silox actif free- flowing• · 2019. 5. 18. · flowing† in rubber formulations based on:...

SILOX Actif Free-Flowing

An Improvement for

the Rubber Industry

SILOX Actif Free-Flowing

Performance and cost saving Quality and environment Formulations examples Comments Dispersion kinetic Data sheet Contact

SILOX Actif Free-FlowingAdvantages

1. Wet process nodular particle shape (no defect initiator and no minute tear initiator).

2. Its particle shape provides far easier and better dispersion.

3. High surface area (over 40 m/g) results in very high reactivity.

4. High reactivity allows to reduce loadings by 50%.

5. Therefore, yields and productivity (shorter curing time) and faster mixing operations.

6. Very significant savings in raw materials and volume cost.

Thanks to a unique process amongst zinc oxide producers, SILOX is able to deliver a unique material on the market.

SILOX Actif Free-Flowing is in combination with fatty acid, a high performance and cost saving crosslinking agent in natural and synthetic rubber applications.

Most interesting characteristics are:

QUALITY:

Mechanical properties of compounds produced with reduced concentration remain unchanged and often better after ageing.

Shape retention in EPDM profiles and better productivity.

Blooming and mould fouling reduced due to the low zinc oxide content.

Very low level of impurities such as lead, cadmium or manganese and copper which are "poisons" for rubber

ENVIRONMENT:

Lower level of zinc in compounds may be desirable environmentally or anyway facilitate FDA approvals where applicable (drinkable water).

Zinc content of latex waste water reduced by more than 50%if zinc oxide is used with a good dispersing agent in the formulation.

Active zinc oxides are also well known to reduce the level of nitrosamine

Very low level of impurities such as lead, cadmium or manganese and copper.

Zinc Oxide nodular structure

SILOX Actif Free-Flowing will also deliver unmatched performances in:

SILOX Actif Free-FlowingDescription

+ Superior flowability+ Precise dosing+ Less/no dust+ Improved dispersion (reduced blending time)+ Nodular structure+ High specific surface(> 40 m/g)+ No/low mould fouling+ No blooming+ Improved ageing+ Reduced reversion+ Lower torque

SILOX Actif Free-Flowing has been developed to provide the market with a binder free zinc oxide with improved handling properties. It can easily and accurately be handled manually or with automated systems. The crush resistance of SILOX Actif Free-Flowing is sufficient to withstand piling of bags or silo storage in the ware house and conveyor belt or pneumatic transportation without being reduced to primary particles.

The efficiency of zinc oxide during vulcanisation is improved bymaximising contact between zinc oxide particles and the components of the formulation. A higher efficiency is obtained with high surface area small particles uniformly dispersed throughout the rubber matrix.

SILOX Actif Free-Flowing can readily and homogeneously dispersed in rubber compared to traditional zinc oxide. This was observed by many rubber compounders and leads to surprising side effects such as reduced blooming, spectacular reduction in mould fouling…

Its superior flow qualities can also bring reduced dusting around dosing equipments compared to powdered standard grades. This is also part of good industrial hygiene practices.

SILOX Actif Free-FlowingScope

This booklet is designed to determine all the benefits associated to SILOX Actif Free-Flowing in rubber formulations based on:

Industrial formulations; most of them have been developed and are commonly used by a European technical moulding parts rubber producer..

Conventional synthetic and natural elastomers formulation of European rubber compounders.

With this study, it will also be possible to get a more complete and comprehensive picture on:

Zinc oxide activity by using 5 phr of French process ZnO* and 2.5 phr of SILOX ZnO Actif.

Main rheometric characteristics. Main mechanical properties of cured

samples.

* Red seal or white seal zinc oxide depending on regional specifications.

Typical industrial formulation examples have been chosen to cover some of the most common elastomers in a typical application (mainly for compression moulded parts):

NR and NR-BR (low hysteresis and mechanism valve).

EPDM (70 Sh-A; 85 Sh-A; high performance compound; window iron-angle; temperature resistant connector and sponge door seal

NBR (membrane). CR (protection bellows). NR-SBR (pulley gasket).

