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Method for preparing 2, 2'-dihydroxybiphenyl by taking dibenzofuran distillate as raw material

A technology of dihydroxybiphenyl and oxyfluorene, which is applied in the field of preparing 2,2'-dihydroxybiphenyl, can solve the problem of the purity not meeting the requirements for use, etc., and achieves the effects of good molding effect, improved yield and resource saving.

Pending Publication Date: 2021-02-09
河北中化鑫宝化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the modernization of the chemical industry, the purity of all chemicals required by the chemical industry has gradually increased with the continuous development of science and technology in our country. In the production of 2,2'-dihydroxybiphenyl, due to the rise of the new material industry, The requirements for the technical level and purity of 2,2'-dihydroxybiphenyl are getting higher and higher, but the decolorization process of the existing 2,2'-dihydroxybiphenyl production process after the alkali fusion reaction is a separate operation. Use activated carbon and sodium sulfite to decolorize, filter and acidify, the finished product contains a certain amount of inorganic salts, and the purity cannot meet the use requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A method for preparing 2,2'-dihydroxybiphenyl by using fluorene distillate as a raw material, including 2,2'-dihydroxybiphenyl, including the following raw materials in the weight ratio: 200 grams of dioxyfluorene distillate, 100 g of potassium hydroxide gram, 20 grams of dilute sulfuric acid and 100 grams of xylene.

[0024] A method for preparing 2,2'-dihydroxybiphenyls with dioxyfluorene cut as raw material, comprising the following steps:

[0025] 1) Add the fluorene distillate into the alkali fusion reaction kettle, heat up to 140°C, then add potassium hydroxide, start stirring after all the materials are melted, and raise the temperature to 275-280°C at a uniform speed, during which time the light components are distilled out . After the temperature reaches 265°C, stop the extraction of light components, and keep stirring at this temperature for 4 hours;

[0026] 2) After the heat preservation is completed, cool down to 120°C and add water to filter, adjust the ...

Embodiment 2

[0035] A method for preparing 2,2'-dihydroxybiphenyl by using oxyfluorene fraction as raw material, including 2,2'-dihydroxybiphenyl, including raw materials in the following weight ratio: 210 grams of oxyfluorene fraction, 95 grams of potassium hydroxide gram, 20 grams of dilute hydrochloric acid and 100 grams of toluene.

[0036] A method for preparing 2,2'-dihydroxybiphenyls with dioxyfluorene cut as raw material, comprising the following steps:

[0037] 1) Add the oxyfluorene fraction to the alkali fusion reaction kettle, heat up to 138°C, then add potassium hydroxide, start stirring after all the materials are melted, and raise the temperature to 275-280°C at a uniform speed, during which time the light components will be distilled out . After the temperature reaches 276°C, stop the extraction of light components, and keep stirring at this temperature for 3 hours;

[0038] 2) After the heat preservation is completed, cool down to 150°C and add water to filter, adjust th...

Embodiment 3

[0047] A method for preparing 2,2'-dihydroxybiphenyl by using oxyfluorene fraction as raw material, including 2,2'-dihydroxybiphenyl, including the following raw materials in the weight ratio: 198 grams of oxyfluorene fraction, 100 grams of potassium hydroxide gram, dilute sulfuric acid 20 grams and mixed solution (mass ratio toluene:xylene=1:1) 100g.

[0048] A method for preparing 2,2'-dihydroxybiphenyls with dioxyfluorene cut as raw material, comprising the following steps:

[0049] 1) Add the oxyfluorene fraction to the alkali fusion reaction kettle, heat up to 128°C, and then add potassium hydroxide. After all the materials are melted, start stirring, and raise the temperature to 275-280°C at a uniform speed, during which time the light components will be distilled out. . After the temperature reaches 278°C, stop the extraction of light components, and keep stirring at this temperature for 3 hours;

[0050] 2) After the heat preservation is completed, cool down to 130°C...

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Abstract

The invention relates to a method for preparing high-purity 2, 2'-dihydroxybiphenyl by taking dibenzofuran distillate as a raw material and belongs to the technical field of synthesis of 2, 2'-dihydroxybiphenyl. According to the method, dibenzofuran distillate (dibenzofuran content of 70-90%) extracted from wash oil is adopted as a raw material, and solid alkali sodium hydroxide, potassium hydroxide or a mixture thereof is adopted as an auxiliary material; the raw material reacts with the solid alkali sodium hydroxide, potassium hydroxide or the mixture thereof according to a feeding ratio of1: (0.5-2). The method comprises the following steps of: adding the dibenzofuran distillate into an alkali fusion reaction kettle; performing heating to 100-140 DEG C; adding the solid alkali, and performing slow heating; and distilling and extracting light components in the heating process. Compared with products obtained by other preparation processes of 2, 2'-dihydroxybiphenyl, a product obtained by the process of the invention is purer and does not contain salt impurities, so that the purity of the product is greatly improved; a large number of raw materials are saved, resource waste is avoided; a novel material processed by using the 2, 2'-dihydroxybiphenyl is better in using effect, and the forming effect of the produced novel material is better.

Description

technical field [0001] The invention relates to the technical field of 2,2'-dihydroxybiphenyl, in particular to a method for preparing 2,2'-dihydroxybiphenyl by using dioxyfluorene distillate as a raw material. Background technique [0002] 2,2'-Dihydroxybiphenyl is an important chemical intermediate, which can be used to synthesize a variety of pharmaceutical products such as nichlorophene, an anti-liver fluke drug, and is also an important polymer material intermediate, which can be used to prepare various polyesters , polycarbonate and epoxy resin macromolecular material modification monomers and the preparation of monomers for liquid crystal materials have great uses in medicine and macromolecular organic chemical industry, and have high production value and economic value. [0003] In the modernization of the chemical industry, the purity of all chemicals required by the chemical industry has gradually increased with the continuous development of science and technology ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/15C07C37/00C07C37/68C07C37/74C07C37/84
CPCC07C37/005C07C37/68C07C37/74C07C37/84C07C39/15
Inventor 吕国华纪烈义张振利
Owner 河北中化鑫宝化工科技有限公司
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