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Preparation method of bisphenol A epoxy ethane additive product

A technology of ethylene oxide and adduct, which is applied in the field of preparation of bisphenol A ethylene oxide adduct, can solve the problems of product performance influence, residue, etc., and achieves a reaction with good reaction selectivity and high yield. Effect

Active Publication Date: 2012-07-04
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] In the above-mentioned method of synthesizing BHE-BPA using ethylene oxide as a raw material, the catalyst remains in the product, which will affect the performance of the product to varying degrees.

Method used

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  • Preparation method of bisphenol A epoxy ethane additive product

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preparation example Construction

[0030] The steps of the preparation method of bisphenol A ethylene oxide adduct are as follows:

[0031] (1) Dissolve 1 mole of bisphenol A and 0.001~0.01 mole of catalyst in 2~10 moles of ether solvent at 80~150°C, and add the solution in 5~10 moles of n-hexane or n-heptane dropwise at this temperature 2.05~2.30 moles of ethylene oxide in the solution, keep it warm until the residual bisphenol A is less than 10ppm;

[0032] (2) Slowly lower the temperature to 0-30°C for crystallization, then filter, wash with n-hexane or n-heptane, and vacuum-dry to obtain a product with a content of more than 98% of bisphenol A plus 2 moles of ethylene oxide;

[0033] (3) The crystallization mother liquor is rectified under normal pressure or vacuum to separate n-hexane or n-heptane, which can be used together with the contained catalyst in the next reaction process.

[0034] The catalyst refers to tri-n-butylamine, tri-n-octylamine or tri-n-decylamine.

[0035]The ether solvent is di-n-pr...

Embodiment 1

[0038] Add 228g (1 mole) bisphenol A, 0.101g (0.001 mole) tri-n-butylamine catalyst and 436g (2 moles) diethylene glycol di-n-butyl ether in a 3L pressure-resistant glass bottle with stirring, and heat up to 150 ℃ to dissolve into a transparent solution; dissolve 90.2g (2.05 moles) of ethylene oxide in 1000g (10 moles) of n-heptane; add the above ethylene oxide dropwise through a constant pressure dropping funnel within 4 hours at a temperature of 150°C The n-heptane solution of alkane, after the dropwise addition, continue the reaction until the residual bisphenol A detected by HPLC is less than 10ppm. After the reaction is completed, slowly lower the temperature to 30°C and keep it warm for 5 hours to fully crystallize, then filter with suction, wash the crystals with 300g of n-heptane, and dry in vacuum at 80°C to constant weight to obtain 301.8g of BHE-BPA finished product, the HPLC detection content is 98.7 %.

Embodiment 2

[0040] The mother liquor obtained in Example 1 was rectified under reduced pressure in a 3000ml three-neck flask with a 50cm rectifying column to obtain 1280g of reclaimed n-heptane and 451g of reclaimed diethylene glycol di-n-butyl ether containing catalyst tri-n-butylamine. Add 228g (1 mole) of bisphenol A and 451g of diethylene glycol di-n-butyl ether recovered above into a 3L pressure-resistant glass bottle with stirring, and dissolve it at 150°C to become a transparent solution; Dissolve ethylene oxide in 1000g (10 moles) of the recovered n-heptane; add the above-mentioned n-heptane solution of ethylene oxide dropwise within 4 hours at a temperature of 150°C, and continue the reaction until bisphenol A is detected by HPLC The residue is less than 10ppm. After the reaction is completed, slowly lower the temperature to 30°C and keep it warm for 5 hours to fully crystallize, then filter with suction, wash the crystals with 300g of n-heptane, and dry in vacuum at 80°C to cons...

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Abstract

The invention discloses a preparation method of a bisphenol A epoxy ethane additive product. The method comprises the following steps of: dissolving 1 mole of bisphenol A and 0.001-0.1 mole of trialkylamine catalyst into 2-10 mole of ether solvent of which the temperature is 80-150 DEG C, and dropwise adding 2.05-2.30 mole of epoxy ethane which can be dissolved into 5-10 mole of n-hexane or n-heptane at the same temperature; and after reacting, slowly cooling to 0-30 DEG C for crystalizing, filtering, washing n-hexane or n-heptane, and performing vacuum drying to obtain 2 mole of bisphenol A-added epoxy ethane product of which the content is over 98 percent. After n-hexane or n-heptane is separated out of a crystalized mother liquor through normal-pressure or reduced-pressure rectification, the crystalized mother liquor can be taken as an ether solvent containing a catalyst for use in a next reacting process. The method has the advantages of high reaction selectivity, high yield, circular usability of the catalyst and suitability for industrial production.

Description

technical field [0001] The invention relates to a preparation method of bisphenol A ethylene oxide adduct. Background technique [0002] Bisphenol A ethylene oxide adducts have different uses according to the degree of ethylene oxide addition. Among them, the 2-mole ethylene oxide adduct of bisphenol A - bishydroxyethylated bisphenol A (hereinafter referred to as BHE-BPA) is widely used because of its structure, which has both the rigidity of the benzene ring and the flexibility of ethoxylate ether. It is used in the synthesis of various polyester resins, photocurable unsaturated polyester monomers, etc. The structure of BHE-BPA is as follows: [0003] [0004] The synthesis methods of BHE-BPA reported in the literature are as follows. [0005] Jiao Jiajun (Acta Functional Polymers, 2003, 16(2): 211-213) and others used 2-chloroethanol as a hydroxyethylation reagent to synthesize BHE-BPA with bisphenol A under alkaline conditions through Williamson reaction. The react...

Claims

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Application Information

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IPC IPC(8): C07C43/23C07C41/03
Inventor 尹红陈志荣郭粟王新荣袁慎峰马定连王胜利
Owner ZHEJIANG UNIV
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