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Synthesis method for 4,4'-biphenyldicarbox ylic acid

A technology of biphenyl dicarboxylic acid and a synthesis method, which is applied in the field of synthesis of 4,4'-biphenyl dicarboxylic acid, can solve the problems of poor economy, large pollution, complicated process and the like, and achieves a low pollution, rich source and simple process. Effect

Pending Publication Date: 2019-01-11
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of this invention is to provide a kind of synthetic method of 4,4'-biphenyl dicarboxylic acid, in order to solve the problem that existing 4,4'-biphenyl dicarboxylic acid synthetic method process is loaded down with trivial details, pollution is big and economical is poor

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  • Synthesis method for 4,4'-biphenyldicarbox ylic acid
  • Synthesis method for 4,4'-biphenyldicarbox ylic acid
  • Synthesis method for 4,4'-biphenyldicarbox ylic acid

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Embodiment 1

[0028] Embodiment 1 of the present invention provides a synthesis method of 4,4'-biphenyl dicarboxylic acid, the reaction steps are as follows:

[0029] In a 250ml three-necked flask equipped with a spherical condenser and a thermometer, add 18.2g (0.10mol) 4,4'-dimethylbiphenyl, 100ml carbon tetrachloride, 81g (0.60mol) sulfuryl chloride and 0.09g ( 0.001mol) tert-butyl hydroperoxide, the above materials were magnetically stirred, and heated to 60°C for reaction, the reaction time was 4h, after the reaction was completed, cooled to room temperature, and nitrogen gas was introduced into the reactant to drive off the reaction. Hydrogen chloride, and the unreacted sulfonyl chloride was distilled off, cooled to room temperature after distilled off, and analyzed by liquid chromatography, the content of 4,4'-bis(trichloromethyl)biphenyl in the mixed solution was 91.7%;

[0030] Add the prepared 4,4'-bis(trichloromethyl)biphenyl mixture and 480g (0.6mol) sodium hydroxide aqueous sol...

Embodiment 2

[0032] Example 2 of the present invention provides a synthesis method of 4,4'-biphenyl dicarboxylic acid, the reaction steps are as follows:

[0033] In a 250ml three-necked flask equipped with a spherical condenser and a thermometer, add 18.2g (0.10mol) 4,4'-dimethylbiphenyl, 100ml carbon tetrachloride, 81g (0.60mol) sulfuryl chloride and 0.09g ( 0.001mol) tert-butyl hydroperoxide, the above materials were magnetically stirred, and heated to 60°C for reaction, the reaction time was 4h, after the reaction was completed, cooled to room temperature, and nitrogen gas was introduced into the reactant to drive off the reaction. hydrogen chloride, and distill under normal pressure to reclaim the unreacted sulfonyl chloride and solvent carbon tetrachloride until no fraction is distilled off, and then down to room temperature to obtain 37.5g 4,4'-bis(trichloromethyl)biphenyl, The liquid chromatography analysis content is 91.9%;

[0034] Add 38.0g of 4,4'-bis(trichloromethyl)biphenyl ...

Embodiment 3

[0036] Embodiment 3 of the present invention provides a synthesis method of 4,4'-biphenyl dicarboxylic acid, the reaction steps are as follows:

[0037] In a 250ml three-necked flask equipped with a spherical condenser and a thermometer, add 18.2g (0.10mol) of 4,4'-dimethylbiphenyl, 100ml of 1,2-dichlorobenzene, 105g (0.78mol) of sulfonyl chloride and 0.25 g (0.0015mol) azobisisobutyronitrile, stir the above materials magnetically, and heat them to 80°C for reaction. The reaction time is 6h. Produced hydrogen chloride, and distill off the unreacted sulfonyl chloride, cool down to room temperature after steaming, and analyze by liquid chromatography, the content of 4,4'-bis(trichloromethyl)biphenyl in the mixed solution is 94.5% ;

[0038] Add the prepared 4,4'-bis(trichloromethyl)biphenyl mixture and 360g (0.9mol) sodium hydroxide aqueous solution into a 1000ml three-necked flask equipped with a spherical condenser and a thermometer, wherein the sodium hydroxide The concentr...

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Abstract

The invention discloses a synthesis method for 4,4'-biphenyldicarbox ylic acid. The method comprises the following specific steps: performing radical chlorination on 4,4'-dimethyl biphenyl used as a raw material under the effect of light or an initiator so as to generate 4,4'-di(trichloromethyl)biphenyl; then performing hydrolysis reaction under an alkaline condition so as to obtain 4,4'-biphenyldicarbox ylic acid; and performing an aftertreatment process, thereby obtaining a finished product. The synthesis method for 4,4'-biphenyldicarbox ylic acid is rich in raw material sources, low in rawmaterial price, simple in synthesis process, high in product recovery rate, free from any purification, high in product yield and product purity, less in pollution, high in conversion rate, high in economical efficiency and suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to the technical field of fine organic synthesis, and more specifically to a method for synthesizing 4,4'-biphenyldicarboxylic acid. Background technique [0002] 4,4'-Biphenyl dicarboxylic acid is an important organic chemical raw material, not only can be used as an intermediate for the synthesis of medicine and polymer materials, but also an important unit for the synthesis of liquid crystal materials, flame retardant polyurethane and flame retardant polyester body. At present, the synthesis methods of 4,4'-biphenyldicarboxylic acid mainly include: 4,4'-dimethylbiphenyl oxidation method, biphenyl chloromethylation oxidation method, 4-iodobenzoic acid coupling method, etc., among which 4 ,The 4'-dimethylbiphenyl oxidation method has the disadvantages of high temperature and high pressure, many by-products, difficult separation and low conversion rate (56%). The synthesis of biphenyl chloromethylation oxidation method requires a...

Claims

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Application Information

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IPC IPC(8): C07C51/093C07C63/333
CPCC07C17/14C07C51/093C07C63/333C07C22/04
Inventor 成西涛南蓉白燕沈寒晰郑阿龙郭鹏涛
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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