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Ultra-high molecular weight polysiloxane synthesis method

A technology of ultra-high molecular weight polysiloxane, which is applied in the field of polymer materials, can solve the problems of unstable rubber materials, many low-molecular polymers, and slow equilibrium reactions, so as to achieve less residual impurities, good product performance, non-degradable effect

Pending Publication Date: 2019-06-04
烟台隆达树脂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Vinyl silicone oil is one of the main raw materials for the synthesis of addition-type silicone rubber. For a long time, potassium hydroxide, amine hydroxide and other alkali catalysts have been used to equilibrate the preparation, and use D4 and vinyl double-headed head to balance the reaction in the catalyst. And the mixing of water during the reaction process will cause a certain amount of Si-OH end groups to exist in the product. When configuring the addition-type liquid silicone rubber base polymer, it is easy to cause bubbles during the vulcanization process, which will affect the performance of the final product.
And it is difficult to neutralize to pH = 7. When configuring addition-type vulcanized silicone rubber, the presence of alkalinity will increase the viscosity of the liquid silicone rubber and make the rubber unstable.
[0003] Using an acidic catalyst for equilibrium reaction to prepare vinyl silicone oil has relatively low activity, and the equilibrium reaction proceeds very slowly
[0004] Although the acidity of trifluoromethanesulfonic acid is much higher than that of others, it can improve the reactivity, but whether it is an alkaline or an acidic catalyst, the final vinyl silicone oil produced by it has unbalanced vinyl arrangement, wide molecular weight distribution and low yield. There are more molecular polymers, which affect the performance of the final product, so there is still room for improvement

Method used

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  • Ultra-high molecular weight polysiloxane synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Put 1,000kg of hydroxyl-terminated polydimethylsiloxane with a viscosity of 5,000mpa.s into a stainless steel reactor and raise the temperature to 120°C. Under 1-2ml / min nitrogen flow, start dehydration treatment for 1 hour, then cool down, and add it to a 2,000-liter kneader , add 100 grams (containing 0.00002 grams of LPNC) of linear chlorinated phosphazene silicone oil solution below 80°C, the material starts to turn white after 10 minutes, the viscosity rises sharply, maintain the temperature at 120°C, and under the negative pressure of 0.06mpa lower than the atmospheric pressure React for 2 hours, release the vacuum, continue to heat up to 230°C, and stir and mix for 3 hours to make the catalyst invalid.

[0031] GPC (gel permeation chromatography) determined Mw 1200000 g / mol.

[0032] 170 ℃ vacuum oven for 2 hours, the volatile content is 0.05%, the color of the glue is transparent, without any smell.

[0033] The product prepared above was mixed with a toluene s...

Embodiment 2

[0036] Put 1,000kg of hydroxyl-terminated polydimethylsiloxane with a viscosity of 10,000mpa.s into a stainless steel reactor and heat up to 130°C. Under 1-2ml / min nitrogen flow, start dehydration treatment for 1 hour, then cool down, and add it to a 2,000-liter kneader , add 150 grams (containing 0.00003 grams of LPNC) of linear chlorinated phosphazene silicone oil solution below 80°C, the material starts to turn white after 5 minutes, the viscosity rises sharply, maintain the temperature at 100°C, and under the negative pressure of 0.1mpa lower than the atmospheric pressure React for 4 hours, release the vacuum, continue to heat up to 250° C., stir and mix for 2 hours, decompose the catalyst, and terminate the reaction.

[0037] GPC determined Mw 1800000 g / mol.

[0038] 170 ℃ vacuum oven for 2 hours, the volatile content is 0.08%, the color of the glue is transparent, without any smell.

[0039] The product prepared above was mixed with a toluene solution to prepare a tolue...

Embodiment 3

[0042] Put 2,000kg of hydroxyl-terminated polydimethylsiloxane with a viscosity of 3,000mpa.s into a stainless steel reactor and heat up to 115°C. Under 1-2ml / min nitrogen flow, start dehydration treatment for 1 hour, then cool down, and add it to a 3,000-liter kneader. Add 130 grams (including 0.000013 grams of LPNC) of linear chlorinated phosphazene silicone oil solution below 80°C. After 7 minutes, the material starts to turn white, and the viscosity rises sharply. Maintain the temperature at 118°C and react under negative pressure 0.06mpa lower than atmospheric pressure. After 3 hours, the vacuum was released, and the temperature was raised to 240° C. for 2 hours to decompose linear phosphazene chloride and terminate the reaction.

[0043] GPC determined Mw 600000 g / mol.

[0044] 170 ℃ vacuum oven for 2 hours, the volatile content is 0.028%, the color of the glue is transparent, without any smell.

[0045]The product prepared above was mixed with a toluene solution to pre...

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Abstract

The invention relates to the technical field of high molecular materials. Unbalanced arrangement of vinyl groups, wide molecular weight distribution and many low molecular polymers will influence performance of the final product. In allusion to the problem, the invention provides an ultra-high molecular weight polysiloxane synthesis method. The technical scheme is as follows: the ultra-high molecular weight polysiloxane synthesis method comprises the following steps: carrying out dehydration treatment on 100 parts by weight of hydroxyl-terminated polydimethyl siloxane, adding 0.01-0.015 partsby weight of a linear phosphonitrilic chloride silicone oil solution containing 20-30 ppm of linear phosphonitrilic chloride and stirring for 5-10 min until viscosity starts to rise, controlling temperature to 100-130 DEG C at negative pressure and stirring and reacting for 2-4 h, recovering normal pressure, continuously heating to 230-250 DEG C, reacting for 2-3 h, decomposing linear phosphonitrilic chloride, and terminating the reaction. By using the linear phosphonitrilic chloride, the arrangement of vinyl groups is ordered, molecular weight distribution is narrow, the content of low molecular volatile cyclosiloxane is low, and the performance of the final product is excellent.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a method for synthesizing ultrahigh molecular weight polysiloxane. Background technique [0002] Vinyl silicone oil is one of the main raw materials for the synthesis of addition-type silicone rubber. For a long time, potassium hydroxide, amine hydroxide and other alkali catalysts have been used to equilibrate the preparation, and use D4 and vinyl double-headed head to balance the reaction in the catalyst. And the mixing of water during the reaction process will cause a certain amount of Si-OH end groups to exist in the product. When configuring the addition-type liquid silicone rubber base polymer, it is easy to cause bubbles during the vulcanization process and affect the performance of the final product. Moreover, it is difficult to neutralize to pH = 7. When configuring addition-type vulcanized silicone rubber, the presence of alkalinity will increase the viscosity ...

Claims

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Application Information

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IPC IPC(8): C08G77/44
Inventor 赵秀华仇进华
Owner 烟台隆达树脂有限公司
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