Clean technology for continuously synthesizing 2,4-binitro-6-chloroaniline

A technology of dinitroaniline and dinitro, which is applied in the clean process field of synthesizing 2,4-dinitro-6-chloroaniline, can solve problems such as unclean production and difficult handling, reduce the amount of hydrochloric acid, avoid Exhaust emissions, significant economic and social benefits

Inactive Publication Date: 2015-05-06
ZHEJIANG LONGSHENG GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the chlorination reaction with sodium chlorate will produce a mother liquor containing sodium chloride, after the mother liquor is applied mechanically for a certain number of times, the sodium chloride content in the mother liquor is too high to be applied mechanically again, and the mother liquor containing high concentration of sodium chloride is difficult to handle. Can not really achieve clean production

Method used

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  • Clean technology for continuously synthesizing 2,4-binitro-6-chloroaniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Such as figure 1 , using three-stage series reactors (2, 3, 4), three parallel filter presses (8, 9, 10) and two parallel mother liquor recovery tanks (11, 12), the first, second, and third stages The volume of the reactor is 50m 3 , control the chlorination temperature at 35-40°C, and the volume of the mother liquor recovery tank is 50m 3 , the volume of the filter press is 500m 3 , the volume of the mother liquor storage tank is 100m 3 , The liquid level of the mother liquid recovery tank is set to 90% of the volume.

[0028] Into the beating kettle (1), feed raw materials simultaneously and continuously for beating, control the feed rate of 2,4-dinitroaniline to be 915kg / h, the feed rate of 31% hydrochloric acid to be 4502kg / h, and 38% dispersant The feed rate of MF is 24kg / h, and the material in the beating tank enters the first-stage reactor (1) at a speed of 5441kg / h; the chlorine gas is passed into the first-stage reactor through the ejector (5) at a flow rat...

Embodiment 2

[0032] According to the operation method described in Example 1, only the hydrochloric acid is replaced with the mother liquor in the mother liquor storage tank, and the filter cake from the filter press is washed and dried to obtain the 2,4-dinitro-6 -Chloroaniline, measured purity (HPLC) 98.2%, yield 96.8%. The collected HCl gas is used for the synthesis of m-acetaniline, and the purity (HPLC) of 99% m-acetaniline can be obtained.

Embodiment 3

[0034] According to the operating method described in Example 1, the difference is the flow rate of raw materials: the feed rate of 2,4-dinitroaniline is 732kg / h, the feed rate of 30% hydrochloric acid is 3893kg / h, and 38% dispersion The feed rate of agent MF is 20kg / h, and the material in the beating kettle enters the first-stage reaction kettle at a speed of 4645kg / h; The material in the reaction kettle is passed into the next-stage reaction kettle at a flow rate of 4918kg / h; then injected into the filter press at a flow rate of 4918kg / h for filtration, and the filter press also enters the mother liquor recovery tank at a flow rate of 4918kg / h; the mother liquor recovery tank The air is blown in the middle, and when the concentration of hydrochloric acid is 30%, the air blowing is stopped, and the mother liquor enters the mother liquor storage tank, and the hydrogen chloride tail gas is collected at the same time; the mother liquor in the mother liquor storage tank can replac...

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Abstract

The invention discloses a clean technology for continuously synthesizing 2,4-binitro-6-chloroaniline. The clean technology comprises the following steps: continuously feeding 2,4-dinitraniline, hydrochloric acid and chlorine gas to a first-stage reaction kettle of a multi-stage tandem reaction kettle; carrying out chlorination reaction under stirring, feeding one part of materials in the previous stage of reaction kettle to the reaction kettle to circulate through a pump, and feeding one part to the next stage of reaction kettle to further carry out chlorination reaction; feeding the tail gas generated by the previous stage of reaction kettle to the next stage of reaction kettle to further carry out chlorination reaction, and feeding one part of the materials in the final stage of reaction kettle to the reaction kettle to circulate through a pump; after reaction is detected to be completed, continuously discharging and filtering one part of materials, wherein the obtained filter cake is a 2,4-binitro-6-chloroaniline product; feeding the filtered mother liquor to a mother liquor recovery tank; and blowing air into the mother liquor in the mother liquor recovery tank, reusing the blown hydrogen chloride tail gas, and pumping into a mother liquor storage tank when the air blown into the mother liquor reaches certain concentration, wherein the mother liquor in the mother liquor storage tank is used in cycle instead of hydrochloric acid.

Description

(1) Technical field [0001] The invention relates to a cleaning process for synthesizing 2,4-dinitro-6-chloroaniline, in particular to a cleaning process for continuously synthesizing 2,4-dinitro-6-chloroaniline. (2) Background technology [0002] 2,4-Dinitro-6-chloroaniline is an important intermediate of disperse dyes, and it is widely used both at home and abroad. Its production method is generally obtained by chlorination of 2,4-dinitroaniline as raw material. Chlorinating agents mainly include: (1) sodium hypochlorite; (2) sodium chlorate; (3) chlorine gas. [0003] (1) Use sodium hypochlorite as the chlorination agent to carry out chlorination reaction in hydrochloric acid medium. The production process of this method is more complicated, and by-products are produced in the reaction process, the product quality is poor, the color is deep, the chlorination time is long, and the equipment productivity is low , and the post-processing is more troublesome. [0004] (2) u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/74
Inventor 余青结曾银城祝培明陆军李世华张桂香周俊锋倪松涛
Owner ZHEJIANG LONGSHENG GROUP
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