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Questionnaire for trials for Gas / Liquid Reactions in the Pilot Plant / Laboratory
CL-175097-4Seite 1 von 14
Please use a separate questionnaire for each product.
The information which you provide in this questionnaire is the basis for the planning and preparation of your trials. We therefore ask you to fill the questionnaire in as conscientiously and completely as possible. If insufficient space is provided, please use additional sheets.
BCT - PROJECT N°
CUSTOMER REFERENCE N°
COMPANY NAME
CONTACT PERSON
DEPARTMENT
STREET
CITY/POST CODE
COUNTRY
TELEPHONE
FAX
© BUSS ChemTech AG, 2006Made by: R. Schaffner
Issue Date: 29.07.2005 Filed by: QM
Questionnaire for trials for Gas / Liquid Reactions in the Pilot Plant / Laboratory
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1. CHEMISTRY
1.1 Reaction equation
1.2. Side reactions
Possible side reactions:
1)
2)
3)
Measures to be taken for the suppression of these reactions:
1)
2)
3)
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2. PRODUCT DATA /SAFETY INFORMATION
2.1. Product data
2.1.1. Starting materials, additives, products and by-products
Please list your starting materials, additives, products and by-products:
starting material or product 1:
starting material or product 2:
starting material or product 3:
starting material or product 4:
starting material or product 5:
starting material or product 6:
Questionnaire for trials for Gas / Liquid Reactions in the Pilot Plant / Laboratory
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starting material / product 1 2 3 4 5 6
chemical formula
molecular weight (g/mol)
melting point ( °C)
boiling point (°C)
density (ambient conditions) (kg/m³)
density (reaktion conditions) (kg/m³)
specific heat cp (ambient conditions) (kJ/kgK)
specific heat cp (reaction conditions) (kJ/kgK)
latent heat of evaporation (kJ/kg)
viskosity (ambient conditions) (cP)
viskosity (reaction conditions) (cP)
reaction enthalpy (kJ/mol)
thermal conductivity (ambient conditions) (W/mK)
thermal conductivity (reaction conditions) (W/mK)
decomposition temperature (°C)
vapour pressure (ambient conditions) (bar)
vapour pressure (reaction conditions) (bar)
Please add curves of vapour pressure, density, viskosity etc. as a funktion of temperature, if available
© BUSS ChemTech AG, 2006Made by: R. Schaffner
Issue Date: 29.07.2005 Filed by: QM
Questionnaire for trials for Gas / Liquid Reactions in the Pilot Plant / Laboratory
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2.1.2. Reaction mixtureDensity (ambient cond.) (kg/m3)
Density (reaction cond.) (kg/m3)
Viscosity (ambient cond.) (cP)
Viscosity (reaction cond.) (cP)
Vapour pressure (ambient cond.) (bar)
Vapour pressure (reaction cond.) (bar)
Reaction enthalpy (kJ/mol)
Thermal stability: At which temperature does the thermal decomposition of the reaction mixture start?: (°C)
2.2 Safety data for the starting materials, additives, products and by-products
1 2 3 4 5 6
Flash point (°C)
Self ignition temperature (°C)
Lower explosion limit (%vol)
MAK-value
UN-N°
Poison classification
Is contact with water dangerous(yes/no)
Melting point (°C)
Boiling point (°C)
Safety sheet N°
Transport classification
Are any special precautions to be taken for the safety and protection of human beings or the enviroment?
All products made in the trials and all unused starting material are best returned to the customer for disposal. To which address should they be dispatched?
© BUSS ChemTech AG, 2006Made by: R. Schaffner
Issue Date: 29.07.2005 Filed by: QM
Questionnaire for trials for Gas / Liquid Reactions in the Pilot Plant / Laboratory
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3. CUSTOMER'S experience
3.1. Experience from laboratory or pilot plant work
What influence does the temperature have on the course of the reaction?
What influence does the pressure have on the course of the reaction?
What different kind of catalysts have been investigated?
What influence does the catalyst type have on the course of the reaction?
What influence does an increase of the catalyst concentration have on the courseof the reaction?
What influence does the starting material concentration have on the course of the reaction?
What kind of solvents have been investigated?
What influence does the solvent have on the course of the reaction?
What influence does the stirrer speed have on the course of the reaction?
(Please add graphs showing the observed influences if available)
What kind of equipment has been used for the laboratory investigations?Please name the type of the equipment or illustrate it with a diagram.
Questionnaire for trials for Gas / Liquid Reactions in the Pilot Plant / Laboratory
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3.2. Experience from production
Please describe the standard operating procedure:
Charge composition:
Starting material 1 : (wt%/total charge)
Starting material 2 : (wt%/total charge)
Starting material 3 : (wt%/total charge)
Starting material 4 : (wt%/total charge)
Additive : (wt%/total charge)
Solvent component 1 : (wt%/total charge)
Solvent component 2 : (wt%/total charge)
Catalyst type : (wt% dry/starting material)
Catalyst supplier :
Reaction pressure : (bar)Reaction temperature : (°C)
Reaction time : (min)
Conversion : (%)
Selectivity : (%)
What kind of equipment has been used to achieve the above mentioned results? Please name the type or add a process diagram.
