Production process for preparing chlorobenzonitrile through ammoxidation

A technology of o-chlorobenzonitrile and ammoxidation method, applied in the chemical industry, can solve the problems of little economic significance and high price of o-chlorobenzoic acid, achieve the effects of suppressing side reactions, improving production technology, and high selectivity

Inactive Publication Date: 2013-05-15
HUBEI JUNTAI PHARMA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Among the above-mentioned methods, the third and fourth methods are the simplest (one-step synthesis), but the price of raw material o-chlorobenzoic acid used in the synthetic method of o-chlorobenzoic acid is high, so the economic significance of synthesis by this method is not large

Method used

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  • Production process for preparing chlorobenzonitrile through ammoxidation
  • Production process for preparing chlorobenzonitrile through ammoxidation
  • Production process for preparing chlorobenzonitrile through ammoxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] First, the activated catalyst VP 0.7 Ce 0.3 Sb 0.5 o 6.1 Fill to In the ebullated bed reactor, the height of the static bed is 2m (about 1.5t of activated catalyst is required), and the heated air (450~480°C) is passed through, and the ammonia is passed through 8m after heating and boiling to 400°C. 3 / h. Continue to pass hot air (350°C) for 3 hours, rise to 500°C, keep warm and activate for 8 hours. Cool down to 370°C, feed ammonia 4m 3 / h, air 200m 3 / h, o-chlorotoluene 56kg / h, water vapor 10m 3 / h, adjust the cooling water to control the reaction temperature at 370~380°C. After the reaction is completed, the crude product with o-chlorobenzonitrile content greater than 99.5% can be collected, and the yield is as high as 94%. The catalyst has not changed after continuous operation for more than one year (no deactivation, no carbon absorption).

Embodiment 2

[0054] First, the activated catalyst VP 2 CaO 12 Fill to In the ebullated bed reactor, the height of the static bed is 2m (about 1.5t of activated catalyst is required), and the heated air (450~480°C) is passed through, and the ammonia is passed through 8m after heating and boiling to 400°C. 3 / h. Continue to pass hot air (350°C) for 3 hours, rise to 500°C, keep warm and activate for 8 hours. Cool down to 370°C, feed ammonia 4m 3 / h, air 200m 3 / h, o-chlorotoluene 56kg / h, water vapor 10m 3 / h, adjust the cooling water to control the reaction temperature at 370~380°C. After the reaction is completed, the crude product with o-chlorobenzonitrile content greater than 99.5% can be collected, and the yield is as high as 92%. The catalyst has been continuously operated for more than one year without change (no deactivation, no carbon absorption).

Embodiment 3

[0056] First, the activated catalyst VPCeSb 0.5 o 8 Fill to In the ebullated bed reactor, the height of the static bed is 2m (about 1.5t of activated catalyst is required), and the heated air (450~480°C) is passed through, and the ammonia is passed through 8m after heating and boiling to 400°C. 3 / h. Continue to pass hot air (350°C) for 3 hours, rise to 500°C, keep warm and activate for 8 hours. Cool down to 370°C, feed ammonia 4m 3 / h, air 200m 3 / h, o-chlorotoluene 56kg / h, water vapor 10m 3 / h, adjust the cooling water to control the reaction temperature at 370~380°C. After the reaction is completed, the crude product with o-chlorobenzonitrile content greater than 99.5% can be collected, and the yield is as high as 93%. The catalyst has been continuously operated for more than one year without change (no deactivation, no carbon absorption).

[0057]In the preparation process of the above-mentioned examples, the waste water from the process of ammoxidation of o-chloro...

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Abstract

The invention provides a production process for preparing chlorobenzonitrile through ammoxidation. The production process comprises the following steps of: portioning air, ammonia, water vapor and o-chlorotoluene together; gasifying the o-chlorotoluene and then mixing the gasified o-chlorotoluene with air, ammonia and water vapor, and conveying the mixture to a fluidized bed reactor for reaction under the action of a catalyst; and after the reaction, cooling and crystallizing the generated product through a cold trap, thereby obtaining crude chlorobenzonitrile, wherein the catalyst is VaPbCecSbdOx multi-component catalyst, and wherein a=1, b=0.7-2, c=0.3-1, d=0.5-1, and the value of x is determined according to valence state balance when V, P, Ce and Sb are +5 valent, +5 valent, +4 valent, +5 valent and -2 valent, respectively. The production process provided by the invention employs the VaPbCecSbdOx as the active catalyst; and the catalyst is simple to fabricate, mild in reaction temperature, long in catalyst service life, high in activity, high in selectivity and the like; as a result, side reaction in the production process is suppressed, the production process of chlorobenzonitrile is improved and the yield of product is obviously improved.

Description

【Technical field】 [0001] The invention relates to the technical field of chemical industry, in particular to a production process for preparing o-chlorobenzonitrile by an ammoxidation method. 【Background technique】 [0002] O-chlorobenzonitrile is an important organic intermediate, which belongs to the field of chemical and pharmaceutical intermediates, and is the source of related technical fields such as medicine. In recent years, the rapid development of medicine and other related fields has promoted the development of chemical raw materials and intermediates, and in turn, the development of chemical raw materials and intermediates has promoted or restricted the development of medicine and other related fields. O-chlorobenzonitrile (OCBN) is a white needle-like crystal with a melting point of 42°C and is easy to sublimate. OCBN molecules contain carbon-nitrogen triple bonds, which are much more active than amide compounds, and can undergo many reactions such as hydrolysi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/50C07C253/28B01J27/198
Inventor 陈川
Owner HUBEI JUNTAI PHARMA CHEM
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