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Synthesis method of para-beta-hydroxyethylsulfonyl sulfate aniline

A technology of hydroxyethyl sulfone sulfuric acid and hydroxyethyl sulfone acetanilide, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of high viscosity of the reaction system, unfavorable later use, large equipment loss and the like , to achieve the effect of reducing reaction energy consumption, reducing equipment loss and improving equipment profit

Active Publication Date: 2015-01-21
ZHEJIANG JINGGUANG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this preparation process, the viscosity of the reaction system is high, the energy consumption is high, and the loss of equipment is large; there are many insolubles in the obtained product, and the product has high hardness and coarse particles, which is not conducive to later use

Method used

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  • Synthesis method of para-beta-hydroxyethylsulfonyl sulfate aniline
  • Synthesis method of para-beta-hydroxyethylsulfonyl sulfate aniline
  • Synthesis method of para-beta-hydroxyethylsulfonyl sulfate aniline

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 850kg of p-β-hydroxyethyl sulfone acetanilide into the mixing pot, then add 2kg of dispersant NNO, mix for 1 hour, add the mixed material to the p-β-hydroxyethyl sulfide with 355kg of sulfuric acid In the synthesis pot of sulfone sulfate aniline, the temperature is raised to 120°C for esterification reaction. After 6 hours of reaction, the semi-finished product of p-β-hydroxyethylsulfone sulfate aniline is obtained; after the semi-finished product of p-β-hydroxyethylsulfone sulfate aniline is crushed Obtain 994kg of p-beta-hydroxyethyl sulfone sulfate aniline and 210kg of 94% acetic acid. Its HPLC purity is 97.23%, the retention time is consistent with commercially available standard products, the ammonia value is 97.5%, and the ester value is 95.5%, which meets the quality requirements of p-β-hydroxyethyl sulfone sulfate aniline. At the same time, the reaction current load is 12A, The hardness is 1.5, and the insoluble matter is 0.05%.

Embodiment 2

[0025] Add 850kg of p-hydroxyethyl sulfone acetanilide into the blending pot, then add 1.5kg of 1:1 dispersant NNO and dispersant MF mixing aids, mix for 1 hour, then add the mixture to In the p-beta-hydroxyethyl sulfone sulfate aniline synthetic pot of the sulfuric acid of band 355kg, 110 ℃ of temperature rises carry out esterification reaction, after reaction 8 hours, get p-beta-hydroxyethyl sulfone sulfate aniline semi-finished product; -Hydroxyethyl sulfone sulfate aniline semi-finished product obtains 215kg of p-beta-hydroxyethyl sulfone sulfate aniline 992.5kg and 93% acetic acid after pulverizing. Its HPLC is 97.8%, the retention time is consistent with the commercially available standard product, the ammonia value is 97.5%, and the ester value is 95.3%, which meets the quality requirements of p-β-hydroxyethyl sulfone sulfate aniline. At the same time, the reaction current load is 10A, the hardness 1.2, insolubles 0.04%.

Embodiment 3

[0027] Add 850kg of p-β-hydroxyethyl sulfone acetanilide into the mixing pot, then add 2kg of dispersant APEO, mix for 1 hour, add the mixture to the p-β-hydroxyethyl sulfide with 355kg of sulfuric acid In the synthesis pot of sulfone sulfate aniline, the temperature is raised to 110°C for esterification reaction. After 8 hours of reaction, the semi-finished product of p-β-hydroxyethylsulfone sulfate aniline is obtained; after the semi-finished product of p-β-hydroxyethylsulfone sulfate aniline is crushed Obtain 993kg of p-beta-hydroxyethyl sulfone sulfate aniline and 210kg of 93.7% acetic acid. Its HPLC is 96.6%, the retention time is consistent with the commercially available standard product, the ammonia value is 96.5%, and the ester value is 94.8%, which meets the quality requirements of p-β-hydroxyethyl sulfone sulfate aniline. At the same time, the reaction current load is 18A, the hardness 3. Insoluble matter is 0.1%.

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Abstract

The invention discloses a synthesis method of para-beta-hydroxyethylsulfonyl sulfate aniline. The synthesis method comprises the following steps: uniformly mixing para-beta-hydroxyethylsulfonyl acetanilide and a catalytic amount of sulfoacid dispersing agent; adding the mixture into sulfuric acid to carry out esterification reaction for removing acetic acid; after the reaction is ended, treating to obtain the para-beta-hydroxyethylsulfonyl sulfate aniline. The synthesis method has the advantages that the sulfoacid dispersing agent used as a performance additive is added into a reaction system to change the state of a material in the reaction process, so that the material is changed from the original peptization state to a foaming peptization state, the reaction efficiency is increased, the reaction energy consumption is reduced, the material crushing effect is improved, the content of insoluble matters in a product is finally reduced, the final material is changed from the original solid particles to non-solid particles with micro air holes, and the later dye preparation can be more favorably realized.

Description

technical field [0001] The invention belongs to the field of synthesis of dye intermediates, in particular to a synthesis method of p-β-hydroxyethyl sulfone sulfate aniline. Background technique [0002] p-β-Hydroxyethyl sulfone sulfate aniline, also known as p-ester, CAS No. 2494-89-5, structure as shown in formula (I), is an important intermediate in the field of reactive dyes, and is the synthesis of KN The necessary raw materials for type\M type reactive dyes can be used to prepare more than a dozen reactive dyes such as reactive green blue KN-G, reactive yellow M-5R, reactive deep blue M-4G, etc. [0003] [0004] In the current synthesis of p-β-hydroxyethyl sulfone sulfate aniline, the p-β-hydroxyethyl sulfone acetanilide (structure shown in formula (II)) is mainly used after drying, adding a certain proportion of sulfuric acid Esterification and deacetic acid removal reaction under reduced pressure for 8 to 12 hours, and then pulverize and refine the reactant to o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/36C07C315/04
Inventor 王国林蒲云秋
Owner ZHEJIANG JINGGUANG IND
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