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Method for preparing chlorotoluene

A technology for p-chlorotoluene and toluene, which is applied in the field of toluene cyclic chlorination, can solve the problems of harsh process conditions, low ratio of p-chlorotoluene and o-chlorotoluene, etc., and achieves the effect of less dosage and high activity

Active Publication Date: 2013-05-15
江苏超跃化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problem that the ratio of p-chlorotoluene to o-chlorotoluene is low or the process conditions are harsh in the method for preparing p-chlorotoluene by toluene ring chlorination, the present invention provides a method with simple process conditions and the combination of p-chlorotoluene and o-chlorotoluene The method for the preparation of p-chlorotoluene with a higher ratio

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0017] Catalyst preparation: In a four-neck flask, add 150ml of ferric chloride aqueous solution with a concentration of 10%, add hydrochloric acid to adjust the pH to 3.5, start stirring, heat up to 60°C, add 75ml of 1nm D418 styrene-based cation exchange resin, heat at 60°C for 2 hours, then filter, rinse the solid with clean water twice and filter dry, the mother liquor can be applied mechanically. The dried solid is packed into a four-necked flask with a water separator, 150ml of toluene is added, heated and dehydrated, and the toluene is filtered to obtain a macroporous chelating resin catalyst.

Embodiment 2

[0019] Load 60 grams of catalyst in a fixed bed reactor with a cooling jacket, and toluene passes through the fixed bed reactor at a flow rate of 0.5 g / min under normal pressure, slowly open the chlorine valve, adjust the chlorine flow rate, and control the conversion rate of toluene 95%, toluene mixed with chlorine enters the reactor from the bottom, and the reaction liquid flows out from the top. The reaction temperature is controlled by adjusting the refrigerant flow rate to 10°C. After the reaction is stable, the content of each component in the product is sampled and analyzed by gas chromatography. The toluene content is 4.6%. p-chlorotoluene:o-chlorotoluene=1.8:1, the content of polychlorinated toluene is 0.87%, and the content of m-chlorotoluene is 0.16%.

Embodiment 3

[0021] Toluene is diluted with one-fold 1,2-dichloroethane; 60 grams of catalysts are loaded into a fixed-bed reactor with a cooling jacket, and toluene passes through the fixed-bed reactor at a flow rate of 0.5 g / min at 0.0 MPa. Slowly open the chlorine valve, adjust the flow rate of chlorine gas, and control the conversion rate of toluene to 95%. After mixing the toluene and chlorine gas, it enters the reactor from the bottom, and the reaction liquid flows out from the top. Control the reaction temperature to 25°C by adjusting the flow rate of the refrigerant. After the reaction is stable, take a sample. The content of each component in the product was analyzed by gas chromatography. The content of toluene was 3.7%, p-chlorotoluene:o-chlorotoluene=2.3:1, the content of polychlorinated toluene was 0.97%, and the content of m-chlorotoluene was 0.18%.

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Abstract

The invention relates to a method of toluene chlorination reaction and particularly relates to a method for preparing chlorotoluene through the toluene chlorination reaction. The method is characterized by adopting a made-to-order macroporous metal chelating resin as a catalyst; and the catalyst is chelated from an iron chloride water solution with the mass concentration of 10% and D418 styrene cation exchange resin with the particle size of 0.5-1.5 millimeters and the aperture of 0.6-1 nanometer at 60 DEG C under the conditions of stirring and ph of 3.5. Thus, electrophilic reaction during toluene chlorination is mainly carried out in a catalyst pore path; because chlorotoluene is smaller than o-chlorotoluene in molecular dimension and has higher diffusion velocity than o-chlorotoluene in a pore path with certain size, more para-position products are obtained; in addition, the method disclosed by the invention has low requirements on temperature and pressure; and the highest content ratio of chlorotoluene to o-chlorotoluene is 4.1:1 under the conditions of 10-80 DEG C and 0.05-0.1 MPa.

Description

technical field [0001] The invention relates to a method for ring chlorination of toluene, in particular to a method for preparing p-chlorotoluene through ring chlorination of toluene. Background technique [0002] Toluene reacts with chlorine gas in the liquid phase under the action of Lewis acid catalysts such as iron trichloride, antimony trichloride, aluminum trichloride, etc., and the mono-substituted aromatic ring product monochlorotoluene is the mixture of o-chlorotoluene and p-chlorotoluene. mixture. If ferric chloride is used as catalyst, the ratio of p-chlorotoluene to o-chlorotoluene in the monochlorotoluene mixture is about 0.5-0.55:1. [0003] Among the toluene ring chlorination products, p-chlorotoluene is an important intermediate in the production of fine chemical products such as pesticides, medicines, and dyes, while o-chlorotoluene has much smaller uses, and a large part of it is used as a low-priced solvent. [0004] For a long time, people have been tr...

Claims

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Application Information

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IPC IPC(8): C07C25/02C07C17/12
Inventor 殷云武任坚跃薛保安
Owner 江苏超跃化学有限公司
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