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Preparation method of alkoxy-terminated linear polydimethylsiloxane

The technology of polydimethylsiloxane and dimethylsiloxane is applied in the field of preparation of linear polydimethylsiloxane, which can solve the difficulty in the reaction between siloxy groups and silanol groups, prolong the reaction time, and increase the reaction time. Process and other problems, to achieve the effect of controllable viscosity range, simple production process and easy industrialization

Active Publication Date: 2022-05-06
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese patent CN103936995A mentions that the reaction product of secondary amine and weak acid can be used as a catalyst to prepare alkoxy-terminated linear polysiloxane, but the catalyst needs to be self-made, which increases the reaction process; CN103382251A mentions the use of tetramethylammonium hydroxide or Alkali gum is used as a catalyst to prepare alkoxy-terminated polysiloxane. There will be mono-alkoxy-terminated by-products in this reaction. The catalyst needs to be decomposed at high temperature, releasing an unfriendly smell, and the requirements for equipment are relatively high. High; CN104558612A mentions to use organic amine salt as catalyst to prepare alkoxy-terminated polysiloxane, although this method can improve the capping efficiency of alkoxy group, it is reported that its alkoxy group capping rate can only reach 95% at the highest ; CN104927058A mentions the use of granular cation exchange resins as catalysts to prepare alkoxy-terminated polysiloxanes, and this patent reports that this reaction is only applicable to the preparation of low-viscosity alkoxy-terminated polysiloxanes; CN106674524A utilizes at least Three alkoxy silsesquioxanes are used as end-capping agents, which can improve the stability and heat resistance of the final alkoxy-terminated polydimethylsiloxane, but because silsesquioxane has a large cage The structure makes the reaction between silanoxy and silanol relatively difficult. Compared with ordinary alkoxysilane, at the same reaction temperature, it is necessary to prolong the reaction time or increase the reaction temperature, and the price of silsesquioxane is much higher. Far higher than the price of ordinary alkoxysilane; CN106905530A discloses a preparation method of alkoxy-terminated polysiloxane, the preparation method is complex, and the catalyst 4-vinylbenzo-18- The crown ether-6 complex has a high boiling point and is difficult to remove, and the price is relatively expensive

Method used

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  • Preparation method of alkoxy-terminated linear polydimethylsiloxane
  • Preparation method of alkoxy-terminated linear polydimethylsiloxane

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Add 60kg of α, ω-dihydroxyl-terminated polydimethylsiloxane, 1.8kg of tetramethoxysilane, 16g of formic acid, and 48g of sodium acetate at 2000mPa·s respectively in a 100L mechanical reaction kettle. After stirring evenly, the reaction The temperature of the kettle was raised to 40°C. After 120 minutes of reaction, the vacuum degree was controlled at -0.06MPa. After evacuating for 100 minutes, alkoxy-terminated polydimethylsiloxane was obtained. The product performance test results are shown in Table 1.

Embodiment 2

[0034] Add 60kg of α, ω-dihydroxyl-terminated polydimethylsiloxane, 1.5kg of vinyltrimethoxysilane, 60g of acetic acid, and 60g of sodium carbonate at 5000mPa·s into a 100L mechanical reactor, and stir evenly. The temperature of the reactor was raised to 60°C. After 80 minutes of reaction, the vacuum degree was controlled at -0.06MPa. After 80 minutes of vacuuming, alkoxy-terminated polydimethylsiloxane was obtained. The product performance test results are shown in Table 1. .

Embodiment 3

[0036] In a 100L mechanical reactor, add 10000mPa·s of α, ω-dihydroxy-terminated polydimethylsiloxane 60kg, methyltrimethoxysilane 980g, acetic anhydride 140g, sodium carbonate 30g, sodium acetate 40g, After stirring evenly, the temperature of the reactor was raised to 80°C. After 60 minutes of reaction, the vacuum degree was controlled at -0.08MPa. After 60 minutes of vacuuming, alkoxy-terminated polydimethylsiloxane was obtained. Product performance test results See Table 1 for details.

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Abstract

The invention provides a preparation method of linear polydimethylsiloxane with an end capped by an alkoxy group. The raw materials for preparing the polydimethylsiloxane by the method are low in price and easy to obtain, the production process is simple, the operation is easy, the reaction temperature is mild, no special requirement on equipment exists, the alkoxy end capping rate is greater than 99%, no side reaction exists, the viscosity range of the product is controllable, the thickening and crosslinking phenomena do not exist after the polydimethylsiloxane is mixed with phthalic ester, and industrialization is easy to realize.

Description

technical field [0001] The invention belongs to the field of organosilicon materials, in particular to a preparation method of alkoxy-terminated linear polydimethylsiloxane. Background technique [0002] The low-molecular-weight alcohol released during the vulcanization of dealcoholized room temperature vulcanized silicone rubber is low-toxic and environmentally friendly, has no irritating odor, and is non-corrosive to metals. It can be widely used in electronic appliances and construction industries. As a green and environmentally friendly sealant, it has great Good development prospects. At present, the dealcoholized silicone rubber sealants on the domestic market mainly use α, ω-dihydroxy-terminated polydimethylsiloxane as the base rubber, alkoxysilane as the crosslinking agent, organic titanium as the catalyst, and fillers. In the preparation process, the viscosity of the system rises sharply or even gels, which is usually called "viscosity peak"; at the same time, duri...

Claims

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Application Information

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IPC IPC(8): C08G77/38C08G77/18C08G77/20C08G77/06
CPCC08G77/38C08G77/18C08G77/20C08G77/06
Inventor 高希银张志杰汪倩刘利谭永霞谢择民戴丽娜张立波
Owner INST OF CHEM CHINESE ACAD OF SCI
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