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Preparation method of bisphenol F

A technology of bisphenol and phenol, applied in the field of preparation of bisphenol F, can solve the problems of high energy consumption of phenol, high consumption of phenol, large energy consumption of recovery and the like

Inactive Publication Date: 2012-06-27
胶州市精细化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the large excess of phenol reduces the production capacity of the equipment on the one hand, and on the other hand, the energy consumption of reclaiming unreacted phenol is very high
[0010] Chinese patent literature (CN 102070409A) also discloses a preparation method of bisphenol F with high 2,4'- and 2,2'-isomer content. The method adopts a two-step synthesis method. Under the conditions (adjusting the pH to 2-3 by phosphoric acid), then add a large amount of catalyst phosphoric acid and formaldehyde to the first step reaction solution to completely react the formaldehyde to obtain a 2,4'-isomer ratio of 42-46 % bisphenol F, but this method also has the defect of excessive phenol consumption
[0011] To sum up, the 4,4'-isomer is the main component of the readily available bisphenol F on the market, and the methods for increasing the ratio of the 2,4'-isomer all have too much phenol, Recycling high energy consumption and other defects

Method used

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  • Preparation method of bisphenol F
  • Preparation method of bisphenol F
  • Preparation method of bisphenol F

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 500ml four-necked flask equipped with mechanical stirring, reflux condenser, thermometer and constant pressure dropping funnel, add molten phenol (225g, 2.4mol), 85% phosphoric acid (74g, 0.64mol) and acetic acid (9.6g) , 0.16mol), stir evenly, heat up to 80°C, slowly add 37% formaldehyde (32.5g, 0.4mol) dropwise within 3h, after the addition, react at 80-85°C for 2h, stop stirring, stand for stratification, in Add solid NaHCO to the organic phase 3 Adjust pH=5, filter at 65-70°C, remove the precipitation insoluble in organic phase (mainly NaH 2 PO 4 / NaAc), the filtrate is distilled under high vacuum (2-5mmHg) under reduced pressure to recover unreacted phenol, the distillation temperature is 120-140 ° C, the residual liquid after removing the phenol is dissolved with 5% NaOH, and transferred to another flask The pH is adjusted to 9-10 with hydrochloric acid again. At this time, there is precipitation, and the filter cake is filtered. After drying, the filter ca...

Embodiment 2

[0032] In a 500ml four-necked flask equipped with mechanical stirring, reflux condenser, thermometer and constant pressure dropping funnel, add molten phenol (225g, 2.4mol), 85% phosphoric acid (74g, 0.64mol) and acetic acid (9.6g) , 0.16mol), stir evenly, heat up to 80°C, slowly add 37% formaldehyde (32.5g, 0.4mol) dropwise within 3h, after adding, react at 95°C for 1h, stop stirring, stand for stratification, in the organic phase Add solid NaHCO 3 Adjust pH=5, filter at 65-70°C, remove the precipitation insoluble in organic phase (mainly NaH 2 PO 4 / NaAc), the filtrate is distilled under high vacuum (2-5mmHg) under reduced pressure to recover unreacted phenol, the distillation temperature is 120-140 ° C, the residual liquid after removing the phenol is dissolved with 5% NaOH, and transferred to another flask The pH is adjusted to 9 with hydrochloric acid again, and a precipitate is precipitated at this time. Filter, and the filter cake is dried to obtain bisphenol F, which...

Embodiment 3

[0037]In a 500ml four-necked flask equipped with mechanical stirring, reflux condenser, thermometer and constant pressure dropping funnel, add molten phenol (225g, 2.4mol), 85% phosphoric acid (74g, 0.64mol) and acetic acid (9.6g) , 0.16mol), stir evenly, heat up to 70°C, add 37% formaldehyde (32.5g, 0.4mol) dropwise within 3h, after the addition, react at 70°C for 2h, stop stirring, stand for stratification, in the organic phase Add solid NaHCO 3 Adjust pH=5, filter at 65-70°C, remove the precipitation insoluble in organic phase (mainly NaH 2 PO 4 / NaAc), the filtrate is distilled under high vacuum (2-5mmHg) under reduced pressure to recover unreacted phenol, the distillation temperature is 120-140 ° C, the residual liquid after removing the phenol is dissolved with 5% NaOH, and transferred to another flask The pH is adjusted to 9 with hydrochloric acid again, and a precipitate is precipitated at this time. Filter, and the filter cake is dried to obtain bisphenol F, which i...

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Abstract

The invention relates to a preparation method of bisphenol F, which is characterized in that under the condition of existence of an acid catalyst, phenol and formaldehyde are reacted to obtain the product. The acid catalyst is a mixture of inorganic acid and organic acid, and the mol ratio of the inorganic acid to organic acid is 10-2:1; the inorganic acid is oxygen-containing acid of phosphor, the organic acid is C1-C4 straight chain or branched chain monoacid or diacid. The invention has the advantages that under the condition that P / F is less than or equal to 10, the bisphenol F with high ortho-isomer (especially 2,4'-isomer ) content can be obtained, the production capability of the device can be increased, and the operation cost and the energy consumption are reduced.

Description

technical field [0001] The invention relates to a preparation method of bisphenol F (bisphenol F). Background technique [0002] Bisphenol F is a key component in the production of epoxy resins. Compared with epoxy resins made from bisphenol A, epoxy resins made from it have the characteristics of low viscosity and excellent workability. For solvent-free and even ultra-high solid content coatings, it can also be used in lining materials, floor materials, injection molding materials, impregnating materials, laminate materials and other fields. [0003] Bisphenol F is generally formed by the condensation of phenol and formaldehyde in the presence of an acidic or Friedel-Grafts catalyst. Its chemical name is dihydroxyphenylmethane, and its structural formula is as follows: [0004] [0005] Bisphenol F is a mixture of 4,4'-dihydroxyphenylmethane (hereinafter referred to as 4,4'-isomer), 2,4'-dihydroxyphenylmethane (hereinafter referred to as 2,4'-isomer) and 2,2'-dihydroxy...

Claims

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Application Information

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IPC IPC(8): C07C39/16C07C37/20
CPCY02P20/52
Inventor 沈永嘉王洪太潘昌艺杨苗宋卫涛王帅
Owner 胶州市精细化工有限公司
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