SILOX Actif Free-FlowingRubber formulation NR (70 2 Sh-A, low hysteresis blend for trailer engine)

0.25OTOS

2Sulphur

0.5DTDM

1MBS

5Semi-naphtenic Oil

10Black HAF 347

55Black SRF 772

0.5TMQ

0.5IPPD

Var.ZnO

3Stearic acid

100Natural Rubber TSR 10

phrFormulation 1

3.2 1.744.830

3.11.825.229.7

3.41.855.430.1

T90Ts2MLCrosslinking rate

SILOX ActifFree-Flowing2,5phr

SILOX ZnOActif

2,5phr

ZnO*5phr

Rheological properties(170C)


SILOX Actif Free-Flowing reduces the T90 of the blend. This can suggest shorter cycle time and productivity increase for the company.The lower minimum torque (ML) obtained with the SILOX Actif Free-Flowing may indicate a lower electrical consumption during mixing which is an additional saving. This lower viscosity is also an indication of easier operating conditions for extrusion, calendering, and moulding.

The lower ZnO content through the use of the SILOX Actif Free-Flowing does not modify the tensile properties of the compound before ageing. After ageing, the compound made with the SILOX Actif Free-Flowing keeps superior mechanical properties compared to the reference blend.

-21.20-25.8

-29.3 -36.2

-24.5 -31.5

Tensile strength at break (%)Elongation (%)

Mechanical properties (7 days 100C)

-7.2-10.9

-8.10-10.8

-6.8-12.2

Tensile strength at break (%)Elongation (%)


16455

15.6525

15.8476

Tensile strength at break (MPa.)Elongation (%)

Mechanical properties (initial)

SILOX Actif Free-FlowingRubber formulation NR-BR (55 5 Sh-A, watertight mechanism valve)

1.5Sulphur

0.4TMTD

1.2CBS

18Semi-naphtenic Oil

30Black FEF 500

20Precipitated CaCO3

0,5TMQ

0.5Phenylbetanaphtylamine

Var.ZnO

2Stearic acid

30Polybutadiene

70Natural Rubber TSR 10

phrFormulation 2



The lower ZnO content through the use of the SILOX Actif Free-Flowing does not modify the tensile properties of the compound before ageing. The compression set is slightly improved.After ageing, the compound made with the SILOX Actif Free-Flowing appears to be less sensitive to degradation.

2.391.555.2

22.6

2.581.565.618.7

2.651.616.119.1



SILOX ZnOActif

2,5phr

ZnO*5phr


-24.6-29.7

-26.4-33.8

-31.8-40.7



-11.6-8.7

-11.9-10.1

-12.9-17.8



13.530520.4

13.331719.1

13.732521.8

Tensile strength at break (MPa.)Elongation (%)CS, 72h 70C (%)


SILOX Actif Free-FlowingRubber formulation NR-BR (60 2 Sh-A, high performance compound with low extractable for water resistant seal)

1.5Sulphur

0.4TMTD

1.2CBS

1PEG 4000

15Semi-naphtenic oil

15Silice VN3

35Black FEF 550

15CaCO3 precipitated

0.5TMQ


Var.ZnO

2Stearic ac.

30Polybutadiene

70NR TSR 10

PhrFormulation 3



The lower ZnO content through the use of the SILOX Actif Free-Flowing does not modify the tensile properties of the compound before ageing. After ageing, the compound made with the SILOX Actif Free-Flowing appears to be less sensitive to degradation.

2.831.676.119.5

2.951.696.218.8

3.241.757.3

16.,9



SILOX ZnOActif

2,5phr

ZnO*5phr


-21.4-29.7

-23.6-31.1

-27.1-34.5



-11.6-13.3

-10-16.1

-11.3-15.6



16.4355

16.6375

16.1403



SILOX Actif Free-FlowingRubber formulation EPDM (70 3 Sh-A, temperature resistant connector for solar panels )

0.6Sulphur

0.6DTDM

0.6ZBDC

0.6ZEDC

0.8MBT

85Paraffinic Oil

140Black FEF 550

0.5TMQ

Var.ZnO

2Stearic acid

25EPDM 2504

75EPDM 9500

phrFormulation 4



The lower ZnO content through the use of the SILOX Actif Free-Flowing does not modify the tensile properties of the compound before ageing. The compression set is slightly improved..After ageing, the compound made with the SILOX Actif Free-Flowing appears to be less sensitive to degradation.

