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Rubber mixtures

A kind of rubber mixture, rubber technology, applied in the compound of elements of Group 4/14 of the periodic table, organic chemistry, chemical instruments and methods, etc.

Inactive Publication Date: 2009-02-25
EVONIK DEGUSSA GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Another disadvantage of using bis(triethoxysilylpropyl) polysulfide coupling agent is that it limits the mixing temperature of the rubber compound to the temperature range of 140-165°C (H.D Luginsland, "AReview on the chemistry and the reinforcement of the silica-silane filler system for rubber applications, Shaker Verlag, Aachen 2002, p. 34)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0229] At room temperature, 400g of bis(triethoxysilylpropyl) polysulfide Si 69 obtained from Degussa AG and 224.2g of triethanolamine, 2g of 2,6-di-tert-butyl-4- Ionol CP is mixed with 0.6g titanium tetrabutoxide. The heating oil bath is heated to 100°C and the ethanol produced is removed by distillation at 200 mbar. After about 150 ml of ethanol was removed by distillation, the temperature of the oil bath rose to 160°C and the pressure dropped to 100 mbar. When ethanol is no longer distilled, the mixture is heated at 160° C. and 50 mbar for another 120 min. Then 2 g of 3-glycidyloxypropyl (triethoxysilane) (Dynasylan GLYEO, available from Degussa AG) was added, and the mixture was stirred for another 30 min at 160° C. in vacuum. The black product was poured into the coated mold under argon and cured. The product obtained is 403.5 g, a black solid.

[0230] according to 1 H NMR analysis showed that the product contained 29.8% by weight of bis(silatranylpropyl) disulfide, 34.1% by...

Embodiment 2

[0233] At room temperature, 400 g of bis(triethoxysilylpropyl) polysulfide Si 261 was mixed with 247.7 g of triethanolamine and 1 g of tetrabutyl titanate in a distillation apparatus. The heating oil bath is heated to 150°C, and the ethanol produced is removed by distillation at 200-600 mbar. The internal temperature rose from 135°C to 148°C within 180 minutes. After the distillation process is over, the brown product is poured into the coated mold under argon and cured. The product obtained is 420.1 g, a dark brown solid.

[0234] According to 29 Si NMR analysis, the product contained 8.7% by weight of bis(silazepine propyl) monosulfide, 77.2% by weight of bis(silazepine propyl) disulfide, and 12.6% by weight Bis(Siazatricyclylpropyl) trisulfide and 1.5% by weight of bis(Siazatricyclylpropyl) tetrasulfide. The measured average chain length of the polysulfide mixture was 2.1 (using the S1-S10 average value).

Embodiment 3

[0236] At room temperature, 400 g of bis(triethoxysilylpropyl) polysulfide Si 262 was mixed with 247.7 g of triethanolamine and 0.7 g of tetrabutyl titanate in a distillation apparatus. The heating oil bath is heated to 160°C, and the ethanol produced is removed by distillation at 50-400 mbar. The internal temperature rose to 159°C within 90 minutes. After the distillation process is over, the black product is poured into the coated mold under argon and cured. The product obtained is 413.7 g, a fragile black solid.

[0237] according to 29 Si NMR analysis showed that the product contained 70.2% by weight of bis(azatricyclylpropyl) disulfide, 22.0% by weight of bis(azatricyclylpropyl) trisulfide, and 3.1% by weight of bis( Siazatricyclyl propyl) tetrasulfide. The measured average chain length of the polysulfide mixture was 2.3 (using the S1-S10 average value).

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Abstract

The invention relates to rubber mixtures, comprising at least one rubber, a filler, an organosilicon compound of the formula I one rubber accelerator and one co-accelerator. The rubber mixtures are prepared by mixing at least one rubber, a filler, an organosilicon compound of the general formula I, one rubber accelerator and one co-accelerator. The rubber mixtures can be used for production of mouldings . The invention further relates to a process for preparation of the organosilicon compound of the formula I via transesterification.

Description

Technical field [0001] The invention relates to rubber mixtures, their preparation and their use. Background technique [0002] It is known that hydrolyzable sulfur-containing organosilicon compounds can react with hydroxyl-containing fillers, such as natural and synthetic silicates, carbonates, glass, and metal oxides. Here they are used for surface modification and adhesion promotion. In the rubber processing industry, they are used as coupling agents between reinforcing fillers and polymers (DE2141159, DE2212239, DE19544469A1, US3978103, US4048206, EP784072A1). [0003] It is also known to use commercially available silane coupling agents having three alkoxy substituents on the silicon atom (DE22 55 577), such as bis[3-triethoxysilylpropyl]tetrasulfide or bis[ 3-Triethoxysilylpropyl] disulfide, resulting in the release of large amounts of alcohol during and after coupling with the filler. Because trimethoxy- and triethoxy-substituted silanes are usually used, the corresponding...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/549C08L21/00C07F7/18
CPCC07F7/1836C08K5/549C08K5/548C07F7/0834C07F7/1804C08L21/00C07F7/18
Inventor A·哈塞K·科尔特I·基弗S·维茨舍P·阿尔贝特O·克洛克曼
Owner EVONIK DEGUSSA GMBH
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