Method for preparing bisphenol F

A phenol and solid acid catalyst technology, applied in the chemical industry, can solve the problems of catalyst waste environmental pollution, difficult to recycle catalysts, serious corrosion of instruments and equipment, etc., and achieve easy separation, recovery and reusability, high catalyst activity and catalytic selectivity, Environmentally friendly effect of catalyst

Inactive Publication Date: 2014-07-23
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent applications JP08198790, JP08268943, and JP09067287 respectively report methods for synthesizing bisphenol F with oxalic acid, phosphoric acid, and hydrochloric acid as catalysts, wherein the phenol-formaldehyde ratio is 4-50:1, and the temperature is within the range of 40-90°C, but the bisphenol F The yields are not high, basically 70-80%, and the catalyst is difficult to recover
Inorganic acid catalysis has the following disadvantages: it is difficult to separate from unreacted raw materials and products after the reaction; it corrodes the equipment seriously; the catalyst waste will cause serious pollution to the environment; the production cost is high
When organic acids are used as catalysts, the reaction temperature is required to be high, resulting in more by-products, high energy consumption in the production process, and the problem of difficult separation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Preparation of catalyst

[0018] Weigh 60.0g of bentonite and roast at 400°C for 2h; then slowly add 50.0g of 10% methanol solution of phosphotungstic acid to 20.0g of roasted bentonite, react at room temperature for 3h, distill off the solvent, and forge at 300°C Burn for 24h to obtain solid acid catalyst C1.

[0019] (2) Synthesis of Bisphenol F

[0020] Weigh 1.56g of solid acid catalyst C1, 83.8g of phenol and 5.20g of formaldehyde (37%), and add them into the reaction flask. Heating, controlling the reaction temperature at 120°C, stirring for 2 hours, removing the catalyst by filtration, to obtain a solution containing bisphenol F, and performing post-processing such as distillation to obtain bisphenol F product with a yield of 93%.

Embodiment 2

[0022] (1) Preparation of catalyst

[0023] Weigh 60.0g of montmorillonite and roast at 200°C for 8h; then slowly add 50.0g of 5% methanol solution of silicotungstic acid to 22.5g of roasted montmorillonite, react at room temperature for 16h, distill off the solvent, Calcined at 200°C for 24 hours to obtain solid acid catalyst C2.

[0024] (2) Synthesis of Bisphenol F

[0025] Weigh 1.30g of solid acid catalyst C2, 83.8g of phenol and 10.40g of formaldehyde (37%), and add them into the reaction flask. Heating, controlling the reaction temperature at 130°C, stirring and reacting for 4 hours, filtering and removing the catalyst to obtain a solution containing bisphenol F, and carrying out post-processing such as distillation to obtain bisphenol F product with a yield of 77%.

Embodiment 3

[0027] (1) Preparation of catalyst

[0028] Weigh 60.0g of diatomite and roast at 500°C for 2h; then slowly add 50.0g of 20% methanol solution of phosphomolybdic acid to 15.0g of roasted bentonite, react at room temperature for 12h, distill off the solvent, 300°C Calcined for 16 hours to obtain solid acid catalyst C3.

[0029] (2) Synthesis of Bisphenol F

[0030] Weigh 1.30g of solid acid catalyst C3, 83.8g of phenol and 5.2g of formaldehyde (37%), and add them into the reaction flask. Heating, controlling the reaction temperature at 100°C, stirring and reacting for 4 hours, filtering and removing the catalyst to obtain a solution containing bisphenol F, and carrying out post-processing such as distillation to obtain bisphenol F product with a yield of 73%.

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Abstract

The invention discloses a method for preparing bisphenol F. The method is characterized in that phenol and formaldehyde serving as raw materials and a solid acid catalyst serving as a catalyst are used to prepare the target product bisphenol F, wherein the solid acid catalyst is prepared from heteropoly acid modified clay, and the mass dosing ratio of the catalyst to formaldehyde is (0.01-0.6):1; and the heteropoly acid is one or more of phosphotungstic acid, phosphomolybdic acid, silicotungstic acid, silicomolybdic acid and the like, wherein the clay is one or more of bentonite, kaoline, montmorillonoid, metakaolin, diatomaceous earth and the like. The method has the prominent advantages that the yield of the product bisphenol F is up to 93 percent, the selection to bisphenol F is 96 percent, the catalyst is friendly to environment, the preparation process is simple, the production cycle is short, the catalyst activity and catalytic selection are high, separation and reclamation are easy, recycling is available, and industrialization is facilitated.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a preparation method of bisphenol F. Background technique [0002] Bisphenol F is a new type of chemical raw material developed in the 1880s. It is mainly used as a raw material for plastics and rubber in fine chemical production. In the synthesis of bisphenol epoxy resin, in addition to all the excellent properties of bisphenol A epoxy resin, the viscosity of the epoxy resin synthesized from bisphenol F is only 1 / 4 to 1 / 7 of that of bisphenol A. Therefore, it has become a very cutting-edge research direction in recent years. my country is a big consumer of synthetic resin in the world. In recent years, the import volume has been ranking first in the world. In foreign countries, the production of bisphenol F has formed a large scale, the synthesis research has been less, and the application research has been deepened, but there is no report of large-scale production in C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/16C07C37/20B01J31/26
CPCB01J23/28B01J23/30B01J27/199C07C37/20C07C39/16
Inventor 夏新年刘冉
Owner HUNAN UNIV
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