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P-phenyl cyanophenyl synthesis method

A technology of p-phenylbenzonitrile and a synthesis method, which is applied in the directions of dehydration preparation of carboxylic acid amides, chemical recovery, organic chemistry, etc., can solve the problems of difficult separation of products and catalysts, harm to the production environment, and difficulty in continuous production, and achieves product yield. The effect of high rate, easy extraction and short production cycle

Inactive Publication Date: 2015-04-08
HUBEI DONGAO CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the acid catalysts used in these chemical production processes are mainly liquid acids. Although the technology is very mature, it has brought harm to the environment during production. At the same time, there are inevitable and insurmountable problems of homogeneous catalysis itself. Disadvantages, such as corrosive equipment, difficult continuous production, poor selectivity, difficult separation of product and catalyst, etc.

Method used

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  • P-phenyl cyanophenyl synthesis method
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Examples

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Embodiment 1

[0018] A 2000-liter enamel reaction kettle with a stirring device, a thermometer, a condenser, and an external jacket cooling and heating device. First check whether the equipment is in good condition and whether the system is dry. The reaction is carried out under water-absent conditions. Add 500 liters of chlorobenzene to the reactor, 60 kilograms of biphenyls, SO 4 2- / ZrO 2 9 kg, start stirring, dissolve for 1 hour, cool the external cooling water to 20°C, add 90 kg of chloroacetyl chloride within 2 hours, stir and react for 2 hours, sample is diluted with methanol and then analyzed by liquid chromatography, when the content of dibenzoyl chloride ≥96%, when the biphenyl content is less than 2%, stop stirring, let it stand for 2 hours to separate and remove the solid catalyst at the bottom, return the acid chloride solution to the reactor, feed liquid ammonia under stirring, and cool the water bath outside, the reaction temperature is less than 15°C, pass The ammonia time...

Embodiment 2

[0020] A 2000-liter enamel reaction kettle with a stirring device, a thermometer, a condenser, and an external jacket cooling and heating device. First check whether the equipment is in good condition and whether the system is dry. The reaction is carried out under water-absent conditions. Add 500 liters of chloroform to the reactor, 100 kilograms of biphenyl, SO 4 2- / ZrO 2 35 kg, start stirring, dissolve for 1 hour, cool the external cooling water to 20°C, add 90 kg of chloroacetyl chloride within 2 hours, stir and react for 5 hours, sample is diluted with methanol and then analyzed by liquid chromatography, when the content of dibenzoyl chloride ≥96%, when the biphenyl content is less than 2%, stop stirring, stand still for 2 hours to separate and remove the solid catalyst at the bottom, return the acyl chloride solution to the reactor, feed liquid ammonia under stirring, and cool the water bath outside, the reaction temperature is less than 15°C, pass ammonia The time is...

Embodiment 3

[0022] A 2000-liter enamel reaction kettle with a stirring device, a thermometer, a condenser, and an external jacket cooling and heating device. First check whether the equipment is in good condition and whether the system is dry. The reaction is carried out under water-absent conditions. Add 500 liters of nitrobenzene to the reactor, 150 kilograms of biphenyls, SO 4 2- / TiO 2 70 kg, start stirring, dissolve for 1 hour, cool the outer cooling water to 20°C, add 90 kg of chloroacetyl chloride within 2 hours, stir and react for 10 hours, sample is diluted with methanol and then analyzed by liquid chromatography. When the content of bibenzoyl chloride ≥96%, when the biphenyl content is less than 2%, stop stirring, stand still for 2 hours to separate and remove the solid catalyst at the bottom, return the acyl chloride solution to the reactor, feed liquid ammonia under stirring, and cool the water bath outside, the reaction temperature is less than 15°C, pass ammonia The time i...

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Abstract

A p-phenyl cyanophenyl synthesis method includes: firstly, feeding biphenyl, solvent and ultrastrong solid acid catalyst into a reaction kettle; secondly, stirring for 2-5h at 0-50 DEG C prior to adding acylating agent, filtering the ultrastrong solid acid catalyst after acyl chlorination reaction for 2-10 hours, then feeding liquid ammonia into the reaction kettle for 5-10 hours at the temperature of 0-50 DEG C for ammoniation, adding thionyl chloride into the reaction kettle for cyanation for 6-10 hours at 50-150 DEG C after ammoniation ends; and distilling off the solvent by pressure reduction of a product obtained by the reaction in the second step, and then obtaining p-phenyl cyanophenyl by means of reduced pressure distillation. The p-phenyl cyanophenyl synthesis method is simple in operation, product extraction is easy after reaction ends, the catalyst is reusable, cost is saved, production cycle is short, environmental pollution is avoided as emission of three wastes is avoided, use ratio of equipment is high, product yield is high, and product quality is good.

Description

technical field [0001] The invention belongs to the field of synthetic methods of organic intermediates, and in particular relates to a method for synthesizing p-phenylbenzonitrile. Background technique [0002] Acid-catalyzed reactions involve petroleum refining processes such as hydrocarbon cracking, reforming, and isomerization, as well as petrochemical and fine chemical processes such as olefin hydration, olefin polymerization, aromatic hydrocarbon alkylation, aromatic hydrocarbon acylation, and alkyd esterification. It can be said that acid catalyst is the basis of this series of solid superacids important industry. At present, the acid catalysts used in these chemical production processes are mainly liquid acids. Although the technology is very mature, it has brought harm to the environment during production. At the same time, there are inevitable and insurmountable problems of homogeneous catalysis itself. Disadvantages, such as corrosive equipment, difficulty in con...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/50C07C253/20
CPCY02P20/584
Inventor 林东翰高艳波
Owner HUBEI DONGAO CHEM TECH