A kind of method that loaded molecular sieve catalyzes toluene to synthesize o-chlorotoluene

A molecular sieve technology for catalyzing toluene and o-chlorotoluene, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as unfavorable industrialization, harsh equipment requirements, strong corrosiveness, etc., and achieve easy product separation. , mild reaction conditions, high catalytic activity

Inactive Publication Date: 2017-09-05
JIANGSU UNIV
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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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  • A kind of method that loaded molecular sieve catalyzes toluene to synthesize o-chlorotoluene
  • A kind of method that loaded molecular sieve catalyzes toluene to synthesize o-chlorotoluene
  • A kind of method that loaded molecular sieve catalyzes toluene to synthesize o-chlorotoluene

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Experimental program
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Effect test

Embodiment 1

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

[0028] ① Preparation of ZSM-5 molecular sieve: 0.03 mol Al 2 (SO 4 ) 3 Added to the prepared 100 mL 1.5 mol / LH 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 a 250 ...

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 3 The 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-chlorotoluene to...

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 temperature wa...

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Abstract

The invention relates to the technical field of preparation of o-chlorotoluene, in particular to a method for catalyzing toluene to synthesize o-chlorotoluene with an AlCl3 loaded HZSM‑5 molecular sieve, and belongs to the technical field of toluene directional chlorination. The method adopts AlCl3 loaded HZSM-5 molecular sieve as a catalyst, Cl2 as a chlorination agent, and adopts a liquid phase chlorination method to carry out selective chlorination of toluene. The selective chlorination of toluene to produce ortho-chlorotoluene has simple synthesis process and mild reaction conditions, and the AlCl3-loaded HZSM-5 molecular sieve used has good catalytic activity, is easy to separate from the product, has little environmental pollution, and has low equipment corrosion. 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 Patents(China)
IPC IPC(8): C07C25/02C07C17/12B01J29/40
Inventor 朱晓燕殷恒波
Owner JIANGSU UNIV
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