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Method for synthesizing carborane polyarylester in greenhouse and carborane polyarylester

A technology for carborane polyarylate and room temperature synthesis, which is applied in the field of carborane polyarylate and carborane polyarylate synthesis at room temperature, can solve the problem of high risk, achieve high molecular weight, simple and easy operation, The effect of excellent thermal stability and mechanical properties

Active Publication Date: 2016-03-23
佛山市南海高拓包装材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, traditional carborane polymers need to react under high temperature conditions above 200 degrees, which is highly dangerous

Method used

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  • Method for synthesizing carborane polyarylester in greenhouse and carborane polyarylester
  • Method for synthesizing carborane polyarylester in greenhouse and carborane polyarylester
  • Method for synthesizing carborane polyarylester in greenhouse and carborane polyarylester

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preparation example Construction

[0039] The preparation method of the carborane polyarylate provided by the invention only needs to be carried out at room temperature, and does not need to be carried out at high temperature like traditional carborane-containing polymers, and is safe and reliable, with high molecular weight and a yield of more than 75%. The process solves the problem of different solubility of the acid chloride phase and phenol relative to the same solvent, resulting in different proportions of raw materials. By controlling the proportion of monomers, the order of feeding, etc., the molecular weight and end group structure of the polymer are regulated; the polymer is dissolved in the organic phase to solve the problem of polymerization The poor solubility of the substance to the system cannot be a problem of increasing the polymer while gradually polymerizing the raw material with a high conversion rate; the operation process is simple and easy. The obtained carborane polyarylate resin has exce...

Embodiment 1

[0049] Synthesis of polyarylate with 4,4-diacid chloride diphenyl ether and 1,2-bis(4-hydroxyphenyl)-o-carborane: in a system equipped with constant pressure funnel, reflux condenser, stirring device, rubber stopper In the 100mL three-necked flask with argon inlet, at room temperature, first add 1,2-bis(4-hydroxyphenyl)-o-carborane (2.05g, 6.25mmol) in the three-necked flask in NaOH aqueous solution ( 0.7M) 15ml, then add benzyltriethylammonium chloride (BTEAC) (0.0125g, 0.055mmol), and slowly add 4,4-diacid chloride diphenyl ether (1.845g, 6.25mmol) dropwise with a constant pressure funnel ) in dichloromethane (37.5ml), stirred slowly, and added dropwise within 30min. Stir vigorously and continue to react at room temperature for 12 hours. The excess solvent was distilled off under reduced pressure, and vacuum-dried at 40 degrees to obtain the white target product: 2.949g, yield 92%; 1100cm in the product -1 The aryl ether peak of R-O-R appears at 2600cm -1 The stretching v...

Embodiment 2

[0051] Synthesis of polyarylate with 4,4-diacid chloride diphenyl ether and 1,7-bis(4-hydroxyphenyl)-m-carborane: in a system equipped with constant pressure funnel, reflux condenser, stirring device, rubber stopper In the 100mL three-necked flask with argon inlet, at room temperature, first add 1,7-bis(4-hydroxyphenyl)-m-carborane (2.05g, 6.25mmol) in the three-necked flask in NaOH aqueous solution ( 0.7M) 8.9ml, then add benzyltriethylammonium chloride (BTEAC) (0.0125g, 0.055mmol), and slowly add 4,4-diacid chloride diphenyl ether (1.845g, 6.25 mmol) in dichloromethane (37.5ml), stirred slowly, and added dropwise within 30min. Stir vigorously and continue to react at room temperature for 12 hours. The excess solvent was distilled off under reduced pressure, and vacuum-dried at 40 degrees to obtain the white target product: 2.55g, yield 89%; 1100cm in the product -1 The aryl ether peak of R-O-R appears at 2600cm -1 The stretching vibration peak of B-H appears at 750cm -1 ...

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Abstract

The invention discloses a method for synthesizing carborane polyarylester in a greenhouse and carborane polyarylester. The method is performed under the protection of inert gas and in a water-free and oxygen-free environment by using diacid chloride dissolved by low-molecular-weight halogenated hydrocarbon as an organic phase, using carborane diphenol dissolved by deionized water as an inorganic phase, using benzyl triethyl ammonium chloride and strong alkali as catalyst, slowly dropping the organic phase into the inorganic phase, and performing quick agitation after full dropping to obtain high-molecular-weight carborane polyarylester. Operation is performed at room temperature instead of high temperature at which the traditional carborane-containing polymer is synthesized, the safety and reliability are high, the molecular weight is great and the yield is above 75 percent.

Description

technical field [0001] The invention relates to the technical field of organic polymers, in particular to a method for synthesizing carborane polyarylate at room temperature and carborane polyarylate. Background technique [0002] Polyarylate (PAR), also known as aromatic polyester, is named for its main chain with aromatic rings and ester bonds. It is a special engineering plastic with thermoplasticity. It is an amorphous polymer similar to polycarbonate and polysulfone, but a higher grade engineering plastic. Due to the large number of aromatic rings in the main chain structure of polyarylate, it conforms to Hückel's rule, has good heat resistance, and has a wide service temperature. Aerospace, electronic appliances, automobile and machinery industries, medical supplies and daily necessities and other industries have a wide range of applications. [0003] Polyarylate was studied in the 1950s. The earliest research report was that in 1957, Belgian Couix first prepared pol...

Claims

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Application Information

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IPC IPC(8): C08G63/698C08G63/79
CPCC08G63/6986C08G63/79
Inventor 霍锦钊白永平李宁张建军吴育荣
Owner 佛山市南海高拓包装材料有限公司
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