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Special catalyst for preparing o-chlorobenzonitrile by ammoxidation method and preparation method and application of catalyst

A technology of ammoxidation and o-chlorobenzonitrile, which is applied in the field of organic chemistry and organic fine chemicals, can solve the problems of rapid catalyst deactivation, unsatisfactory activity and selectivity, achieve high activity and selectivity, and reduce catalyst The effect of loss of components and prolonging the service life

Active Publication Date: 2019-06-14
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the large steric hindrance of the ortho-chlorine and the passivation effect of electron-withdrawing in o-chlorotoluene, the activity and selectivity of the current industrial catalysts for the ammoxidation of o-chlorotoluene are still not ideal, the catalyst deactivates quickly, and the catalyst life needs to be further improved. extend

Method used

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  • Special catalyst for preparing o-chlorobenzonitrile by ammoxidation method and preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 28.62 g H 2 C 2 o 4 2H 2 O was dissolved in 100 mL of 80°C distilled water, and 8.61 g of V were added 2 o 5 and 2.84 g CrO 3 React until no gas is produced, then add 25.24 grams of Sm(NO 3 ) 3 .6H 2 O, 16.37 grams of 85% H 3 PO 4 , 1.47 g H 3 BO 3 and 0.32 g K 2 CO 3 After forming a uniform solution, slowly add 100 mL of 30% silica sol, and then add 5 g of aminohexyltrichlorosilane. After stirring evenly, the catalyst precursor was obtained by high-speed spray centrifugal drying, dried in a muffle furnace at 110° C., and then gradually raised to 550° C. for 6 hours. After natural cooling, set aside. The active composition of the catalyst is: VP 1.5 SM 0.6 Cr 0.3 B 0.25 K 0.05 .

[0024] 20g of the above-mentioned solid catalysts are filled in a quartz tube fixed-bed reactor with an internal diameter of 30mm, and the molar ratio of the reaction raw materials is: o-chlorotoluene:NH 3 :Air=1:3:20, the reaction temperature is 673±1K, and the catalyst ...

Embodiment 2～8

[0026] Catalyst formula is different, and reaction condition is with embodiment 1, and result is as follows:

[0027]

[0028] The catalyst of the present invention containing other co-catalysts can be prepared according to the above method, wherein the corresponding precursors can be oxides, salts, acids or bases of other co-catalyst components. During the preparation, the desired catalyst can be obtained by replacing the corresponding precursor substances in proportion with reference to the above-mentioned examples.

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Abstract

The invention discloses a special catalyst for preparing o-chlorobenzonitrile by an ammoxidation method. A carrier of the special catalyst is organic silicon modified silica gel, a main catalyst comprises three components of V, P and rare earth metal Re, and a cocatalyst comprises at least one of three components of D, E and G; the active component of the catalyst is represented by VPRe<c>D<d>E<e>G<g>O<x>; the rare earth metal Re is lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium or scandium; D is titanium, chromium, molybdenum, manganese, antimony or bismuth; E is boron, iron, cobalt, nickel, zinc or tin; and G is lithium, sodium, potassium, caesium, magnesium or calcium. The invention also discloses a preparation method and application of the catalyst. The rare earth metal is used for adjusting the acidity and alkalinity, the oxidation-reduction capacity and the coordinationcapacity with reactants of the catalyst, and improving the activity of the catalyst and the selectivity of products, and the service life of the industrial catalyst is prolonged by utilizing organic silicon to reinforce the action of an inorganic oxide and the carrier. The catalyst is simple in preparation method and good in thermal stability and mechanical strength.

Description

technical field [0001] The invention relates to a special catalyst for preparing o-chlorobenzonitrile by an ammoxidation method, a preparation method and an application. It belongs to the technical field of organic chemistry and also belongs to the technical field of organic fine chemicals. Background technique [0002] O-chlorobenzonitrile, also known as o-chlorobenzonitrile, is an important fine chemical and an intermediate in organic synthesis. Using o-chlorobenzonitrile as raw material, the corresponding o-chlorobenzoic acid, o-chlorobenzamide, o-chlorobenzylamine, o-chloroaniline, o-fluorobenzonitrile, o-fluorobenzoic acid, o-fluoroaniline, etc. can be prepared, widely Used in industries such as dyes, medicines, pesticides and spices. For example, 2-cyano-4-nitroaniline, an important intermediate of multi-purpose azo disperse dyes, can be produced through nitration and ammonolysis of o-chlorobenzonitrile; biphenyl compounds can be synthesized with halogenated benzene ...

Claims

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Application Information

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IPC IPC(8): B01J27/198C07C255/50C07C253/28
Inventor 谢光勇张倩黄业迎郑浩熊焰周新花
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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