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Alpha, omega-hydroxyl-terminated diphenyl siloxane and dimethhyl siloxane copolymer and preparation method thereof

A technology of dimethylsiloxane and diphenylsiloxane, which is applied in the field of organic silicon materials, can solve the problems of complex preparation process, complex process, easy breakage and the like of a mixed ring body, and achieves improved storage stability and simple process. , less corrosive effect

Inactive Publication Date: 2012-09-19
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can improve the poor activity of phenyl rings to a certain extent, the preparation process of mixed rings is complicated and the cost is high, especially the silicon-phenyl bond is easily broken under high temperature and strong alkalinity during the cleavage reaction.
Therefore, the process of producing α, ω-dihydroxyl-terminated diphenylsiloxane-dimethylsiloxane copolymers with medium and high phenyl content by this method is complicated and the cost is high

Method used

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  • Alpha, omega-hydroxyl-terminated diphenyl siloxane and dimethhyl siloxane copolymer and preparation method thereof
  • Alpha, omega-hydroxyl-terminated diphenyl siloxane and dimethhyl siloxane copolymer and preparation method thereof
  • Alpha, omega-hydroxyl-terminated diphenyl siloxane and dimethhyl siloxane copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039]Preparation of hydroxyl-terminated diphenylsiloxane-dimethylsiloxane copolymer

[0040] Add 45g of octaphenylcyclotetrasiloxane (D 4 Ph2 ) and 300g of dimethylsiloxane ring body (DMC), then add 0.2g of potassium silanolate catalyst and 1.5g of dimethyl sulfoxide. After closing the reaction system, start stirring, and raise the temperature to 150°C. After 20 minutes, the solid powder in the reaction bottle almost disappeared. Continue the reaction for 40 minutes. Add 4.0 g of deionized water to the reaction system for degradation reaction, and continue stirring for 2 hours.

[0041] After the degradation reaction, add 0.3g of propionic acid, neutralize the reaction for 1 hour, heat up to 160°C and vacuumize to 1mmHg for 4 hours to remove low molecular weight, and obtain a colorless, transparent, odorless hydroxyl-terminated diphenylsiloxane after cooling Alkane-dimethylsiloxane copolymer products. The viscosity of gained product is 4500mPas, and volatile matter content...

Embodiment 2

[0043] As described in Example 1, the difference is:

[0044] Add 130 g of D to the reaction vial 4 Ph2 And 300g of DMC, 0.3g of potassium silanolate catalyst and 2.5g of N,N-methylacetamide. Close the reaction system and raise the temperature to 150°C. After about 30 minutes, the solid powder in the reaction bottle almost completely disappears, and the reaction is continued for 50 minutes. The rest is the same as in Example 1, and a colorless, transparent, and odorless hydroxyl-terminated diphenylsiloxane is obtained. -Dimethicone copolymer products.

[0045] The viscosity, volatile content, refractive index, phenyl chain segment content and surface vulcanization time of the product were tested respectively, and the results are shown in Table 1.

Embodiment 3

[0047] As described in Example 1, the difference is:

[0048] Add 270 g of D to the reaction vial 4 Ph2 And the DMC of 300g, potassium siliconate catalyst 0.3g and tri-n-butyl phosphorus oxide 5.5g. Close the reaction system and raise the temperature to 150°C. After about 40 minutes, almost all the solid powder in the reaction bottle disappears, and the reaction is continued for 50 minutes. The rest is the same as in Example 1, and a colorless, transparent, odorless hydroxyl-terminated diphenylsiloxane is obtained. -Dimethicone copolymer products.

[0049] The viscosity, volatile content, refractive index, phenyl chain segment content and surface vulcanization time of the product were tested respectively, and the results are shown in Table 1.

[0050] from figure 1 As can be seen in , 3071cm -1 、3052cm -1 、3004cm -1 Both are absorption peaks of hydrogen on the benzene ring, 1590cm -1 and 1120cm -1 It is the absorption peak of silicon phenyl group, 1260cm -1 It is the...

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Abstract

The invention relates to an alpha, omega-hydroxyl-terminated diphenyl siloxane and dimethhyl siloxane copolymer and a preparation method thereof, and belongs to the field of organic silicon materials. The alpha, omega-hydroxyl-terminated diphenyl siloxane and dimethhyl siloxane copolymer is characterized in that the structural formula of the copolymer is shown as follows, and n and m in the formula are positive integers, and 0<n / (n+m)<70%. Octaphenyl-cyclotetrasiloxane is used as a phenyl-contained raw material, silanol sylvine is used as a catalyst, dimethyl sulfoxide and the like are used as accelerators, propionic acid and the like are used as neutralizers, and the raw materials are high in purity, easy to purchase or prepare according to the prior art, low in corrosivity and less toxic to human bodies and environment. The alpha, omega-hydroxyl-terminated diphenyl siloxane and dimethhyl siloxane copolymer and the preparation method thereof are simple and convenient in process and easy to operate, have no special requirements on equipment and avoid massive use of organic solvents so as to be environment-friendly and convenient for industrialization.

Description

technical field [0001] The invention relates to an α,ω-hydroxyl-terminated diphenylsiloxane-dimethylsiloxane copolymer and a preparation method thereof, belonging to the field of organic silicon materials. Background technique [0002] α,ω-Dihydroxy polydimethylsiloxane (low viscosity products are usually called hydroxy silicone oil, and the domestic trade name of high viscosity products is 107 glue), which is widely used in the processing of silicone rubber as a structural control agent, fabric Finishing agent, base polymer of condensation type RTV silicone rubber and other products. Hydroxyl-terminated diphenylsiloxane-dimethylsiloxane copolymers or methylsiloxanes obtained by introducing phenylsiloxane segments into α,ω-dihydroxypolydimethylsiloxane-containing molecules phenylsiloxane-dimethylsiloxane copolymer (the structural formula is shown in formula (1) and formula (2) respectively, Ph represents phenyl, x, y, m are positive integers, n is 0 or positive Integer), c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/18C08G77/08
Inventor 胡生祥桑圣凯付佃亮张停
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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