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Synthetic method of m-dichlorobenzene

A synthesis method and technology of m-dichlorobenzene, which are applied in chemical instruments and methods, halogenated hydrocarbon preparation, chemical recovery and other directions, can solve problems such as low conversion rate and complicated separation, and achieve high conversion rate, low cost and long life. Effect

Inactive Publication Date: 2010-04-21
JIANGSU EQUALCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] ① Transposition under normal pressure in the presence of water can only be operated intermittently, and the product is a mixture of three isomers, ortho, meta, and para, with low conversion and complicated separation;

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 300 grams of o-dichlorobenzene into the reactor with a condenser on top, heat to 150°C, add 30 grams of aluminum trichloride, continue heating to and maintain a reflux state, and introduce a weak HCl gas flow (about 3 liters / hour) After transposition reaction for 1.5 hours, mixed dichlorobenzenes were obtained. Sample analysis showed that 55% of the meta-position, 20% of the para-position, and 25% of the ortho-position.

Embodiment 2

[0023] A rectifying column with a theoretical plate number of 70 is installed above the reactor, 200 grams of o-dichlorobenzene, 100 grams of aluminum trichloride, 50 grams of binding agent magnesium chloride are added, and a weak HCl airflow (about 3 liters / hour) is introduced, Raising the temperature to 170-180°C, until there is reflux at the top of the column, drop in o-dichlorobenzene at a speed of 50 grams per hour, and 50 grams per hour of product flows out from the top, wherein the middle dichlorobenzene is 90%, and p-dichlorobenzene is 90%. 10%, no o-dichlorobenzene. When the top reflux flow drops significantly (<30 g / h), it indicates that the catalyst is invalid, and about 7000 g of m-dichlorobenzene can be obtained.

Embodiment 3

[0024] Embodiment 3: a rectifying column with a theoretical plate number of 70 is installed above the reactor, 200 grams of p-dichlorobenzene and 100 grams of titanium trichloride are added, and a weak HCl airflow (about 3 liters / hour) is introduced, and the temperature is raised to 160-175°C, until there is reflux at the top of the column, drop in p-dichlorobenzene at a rate of 50 g / h, and 50 g / h of product flows out from the top, of which m-dichlorobenzene is 75% and p-dichlorobenzene is 25% , no o-dichlorobenzene. When the top reflux flow drops significantly (<30 g / h), it indicates that the catalyst is invalid, and about 6000 g of m-dichlorobenzene can be obtained.

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PUM

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Abstract

The invention discloses a synthetic method of m-dichlorobenzene which is obtained by transposition in the presence of a catalyst by taking o-dichlorobenzene and / or p-dichlorobenzene as raw materials. The catalyst is a composite catalyst comprising a solid phase catalyst and a gas phase catalyst, wherein the solid phase catalyst is aluminum trichloride or halide of transition metal, and the gas phase catalyst is anhydrous hydrogen chloride or other anhydrous halogen acids. The raw materials have no limitation of water, have arbitrary ortho-para proportion and react under normal pressure; the solid catalyst has long service life, and the gas catalyst can be recycled after gas-liquid separation and has high conversion ratio; and the synthetic method can be used for large-scale industrial production. The process realizes the automatic control easily and has energy saving, safety, environment protection and low cost.

Description

Technical field: [0001] The invention relates to a synthesis method of m-dichlorobenzene. Background technique: [0002] m-dichlorobenzene is a basic organic chemical raw material. As one of the important raw materials for pesticides, pharmaceuticals and dye intermediates, its market prospect is quite broad. [0003] Since chlorine is an ortho- and para-positioning group, usually the chlorination of benzene to dichlorobenzene is a mixture of three isomers, o-, p-, and meta-isomers, which also contains a small amount of trichlorobenzene. In the mixed solution, due to the difference in the types of catalysts used, the ratio of the ortho-position and the para-position can be adjusted, but the ratio of m-dichlorobenzene is about 3%. Among the three isomers, m-dichlorobenzene is relatively more valuable because it is difficult to obtain and has a wide range of uses. In order to ensure accurate positioning, m-nitrochlorobenzene or m-dinitrobenzene is usually thermally chlorinate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C25/08C07C17/358
CPCY02P20/584
Inventor 毕亚铃阮文林易江华陈燚毛晓宇
Owner JIANGSU EQUALCHEM
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