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Method for preparing biphenyl through catalyzing loop opening of dibenzofuran

A technology of benzofuran and biphenyl, which is applied in the field of fine chemical synthesis, can solve the problems of low selectivity, cumbersomeness, and many process steps, and achieves the effects of long operation time, avoidance of post-treatment, and small environmental impact.

Inactive Publication Date: 2018-12-07
斯爱玲
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The use of active metal sodium requires many process steps, which is relatively cumbersome and has certain risks.
[0004] Chinese patent, publication number: CN106495991A discloses a method for dibenzofuran ring-opening to prepare biphenyl, using a solvent to dissolve dibenzofuran in a dissolution tank, the dissolution temperature is 80-100°C, and the dissolved dibenzofuran The furan organic solution is injected into a fixed-bed reactor equipped with a selective hydrofining catalyst for hydrofining reaction. After the hydrofinishing reaction, the product is directly rectified in a rectification tower, and o-phenylphenol is directly granulated as a product. The yield of o-phenylphenol is about 10%, and the selectivity is low

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  • Method for preparing biphenyl through catalyzing loop opening of dibenzofuran

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Experimental program
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Embodiment 1

[0020] Alumina is used as a carrier, nickel hypophosphite is used as a nickel source, and sodium hypophosphite is used as a phosphorus source. The impregnating solution is configured by 1 part by weight of nickel hypophosphite, 1 part by weight of sodium hypophosphite and 4 parts by weight of distilled water. The volume of the impregnating solution is equal to the volume of the maximum adsorbed water of the catalyst carrier. The molar ratio of nickel and phosphorus atoms in the impregnating solution is 1:3. The impregnation at room temperature is carried out according to the impregnation method of equal volume, and 2 parts by weight of the impregnating solution are added dropwise to 1 part by weight of the alumina carrier, and the stirring is continued. After the dropwise addition, it was allowed to stand at room temperature for 5h. Dry at a temperature of 60°C for 6h; then, put the dried catalyst precursor into a tubular reactor and feed nitrogen with a volumetric space velo...

Embodiment 2

[0022] Alumina is used as a carrier, nickel hypophosphite is used as a nickel source, and sodium hypophosphite is used as a phosphorus source. The impregnating solution is configured by 1 part by weight of nickel hypophosphite, 1 part by weight of sodium hypophosphite and 4 parts by weight of distilled water. The volume of the impregnating solution is equal to the volume of the maximum adsorbed water of the catalyst carrier. The molar ratio of nickel and phosphorus atoms in the impregnating solution is 1:3. The impregnation at room temperature is carried out according to the impregnation method of equal volume, and 2 parts by weight of the impregnating solution are added dropwise to 1 part by weight of the alumina carrier, and the stirring is continued. After the dropwise addition, it was allowed to stand at room temperature for 5h. Dry at a temperature of 60°C for 6h; then, put the dried catalyst precursor into a tubular reactor and feed nitrogen with a volumetric space velo...

Embodiment 3

[0024] Alumina is used as a carrier, ferric nitrate is used as an iron source, and sodium hypophosphite is used as a phosphorus source. The impregnating solution is prepared by 1 weight part of ferric nitrate, 2 weight parts of sodium hypophosphite and 4 weight parts of distilled water, and the volume of the impregnating solution is equal to the volume of the maximum water absorbed by the catalyst carrier. The impregnation at room temperature is carried out according to the impregnation method of equal volume, and 1 part by weight of impregnating solution is added dropwise to 1 part by weight of alumina carrier, and stirred continuously. After the dropwise addition, it was allowed to stand at room temperature for 5h. Dry at a temperature of 60°C for 6h; then, put the dried catalyst precursor into a tubular reactor and feed nitrogen with a volumetric space velocity of 450h -1 , the pressure is 1.0MPa, the temperature is raised to 250°C at a rate of 2°C / min, and the constant te...

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Abstract

The invention discloses a method for preparing biphenyl through catalyzing the loop opening of dibenzofuran. According to the method, dibenzofuran is taken as a raw material, an adopted supported transition metal phosphide catalyst has good activity stability, and the stable operation time of a device is long, so that the frequent switching between the reaction and regeneration of a reactor can beavoided; the catalyst can be regenerated, so that the after-treatment of a large number of waste catalysts can be avoided, the environmental influence is low, the selectivity of produced biphenyl isover 70%, the yield of o-phenylphenol is about 12%, and the total yield of benzene and cyclohexane is below 10%.

Description

technical field [0001] The invention belongs to the field of synthesis of fine chemicals and relates to a method for preparing biphenyl by ring opening of dibenzofuran. Background technique [0002] Biphenyl (BP) is an important organic raw material, which is widely used in medicine, pesticides, dyes, liquid crystal materials and other fields. It can be used to synthesize plasticizers and preservatives, and can also be used to make fuels, engineering plastics and high-energy fuels. Biphenyl is present in coal tar, crude oil and natural gas. The preparation methods of biphenyl include chemical synthesis of biphenyl by benzene pyrolysis and separation and extraction of biphenyl by various coal tar fractions. The mass fraction of biphenyl in coal tar is 0.20%-0.40%. At present, coal tar extraction method and chemical synthesis method coexist. O-phenylphenol (OPP), as an important new type of fine chemical product and organic synthesis intermediate, is widely used in steriliz...

Claims

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Application Information

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IPC IPC(8): C07C1/20C07C1/247C07C15/14B01J27/185
CPCB01J27/185B01J27/1853C07C1/20C07C1/247C07C15/14Y02P20/10Y02P20/584
Inventor 斯爱玲
Owner 斯爱玲