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Polysiloxane intermediate, its preparing process and application

A polysiloxane and intermediate technology, applied in the field of polysiloxane intermediates and its preparation and application, can solve the problems of large limitations, physical state and physical properties, etc., and achieve the effect of enriching content

Inactive Publication Date: 2006-01-11
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of polysiloxane polymer materials is mostly the ring-opening polymerization of monomers, and the control of the molecular weight, physical state and physical properties of the product is not easy, so its limitations are relatively large

Method used

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  • Polysiloxane intermediate, its preparing process and application
  • Polysiloxane intermediate, its preparing process and application
  • Polysiloxane intermediate, its preparing process and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] When the coefficient x is 0.90 and m is 3, the synthesis route is as follows:

[0016]

[0017] The synthesis method is: in a Schlenk tube equipped with a stirring magnet, add hydrogen-containing silicone oil, N-allyl indole, a little dichlorodicyclopentadiene platinum catalyst, anhydrous toluene, under the condition of argon protection The reaction was stirred at 60°C for 48 hours, cooled to room temperature, and a large amount of solvent was distilled off under reduced pressure. Then add an appropriate amount of methanol, put it in the refrigerator for two hours, pour out the supernatant, dissolve the precipitate in a small amount of chloroform, and then reprecipitate with methanol, and do this several times to obtain a light green viscous solid P1, which is vacuum-dried at 40°C . Wherein the molar ratio of hydrogen-containing silicone oil to N-allylindole is 1:2.

[0018] Under the protection of an argon atmosphere, the molar ratio of P1:phosphorus oxychloride i...

Embodiment 2

[0025] When the coefficient x is 0.20 and m is 11, the synthesis route is as follows:

[0026]

[0027] The synthesis method is as follows: in a Schlenk tube equipped with a stirring magnet, add hydrogen-containing silicone oil, N-undecenyl indole, a little dichlorodicyclopentadiene platinum catalyst, anhydrous toluene, The reaction was stirred at 60°C for 48 hours under the condition, cooled to room temperature, and a large amount of solvent was distilled off under reduced pressure. Then add an appropriate amount of methanol, put it in the refrigerator for two hours, pour out the supernatant, dissolve the precipitate in a small amount of chloroform, and then re-precipitate with methanol, and do this several times to obtain a light green viscous liquid P7, which is vacuum-dried at 40°C . Wherein the molar ratio of hydrogen-containing silicone oil to N-undecenylindole is 1:2.

[0028] Under the protection of argon atmosphere, the molar ratio of P7:phosphorus oxychloride is...

Embodiment 3

[0035] When the coefficient x is 0.05 and m is 3, the synthesis route is as follows:

[0036]

[0037] The synthesis method is as follows: see Example 1 for the synthesis of P1.

[0038] Under the protection of an argon atmosphere, the molar ratio of P1:phosphorus oxychloride is 1:0.07, and phosphorus oxychloride is added to the N,N-dimethylformamide solution of P1 (concentration is 6~15wt%) ), react at 0°C for 50 minutes; then react at 50°C for 20 minutes, separate and purify to obtain the desired polysiloxane intermediate P13.

[0039] Examples of synthetic applications are as follows (synthesis of polysiloxane polymers with second-order nonlinear optical chromophores):

[0040] The synthesis methods are generally similar, and the usual synthesis steps are as follows:

[0041] Under the protection of argon atmosphere, dissolve P13 (2.5 mmol), cyanoacetylated chromophore (0.2 mmol) and hexahydropyridine (three drops) in 1.5 mL of freshly distilled N,N-dimethylformaldehyd...

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Abstract

The invention relates to a polysiloxane reaction intermediate having a structural formula disclosed in the specification, where x=0.05-1.00, m=2-11, n=30-100. The invention also discloses the process for preparing the polysiloxane intermediate. The required polysiloxane intermediate can be obtained through the reaction between poly (indolyl) oxosilane and phosphorus oxytrichloride in N, N-dimethyl formamide. The compound has good stability and special reaction activity, thus can be used in preparing various functional polysiloxane macromolecule material.

Description

technical field [0001] The invention relates to a polysiloxane reaction intermediate and its preparation method and application. Background technique [0002] Polysiloxane is a kind of polymer with inorganic main chain, which has various good properties. It is the most studied inorganic main chain polymer. Various polysiloxane polymer materials have been developed. has been more widely used. At present, the preparation of polysiloxane polymer materials is mostly the ring-opening polymerization of monomers, and the control of the molecular weight, physical state and physical properties of the product is not easy, so its limitations are relatively large. Contents of the invention [0003] The object of the present invention is to provide a stable polysiloxane intermediate with high reactivity and its preparation method and application. [0004] The technical solution provided by the invention is: a polysiloxane intermediate having the following general formula: [0005] ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/52C08G77/54
Inventor 李振秦金贵
Owner WUHAN UNIV
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