4.011.375.120.2

4.411.415.520.7

4.721.456.518.6



SILOX ZnOActif

2,5phr

ZnO*5phr


-6.5-10.9

-10.4-12.9

-11.8-23.5



-3.2-8

-2.8-7.2

-2.7-7.8



12.834322.6

12.636522.8

12.936424.1



SILOX Actif Free-FlowingRubber formulation EPDM (85 3 Sh-A, drinking water raccort cast iron-PVC)

1.5Sulphur

3.0CBS

55Paraffinic Oil

130Black FEF 550

2Epolene 34

0.5TMQ

Var.ZnO

0.3Stearic acid

25EPDM 4038

75EPDM 378

phrFormulation 5


In this slow curing EPDM formulation, SILOX Actif Free-Flowing is not adversely modifying the crosslinking behaviour. The lower minimum torque (ML) obtained with the SILOX Actif Free-Flowing may indicate a lower electrical consumption during mixing which is an additional saving. This lower viscosity is also an indication of easier operating conditions for extrusion, calendering, and moulding.

The lower ZnO content through the use of the SILOX Actif Free-Flowing does not modify the tensile properties of the compound before ageing. After ageing, the compound made with the SILOX ActifFree-Flowing appears to be less sensitive to degradation.

9.981.4711.131.8

10.061.4510.733.1

9.431.431133



SILOX ZnOActif

2,5phr

ZnO*5phr


-13.9-13.3

-16.9-17.4

-15.6-21.4



-5-9.1

-6.7-11.8

-5.1-10.4



11.4320

11.7324

11.7312



SILOX Actif Free-FlowingRubber formulation EPDM (62 5 Sh-A, window iron-angle)

1.5DPTT

0.8Sulfur

0.8ZBDC

0.8ZEDC

1MBTS

60Flexon 876

100Black FEF 550

Var.ZnO

2stearic Ac.

50Vistalon 2504

50Vistalon 9500

PhrFormulation 6



In this EPDM formulation reducing the zinc oxide content through the use of the SILOX Actif Free-Flowing is leading to mixed but equivalent mechanical properties.After ageing 7 days at 70C or 100C the mechanical properties of both blends remain similar.

3.71.66

837.7

3.751.628.234.3

3.821.768.234.9



SILOX ZnOActif

2,5phr

ZnO*5phr


7.9-14.1

+9.9-12.2

+11.1-14.3



+3-8.1

+4,5-8.4

+5.5-8.7



13.1315

12.85287

12.6330



SILOX ActifRubber formulation EPDM (59 4 Sh-A, sponge door seal)

2Genitron ACR

0.5Rhenocure S/G

1ZBEC

1.5Geniplex 80

1.4MBT

0.5Genitron OB

1.7Sulphur

2Calcium oxide

2Carbowax 3350

0.5Stearic Ac.

Var.ZnO

55Flexon 876

30OMYA BSH

65N539

100Vistalon 8600

PhrFormulation 6


8.790.6710.9249.46

10.420.888.6644.33


SILOX ZnO Actif 6phr

ZnO*10phrRheological properties 170C

13402709.860

1.74E-04

140037014.259

1.57E-04

Tensile strength at break (MPa.)Elongation (%)Compression setShore A DurometerCrosslinking density


SILOX Actif reduces the T90 of the blend. This can suggest shorter cycle time and productivity increase for the company. The higher viscosity and the reduced scortch time obtained with such a formulation has given an extra advantage to the EDPM profiles producers as they give more shape stability before complete curing.

In this sponge EPDM formulation reducing the zinc oxide content through the use of the SILOX is leading to a higher crosslinked density but also a tremendous improvement of the compression set.

SILOX Actif Free-FlowingRubber formulation NBR (55 3 Sh-A, ballcock membrane/moving part seal)

0.6Ferrusoufre

0.5CaCO3 sulfonamide

2TMTD

1CBS

3PE wax

1Stucktol WB12

8DOP

10CaCO3

15Black HAF 347

20Black SRF 772

1Phenylbetanaphtylamine

Var.ZnO

1Stearic Ac.

