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Directly-thermocurable organic siloxane, manufacture method and application

A technology for curing products and reactions, applied in chemical instruments and methods, organic chemistry, organic insulators, etc., can solve the problems of difficult to control pre-polymerization, high cost of aryne resin synthesis, and large heat release.

Inactive Publication Date: 2015-02-04
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the synthesis cost of the above-mentioned aryne resins is relatively high, and noble metal palladium needs to be used as a catalyst; in addition, the high curing temperature of these resins (usually greater than 300 ° C) has a large heat release during curing, which limits their use.
What needs to be pointed out in particular is that many such aryne resins need to be pre-polymerized before use to obtain better film-forming properties, and pre-polymerization is generally difficult to control

Method used

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  • Directly-thermocurable organic siloxane, manufacture method and application
  • Directly-thermocurable organic siloxane, manufacture method and application
  • Directly-thermocurable organic siloxane, manufacture method and application

Examples

Experimental program
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Effect test

Embodiment 14

[0127] The preparation of embodiment 14-(methylpropargyloxy)-1-bromobenzene

[0128]

[0129] Under argon protection, add 51.9 grams of 4-bromo-phenol (0.3mol), 66.5 grams of methyl bromide propyne (0.5mol) and 300 milliliters of DMSO (dimethyl sulfoxide) steamed now in the reaction device, room temperature After stirring for 30 minutes, 53 grams of anhydrous sodium carbonate (0.5mol) was added. After reacting at room temperature for 10 hours, the reaction mixture solution was poured into water, stirred vigorously for 20 minutes, and the product was extracted with chloroform in batches. After washing with sodium chloride aqueous solution, chloroform was removed by rotary evaporation, and the obtained solid was washed with water and a small amount of ethanol to obtain 60 g of the product, with a yield of 89%. Hydrogen spectrum characterization ( 1 H NMR, 300MHz, CDCl 3 )7.55(d,2H),6.70(d,2H)4.55(s,2H),0.39(s,3H)

Embodiment 24

[0130] The preparation of embodiment 24-(methylpropargyloxy)-1-bromobenzene

[0131]

[0132] Under argon protection, add 51.9 grams of 4-bromo-phenol (0.3mol), 45.5 grams of methyl chloride propyne (0.5mol) and 300 milliliters of DMSO (dimethyl sulfoxide) steamed now in the reaction device, room temperature After stirring for 30 minutes, 53 grams of anhydrous sodium carbonate (0.5mol) was added. After reacting at room temperature for 10 hours, the reaction mixture solution was poured into water, stirred vigorously for 20 minutes, and the product was extracted with chloroform in batches. After washing with sodium chloride aqueous solution, chloroform was removed by rotary evaporation, and the obtained solid was washed with water and a small amount of ethanol to obtain 55 g of the product, with a yield of 81.5%. Hydrogen spectrum characterization ( 1 H NMR, 300MHz, CDCl 3 )7.55(d,2H),6.70(d,2H),4.55(s,2H),0.39(s,3H).

Embodiment 34

[0133] The preparation of embodiment 34-(methylpropargyloxy)-1-chlorobenzene

[0134]

[0135] Under argon protection, add 38.7 grams of 4-chloro-phenol (0.3mol), 66.5 grams of methyl bromide propyne (0.5mol) and 300 milliliters of DMSO (dimethyl sulfoxide) steamed now in the reaction apparatus, room temperature After stirring for 30 minutes, 53 grams of anhydrous sodium carbonate (0.5mol) was added. After reacting at room temperature for 10 hours, the reaction mixture solution was poured into water, stirred vigorously for 20 minutes, and the product was extracted with chloroform in batches. After washing with sodium chloride aqueous solution, chloroform was removed by rotary evaporation, and the obtained solid was washed with water and a small amount of ethanol to obtain 45 g of the product, with a yield of 82.9%. Hydrogen spectrum characterization ( 1 H NMR, 300MHz, CDCl 3 ) 7.55 (d, 2H), 6.70 (d, 2H), 4.55 (s, 2H), 0.36 (s, 3H).

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Abstract

The invention provides directly-thermocurable organic siloxane, a manufacture method and application, and concretely provides a polymer with the structure shown as the following formula A, and in the formula A, n is an integer between 10-20. The polymer can be cured to prepare a cured product which has excellent mechanical properties, good thermal stability and relatively low dielectric constant.

Description

technical field [0001] The invention belongs to the production field of high-performance polymer monomers, and in particular relates to a production method of organosiloxane containing methyl propargyl aryl ether which can be directly thermally cured. Background technique [0002] Silicone resins have high heat resistance, easy processing and excellent optical properties, and have been widely used in many industrial sectors. Typically, however, silicone resins need to be crosslinked in order to be useful. Commonly used cross-linking methods generally include hydrosilylation and free radical chain extension, and in most cases, such cross-linking methods either require a catalyst (metal platinum) or an initiator. [0003] It is known that polyfunctional organic molecules containing alkyne groups can undergo polymerization reactions under heating. Based on this feature, many alkyne polymers have been developed. Typically, aryl acetylene resins (J.Adv.Mater.1995, 4, 21), ethy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C08G77/14C08F283/12C08F222/40C08F299/08C08J5/18H01B3/46
Inventor 房强罗乙杰朱芝田
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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