Preparation method of high-yield 4, 4'-biphenol

A high-yield technology for biphenol, which is applied in the field of preparation of 4,4'biphenol, can solve the problems of difficult product purification, harsh reaction conditions, and high equipment requirements, and achieve easy product purification, fast reaction speed, The effect of low equipment requirements

Pending Publication Date: 2022-01-21
宁夏清研高分子新材料有限公司
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Problems solved by technology

[0006] (3) Biphenyl halogenation high-pressure hydrolysis method: use biphenyl as raw material, and 4,4' biphenyldiphenol can be obtained through halogenation, hydrolysis and other reactions. This method has harsh reaction conditions, high requirements on equipment, and also has environmental pollution The problem;
[0008] The above-mentioned several traditional methods for preparing 4,4'biphenyldiphenol usually use an organic medium as a reaction solvent. After the reaction, the treatment of the organic solvent will cause certain pollution to the environment, and the by-products in the reaction process The reaction will lead to low conversion rate, and the preparation of 4,4'biphenol by oxidative coupling method requires three steps of oxidation, reduction and de-isobutylation, and the de-tert-butyl step requires a large amount of three Aluminum chloride brings difficulties to product purification

Method used

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  • Preparation method of high-yield 4, 4'-biphenol
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  • Preparation method of high-yield 4, 4'-biphenol

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preparation example Construction

[0032] The preparation method of the high-yield 4,4'biphenyldiol of the present application is characterized in that it comprises the following steps:

[0033] S1: Utilizing metal sources on CeO 2 Loading is carried out to prepare a metal-loaded semiconductor material;

[0034] S2: After adding the metal-supported semiconductor material prepared in S1 and 2,6-di-tert-butylphenol into the reaction vessel, oxygen was introduced to carry out the oxidation coupling reaction of 2,6-di-tert-butylphenol, and then the The reaction product was filtered and dried to obtain product A;

[0035] S3: Add the product A and ethanol prepared in S2 into the reaction vessel, add the catalyst after it is completely dissolved, and perform a reduction reaction at 60-80°C for 1-3 hours with stirring, then spin evaporate the ethanol, and pump the remaining substance while it is hot After filtering, washing, and finally drying to obtain product B;

[0036] S4: Add the product B, m-xylene and sodium...

Embodiment 1

[0049] S1: Weigh 2g of CeO in a beaker 2 Nano powder, then add 20ml of lysine solution (concentration is 0.53mol / L), mix well and add 20ml of 0.1mol / L HAuCl 4 solution, and then move it to an oil bath at 80°C, slowly add 0.5mol / L sodium carbonate solution dropwise under stirring until the pH is 7, filter it with a Buchner funnel after constant temperature for 2 hours, and then filter the filter cake with a deionized Washed with water for 3 times, then placed it in an oven at 60 °C to dry, and finally dried the catalyst in N 2 Calcined in a muffle furnace at 400°C under protection for 4 hours, and after grinding, a noble metal-supported semiconductor catalyst was obtained;

[0050] S2: First add 2g of 2,6-di-tert-butylphenol into a 25mL three-necked flask, then add 5g of water and 0.2g of sodium dodecylbenzenesulfonate, stir for 20min and then add 0.02g of precious metal loaded For semiconductor catalysts, evacuate and then pass through O 2 , carry out oxidative coupling rea...

Embodiment 2

[0054] S1: Weigh 2g of CeO in a beaker 2 Nano powder, then add 20ml of lysine solution (concentration is 0.53mol / L), mix well and add 12ml of 0.1mol / L PdCl 2 solution, and then move it to an oil bath at 60°C, slowly add 0.5mol / L sodium carbonate solution dropwise under stirring until the pH is 7, filter it with a Buchner funnel after constant temperature for 3 hours, and then filter the filter cake with a deionized Washed with water for 3 times, then placed it in an oven at 60 °C to dry, and finally dried the catalyst in N 2 Calcined in a muffle furnace at 450°C under protection for 3 hours, and obtained a noble metal-supported semiconductor catalyst after grinding;

[0055] S2: First add 2g of 2,6-di-tert-butylphenol into a 25mL three-necked flask, then add 5g of water and 0.2g of sodium dodecylbenzenesulfonate, stir for 20min and then add 0.02g of precious metal loaded For semiconductor catalysts, evacuate and then pass through O 2 , carry out oxidative coupling reaction ...

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Abstract

The invention relates to the technical field of organic synthesis, and concretely relates to a preparation method of high-yield 4, 4'-biphenol. According to the preparation method, a metal-loaded semiconductor material is used as a catalyst, oxygen is used as an oxidizing agent, an oxidative coupling reaction of 2, 6-di-tert-butylphenol is realized, the reaction is carried out at normal temperature, the reaction speed is high, the conversion rate is high, and then a small amount of by-products are reduced into 4, 4 '-biphenol through a reduction reaction, purification and filtration are performed, tert-butyl is efficiently removed from the filtered product with p-toluenesulfonic acid as a catalyst, the target product is obtained, and the obtained 4, 4'-biphenol is high in yield and good in quality. The metal-loaded semiconductor material can be recycled, and a large amount of organic medium solvent and a large amount of aluminum trichloride are not used in the preparation process, so the method has the advantages of low environmental pollution, easiness in product purification, mild reaction conditions, low equipment requirements and good application prospects, and meets the requirements of large-batch production and manufacturing.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing 4,4' biphenol with high yield. Background technique [0002] As an important organic intermediate, 4,4'biphenyldiphenol can be used to manufacture engineering plastics and their composite materials, etc. Because 4,4' biphenyl has anti-oxidation, anti-aging and non-polluting properties, it is widely used in food packaging, colorless or light-colored vulcanized rubber products and medical latex products. At the same time, 4,4' biphenyl Diphenol also has the property of high temperature resistance, and can be used as a modified monomer such as polyester, polycarbonate (PC), polyphenylsulfone, polyurethane and epoxy resin. In addition, it can also be used as a raw material for liquid crystal polymers. Used in the manufacture of high-strength fibers, reinforced optical fibers, etc. As early as the 1970s, 4,4'biphenol was used in the production of liq...

Claims

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Application Information

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IPC IPC(8): C07C37/50C07C39/15C07C37/70C07C37/82B01J23/63B01J23/66
CPCC07C37/50C07C37/70C07C37/82B01J23/63B01J23/66C07C39/15Y02P20/584
Inventor 张东宝于冉徐良
Owner 宁夏清研高分子新材料有限公司
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