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Preparation method of high-content 4, 4 minute-isomer bisphenol F

A technology of isomers and content, applied in the field of organic catalytic synthesis, can solve the problems of strong corrosion of inorganic acid catalysts, high molar ratio of phenol and formaldehyde, difficult separation and recovery, etc., to reduce operating costs and environmental pressure, and low molar ratio , the effect of low operating cost

Inactive Publication Date: 2015-09-02
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a kind of high-efficient green preparation method of bisphenol F with high 4,4'-isomer content, to solve the 4,4'-isomer content in existing phenol, formaldehyde synthesis bisphenol F product Not high, high molar ratio of phenol to formaldehyde, synthetic products need to be separated and purified by organic solvents, inorganic acid catalysts are highly corrosive, difficult to separate and recover, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Embodiment 1 Add 1 mole of phenol, 1 mole of ionic liquid catalyst [C 4 mim][HSO 4 ], heated to 65°C, fully stirred at a stirring speed of 500 rev / min (the present embodiment, the same below), adding 68.5 grams of formaldehyde solution with a mass percentage of 22%, so that phenol, [C 4 mim][HSO 4 ], formaldehyde, and water in a molar ratio of 2:2:1:6, reflux and stir at a constant temperature of 65°C for 6 hours, finish the reaction, cool to room temperature, add 1 mole of ethyl acetate to the reaction solution, stir and mix well, The reaction solution was left to stand and separated, and the upper organic phase was distilled under reduced pressure to recover ethyl acetate and phenol in stages to obtain the bisphenol F product, wherein the mass percentage of 4,4'-isomer bisphenol F was 69.1% , the mass yield of bisphenol F was 42.0%. The ethyl acetate and phenol recovered from the upper organic phase and the ionic liquid aqueous phase directly recovered from the lowe...

Embodiment 2

[0014] Embodiment 2 is the same as embodiment 1, but the ionic liquid catalyst is changed into [C 2 mim][HSO 4 ], in the bisphenol F product, the 4,4'-isomer bisphenol F mass percent content is 59.2%, and the bisphenol F mass yield is 41.9%.

Embodiment 3

[0015] Embodiment 3 is the same as embodiment 1, but the ionic liquid catalyst is changed into [C 6 mim][HSO 4 ], in the bisphenol F product, the 4,4'-isomer bisphenol F mass percent content is 63.2%, and the bisphenol F mass yield is 49.5%.

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PUM

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Abstract

The invention discloses a preparation method of high-content 4, 4 minute-isomer bisphenol F. The preparation method comprises the following steps of (1) the catalysis and aqueous solution characteristics of water-soluble acid imidazole salt ionic liquids are utilized to catalyze phenol and formaldehyde to compound the bisphenol F under the condition of keeping appropriate water volume, low phenol and formaldehyde mole ratio sum, and lower reaction temperature, and a compound reaction effect of the high-content 4, 4 minute-isomer bisphenol F is obtained; (2) an ionic liquid catalyst water phase can be directly separated, recovered and reused through adding ethyl acetate, stirring, mixing, standing and layering, so that the corrosivity on equipment is obviously reduced; (3) the reaction batch charging phenol and formaldehyde mole ratio is low, and the recovered phenol amount, the operation cost and the environment pressure are obviously reduced; (4) the ethyl acetate is low in boiling point so as to be convenient to evaporate and recover; (5) the whole preparation process is low in operation cost, low in corrosivity, high in material utilization, green and environmental-friendly.

Description

technical field [0001] The invention relates to a preparation method of bisphenol F with high 4,4'-isomer content, which belongs to the field of organic catalytic synthesis. Background technique [0002] Bisphenol F has three isomers, 4,4'-, 2,4'-, and 2,2'-, and is usually synthesized by acid-catalyzed phenol and formaldehyde. When the content of 4,4'-isomer in bisphenol F is high, it is beneficial to the curing of functional groups to form a linear network structure, with low viscosity and good fluidity. No diluent added. At present, it has been reported that in the methods for synthesizing bisphenol F, the content of 4,4'-isomer bisphenol F in the synthetic product (referring to mass percentage, the same below) is mostly in the range of 42% to 55%. Patent CN101440022A reports that the 4,4'-isomer bisphenol F content is 49.5% in the phosphoric acid catalysis method, and the patent US43384706 reports that the 4,4'-isomer bisphenol F content is 55% in the phosphoric acid c...

Claims

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Application Information

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IPC IPC(8): C07C39/16C07C37/20
CPCY02P20/584C07C37/20C07C39/16
Inventor 刘跃进何志成吴志民王丹凤李勇飞潘浪胜
Owner XIANGTAN UNIV
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