Special catalyst for preparing 2, 6-dichlorobenzonitrile by ammonia oxidation method and preparation method and application of special catalyst

A technology of ammoxidation and dichlorobenzonitrile, which is applied in the field of organic chemistry and organic fine chemicals, can solve the problem of high catalyst strength, long life, high load, high activity and high selectivity, product yield and Low reaction selectivity, low mechanical strength of the catalyst, etc., to achieve good application value, good thermal stability and mechanical strength, and low cost

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

AI Technical Summary

Problems solved by technology

[0005] There are more than ten kinds of preparation methods for 2,6-dichlorobenzonitrile, generally using corresponding aldehydes, aldoximes or acids as raw materials. These methods have high raw material prices, long reaction routes, low product yields and low reaction selectivity. serious environmental pollution
Most of the measures in the above patents complicate the production process and increase the investment; or cause equipment corrosion and low product purity.
Martin et al prepared 2,6-dichlorobenzonitrile with the unloaded VPO composite oxide prepared by sol-gel method as ammoxidation catalyst, the product yield is low, and it is difficult to reach the requirements of industrial production; in addition, the catalyst mechanism Not strong enough to be used in fluidized bed reactors (Journal of Catalysis, 2006, 240:8-17; Catalysis Today, 2009, 142: 158-164)
In Chinese patent CN1055028C, V is prepared by silica gel impregnation method. a Ti b P c Cr d o x The four-component silica gel-supported catalyst catalyzes the ammoxidation of 2,6-dichlorotoluene to prepare 2,6-dichlorobenzonitrile, and the yield can reach 85%. However, the silica gel-supported catalyst generally has a short service life in industry.
The catalysts used in these patents are still difficult to meet the industrial requirements for high catalyst strength, long life, high load, high activity and high selectivity

Method used

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  • Special catalyst for preparing 2, 6-dichlorobenzonitrile by ammonia oxidation method and preparation method and application of special catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Dissolve 4g of melamine in 10mL of hot water and mix evenly with 90mL of 30% silica sol; mix 18.30g of H 2 C 2 o 4 2H 2 Dissolve O in 100 mL of 80°C distilled water, add 8.80 g of V 2 o 5 React to produce without gas, then add 20.48 grams (NH 4 ) 6 Mo 7 o 24 4H 2 O, 3.60 g H 3 BO 3 , 8.44 g Co(NO 3 ) 2 ·6H 2 O and 0.36 g Li 2 CO 3 , after the formation of a uniform solution, slowly add the above-mentioned melamine-dissolved silica sol mixture. After stirring evenly, it was concentrated to a solid content of 35%, and then the catalyst precursor was obtained by high-speed spray centrifugal drying, dried in a muffle furnace at 110°C, and then gradually heated to 500°C, and kept for 8 hours. After natural cooling, set aside. The active composition of the catalyst is: VMo 1.2 B 0.6 co 0.3 Li 0.1 o 7.35 The active component content is 50%, and the weight percentage of carbon nitride in the silica gel-carbon nitride composite carrier is about 10%. The av...

Embodiment 3～7

[0028] Catalyst formula is different, and reaction condition is with embodiment 1, and result is as follows:

[0029]

[0030] It is well known to those skilled in the art that the catalyst of the present invention containing other cocatalysts can also be prepared according to the above method. During preparation, the desired catalyst can be obtained by replacing the corresponding precursor substances of other cocatalyst components in proportion with reference to the above examples. The corresponding precursors of other cocatalyst components can be their oxides, salts, acids or bases and the like.

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Abstract

The invention discloses a special catalyst for preparing 2, 6-dichlorobenzonitrile by an ammonia oxidation method. The special catalyst is a multi-component inorganic composite oxide loaded by a silica gel-carbon nitride composite carrier, and the composition of the active component of the catalyst is shown as VMobBcCodDeOx, wherein D is lithium, sodium, potassium, rubidium, cesium, magnesium, calcium or barium. The invention also discloses a preparation method and application of the catalyst. Organic matters containing nitrogen and carbon and silica sol are respectively added as precursors ofcarbon nitride and silica gel for mixed calcination to form the silica gel-carbon nitride composite carrier. compared with a common silica gel carrier, the silica gel-carbon nitride composite carrierhas the advantages that the effects of the inorganic oxide and the carrier are enhanced, the strength and the wear resistance of the catalyst are improved, the inorganic oxide is dispersed more uniformly, the loss of catalyst components is reduced, and the service life of the catalyst is prolonged; meanwhile, the carbon nitride can also adjust the acid-base property, oxidation-reduction capability and coordination capability with reactants of the catalyst so that the activity and the selectivity of the catalyst are improved. 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 2,6-dichlorobenzonitrile by an ammoxidation method, a preparation method and application thereof. It belongs to the technical field of organic chemistry and also belongs to the technical field of organic fine chemicals. Background technique [0002] 2,6-dichlorobenzonitrile is also known as 2,6-dichlorobenzonitrile. As a high value-added fine chemical, chlorobenzonitrile is a key raw material for the manufacture of some high-efficiency and low-toxicity pesticides, new medicines, high-performance materials, dyes, etc., and is widely used in various fields of the national economy. [0003] 2,6-Dichlorobenzonitrile (2,6-DCBN) is mainly an essential intermediate of ultra-efficient, pollution-free, and low-residue "benzoylurea" pesticides. At present, the use, sale and production of low-efficiency and high-toxic pesticides have been banned by law in my country, so there is an urgent need for a larg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J23/887B01J35/02B01J35/10C07C253/28C07C255/50
CPCB01J27/24B01J23/8877B01J23/002B01J35/0026B01J35/023B01J35/1014C07C253/28B01J2523/00C07C255/50B01J2523/13B01J2523/305B01J2523/55B01J2523/68B01J2523/845B01J2523/15B01J2523/23B01J2523/12
Inventor 谢光勇丁爽郑浩董运召熊焰
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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