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A method for removing impurities in poly-2,6-diphenyl-p-phenylene ether

A technology of diphenyl, tetraphenyl diphenoquinone, applied in the field of chemistry, can solve problems such as poor cleaning effect and influence

Active Publication Date: 2019-01-18
派瑞科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In addition to the main product poly-2,6-diphenyl-p-phenylene ether, there is also a by-product 3,3',5,5-tetraphenyldiphenoquinone in the product obtained by the oxidative coupling method, and the diphenoquinone is almost Insoluble in precipitating agents, it will co-precipitate with the main product poly-2,6-diphenyl-p-phenylene ether during precipitation; solvent cleaning is currently used to remove the diphenoquinone, but the cleaning effect is not good, affecting poly-2,6-diphenylene ether The mass of phenyl p-phenylene ether

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0033] Add 150mL of benzene, 0.006mol of cuprous bromide, 0.006mol of 1,3-butanediamine and 15g of 2,6-diphenylphenol into a 250mL three-necked flask, heat to 55°C, and flow at 100mL / min Introduce oxygen, stir and react for 3 hours to obtain about 150 mL of solution, which is the product after the oxidation coupling reaction is complete; add 5 mL of aqueous hydrochloric acid with a mass concentration of 15% to the product, stir for 15 minutes, and remove cuprous bromide in the product And 1,3-butanediamine, liquid separation, take upper layer solution B, sample 5mL from upper layer solution B, dry, obtain 0.5g dry matter, be dissolved in 5mL chloroform, in Shimadzu UV-1501 ultraviolet-visible spectrophotometer Using colorimetric analysis, it can be seen that the characteristic absorption peak of poly-2,6-diphenyl-p-phenylene ether is at 347nm, the content is 0.47g, and the characteristic absorption peak of 3,3',5,5-tetraphenyldiphenoquinone is at 256nm , the content is 0.03g, ...

Embodiment 2

[0036] Add 150mL of benzene, 0.006mol of cuprous chloride, 0.006mol of ethylenediamine and 15g of 2,6-diphenylphenol into a 250mL three-necked flask, heat to 55°C, and feed oxygen at a flow rate of 100mL / min. Stir the reaction for 3 hours to obtain about 150 mL of solution, which is the product after the oxidation coupling reaction is complete; add 7.5 mL of acetic acid aqueous solution with a mass concentration of 25% to the product, stir for 15 minutes, and remove cuprous chloride and ethylene dichloride in the product. Amine, liquid separation, take upper layer solution B, sample 5mL from upper layer solution B, dry, obtain 0.5g dry matter, dissolve in 5mL chloroform, adopt colorimetric method analysis on Shimadzu UV-1501 ultraviolet-visible spectrophotometer, It can be seen that the characteristic absorption peak of poly-2,6-diphenyl-p-phenylene ether is at 347nm, and the content is 0.45g; the characteristic absorption peak of 3,3',5,5-tetraphenyldiphenoquinone is at 256nm,...

Embodiment 3

[0039]Add 150mL of benzene, 0.006mol of cuprous iodide, 0.006mol of 1,3-propylenediamine and 15g of 2,6-diphenylphenol into a 250mL three-necked flask, heat to 55°C, and flow at 100mL / min Feed oxygen, stir and react for 3 hours to obtain about 150 mL of solution, which is the product after the oxidation coupling reaction is complete; add 7.5 mL of acetic acid aqueous solution with a mass concentration of 15% to the product, stir for 15 minutes, and remove cuprous iodide and 1,3-propanediamine, liquid separation, take the upper layer solution B, sample 5mL from the upper layer solution B, dry to obtain 0.5g dry matter, dissolve in 5mL chloroform, and use it on Shimadzu UV-1501 UV-visible spectrophotometer Using colorimetric analysis, it can be seen that the characteristic absorption peak of poly-2,6-diphenyl-p-phenylene ether is at 347nm, and the content is 0.44g; the characteristic absorption peak of 3,3',5,5-tetraphenyldiphenoquinone is at 256nm, The content is 0.06g, 145mL o...

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Abstract

The invention relates to a method for removing impurities from poly 2,6-diphenyl-p-phenylene oxide, and belongs to the field of chemistry. The method comprises the following steps of mixing and dissolving the poly 2,6-diphenyl-p-phenylene oxide and impurities of 3,3',5,5'-tetraphenyl biphenyl quinone in an organic solvent to obtain a raw material solution; adding a reducing agent; under protection gas, performing stirring reduction reaction at 10 to 70 DEG C; performing stirring and liquid separation; taking an upper layer solution A; stirring and simultaneously adding a precipitating agent into the upper layer solution A; filtering, cleaning and drying to obtain the impurity-removed poly 2,6-diphenyl-p-phenylene oxide. The method has the advantages that after the impurities are reduced into 3,3',5,5'-tetraphenyl biphenyl quinone, the easy dissolution into the precipitating agent is realized; in the poly 2,6-diphenyl-p-phenylene oxide precipitating process, precipitates are not separated out; 3,3',5,5'-tetraphenyl diphenol mixed in the poly 2,6-diphenvl-p-phenvlene oxide precipitates can be removed through cleaning; the impurities can be fast and thoroughly removed.

Description

technical field [0001] The invention relates to a method for removing impurities in poly-2,6-diphenyl-p-phenylene ether, in particular to a reduction method for removing impurities 3,3' in poly-2,6-diphenyl-p-phenylene ether , The method for 5,5-tetraphenyldiphenoquinone belongs to the field of chemistry. Background technique [0002] Poly(2,6-diphenyl-p-phenylene ether) is a kind of polyphenylene ether resin, and its structure has high thermal stability. Poly-2,6-diphenyl-p-phenylene ether is used as an adsorption material in the sampling and analysis of organic matter, which has the advantages of high adsorption efficiency and reproducibility; in addition, poly-2,6-diphenyl-p-phenylene ether is also used as a chromatographic packing . [0003] In the prior art, poly-2,6-diphenyl-p-phenylene ether is usually prepared by 2,6-diphenylphenol through an oxidative coupling reaction (abbreviated as an oxidative coupling method) in the presence of a copper amine complex catalyst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/46
CPCC08G65/46
Inventor 许东海陈欢姜燕石晶蔡淑红顾秀杰王峰
Owner 派瑞科技有限公司
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