100NBR 33C50

PhrFormulation 7



The lower ZnO content through the use of the SILOX Actif Free-Flowing does not modify the tensile After ageing, the compound made with the SILOX Actif Free-Flowing appears to be less sensitive to degradation.

4.752.192.314.4

4.872.312.713.2

5.362.23.412.2


SILOX ActifFree-Flowing 2,5phr

SILOX ZnOActif

2,5phr

ZnO*5phr


7.3-10.7

+9.2-12.4

+8.1-16



+3.3-4.4

+3.7-4

+2.2-5.1



14.439641.7

13.639840.1

13.940535.7

Tensile strength at break (MPa.)Elongation (%)Tear resistance (MPa.)


SILOX Actif Free-FlowingRubber formulation CR (55 5 Sh-A, protection bellows)

4MgO

0.25TMTD

1ETU

20DOP

18Black HAF 347

12Black SRF 772

20Silicium Oxide

2PE wax

1IPPD

1Octylated diphenylamine

Var.ZnO

0.5Stearic Ac.

25Polychloroprene WD

75Polychloroprene GW

PhrFormulation 8



The lower ZnO content through the use of the SILOX Actif Free-Flowing does not modify the tensile properties of the compound before ageing. The compression set is slightly improved..After ageing, the compound made with the SILOX Actif Free-Flowing keeps mechanical properties equivalent to the reference blend.

3.811.165.229.1

3.841.185.230.3

3.931.255,828.3



SILOX ZnOActif

2,5phr

ZnO*5phr


-3.5-13.1

-4.4-12.2

-4.8-13.1



Not applicable for this

formulation


formulation


formulation



18.343218.9

18,544018.7

18.344819.2



SILOX Actif Free-FlowingRubber formulation NR-SBR(80 5 Sh-A, pulley gasket)

3Sulphur

1.5CaCO3 sulfonamide

0.75TMTD

1.5MBTS

1.5Refined paraffin wax

5Coumarone Resin

100CaCO3 precipitated

45Black SRF 772

15Black HAF 347


Var.ZnO

1,5Stearic ac.

90SBR 1778

30NR TSR 10

PhrFormulation 9



In this SBR-NR formulation, despite a 50% reduction of the zinc oxide content through the use of the SILOX Actif Free-Flowing , the initial and after ageing mechanical properties of the compounds remain equivalent.

2.471.337.538.6

2.561.377.536.7

3.011.438.534.2



SILOX ZnOActif

2,5phr

ZnO*5phr


-21-25.7

-23.7-27.6

-19.3-24.2



10.10-14.5

-10.2-16.3

-8.8-14.2



14.233133.2

14.431034.1

14.633732.4

Tensile strength at break (MPa.)Elongation (%)Tear resistance (MPa.)


SILOX Actif Free-FlowingObservations

Information's extracted from the rheology:

In most of the rubber formulations SILOX Actif Free-Flowing slightly reduces the crosslinkingtime (t90) of the blend. Often this little change will not require any reformulation but will lead to a shorter cycle time resulting in a productivity increase for the company.In some cases, the lower torque (ML) obtained with the SILOX Actif Free-Flowing may indicate a lower electrical consumption (in particular for internal mixer operation) which is an additional saving A lower viscosity is also a good indication for the operating conditions in compression moulding, calendering, extrusion…

Information's extracted from the mechanical testing:

The lower ZnO content through the use of the SILOX Actif Free-Flowing does not modify the tensile properties of the rubber compounds before ageing. After ageing, all of the formulations made with the SILOX Actif Free-Flowing keep superior or equivalent mechanical properties compared to the reference blends.Compression set and tear resistance are also taking benefit from SILOX Actif Free-Flowing .

SILOX Actif Free-FlowingConclusions

1.SILOX Actif Free-Flowing shows it is possible to work with reduced concentration of zinc oxide in the compound and keep all mechanical and rheological properties equivalent or even slightly improved.

2.After ageing, the mechanical properties of the rubber blend are superior or equivalent to the reference formulation.

3.SILOX Actif Free-Flowing is a good ecological and economical way to improve performance of rubber formulations and significant reduction of heavy metals in wastes and latex effluent.

4.High reactivity allows to reduce loadings by 50 percent or even more.

