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A continuous sulfonation process for the synthesis of p-aminophenyl-β-hydroxyethyl sulfone sulfate

A technology of p-aminophenyl and hydroxyethyl sulfone, which is applied in the field of continuous sulfonation process for the synthesis of p-aminophenyl-β-hydroxyethyl sulfone sulfate, can solve the problem of difficult temperature control, prolong production cycle, increase energy Consumption and other problems, to achieve the effect of easy control of reaction temperature, easy industrial production, and overcome complicated operation

Active Publication Date: 2016-09-07
ZHEJIANG QICAI ECO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 1. Batch reaction, the raw material acetanilide needs to be cooled and sliced ​​into flake solids, and then the solids are slowly added to the sulfonation kettle to react with chlorosulfonic acid. The solids must be dissolved before reacting, and heat will be generated locally, resulting in local The reaction temperature is too high, thereby causing the by-product p-chloroaniline to exceed the standard, which not only increases energy consumption but also affects product conversion;
[0008] 2. The reaction mass transfer effect of the batch method is poor, the temperature is not easy to control, and the waste gas generated is not easy to get rid of;
[0009] 3. The reaction time of the batch method is long, which prolongs the production cycle and has the disadvantage of high synthesis cost

Method used

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  • A continuous sulfonation process for the synthesis of p-aminophenyl-β-hydroxyethyl sulfone sulfate
  • A continuous sulfonation process for the synthesis of p-aminophenyl-β-hydroxyethyl sulfone sulfate
  • A continuous sulfonation process for the synthesis of p-aminophenyl-β-hydroxyethyl sulfone sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Turn on the sulfonation circulating pump 4, adjust the flow rate of chlorosulfonic acid to 1500kg / h, pump the chlorosulfonic acid feed pipe b from the chlorosulfonic acid transfer tank to the sulfonation batching kettle 5 through the feed pump, and enter the mouth of the sulfonation batching kettle Equipped with the first atomizing distributor c, it can instantly atomize the chlorosulfonic acid so that it is sprayed into the sulfonated batching kettle 5 in an atomized state, and at the same time, the flow rate of the molten acetanilide is adjusted to be 600kg / h, and the acetanilide is fed into the The material pipe a is transferred from the acetanilide transfer tank 1 to the sulfonation batching kettle 5 through the acetanilide feed pump 2, and the second atomization distributor d is installed at the mouth of the sulfonation batching kettle, which can instantly atomize the acetanilide, so that It is sprayed into the sulfonation batching kettle 5 in an atomized form, the ...

Embodiment 2

[0051] Turn on the sulfonation circulating pump 4, adjust the flow rate of chlorosulfonic acid to 1500kg / h, pump the chlorosulfonic acid feed pipe b from the chlorosulfonic acid transfer tank to the sulfonation batching kettle 5 through the feed pump, and enter the mouth of the sulfonation batching kettle Equipped with the first atomizing distributor c, it can instantly atomize the chlorosulfonic acid so that it is sprayed into the sulfonated batching kettle 5 in an atomized state, and at the same time, the flow rate of the molten acetanilide is adjusted to be 600kg / h, and the acetanilide is fed into the The material pipe a is transferred from the acetanilide transfer tank 1 to the sulfonation batching kettle 5 through the acetanilide feed pump 2, and the second atomization distributor d is installed at the mouth of the sulfonation batching kettle, which can instantly atomize the acetanilide, so that It is sprayed into the sulfonation batching kettle 5 in an atomized form, the ...

Embodiment 3

[0053] Turn on the sulfonation circulation pump 4, adjust the flow rate of chlorosulfonic acid to 2000kg / h, pump the chlorosulfonic acid feed pipe b from the chlorosulfonic acid transfer tank to the sulfonation batching kettle 5 through the feed pump, and enter the mouth of the sulfonation batching kettle Equipped with the first atomizing distributor c, it can instantly atomize the chlorosulfonic acid so that it is sprayed into the sulfonated batching kettle 5 in an atomized state, and at the same time, the flow rate of the molten acetanilide is adjusted to be 600kg / h, and the acetanilide is fed into the The material pipe a is transferred from the acetanilide transfer tank 1 to the sulfonation batching kettle 5 through the acetanilide feed pump 2, and the second atomization distributor d is installed at the mouth of the sulfonation batching kettle, which can instantly atomize the acetanilide, so that It is sprayed into the sulfonation batching kettle 5 in an atomized form, the ...

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Abstract

The invention discloses a continuous sulfonating process for synthesizing p-aminophenyl-beta-hydroxyethyl sulfone sulphate. The process comprises the steps: performing reaction on chlorosulfonic acid and acetanilide which serve as raw materials; respectively atomizing chlorosulfonic acid and molten-state acetanilide and contacting with each other during feeding to perform reaction. According to the continuous sulfonating process for synthesizing p-aminophenyl-beta-hydroxyethyl sulfone sulphate, the molten-state acetanilide is used as a raw material, and the reaction on the acetanilide in an atomizing state and chlorosulfonic acid which is also in an atomizing state are carried out and the reaction temperature is easily controlled, so that the production of byproducts such as parachloroaniline is avoided, and the conversion rate of acetanilide serving as a raw material is high. The process is convenient to operate, short in production period, controllable in reaction process, less in labor demands, low in cost and easy for industrial production.

Description

technical field [0001] The invention relates to the technical field of production of dye intermediates, in particular to a continuous sulfonation process for synthesizing p-aminophenyl-β-hydroxyethyl sulfone sulfate. Background technique [0002] p-Aminophenyl-β-hydroxyethyl sulfone sulfate is an important organic raw material and reactive dye intermediate, widely used, such as for the manufacture of reactive black KN-B, reactive red 3BS, reactive blue 3GF, etc. [0003] About p-aminophenyl-beta-hydroxyethyl sulfone sulfuric acid ester process research existing many patents, bibliographical reports both at home and abroad, as publication number is disclosed in the Chinese patent literature of CN1869017A by making mol ratio be 1:1~1.2 Mix β-hydroxyethyl sulfone aniline and sulfuric acid evenly to obtain a reaction material, dry and solidify the reaction material at 110-200°C to obtain a cured product, and the cured product is reacted under reduced pressure at 150-180°C in a m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/88C07C303/02C07C309/51C07C303/08
Inventor 胡章云杜志超李学坤陆建祥李军
Owner ZHEJIANG QICAI ECO TECH CO LTD