Preparation method of bisphenol F with high ortho-position isomer content

A technology of isomers and high ortho positions, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of easy crystallization of resins, slow curing speed of bisphenol F epoxy resins, and vicinal problems in bisphenol F. low content of isomers, etc., to achieve the effect of simple and easy process operation

Active Publication Date: 2011-05-25
NANTONG XINGCHEN SYNTHETIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to propose a kind of preparation method of high ortho isomer content bisphenol F, to solve the low ortho isomer content in the bisph

Method used

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  • Preparation method of bisphenol F with high ortho-position isomer content
  • Preparation method of bisphenol F with high ortho-position isomer content

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Embodiment 1

[0018] Add 540g of molten phenol in a 1000ml three-necked flask, and protect it with nitrogen. Start stirring, and adjust the pH value to 2 with phosphoric acid with a mass concentration of 65%, and heat up to 70°C, and drop 20g of formaldehyde solution with a mass concentration of 37.2% within 1h, and react at 70°C for 1.5h; Then add 100g of phosphoric acid solution with a mass concentration of 65% to the reaction solution, and maintain the temperature at 60°C, add 6g of formaldehyde solution with a mass concentration of 37.2% dropwise within 30min, and keep it at 60°C for about 2h, and end reaction. Then the reaction solution is placed in a separatory funnel, allowed to stand for layers, and the phosphoric acid phase of the lower layer is separated; then neutralize the organic phase with 5% sodium hydroxide solution, so that the pH of the organic phase is 5; Phenol, until the temperature is 190°C, the bisphenol F product is obtained. (The concentrations of the above-mentio...

Embodiment 2

[0022] Add 552g of molten phenol in a 1000ml three-necked flask, and protect it with nitrogen. Start stirring, and adjust the pH value to about 2 with 65% phosphoric acid, and heat up to 70°C, and drop 20g of formaldehyde solution with a mass percentage of 37.2% within 1h, and react at 70°C for 1.5h; Add 100g of phosphoric acid solution with a concentration of 65% to the reaction solution, and maintain the temperature at 60°C, add 6g of formaldehyde solution with a concentration of 37.2% dropwise within 30min, and maintain the reaction at 62°C for 2h to end the reaction. Then the reaction solution was placed in a separatory funnel, allowed to stand for layers, and the phosphoric acid phase in the lower layer was separated; then neutralized the organic phase with 5% sodium hydroxide solution, so that the pH of the organic phase was 6; Phenol, until the temperature is 190°C, the bisphenol F product is obtained. (The concentrations of the above-mentioned solutions are all in mas...

Embodiment 3

[0026] Add 564g of molten phenol in a 1000ml three-necked flask, and protect it with nitrogen. Start stirring, and adjust the pH value to 2 with phosphoric acid with a mass concentration of 65%, and heat up to 70°C, and drop 30g of formaldehyde solution with a mass concentration of 37.2% within 1h, and react at 70°C for 1.5h; Then add 100g of phosphoric acid solution with a mass concentration of 65% to the reaction solution, and maintain the temperature at 61°C, add 22g of a formaldehyde solution with a mass concentration of 37.2% dropwise within 30min, and keep it at 61°C for 2h to end the reaction . Then the reaction solution is placed in a separatory funnel, allowed to stand for layers, and the phosphoric acid phase of the lower layer is separated; then neutralize the organic phase with 5% sodium hydroxide solution, so that the pH of the organic phase is 5; Phenol, until the temperature is 190°C, the bisphenol F product is obtained.

[0027] The composition analysis of th...

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Abstract

The invention discloses a preparation method of bisphenol F with high ortho-position isomer content. The preparation method comprises the following steps: synthesizing the bisphenol F by adopting a two-step method, separating an organic phase and a phosphoric acid phase, neutralizing the organic phase and removing salt, and recovering phenol under the reduced pressure to obtain the bisphenol F product, wherein in the first step of the two-step synthesis method, the phenol reacts with formaldehyde under the weakly acidic condition; and in the second step, a large amount of catalyst phosphoric acid and formaldehyde are added into the reaction liquid obtained in the first step, and the formaldehyde completely reacts. The invention overcomes the defects that the content of the ortho-position isomer in the bisphenol F prepared by the existing bisphenol F preparation method is low, the curing speed of the synthesized bisphenol F epoxy resin is slow, the resin is easy to crystallize and the like.

Description

technical field [0001] The invention relates to a preparation method of bisphenol F, in particular to a preparation method of bisphenol F with high ortho isomer content. Background technique [0002] Bisphenol F (BPF) The chemical name of bisphenol F is 4,4'-dihydroxydiphenylmethane, which is an important chemical intermediate. It is formed by condensation of phenol and formaldehyde, and its structural formula is as follows: [0003] [0004] Due to the characteristics of the reaction raw materials, bisphenol F is difficult to obtain a higher purity product, and it often exists simultaneously with 2,4-dihydroxydiphenylmethane and 2,2'-dihydroxydiphenylmethane. Due to its chemical structure characteristics, when synthesizing epoxy resin, polyester resin, polycarbonate and as a modifier and stabilizer of phenolic resin, the heat resistance, moisture resistance, insulation, processability and injection casting of the obtained product The performance is far superior to simi...

Claims

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Application Information

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IPC IPC(8): C07C39/16C07C37/20
Inventor 陈明蒋超
Owner NANTONG XINGCHEN SYNTHETIC MATERIAL
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