Catalyst for preparing 3, 4-dichlorobenzonitrile and preparation method and application thereof

A technology of dichlorobenzonitrile and catalyst, applied in chemical instruments and methods, chemical elements of heterogeneous catalysts, catalysts for physical/chemical processes, etc., can solve problems such as short lifespan, long reaction route, and difficulty in industrialized production. , to achieve the effect of improving strength and wear resistance, improving activity and selectivity, and prolonging service life

Pending Publication Date: 2020-08-25
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional preparation methods of 3,4-dichlorobenzonitrile are generally prepared from corresponding aldehydes, aldoximes or acids as raw materials. These methods have high raw material prices, long reaction routes, and serious environmental pollution.
Martin et al. (NH 4 ) 2 [(VO) 3 (P 2 o 7 ) 2 ] prepare 3,4-dichlorobenzonitrile as ammoxidation catalyst, product yield is only 50%, is difficult to reach the requirement of industrialized production; In addition, this catalyst mechanical strength is not high, also can't be used in fluidized bed reactor ( Catalysis Letters, 1995, 33:349; Catalysis Today, 1996, 32:279)
Wuhan University once applied for a patent (CN1328875A) on a method for preparing 3,4-dichlorobenzonitr...

Method used

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  • Catalyst for preparing 3, 4-dichlorobenzonitrile and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Dissolve 10g of urea in 20mL of water and mix evenly with 80mL of 30% silica sol; 15.73g of H 2 C 2 o 4 2H 2 O was dissolved in 100 mL of 80°C distilled water, and 7.57 g of V was added 2 o 5 React until no gas is produced, then add 18.63 grams of HSb(OH) 6 , 5.75 grams of 85% H 3 PO 4 , 2.58 g H 3 BO 3 , 4.84 g Co(NO 3 ) 2 ·6H 2 O and 0.09 g Na 2 CO 3 , after forming a homogeneous solution, slowly add to the above-mentioned urea-dissolved silica sol mixed solution. 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: VSb 1 P 0.6 B 0.5 co 0.2 Na 0.02 o 7.46 ; The weight percentage of carbon nitride in the silica gel-carbon nitride composite carrier is about 20%. The average particle size of the catalyst is 53μm, the bulk density is 1.02g / ml,...

Embodiment 3～8

[0027] Catalyst formula is different, and reaction condition is with embodiment 1, and result is as follows:

[0028]

[0029] 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 3, 4-dichlorobenzonitrile. The carrier of the special catalyst is a silica gel-carbon nitride composite carrier formed by doping carbon nitridewith silica gel, and the composition of a loaded active component is shown as VSbbPcDdEeGgOx, wherein D is boron, lanthanum, cerium, samarium, europium, scandium, chromium, molybdenum, bismuth or tungsten, E is titanium, zirconium, manganese, iron, cobalt, nickel, copper, zinc or tin, and G is lithium, sodium, potassium, rubidium, cesium, beryllium, magnesium, calcium or barium. The invention also discloses a preparation method and application of the catalyst. In the composite carrier of the special catalyst prepared by the method, carbon nitride is used as Lewis base to perform Lewis acid-base reaction with an active component used as Lewis acid so that the action of the active component and the carrier is enhanced, the loss of the active component is reduced, the active component is dispersed more uniformly, and the strength and wear resistance of the catalyst are improved; the service life is prolonged; and the oxidation-reduction capability of the catalyst and the coordination capability with reactants can be adjusted by utilizing the carbon nitride so that the activity and the selectivity of the catalyst are improved.

Description

technical field [0001] The invention relates to a catalyst for preparing 3,4-dichlorobenzonitrile by using 3,4-dichlorotoluene as a raw material through ammoxidation reaction, 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] 3,4-dichlorobenzonitrile, also known as 3,4-dichlorobenzonitrile, is an important fine chemical and an intermediate in organic synthesis. With the continuous emergence of new pesticides and pharmaceuticals containing fluorine, the demand for fluorinated aromatic compounds has increased sharply. The fluorinated derivatives of 3,4-dichlorobenzonitrile, 3,4-difluorobenzonitrile, 4-fluoro- 3-chlorobenzonitrile, 3,4-difluorobenzoic acid, 4-fluoro-3-chlorobenzoic acid, etc., can be widely used in pesticides, medicines, pigments, dyes and other industries; such as 3,4-difluorobenzonitrile It is an important intermedia...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J27/198B01J27/199B01J35/10B01J35/02C07C253/28C07C255/50
CPCB01J27/24B01J27/198B01J27/199B01J23/002B01J35/0026B01J35/1014B01J35/023C07C253/28B01J2523/00B01J2523/12B01J2523/305B01J2523/51B01J2523/53B01J2523/55B01J2523/845B01J2523/11B01J2523/67B01J2523/22B01J2523/47B01J2523/68B01J2523/13B01J2523/3743B01J2523/842B01J2523/23C07C255/50Y02P20/584
Inventor 谢光勇郑浩丁爽董运召熊焰
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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