissipation rate to identify zones where particles break up is more likely to occur;

Furthermore, a simplified 1D Population Balance Model (PBM) was developed to evaluate the evolution of Particle Size Distributions (PSD). The breakage of Aerosil 200V nanoparticle clusters using the Ytron ZC1 was modelled. The numerical model assumes a simplified 1D flow pattern in the system and the evolution of particle size distribution is modelled using the discrete form of population balance equations. Comparisons with experimental data are also presented.

DOM67 December 2014 Proposed workplans for 2014-15 Dr Gul Ozcan-Taskin

DOM68 January 2015 Power characteristics and break up of nanoparticle clusters using the Ytron Z-Lab in-line rotor-stator Dr Gustavo Padron Executive Summary Since its inception, several different in-line rotor-stator mixers have been used in DOMINO for de-agglomerating nanoparticle clusters. Of these, Ytron Z-Lab was previously studied with its rotor fitted with a pumping wheel in order to make it self-pumping. During subsequent experiments conducted with Ytron Z130, a pumping wheel was not present and an external pump had to be used to provide flow. The main purpose of this new study has been to establish the performance of Ytron Z-Lab with an external pump instead of the pumping wheel, in order to compare the different Ytron units directly.




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To be able to analyse the data and compare these devices on the basis of power consumption and/or energy density, the power characteristics of all units have been determined using the calorimetry technique.

DOM69 May 2015 Emulsification using a power intensive process device- Microfluidizer M110-P Dr Gul Ozcan-Taskin Executive Summary Among several applications that require the formation of emulsions- varying from pharmaceutical to food, personal care and cosmetics to agrochemicals- nanoemulsions have been reported to be of particular interest to pharmaceutical and personal care\cosmetic products (Sadeghpour et al, 2013; Gupta and Rousseau, 2012; Garrec et al, 2012; Maali and Mossavian, 2013). Nanoemulsions typically have droplets in the range of 10 to 100 nm and are obtained using power intensive devices, such as a high pressure valve homogeniser or Microfluidizer. Continuing from previous DOMINO work on emulsification using the ultrasonicator and deagglomeration using the Microfluidizer, further work has been undertaken using the Microfluidizer, to investigate the emulsification process of a given test system: 10%v:v 10 cSt silicone oil-in-water. Power input was determined over a range of pressure values and results obtained on the break up of silicone oil-in-water were compared to those obtained using the ultrasonicator. DOM70 June 2015 Modelling of Ytron Z130 device: PBM for break up with the QMOM Dr Carlos Fonte Executive Summary This report details the results of a study undertaken within DOMINO on the modelling of the Ytron Z130 in-line rotor stator device, used for the break-up of silica nanoparticle clusters. This model makes use of the 3D Computational Fluid Dynamics (CFD) model developed in a previous DOMINO work (DOM 53) including its flow field and distribution of turbulent energy dissipation rate for the implementation of a new approach of Population Balance Modelling (PBM) for the deagglomeration of nanoparticles. The PBM was implemented in ANSYS Fluent and calculates the evolution of local particle size inside the device using the Quadrature Method of Moments (QMOM). The breakage of Aerosil 200V nanoparticle clusters processed in this rotor-stator device was modelled. Erosion was observed to be the main breakage mechanism from experimental work and was selected in the population balance modelling. The results obtained from numerical simulations




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are compared with experimental data and simulation results of PBM using a simplified model developed in previous work of DOMINO (DOM 53). DOM71August 2015 Effect of dispersion volume on milling of nanoparticle clusters Dr Gul Ozcan-Taskin Executive Summary The study reported in this document relates to the effect of residence time on de-agglomeration using a stirred bead mill (WAB Dyno-mill Multi Lab) by changing the dispersion volume. The test system used was 15 wt.% Aerosil 200V in water. The study follows on from previous work performed at a given dispersion volume of 2 l where residence time was varied by changing the flow rate.

DOM72 October 2015 Effect of deagglomeration of two carbon black dispersions using the Microfluidiser 110-P and ultrasonicator Dr Gul Ozcan-Taskin Executive Summary Two coarse dispersions of carbon black were further processed using power intensive process devices- Microfluidizer M110-P and Hielscher ultrasonicator- and the results obtained in this preliminary study are presented in this report. DOM73 October 2015 Combined effect of particle concentration, continuous phase viscosity and milling speed on the deagglomeration of silica nanoparticle clusters using the WAB stirred bead mill. Dr Gul Ozcan-Taskin Executive Summary This study has been performed to investigate the combined effect of continuous phase viscosity and particle concentration over a range of mill speeds. 10 cP Newtonian glycerol solution was used as the continuous phase and the dispersed phase was10 and 15% w:w Aerosil 200V particles. The study was performed using 2 litres of dispersions and one experiment was performed at a higher volume, 4 l. The predominant mechanism of breakup was found and compared with the fiindings obtained using an in-line rotor-stator, ultrasonicator and Microfluidizer.




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DOM74 November 2015 Incorporation of Zeolite powder into water using Ytron ZC1 Dr Gul Ozcan-Taskin Executive Summary The incorporation of Zeolite into water was studied using the in-line rotor-stator Ytron ZC01. The Zeolite concentration used was up to 10% w:w. A funnel connected to the powder inlet of ZC1 was used as well as a hose, and powder incorporation times measured. DOM75 November 2015 Effect of particle concentration on break-up of nanoscale silica clusters using the in-line rotor-stator Ytron ZC1 Dr Gustavo A Padron

Executive Summary A number of different in-line rotor-stators have been studied within DOMINO for the breakup of nanoparticle clusters. Most of the work has been carried out using Aerosil 200V as a model material but other particles including different types of silica, and nanoclays have also been used. This report summarises the most recent work undertaken with the Ytron ZC1, which focuses on the effect of solids concentration on simultaneous incorporation and breakup of silica clusters. DOM76 December 2015

DOMINO future work plan proposals 2015-2016

Dr Nigel Heywood, Dr Gul Ozcan-Taskin, Dr Gustavo A Padron Executive Summary In this report the proposed work programme for DOMINO in the 2015 – 2016 year is presented. For completeness, a description of the DOMINO project is given in Sections 2 and 3, followed by proposed work packages presented in Section 4. Following on from the voting process, the report containing the final work plans was issued to all DOMINO Members as Version 2 of DOM76.

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