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Method for producing high-purity o-chlorotoluene by adsorption separation method

An o-chlorotoluene, adsorption separation technology, applied in chemical instruments and methods, organic chemistry, halogenated hydrocarbon preparation, etc., can solve problems such as the inability to obtain high-purity o-chlorotoluene, affecting downstream high-end pharmaceutical applications and development, etc., to avoid The recycling steps and processes are simplified and easy to implement, and the effect of reducing the processing cost

Pending Publication Date: 2022-05-06
常州新东化工发展有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

o / p-chlorotoluene mainly through toluene and Cl 2 Under the action of Fe catalyst, it is obtained by chlorination on the toluene ring, and then o / p-chlorotoluene is separated by rectification to obtain o / p-chlorotoluene products. It is calculated that even if a rectification separation tower with more than 100 theoretical plates is used, high-purity (≥99.95%) o-chlorotoluene cannot be obtained, so it directly affects the application and development of downstream high-end medicine and fine chemicals

Method used

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  • Method for producing high-purity o-chlorotoluene by adsorption separation method
  • Method for producing high-purity o-chlorotoluene by adsorption separation method
  • Method for producing high-purity o-chlorotoluene by adsorption separation method

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Experimental program
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Effect test

Embodiment 1

[0045] Take 50 g of o-chlorotoluene solutions of different production batches, add different kinds of adsorbents, filter after stirring for a certain period of time, analyze the mass fraction of o-chlorotoluene in the filtrate, and compare the adsorption effects of different adsorbents. The results are shown in Table 2.

[0046] Table 2 Adsorption effect of different adsorbents

[0047]

Embodiment 2

[0049] Take 50 g of o-chlorotoluene with production batch number 20210321 and put it into a 250 mL three-necked flask, add 5 g of IM-5 molecular sieve, stir for 30 minutes and then filter to obtain o-chlorotoluene solution. IM-5 adsorbent uses 30 g of toluene as a desorbent to desorb it Washing, the adsorbent IM-5 obtained after washing remains in the three-necked flask, put the three-necked flask into a bowl-shaped electric furnace, feed 0.83L / min nitrogen, control the temperature of the electric furnace to 180°C, and regenerate at this temperature for 3h Then, cool to room temperature. After cooling down to room temperature, the adsorbent is used again, and the cycle is applied in this way, and the result is as follows: figure 1 As shown, the adsorption regeneration of the adsorbent is recycled 50 times, and the mass fraction of o-chlorotoluene is above 99.95%.

Embodiment 3

[0051] Take 50 g of o-chlorotoluene with the production batch number of 20210915 and add it to a 250 mL three-neck flask, add 6.25 g of ZSM-5 molecular sieve, stir for 30 minutes, and then filter to obtain an o-chlorotoluene solution. ZSM-5 adsorbent uses 35 g of toluene as a desorbent to desorb it. After washing, the adsorbent ZSM-5 obtained after washing remains in the three-necked flask. Put the three-necked flask into a bowl-shaped electric furnace, feed 0.11L / min nitrogen, control the temperature of the electric furnace to 180°C, and regenerate at this temperature After 4h, cool to room temperature. After cooling down to room temperature, the adsorbent is used again, and the cycle is applied in this way, and the result is as follows: figure 2 As shown, the adsorption regeneration of the adsorbent is recycled 50 times, and the mass fraction of o-chlorotoluene is above 99.95%.

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Abstract

The invention relates to a method for producing high-purity o-chlorotoluene by an adsorption separation method, and belongs to the technical field of chemical raw material preparation. According to the method for selectively adsorbing the parachlorotoluene contained in the o-chlorotoluene to produce the high-purity o-chlorotoluene, the mass fraction of the parachlorotoluene in the o-chlorotoluene can be reduced to 0.05 wt% or below, after adsorption saturation of the adsorbent, the adsorbent can be recycled through toluene washing, filtering and normal-pressure drying, and the method is suitable for industrial production. The used adsorbent can be recycled for more than 50 times, the regenerant toluene is a raw material for producing ortho / parachlorotoluene, and ortho / parachlorotoluene-containing liquid washed by toluene can be continuously used as a reaction raw material, so that a new regenerant does not need to be purchased, meanwhile, the recycling procedure of the regenerant is omitted, the process route is simplified, and the treatment cost is reduced; the method has the advantages that the operation is simple, the purity of the produced o-chlorotoluene is high, the energy consumption is low, and the like.

Description

technical field [0001] The invention relates to a method for producing high-purity o-chlorotoluene by an adsorption separation method, and belongs to the technical field of chemical raw material preparation. Background technique [0002] At present, there are three isomers of chlorotoluene, namely o-chlorotoluene, m-chlorotoluene and p-chlorotoluene. Among them, o-chlorotoluene is a methyl-substituted halogenated benzene, which is used as an intermediate in the pesticide, pharmaceutical and dye industries. o / p-chlorotoluene mainly through toluene and Cl 2 Under the action of Fe catalyst, it is obtained by chlorination on the toluene ring, and then o / p-chlorotoluene is separated by rectification to obtain o / p-chlorotoluene products. It is calculated that even if a rectification separation tower with more than 100 theoretical plates is used, high-purity (≥99.95%) o-chlorotoluene cannot be obtained, so it directly affects the application and development of downstream high-end...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C25/02C07C17/389C07C17/12
CPCC07C17/389C07C17/12C07C25/02Y02P20/584
Inventor 李景林崔咪芬陈献顾苏平赵婕
Owner 常州新东化工发展有限公司
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