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Method for synthesizing high content of 4,4'-dihydroxydiphenylmethane by one-step method

A technology of dihydroxydiphenyl and step method, which is applied in the field of synthetic compounds, can solve problems such as too long process routes, and achieve the effects of simple synthesis process, convenient operation and high yield

Inactive Publication Date: 2009-05-27
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0029] Shenyang Institute of Comprehensive Utilization of Chemical Industry used a two-step method to synthesize bisphenol F in the invention patent application with the publication number CN 1160704A, but the process route was too long

Method used

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  • Method for synthesizing high content of 4,4'-dihydroxydiphenylmethane by one-step method
  • Method for synthesizing high content of 4,4'-dihydroxydiphenylmethane by one-step method
  • Method for synthesizing high content of 4,4'-dihydroxydiphenylmethane by one-step method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Add 37.6g of phenol into a four-neck flask equipped with an electric stirrer, a thermometer and a reflux condenser, heat in a water bath, and after the phenol is fully melted, drop in 5.4ml of phosphoric acid, stir vigorously to fully mix the phenol and phosphoric acid, and then slowly drop Add 8.2 g of formaldehyde solution (according to mass percentage, the concentration of formaldehyde solution is 37%), make the molar ratio of phenol and formaldehyde 4: 1, and react at a constant temperature at 45°C for 4 hours, stop stirring, and separate the acid and oil phase with a separatory funnel Neutralize with sodium bicarbonate to pH 5.6, then separate the water from the organic phase, then use a rotary evaporator for vacuum distillation to remove phenol and water, cool, crystallize, and filter to obtain the product.

[0047] see figure 1 , the peaks of chemical shift 3.931 and 3.924 belong to the methylene nuclei of 2,2'-structure and 2,4'-structure respectively, and the p...

Embodiment 2

[0050] Similar to Example 1, the difference is that the concentration of formaldehyde solution is 40%, the molar ratio of phenol to formaldehyde is 5:1, and the oil phase is neutralized to pH 6 with sodium bicarbonate.

Embodiment 3

[0052] As described in Example 1, the amount of phenol was changed to 28.3g, so that the molar ratio of phenol to formaldehyde was 3:1, and the concentration of formaldehyde was 38% by mass percentage, and the oil phase was neutralized with sodium bicarbonate until the pH value was 5.5 .

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Abstract

The invention discloses a method for synthesizing dihydroxy diphenyl methane with high 4, 4' site content by one stage process, relates to a method for synthesizing bisphenol F with high 4, 4' site content and provides a method for synthesizing dihydroxy diphenyl methane with high 4, 4' site content by one stage process, which reduces dosage of phenol and production cost and has yield of more than 60 percent. The method comprises the following steps: adding the phenol into a container provided with an electric stirrer, a thermometer and a reflux condensation tube, heating the phenol in water bath, adding phosphoric acid after the phenol is fully melted, stirring the mixture, and fully mixing the phenol and the phosphoric acid to obtain mixed solution; adding formaldehyde solution into the mixed solution, separating acid after reaction, neutralizing an oil phase by sodium bicarbonate, separating water and an organic phase, decompressing and distilling the mixed solution, removing the phenol and the water, and cooling, crystallizing and filtering the mixed solution to obtain products.

Description

technical field [0001] The invention relates to a method for synthesizing bisphenol F with high 4,4' content, in particular to a method for synthesizing dihydroxydiphenylmethane with high 4,4' content in one step. Background technique [0002] Bisphenol F (Bisphenol F) is a new type of chemical raw material developed in the 1980s. It is a common name for dihydroxydiphenylmethane. It is a bisphenol compound produced by condensation reaction of phenol and formaldehyde under the action of an acidic catalyst. . [0003] Bisphenol F is mainly used as a raw material for low-viscosity epoxy resins, special polyesters, and additives for information recording paper. Due to the characteristics of its chemical structure, when synthesizing epoxy resin, polyester resin, polycarbonate resin and as an additive to phenolic resin, the heat resistance, moisture resistance, insulation, especially processability and mechanical properties of the products obtained Both are far superior to simil...

Claims

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Application Information

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IPC IPC(8): C07C39/16C07C37/20
Inventor 邹友思赵军温庆如林睿许锐林华端
Owner XIAMEN UNIV
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