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Method for reducing product yellowing in hydrosilylation reaction process

A technology for hydrosilylation reaction and hydrosilylation is applied in the field of reducing the yellowing of products in the process of hydrosilylation, and can solve the problems of shortened product shelf life, yellowing of hydrosilylation products, yellowing of products, etc.

Active Publication Date: 2022-05-27
JIANGXI BLUESTAR XINGHUO SILICONE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During processing, storage and application, polymer compounds containing double bonds such as polyether will be in contact with the air. At a certain temperature, autoxidation reaction will easily occur to form peroxides. It will oxidize zero-valent platinum to form platinum black, and the zero-valent platinum remaining in the product will be gradually oxidized to form platinum black, which not only leads to yellowing of the hydrosilylation product, but also leads to the decolorization of the product The re-yellowing of the product shortens the shelf life of the product

Method used

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  • Method for reducing product yellowing in hydrosilylation reaction process
  • Method for reducing product yellowing in hydrosilylation reaction process
  • Method for reducing product yellowing in hydrosilylation reaction process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) 100g of low hydrogen-containing silicone oil with a hydrogen content of 0.03% and 6.54g of 4-(allyloxy)-2,2,6,6-tetramethylpiperidine were added to the reactor, and 0.02g of 1,3-Divinyl-1,1,3,3-tetramethyldisiloxane platinum complex and 0.03g of acetylacetone were heated to 80°C and reacted for 2h;

[0043] (2) 0.1 g of disodium EDTA was added to the product of step (1), stirred at 30° C. for 1 h, and the product obtained by filtration was recorded as S1.

[0044] Comparative Example 1*

[0045] (1) 100g of low hydrogen-containing silicone oil with a hydrogen content of 0.03% and 6.54g of 4-(allyloxy)-2,2,6,6-tetramethylpiperidine were added to the reactor, and 0.02g of 1,3-Divinyl-1,1,3,3-tetramethyldisiloxane platinum complex and 0.03g of acetylacetone were heated to 80°C and reacted for 2h;

[0046] (2) The product of step (1) was stirred at 30° C. for 1 h, and the product obtained by filtration was recorded as Q1*.

Embodiment 2

[0054] (1) 250g of allyl polyether with the brand name of HMS-284M was added to the reactor, and 0.035g of 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum complexed and 0.05g of acetylacetone, the temperature was raised to 90°C, a total of 100g of heptamethylmonohydrogentrisiloxane was added in batches, and the reaction was carried out for 4h;

[0055] (2) 0.2 g of disodium EDTA was added to the product of step (1), stirred at 30° C. for 1 h, and the product obtained by filtration was recorded as S2.

[0056] Comparative Example 2*

[0057] (1) 250g of allyl polyether with the brand name of HMS-284M was added to the reactor, and 0.035g of 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum complexed and 0.05g of acetylacetone, the temperature was raised to 90°C, a total of 100g of heptamethylmonohydrogentrisiloxane was added in batches, and the reaction was carried out for 4h;

[0058] (2) The product of step (1) was stirred at 30° C. for 1 h, and the product obtained by f...

Embodiment 3

[0066] (1) 100g of low hydrogen-containing silicone oil with a hydrogen content of 0.1%, 4.25g of HMS-211M allyl polyether and 10.5g of 80HA-1050 polyether were added to the reactor, and 0.02g of 1,3 - Divinyl-1,1,3,3-tetramethyldisiloxane platinum complex and 0.03g acetylacetone, heated to 80°C for 3h reaction;

[0067] (2) 0.1 g of disodium EDTA was added to the product of step (1), stirred at 30° C. for 1 h, and the product obtained by filtration was recorded as S3.

[0068] Comparative Example 3*

[0069] (1) 100g of low hydrogen-containing silicone oil with a hydrogen content of 0.1%, 4.25g of HMS-211M allyl polyether and 10.5g of 80HA-1050 polyether were added to the reactor, and 0.02g of 1,3 - Divinyl-1,1,3,3-tetramethyldisiloxane platinum complex and 0.03g acetylacetone, heated to 80°C for 3h reaction;

[0070] (2) The product of step (1) was stirred at 30° C. for 1 h, and the product obtained by filtration was recorded as Q3*.

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Abstract

The invention relates to a method for reducing yellowing of a product in a hydrosilylation reaction process, which is characterized in that different auxiliaries are introduced in different stages of the hydrosilylation reaction, and finally, a metal catalyst in the product is complexed and adsorbed by the auxiliaries to form an insoluble substance, so that the yellowing degree of the product in the hydrosilylation reaction process is reduced, and the yield of the product is improved. Meanwhile, metal catalyst recovery is facilitated, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the field of organosilicon compound synthesis, and in particular relates to a method for reducing the yellowing of a product during a hydrosilylation reaction process. Background technique [0002] Hydrosilylation reaction is one of the most studied and widely used reactions in organosilicon chemistry. Since the discovery of this reaction by Sommer et al. in 1947, a lot of research work has been done on this reaction, especially on transition metal catalysts, and a lot of progress has been made. Ultraviolet rays, γ-rays, high temperatures, peroxides, and azo compounds can all make the hydrosilylation reaction, but due to the low selectivity, especially in some systems, it is difficult to avoid the polymerization of unsaturated compounds. Subject to many restrictions, is now less used. Since Speier discovered chloroplatinic acid, a very effective homogeneous hydrosilylation catalyst in 1957, transition metal catalysts formed f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388C08G65/00C08G77/46
CPCC08G77/388C08G65/00C08G77/46
Inventor 王璐王聪吕玉霞袁学宇杨艳飞
Owner JIANGXI BLUESTAR XINGHUO SILICONE CO LTD