5.Therefore, yields and productivity (faster curing time) will increase but also energy saving.

6.SILOX Actif Free-Flowing brings significant savings in raw materials and volume cost.

7.Another advantage with SILOX Actif Free-Flowing is the transparency to visible light due to the small particles size. This means reduced level of pigments for colored and semi-transparent products.

8.SILOX Actif Free-Flowing is readily dispersed in the rubber matrix compared to traditional ZnO*.


Dispersion kinetics of ZnO*and ZnO Actif in presence of stearic acid

Red seal versus SILOX ZnO Actif

ZnO* SILOX ZnO Actif

15 phr ZnO; 3 phr Stearic ac; 100 phr EPDM; 30 phr paraffin oil; 0,25 % carbon black2 rolls mill; 120C

120 seconds90 seconds

60 seconds45 seconds


The efficiency of zinc oxide during vulcanisation is improved by maximising contact between zinc oxide particles and the components of formulation. Higher efficiency is obtained with high surface area small particles uniformly dispersed throughout the rubber matrix.. SILOX ZnO Actif can readily and homogeneously dispersed in rubber compared to traditional zinc oxide.This also gives to the formulators a safer process and/or opportunities to increase its productivity.

Mould fouling (EPDM-NR)

0

20

40

60

80

100

120

0 100 200 300 400 500

Time (hours)

Foul

ing

(%)

Red sealActif FF

SILOX Actif Free-FlowingMould fouling effect

No mould fouling for production time doubled; less maintenance required; higher productivity

100% fouling= all cavities of the mould are dull

SILOX Actif Free-FlowingPRODUCT DATA SHEET

Yellow pale powder with 100 % nodular particlesAppearence

45 +/- 5 m2/g5,5/5,7900 g/l approx.0,08 % max.

ELC 30 - Measure of the surface area B.E.T.

ELC 56 - Granulometry

Surface area B.E.T.Specific gravityPacking density45μ sieve retention

SpecificationTest methodsPhysical properties

ZnOCuMnPbCdLoss on drying(2 hrs at 105C)

Chemical properties

94 min.7 valeur typique4 valeur typique20 valeur typique2 valeur typique0.5 max.**

ELC 51 – GravimtrieEICP 19 – ICP*EICP 19 – ICP*EICP 19 – ICP*EICP 19 – ICP*ELC 14 – Gravimtrie

% PpmPpmPpmppm%

SpecificationTest methods

* CP : Inductively Coupled Plasma** H2O specification is guaranteed at packing

OXYDE DE ZINC "SILOX ACTIVE FREE-FLOWING

SILOX ACTIVE is a chemically produced zinc oxide in powder form with excellent flow and reactivity characteristics in use.

SILOX Actif Free-FlowingContact

SILOX s.a.144, Rue Joseph WautersB-4480 ENGIS - BelgiumTel. : + 32 4 273 92 85 • Fax : + 32 4 273 96 [email protected]

www.silox.com

TRANSPEK-SILOX INDUSTRY LimitedKalali RoadATLADRA, VADODARA 390 012 IndiaTel. : + 91 265 2680401 to 05 • Fax : + 91 265 2680407/[email protected]

HYDRO TECHNOLOGIES (CANADA) Inc.2324, Rue Einstein STE-FOY, QUEBEC G1P 3S2 - CanadaTel : +1 418 650 9422 • Fax : +1 418 650 [email protected]

SILOX Actif Free-FlowingRecommendations

DISCLAIMER OF LIABILITY The information in this booklet is to our knowledge true and accurate obtained from sources which we believe are reliable. However, the information is provided without any warranty, express or implied, regarding its correctness. Customers ofSILOX must make their own assessment to determine the suitability of a SILOX ZnO Actif Free-Flowing product for a particular purpose.

The conditions or methods of handling, storage, use or disposal of the product are beyond our control and may be beyond of our knowledge. For this and other reasons, we do not assume responsibility and expressly disclaim liability for loss, damage or expense arising out of or in any way connected with the handling, storage, use or disposal of the product. This booklet was prepared and is to be used only for this product.

silox actif free- flowing• · 2019. 5. 18. · flowing† in rubber formulations based on:...

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