Method for preparing cyanobenzene by ammonifying benzoic acid gaseous phase

A technology of benzoic acid and benzonitrile, which is applied in the fields of ammonia-carboxylic acid reaction preparation, organic chemistry, etc., can solve the problems of high requirements for condition control, complicated three-waste treatment technology, and complicated technological process.

Active Publication Date: 2014-06-18
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are factories in China that have developed related processes, but the process flow is relatively complicated, the requirements for condition control are high, and the three wastes treatment technology is complicated

Method used

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  • Method for preparing cyanobenzene by ammonifying benzoic acid gaseous phase

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Embodiment 1

[0018] The catalyst was filled in a tubular fixed-bed reactor, and hydrogen was continuously fed into the fixed-bed reactor at 300° C. to activate the catalyst for 2 hours. Nitrogen is used as the carrier gas to pass into the preheater. When nitrogen flows through the vaporization chamber, it is mixed with vaporized benzoic acid and ammonia to form a mixed gas of benzoic acid-ammonia-nitrogen. The molar ratio of each substance in the mixed gas is benzoic acid : ammonia: nitrogen = 1:1:5; benzoic acid-ammonia-nitrogen mixed gas reacts at 400°C when it passes through the catalyst bed, and the crude product obtained by the reaction is liquefied in the condenser, and the cooling medium in the condenser is water , The crude product can be rectified after separating the water phase, and the benzonitrile content in the crude product is 85wt%. The unliquefied gas can be back-pressurized by the compressor to the gas tank for recycling. The present invention prepares the technological ...

Embodiment 2

[0021] The catalyst is filled in a tubular fixed-bed reactor, and hydrogen is continuously fed into the fixed-bed reactor at 320°C to activate the catalyst for 2 hours; hydrogen and nitrogen are mixed and passed into the preheater as a carrier gas, in which hydrogen and nitrogen The molar ratio of the hydrogen-nitrogen mixture is 1:1; when the hydrogen-nitrogen mixed gas flows through the vaporization chamber, it is mixed with the vaporized benzoic acid and urea to form a mixed gas of benzoic acid-urea-hydrogen-nitrogen, and the molar ratio of each substance in the mixed gas is benzene Formic acid: urea: hydrogen: nitrogen = 1:2:20:20; when the mixed gas of benzoic acid-urea-hydrogen-nitrogen passes through the catalyst bed, the reaction occurs at 350°C, and the crude product obtained by the reaction is liquefied in the condenser and then The cooling medium is glycerin, and the crude product can be rectified after separating the water phase. The benzonitrile content in the cru...

Embodiment 3

[0024] Fill phosphoric acid-diatomaceous earth in a tubular fixed reactor as a catalyst, and continuously pass hydrogen gas into the fixed-bed reactor at 250°C to activate phosphoric acid-diatomite for 2 hours; use water vapor as carrier gas to preheat When water vapor flows through the vaporization chamber, it is mixed with vaporized benzoic acid and ammonium bicarbonate to form a mixed gas of benzoic acid-ammonia-steam, and the molar ratio of each substance in the mixed gas is benzoic acid: ammonium bicarbonate: water Steam=1:5:30; benzoic acid-ammonia-steam mixed gas reacts at 250°C when it passes through the catalyst bed, and the crude product obtained from the reaction is liquefied in the condenser, and the cooling medium in the condenser is heat transfer oil , The crude product can be rectified after separating the water phase, and the content of benzonitrile in the crude product is 80 wt%. Unliquefied gas can be vented.

[0025]

[0026] The ammoniating agent ammonia,...

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Abstract

The invention discloses a method for preparing cyanobenzene by ammonifying benzoic acid gaseous phase. The method comprises the following steps: mixing gaseous benzoic acid and an ammonifying agent and carrier gas, and performing catalysis through a catalyst fixed bed, wherein the mol ratio of the benzoic acid to the ammonifying agent to the carrier gas is 1: (1-5): (5-40); the adopted carrier gas can be reaction raw material gas or inert gas, a condenser is arranged behind the reactor, the crude product is condensed to separate out the water phase, and then the rectifying and purifying are performed. The reaction flow is simple, the cyanobenzene is prepared by ammonifying the benzoic acid gaseous phase, the three wastes are prevented, and the economic benefit and the environment benefit are obvious.

Description

[0001] technical field [0002] The invention belongs to the field of organic chemical industry, in particular to a method for preparing benzonitrile by gas-phase ammoniation of benzoic acid. Background technique [0003] Benzonitrile is an important organic intermediate, which is widely used in the synthesis of benzylamine and benzomelamine, etc. It can also be used in solvents, antioxidants and non-ionic surfactants, used in benzyl rubber, resins, coatings and Polymer Synthesis. [0004] Benzonitrile is mainly produced industrially by the ammoxidation of toluene. At 380°C, the ratio of raw materials is toluene: ammonia: oxygen = 1:4.7:3, and the space velocity is 800h -1 , under the action of vanadium series catalyst, the yield of benzonitrile can reach 85%. At present, there are factories in China that have developed related processes, but the process flow is relatively complicated, the requirements for condition control are high, and the three wastes treatment technol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/50C07C253/22
Inventor 郭泽军于萍罗运柏
Owner WUHAN UNIV
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