Stirred tank type :
Working volume : (m3)
Maximal operating pressure : (bar)
Maximal operating temperature : (°C)
Stirring rate : (1/min)
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How does the equipment have to be cleaned after the trials?
What are the requirements for the material of construction? Please name the appropriate materials of construction.
What kind of additional actions or precautions have to be taken to influence the course of the reaction positively?
Is there a possibility of crystallisation of intermediates or products below a certain temperature?
no
yes(please give crystallisation temperature and describetype of crystals): [°C]
What impurities or substances that are known to be a catalyst poison or can act as such are there in the reaction mixture or in the starting materials and additives?
Questionnaire for trials for Gas / Liquid Reactions in the Pilot Plant / Laboratory
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4. BUSS-CT PILOT PLANT TESTS
4.1. Objectives
4.1.1. Aim of the trials
Please list the goals you would like to achieve:
actual target
Yield (%)
Selectivity (%)
Reaction time (min)
Catalyst amount (wt% dry/starting material)
Re-use of the catalyst (N° of recycles)
Starting material concentration (wt%/total charge)
Which of the above mentioned parameters are critical for the economy of the process?
4.1.2. Product requirements:
Please add the specifications you would like to achieve:
4.2. Performance of trials
4.2.1. Working procedure
Please give the chronological order of the required working procedure. What effect does a deviation from this given procedure cause?
Questionnaire for trials for Gas / Liquid Reactions in the Pilot Plant / Laboratory
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4.2.2. Charge
Starting material 1 : (wt%/total weight)
Starting material 2 : (wt%/total weight)
Starting material 3 : (wt%/total weight)
Starting material 4 : (wt%/total weight)
Additives : (wt%/total weight)
Solvent component 1 : (wt%/total weight)
Solvent component 2 : (wt%/total weight)
Catalyst : (wt%/starting material)
4.2.3. Catalyst details
Type :
Supplier :
In what form will the catalyst be delivered?
powder
humid e.g. Pt/C : % H20 content :
Raney-Nickel in H2O
other forms
in case of Ra-Ni:
are there any special instructions for weighing out the catalyst?
4.2.4. Reaction conditions
Pressure : (bar)
Temperature : (°C)
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4.2.5. Further information
Which of the following pump seal flushing liquids are preferable for your product?
paraffin oil
water/glycerine mixture
Is the starting material dissolved or is it a slurry?
If a slurry, how many wt% of the total reaction mixture are not dissolved?
(wt%)
Does the starting material dissolve as the reaction proceeds?
Pre-treatment:What steps are required before the reaction?
Post-treatment:Is a work-up of the product after the reaction and catalyst filtration necessary or desired?
4.3. Analyses
Which substances are analyzed using a.) physical determinations :
b.) chemical determinations :
Please add the required analytical methods. Please use the forms in the appendix if possible.
So that we can reproduce, your analyses before trials begin, please let us have the reference substances, column(s) and chromatograms 4 weeks before the start of the trials at the latest.
To reach an optimal and efficient utilisation of the laboratory equipment it is usually advisable for an analytical specialist to come to BCT to advise our laboratory staff on the details of the procedures to be used.
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APPENDIX
1. Gas chromatography
1.1. Column
Supplier :
Type/Support :
Length : (m)
Diameter : (mm)
1.2. GC-Method
Start-Temperature-Oven : (°C)
End-Temperature-Oven : (°C)
Initial-Time : (min)
Rise of temperature : (°C/min)
End-Time : (min)
Detector : (°C)
Injector : (°C)
1.3. Sample preparation
Solvent :
Concentration :
Injection volume : (ul)
Sample preparation (please describe the preparation exactly):
1.4. Integration method: Area %
Internal Standard method
External Standard method
1.5. Customer's equipment
Supplier :
Equipment type :
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2. HPLC2.1. Column
Supplier :
Type :
Support :
Particle size : (um)
Diameter : (mm)
Length : (mm)
2.2. Conditions
Wavelength : (nm)
Flow : (ml/min)
Range : (AUFS)
Pressure : (bar)
Column temperature : (°C)
Method Pump A Pump B
isocratic
gradient
Gradient program
Time Initial (min)
Flow
%A
%B
2.3 Sample preparation
Solvent
Concentration
Injection volume (ul)
Sample preparation (Please describe the preparation exactly):
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2.4. Integration method:
Area %
Internal Standard method
External Standard method
2.5. Customers equipment
Supplier :
Type :
3. IR/UV
3.1. Conditions
Cell thickness : (mm)
Concentration :
Wavelength : (nm)
Reference solution :
3.2. Sample preparation
Sovent :
Concentration :
Sample preparation :
(please describe the preparation exactly)
3.3. Customer's Equipment
Supplier :
Type :
Appendix
Summary of the analytical capabilities of the BCT laboratory (see FF-477339-0)
Please complete this Questionnaire formand send it to: or contact us please by:BUSS ChemTech AG Fax: +41 61 82 56 737Hohenrainstrasse 10 Phone: +41 61 82 56 668CH-4133 Pratteln1, Switzerland e-mail: [email protected] site address of Buss ChemTech AG: www.buss-ct.com