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Method for catalyzing methylbenzene to compound orthochlorotoluene through supported molecular sieves

A technology for catalyzing toluene and o-chlorotoluene with molecular sieves, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc.

Inactive Publication Date: 2015-09-30
JIANGSU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the existing technology for preparing o-chlorotoluene, common Lewis acids are mainly used as catalysts, including SbCl3, FeCl3 , AlCl3, etc. Although Lewis acid catalysts have good catalytic activity, they are highly corrosive when used alone, require harsh equipment, and have many three wastes, which are not conducive to industrial production

Method used

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  • Method for catalyzing methylbenzene to compound orthochlorotoluene through supported molecular sieves
  • Method for catalyzing methylbenzene to compound orthochlorotoluene through supported molecular sieves
  • Method for catalyzing methylbenzene to compound orthochlorotoluene through supported molecular sieves

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of HZSM-5 molecular sieve

[0028] ① ZSM-5 molecular sieve preparation: 0.03 mol Al 2 (SO 4 ) 3 Added to the prepared 100 mL 1.5 mol / L H 2 S0 4 solution, stir to dissolve it completely, add 15 mL of ammonia water (mass fraction 25%) into 100 mL of distilled water, stir and mix evenly, slowly add this solution to the above Al 2 (SO 4 ) 3 / H 2 S0 4 In the solution, stir evenly to obtain solution A; add 150g of water glass (modulus 3.2) into 225 mL of distilled water, and stir evenly to obtain solution B; under stirring conditions, use a peristaltic pump to slowly add solution A to solution B reaction at 30 °C, after 2 h, put the mixture into a hydrothermal kettle, crystallize at 170 °C for 120 h, wash the prepared ZSM-5 molecular sieve with distilled water to neutrality, and dry it at 120 °C for 2 h, spare.

[0029] ② Preparation of HZSM-5 molecular sieve: 10 g of ZSM-5 molecular sieve and 100 mL NH 4 NO 3 (30wt%) solution was added to ...

Embodiment 2

[0037] Adopt the same method of embodiment 1 to prepare AlCl 3 Load HZSM-5 molecular sieve, toluene chlorination reaction step is the same as embodiment 1, changes AlCl 3The amount of loaded HZSM-5 molecular sieve is 0.05 g, 0.5 g, and 1.0 g, and the influence of catalyst amount on the toluene chlorination reaction process can be obtained, as shown in Table 2:

[0038] Table 2 Effect of catalyst dosage on toluene chlorination reaction

[0039]

[0040] Table 2 shows the effect of catalyst dosage on toluene chlorination reaction. As the amount of catalyst increased from 0.1% to 2.0%, the conversion rate of toluene increased from 62.5% to 100.0%; the ratio of o-chlorotoluene and p-chlorotoluene increased from 2.59 to 2.82, and then dropped to 2.60; as can be seen from Table 2 It is concluded that increasing the amount of catalyst is beneficial to increase the rate of toluene chlorination, but at the same time it will also lead to a decrease in the ratio of o-chlorotolue...

Embodiment 3

[0042] Adopt the same method of embodiment 1 to prepare AlCl 3 Loading HZSM-5 molecular sieve, the toluene chlorination reaction steps are the same as in Example 1, changing the reaction temperature to 50 °C and 80 °C, the influence of different reaction temperatures on the toluene chlorination process can be obtained, as shown in Table 3:

[0043] Table 3 Effect of different reaction temperatures on the chlorination of toluene

[0044] Reaction temperature / ℃ Toluene conversion / % o-Chlorotoluene / P-Chlorotoluene 50 86.4 2.59 65 98.2 2.82 80 100.0 2.50

[0045] Table 3 reflects the influence of reaction temperature on toluene chlorination reaction; as can be seen from Table 3, the conversion rate of toluene increases with the raising of reaction temperature. When the reaction temperature is 65 ℃, the ratio of o-chlorotoluene to p-chlorotoluene in the product is the highest, which is 2.82.

[0046] The results showed that high temperatu...

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Abstract

The invention relates to the preparation technical field of orthochlorotoluene, in particular to a method for catalyzing methylbenzene to compound orthochlorotoluene through aluminum chloride (AlCl3) supported HZSM-5 molecular sieves, which belongs to the technical field of methylbenzene directional chlorination. The method for catalyzing the methylbenzene to compound the orthochlorotoluene through the AlCl3 supported HZSM-5 molecular sieves uses the AlCl3 supported HZSM-5 molecular sieves as catalysts, uses Cl2 as chlorinating agents, and selectively chloridizes the methylbenzene by adopting a liquid phase chlorination process. The method for selectively chloridizing to prepare the orthochlorotoluene is simple in synthetic process, mild in reaction condition, excellent in catalytic activity of the used AlCl3 supported HZSM-5 molecular sieves, easy to separate from products, small in environment pollution and small in corrosivity, and has extremely high industrial application value.

Description

technical field [0001] The invention relates to the technical field of preparing o-chlorotoluene, in particular to a kind of AlCl 3 The invention relates to a method for catalyzing the synthesis of o-chlorotoluene from toluene by loading HZSM-5 molecular sieve, which belongs to the technical field of directional chlorination of toluene. Background technique [0002] O-chlorotoluene is an important fine chemical raw material, which is widely used in pesticides, medicines, dyes and paints. Using o-chlorotoluene as raw material, it can produce o-chlorobenzyl, o-chlorobenzaldehyde, o-chlorobenzoyl chloride, O-chlorobenzoic acid, cresol, dichlorotoluene, etc. are mainly used as raw materials for the production of fungicides and insecticides. [0003] In the existing technology for preparing o-chlorotoluene, common Lewis acids are mainly used as catalysts, including SbCl 3 , FeCl 3 , AlCl 3 etc. Although the Lewis acid catalyst has good catalytic activity, it is highly corrosi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C25/02C07C17/12B01J29/40
Inventor 朱晓燕殷恒波
Owner JIANGSU UNIV
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