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Low-molecular-weight poly (arylene ether) and preparation method thereof

An arylene ether, low molecular weight technology, applied in the field of polyresin, can solve the problems of short preparation process, poor high temperature decomposition resistance, wide molecular weight distribution, etc., and achieve short process, high glass transition temperature and narrow molecular weight distribution. Effect

Pending Publication Date: 2021-12-17
NANTONG XINGCHEN SYNTHETIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, prepare low-molecular-weight poly(arylene ether) by the direct synthesis method that has been disclosed, mostly adopt complete detachment method to obtain low-molecular-weight poly(arylene ether), and complete detachment method has characteristics such as preparation procedure is short, easy production, but The complete detachment method retains impurities in the polymerization process (for example, red quinone), and has defects such as wide molecular weight distribution and poor resistance to pyrolysis

Method used

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  • Low-molecular-weight poly (arylene ether) and preparation method thereof
  • Low-molecular-weight poly (arylene ether) and preparation method thereof
  • Low-molecular-weight poly (arylene ether) and preparation method thereof

Examples

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Effect test

Embodiment 1

[0090] (1) Take 10Kg of 2,6-dimethylphenol monomer, 150Kg of toluene and 2Kg of copper ammonium composite catalyst to prepare a solution, inject it into the reaction kettle, start stirring, and pour it into the reaction kettle within the temperature range of 20±5°C Introduce 99.99% oxygen into the reactor, start the oxidative polymerization reaction at 40±2°C, then add 40Kg of 2,6-dimethylphenol into the reactor at a uniform speed within 60 minutes, continue the reaction after the dropwise addition, and take samples online until polymerization The intrinsic viscosity of the product reaches 0.12dl / g, and the polymerization is stopped.

[0091] (2) Add an aqueous solution of copper ion chelating agent to the mixed solution of low molecular weight poly(arylene ether), stir and extract for 15 minutes, then let stand for 20 to 30 minutes, separate and remove the lower aqueous phase. Wherein, the concentration of the aqueous solution of the copper ion chelating agent is 0.1mol / L, an...

Embodiment 2

[0099] (1) Get 10Kg of 1:0.8 molar ratio of 2,6-dimethylphenol monomer and mixed monomer of tetramethylbisphenol A, 150Kg of toluene and 2Kg copper ammonium composite catalyst to prepare solution, inject In the reaction kettle, start stirring, feed 99.99% oxygen into the reaction kettle within the temperature range of 20±5°C, start the oxidative polymerization reaction at 40±2°C, and then add 40Kg of 2, 6 Xylenol, continue to react after the dropwise addition is completed, take samples online for detection until the intrinsic viscosity of the polymerized product reaches 0.09dl / g, then stop the polymerization.

[0100] (2) Add an aqueous solution of copper ion chelating agent to the mixed solution of low molecular weight poly(arylene ether), stir and extract for 15 minutes, then let stand for 20 to 30 minutes, separate and remove the lower aqueous phase. Wherein, the concentration of the aqueous solution of the copper ion chelating agent is 0.1mol / L, and the dosage is 35L.

[...

Embodiment 3

[0108] (1) Take 10Kg of 2,6-dimethylphenol monomer, 150Kg of toluene and 3Kg of copper ammonium composite catalyst to prepare a solution, inject it into the reaction kettle, start stirring, and pour into the reaction kettle within the temperature range of 20±5°C Introduce 99.99% oxygen into the reactor, oxidatively polymerize at 40±2°C, then add 40Kg of 2,6-dimethylphenol to the reactor at a uniform speed within 60 minutes, continue the reaction after the dropwise addition, and take samples online until the polymerization product When the intrinsic viscosity reaches 0.28dl / g, the polymerization is stopped.

[0109] (2) Add an aqueous solution of copper ion chelating agent to the mixed solution of low molecular weight poly(arylene ether), stir and extract for 15 minutes, then let stand for 20 to 30 minutes, separate and remove the lower aqueous phase. Wherein, the concentration of the aqueous solution of the copper ion chelating agent is 0.1mol / L, and the dosage is 52.5L.

[0...

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Abstract

The invention provides low-molecular-weight poly (arylene ether) and a preparation method thereof. The preparation method comprises the following steps of: (1) in the presence of an oxidant and a catalyst, carrying out oxidative polymerization on a phenol monomer in agood poly (arylene ether) solvent to obtain a low-molecular-weight poly (arylene ether) mixed solution with intrinsic viscosity of 0.05-0.3 dl / g in a chloroform solution at 25 DEG C; (2) washing the mixed solution; (3) adding the washed mixed solution into a poor poly (arylene ether) solvent under stirring and inert atmosphere to form slurry, and filtering the slurry to obtain a wet material, the solid content of the low-molecular-weight poly (arylene ether) in the washed mixed solution being controlled to be 30-80wt%, and the weight ratio of the poor poly (arylene ether) solvent to the washed poly (arylene ether) mixed solution being 3 or more; and (4) drying the wet material to obtain low-molecular-weight poly (arylene ether). The low-molecular-weight poly (arylene ether) prepared by the method is low in quinone content, narrow in molecular weight distribution and high in glass-transition temperature.

Description

technical field [0001] The invention belongs to the technical field of poly(arylene ether) resins, and in particular relates to low molecular weight poly(arylene ether) and a preparation method thereof. Background technique [0002] Poly(arylene ether) is one of the five general-purpose engineering plastics, and has a wide range of applications in electronic appliances, automobiles, household appliances, office equipment, and industrial machinery. In recent years, with the rapid development of communication technology, the 5th generation (5G) communication technology has been promoted and used globally. 5G communication is a high-frequency communication technology that requires high electrical properties of materials, especially dielectric properties. Communication equipment The dielectric loss factor of basic materials, especially copper-clad laminates, has very high requirements. The smaller the dielectric loss factor within a certain range, the better the signal transmiss...

Claims

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Application Information

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IPC IPC(8): C08G65/44
CPCC08G65/44
Inventor 郝景峰戴伍国凌俊杰
Owner NANTONG XINGCHEN SYNTHETIC MATERIAL
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