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A kind of sulfonation process and device of alkyl diphenyl ether

A technology for the sulfonation of alkyl diphenyl ethers, which is applied in the field of sulfonation processes and devices for alkyl diphenyl ethers, can solve the problems of restricting the industrialization process of alkyl diphenyl ether sulfonates, increasing the difficulty of separating sulfonate products, Problems such as low content of effective substances in the product can achieve the effect of shortening the residence time, suppressing side reactions, and fast speed

Active Publication Date: 2019-10-01
中轻化工绍兴有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the reported literature, the sulfonating agent used in the preparation of the intermediate alkyl diphenyl ether sulfonic acid of the alkyl diphenyl ether sulfonate at present in China is mainly concentrated sulfuric acid, oleum and chlorosulfonic acid. The sulfonating agent will not only increase the difficulty of separating the sulfonate product, but also produce a large amount of acid waste water or acid gas HCl in the sulfonation process, which will lead to environmental pollution, equipment corrosion and cost increase; at the same time, the reactor used is a stirred "kettle "type" (reaction kettle and flask) reactor, although the reactor has a simple structure and less equipment investment, but the material has a long residence time, serious back-mixing, many side reactions, low content of effective substances in the product, and poor color, which limits the alkane The industrialization process of diphenyl ether sulfonate

Method used

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  • A kind of sulfonation process and device of alkyl diphenyl ether

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Effect test

Embodiment 1

[0020] Realize the object device of the present invention, it comprises membrane type sulfonation reactor 1, tank type sulfonation reactor 2, organic matter / inert solvent storage tank 3, condenser 4 and inert solvent recovery tank 5, it is characterized in that membrane type sulfonation reaction The outlet at the bottom of device 1 is connected to the inlet of tank-type sulfonation reactor 2, the top of membrane-type sulfonation reactor 1 has a mixed gas inlet, and the top of membrane-type sulfonation reactor 1 is connected to organic matter / inert solvent storage tank 3, tank-type The gas outlet of the sulfonation reactor 2 is connected to the condenser 4, the condenser 4 is connected to the inert solvent recovery tank 5, the upper part of the condenser has an exhaust port 9, and the membrane type sulfonation reactor 1 and the tank type sulfonation reactor 2 have cooling Water inlet 6 and cooling water outlet 7.

[0021] Add 500Kg of monododecyl diphenyl ether and 1,2-dichloro...

Embodiment 2

[0023] Add 500Kg of dodecyl diphenyl ether and dichloromethane into the organic matter / inert solvent storage tank 3 according to the ratio of 1:1 (mass ratio) and stir to form an organic mixture, and pump the organic mixture into the membrane sulfur In the reactor 1, while passing SO 3 / air mixture to control the SO in the initial sulfonation reaction process 3 gas concentration (SO 3 The volume ratio of mixed gas) is 2%, gas SO 3 The molar ratio to the organic mixture is 0.8:1, the temperature of the circulating cooling water is 25°C, and the residence time in the membrane sulfonator is 7min. After the preliminary sulfonation reaction, stop feeding SO 3 / air mixture. Put all the products after preliminary sulfonation into the tank type sulfonator 2, and feed SO at the same time 3 / air mixture to control the SO in the sulfonation reaction process 3 gas concentration (SO 3 The volume ratio of mixed gas) is 3%, gas SO 3 The molar ratio with the organic mixture is 2:1, the...

Embodiment 3

[0025] Add 500Kg of isodecyl diphenyl ether and chloroform into the organic matter / inert solvent storage tank 3 according to the ratio of 1:3 (mass ratio) and stir to form an organic mixture, and use a metering pump to pump the organic mixture into the membrane sulfonator 1, while feeding SO 3 / air mixture to control the SO in the initial sulfonation reaction process 3 gas concentration (SO 3The volume ratio of mixed gas) is 4%, gas SO 3 The molar ratio to the organic mixture is 1.5:1, the temperature of the circulating cooling water is 35°C, and the residence time in the membrane sulfonator is 7min. After the preliminary sulfonation reaction, stop feeding SO 3 / air mixture. Put all the products after preliminary sulfonation into the tank type sulfonator 2, and feed SO at the same time 3 / air mixture to control the SO in the sulfonation reaction process 3 gas concentration (SO 3 The volume ratio of mixed gas) is 6%, gas SO 3 The molar ratio to the organic mixture is 2.5...

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Abstract

The invention relates to a sulfonating process of alkyl diphenyl ether, and the sulfonating process comprises the concrete steps: initially sulfonating a mixture of SO3 gas, alkyl diphenyl ether and an inert solvent at 10-35DEG C in a film sulfonator, then conducting further sulfonating at 10-80DEG C in a kettle sulfonator, finally recovering the inert solvent from the further sulfonated product by an evaporative condenser and delivering the inert solvent into a solvent recovery tank, exhausting the tail gas through an exhaust outlet into a tail gas treatment system, and then obtaining the alkyl diphenyl ether sulfonic acid product. The sulfonating process has the characteristics of high efficiency of process, low cost, high product purity, good color and the like.

Description

technical field [0001] The invention relates to a sulfonation process and device of alkyl diphenyl ether. Background technique [0002] Alkyl diphenyl ether sulfonates are widely used in tertiary applications because of their good water solubility, surface activity, and good solubility and stability in strong acids, strong alkalis, high-concentration inorganic salts, and bleach solutions. Oil extraction, textile printing and dyeing, daily chemical industry, emulsion polymerization and soil purification and other fields. At present, this kind of products has not yet realized industrial production in China, and all products rely on imports. Patent CN 103265460 discloses a preparation method of alkyl diphenyl ether sulfonate, put alkyl diphenyl ether and inert organic solvent into sulfonation kettle, add sulfonating agent to keep warm for sulfonation for a period of time, add water and let stand for acid analysis After layering, the waste acid water layer was removed, and the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/06C07C309/42
Inventor 李萍郭朝华杨效益李全红李建波耿卫东李慧芳荆春萍
Owner 中轻化工绍兴有限公司
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