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A kind of carboxyl functionalized polysiloxane and its preparation method

A technology of polyalkylhydridosiloxane and polysiloxane, which is applied in the field of carboxyl-functionalized polysiloxane and its preparation, can solve the problems of difficult purification, difficulty in expanding production, and high energy consumption of distillation process, and achieve Solve the problem of product separation and purification, reduce energy consumption, and improve the effect of reaction yield

Active Publication Date: 2019-10-01
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this invention, the reaction yield is low, thereby making the industrialization cost increase
Patent CN102731787B discloses a preparation method of carboxyl silicone oil, using undecylenic acid and methylhydrogen dichlorosilane as raw materials, and directly hydrosilylation under the catalysis of platinum / carbon catalyst to obtain 11-carboxyundecylmethyl Dichlorosilane, the preparation process of this invention is complicated, the distillation process involved is high in energy consumption, heavy in pollution, the molecular weight distribution of the obtained product is wide, the purification is difficult, and it is difficult to expand production
On the other hand, the carboxyl-functional polysiloxane obtained by the current preparation method has a low hydrosilylation rate
There are still a lot of active hydrogen in the product, which leads to many side reactions and unstable physical and chemical properties in subsequent applications

Method used

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  • A kind of carboxyl functionalized polysiloxane and its preparation method
  • A kind of carboxyl functionalized polysiloxane and its preparation method
  • A kind of carboxyl functionalized polysiloxane and its preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Step 1: in the drying four-neck flask that thermometer, condenser, dropping funnel, Ar pass inlet are housed, add 150g anhydrous toluene, start stirring, 72g methyl methacrylate (R 7 is methyl, R 8 is methyl, p is 0, 0.72mol) is added to toluene, and then 75g of polyalkylene with hydrogen content of 0.8wt% (Mn~950, m / n is 1 / 1, 0.6mol per mole of SiH) Hydrosiloxane is added to the mixed reaction system of toluene and methyl methacrylate. Then 300mg of Karstedt platinum catalyst (2wt% Pt in xylene solution) was added dropwise into the mixed reaction system. After the dropwise addition, the temperature was controlled at 20° C., and the reaction was continued for 12 hours. After the reaction was finished, 128.5 g of polysiloxane functionalized with methyl methacrylate was obtained by distillation under reduced pressure, with a yield of 95.2%. through 1 According to H NMR, the hydrosilylation rate is 98.5%.

[0075] The reaction equation is as follows:

[0076]

[0...

Embodiment 2

[0086] Step 1: in the drying four-neck flask that thermometer, condenser, dropping funnel, Ar pass inlet are housed, add 150g anhydrous toluene, start stirring, 72g methyl methacrylate (R 7 is methyl, R 8is methyl, p is 0, 0.72mol) is added to toluene, and then 75g of polyalkylene with hydrogen content of 0.8wt% (Mn~950, m / n is 1 / 1, 0.6mol per mole of SiH) Hydrosiloxane is added to the mixed reaction system of toluene and methyl methacrylate. Then 300mg of Karstedt platinum catalyst (2wt% Pt in xylene solution) was added dropwise into the mixed reaction system. After the dropwise addition, the temperature was controlled at 20° C., and the reaction was continued for 12 hours. After the reaction was finished, 128.5 g of polysiloxane functionalized with methyl methacrylate was obtained by distillation under reduced pressure, with a yield of 95.2%. through 1 According to H NMR, the hydrosilylation rate is 98.5%.

[0087] The reaction equation is as follows:

[0088]

[00...

Embodiment 3

[0095] Step 1: in the drying four-neck flask that thermometer, condenser, dropping funnel, Ar pass inlet are housed, add 150g anhydrous toluene, start stirring, 72g methyl methacrylate (R 7 is methyl, R 8 is methyl, p is 0, 0.72mol) is added to toluene, and then 75g of polyalkylene with hydrogen content of 0.8wt% (Mn~950, m / n is 1 / 1, 0.6mol per mole of SiH) Hydrosiloxane is added to the mixed reaction system of toluene and methyl methacrylate. Then 300mg of Karstedt platinum catalyst (2wt% Pt in xylene solution) was added dropwise into the mixed reaction system. After the dropwise addition, the temperature was controlled at 20° C., and the reaction was continued for 12 hours. After the reaction was finished, 128.5 g of polysiloxane functionalized with methyl methacrylate was obtained by distillation under reduced pressure, with a yield of 95.2%. through 1 According to H NMR, the hydrosilylation rate is 98.5%.

[0096] The reaction equation is as follows:

[0097]

[0...

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Abstract

The invention discloses carboxyl functionalized polysiloxane and a preparation method thereof. The method comprises the following steps: 1), subjecting polyalkyl hydrogenated siloxane and alkyl olefine acid derivatives to hydrosilylation to obtain carboxylate-functionalized polysiloxane; 2), subjecting the obtained carboxylate-functionalized polysiloxane successively to hydrolysis, acidification, extraction and vacuum drying to obtain the carboxyl functionalized polysiloxane. The hydrosilylation of the method provides complete addition, a synthetic process is simplified, reaction yield is increased, and side effects are reduced.

Description

technical field [0001] The invention belongs to the technical field of organosilicon products, and in particular relates to a carboxyl-functionalized polysiloxane and a preparation method thereof. Background technique [0002] Organosilicon materials are mainly a kind of polymer compound with Si-O bond as the main chain, and organic groups are introduced as side chains on Si, which have excellent performance and unique functions. In the past ten years, silicone materials have been widely used in military, construction, textile, electronics, medicine, electric power, automobile, chemical industry, aerospace and other fields, and have become a very popular industry. [0003] Polysiloxane, such as polydimethylsiloxane (PDMS), is a common silicone material in industrial production and scientific research. By modifying polysiloxane with functional groups, such as polyether, amino, epoxy, mercapto, carboxyl, anhydride, and hydroxyl, the application range of polysiloxane is greatl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/38C08G77/34
Inventor 李承辉游效曾赖建诚
Owner NANJING UNIV
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