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Catalyst for toluene chlorination and preparation method thereof

A catalyst and main catalyst technology, applied in the field of chemistry, can solve the problems of restricting industrial application, high production cost, destroying the lattice of zeolite molecular sieve and the like

Active Publication Date: 2012-10-17
常州新东化工发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When zeolite molecular sieve is used as catalyst for toluene chlorination, the selectivity of p-chlorotoluene is relatively high, the reaction conversion rate is also high, and the product is easy to separate, but the HCl generated in the reaction is easy to react with zeolite molecular sieve to destroy the crystal lattice of zeolite molecular sieve
Therefore, the regeneration and short service life of zeolite molecular sieves lead to high production costs and harsh technical conditions, which have become the key to restricting its industrial application.

Method used

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  • Catalyst for toluene chlorination and preparation method thereof
  • Catalyst for toluene chlorination and preparation method thereof
  • Catalyst for toluene chlorination and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1.8gNa 2 HPO 4 12H 2 O and 14.5gNa 2 MoO 4 2H 2 O was dissolved in 30 mL and 100 mL of distilled water respectively, and the two solutions were mixed and added into a 250 mL three-neck flask, heated to boiling, refluxed for 1 hour, stopped heating, and added 30% hydrochloric acid while stirring until the pH of the solution = 2.0, And continue to stir to room temperature, add 80mL ether to the reaction solution, shake fully, then add 30% hydrochloric acid and continue shaking until the solution is divided into three layers after standing, and the yellow oily substance in the lower layer is heteropolyacid ether compound. Take out the ether compound in the lower layer, blow off the ether, add 2 mL of distilled water, put it in a vacuum desiccator until the crystals are completely precipitated, filter and dry to obtain 12-molybdophosphoric acid (H 3 PMo 12 o 40 ) crystal 7.8g. The resulting 12-molybdophosphoric acid (H 3 PMo 12 o 40 ) is activated in a muffle fur...

Embodiment 2

[0030] 1.8gNa 2 HPO 4 12H 2 O and 20.0gNa 2 WO 4 2H 2O was dissolved in 30 mL and 100 mL of distilled water respectively, and the two solutions were mixed and added into a 250 mL three-neck flask, heated to boiling, refluxed for 1 hour, stopped heating, and added 30% hydrochloric acid while stirring until the pH of the solution = 2.0, And continue to stir to room temperature, add 80mL ether to the reaction liquid, shake fully, then add 30% hydrochloric acid and continue shaking until the solution is divided into three layers after standing, the lower white oily substance is heteropoly acid ether compound. Take out the ether compound in the lower layer, blow off the ether, add 2mL of distilled water, put it in a vacuum desiccator until the crystals are completely precipitated, filter and dry to obtain 12-tungstophosphoric acid (H 3 PW 12 o 40 ) crystal 12.9g. The resulting 12-tungstophosphoric acid (H 3 PW 12 o 40 ) is activated in a muffle furnace, the activation te...

Embodiment 3

[0036] 1.8gNa 2 HPO 4 12H 2 O and 13.3gNa 2 MoO 4 2H 2 O was dissolved in 30mL and 100mL of distilled water respectively, and the two solutions were mixed and added into a 250mL three-neck flask, heated to boiling, and refluxed for 1h; 1.65gNa 2 WO 4 2H 2 O was dissolved in 15mL of distilled water, and the solution was added to the above reaction solution under stirring conditions, heated to reflux for 6 hours, stop heating, add 30% hydrochloric acid to the solution pH = 2.0 while stirring, continue to stir to room temperature, add Add 80mL of diethyl ether to the reaction solution. After fully shaking, add 30% hydrochloric acid and continue shaking until the solution is divided into three layers after standing still. The yellow oily substance in the lower layer is heteropolyacid ether compound. Take out the ether compound in the lower layer, blow off the ether, add 2 mL of distilled water, put it in a vacuum desiccator until the crystals are completely precipitated, fi...

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Abstract

The invention provides a catalyst for toluene chlorination and a preparation method thereof. The catalyst comprises a main catalyst heteropoly acid compound B and a cocatalyst compound A, wherein the ratio of B to A is 2:1(mol / mol); the main catalyst heteropoly acid compound B is 12-molybdenum phosphate (H3PMo12O40), 12 tungstophosphoric acid (H3PW12O40), 11-molybdenum tungsten phosphoric acid (H3PMo11O40), 10-molybdenum tungsten phosphoric acid (H3PMo10W2O40) or 9- molybdenum tungsten phosphoric acid (H3PMo9W3O40); and the cocatalyst compound A is inorganic sulfur powder or diphenylsulfide. The invention also provides the preparation method of the catalyst used for toluene chlorination. The technical scheme of the invention has the advantages of improving the toluene conversion when toluene is chlorinated, and highly selective regulation of the isomer ration when toluene is chlorinated.

Description

technical field [0001] The invention belongs to the technical field of chemistry, and relates to a catalyst and a preparation method thereof, in particular to a catalyst for toluene chlorination and a preparation method thereof. Background technique [0002] Chlorination of toluene mainly produces three isomers of o-chlorotoluene, m-chlorotoluene and p-chlorotoluene, among which p-chlorotoluene is the most widely used. When chlorination is carried out with Lewis acid as a catalyst, there are more o-chlorotoluene in the chlorination products, accounting for 55% to 65%; less p-chlorotoluene, accounting for 35%-45%; m-chlorotoluene is less than 1%. The study found that choosing a suitable toluene chlorination catalyst can greatly increase the content of p-chlorotoluene in the chlorination products. Studies have shown that using or changing catalysts is the main way to adjust the isomer ratio. There are many industrialized or industrialized toluene chlorination catalytic metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18C07C17/12C07C25/06
Inventor 葛裕华俞志宏陶文平顾留杰王明亮苏向华沈丹丹
Owner 常州新东化工发展有限公司
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