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Method of using SO<3>-air mixture to produce alkylphenol sulfonic acid and salts thereof via film sulfonator sulfonated alkylphenol

A technology of alkylphenol sulfonate and alkylphenol sulfonic acid, which is applied to the preparation of sulfonate, the reaction of thin-film liquid and gas, and the preparation of sulfonic acid. It can solve the problems of high inorganic salt content and recovery of sulfonated phenol. Low yield, large consumption of organic solvents, etc., to achieve the effects of low inorganic salt content, environmental protection, and high sulfonation rate

Active Publication Date: 2012-05-23
TAIXING LINGFEI CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN 1239477C once disclosed a method for intermittently sulfonating phenols with chlorosulfonic acid in an organic solvent phase, but this patent mainly sulfonates short-chain dihydric phenols or benzophenone phenol derivatives, The recovery yield of sulfonated phenol produced is low, and a large amount of organic solvent is consumed, and the sulfonated phenol product produced by chlorosulfonic acid sulfonation process has the disadvantage of high content of inorganic salts after neutralization

Method used

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  • Method of using SO&lt;3&gt;-air mixture to produce alkylphenol sulfonic acid and salts thereof via film sulfonator sulfonated alkylphenol
  • Method of using SO&lt;3&gt;-air mixture to produce alkylphenol sulfonic acid and salts thereof via film sulfonator sulfonated alkylphenol

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Experimental program
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Effect test

Embodiment 1

[0017] Embodiment 1: the preparation of mixing potassium cresyl sulfonate

[0018] mixed cresol with SO 3 - The air mixture is metered separately into the membrane sulfonator, where the SO 3 The molar ratio with mixed cresol is 1.05:1, SO 3 - SO in the air mixture 3 The volume concentration is 3%; the sulfonation temperature is 30°C, and the sulfonation reaction is an instantaneous continuous reaction; after the reaction product passes through the gas-liquid separator, the liquid part enters the aging kettle and is aged at the sulfonation temperature for half an hour to obtain mixed cresolsulfonic acid ; Add process water to the neutralization kettle, add mixed cresolsulfonic acid and potassium hydroxide solution, carry out neutralization reaction at 30°C, stir for 2 hours, make the product pH value reach 7-9, and obtain a mass concentration of 50% Mix Potassium Cresol Sulfonate.

Embodiment 2

[0019] Embodiment 2: the preparation of 2-sec-butylphenol ammonium sulfonate

[0020] Combine 2-sec-butylphenol with SO 3 - The air mixture is metered separately into the membrane sulfonator, where the SO 3 The molar ratio to 2-sec-butylphenol is 1.3:1, SO 3 - SO in the air mixture 3 The volume concentration is 4%; the sulfonation temperature is 40°C, and the sulfonation reaction is an instantaneous continuous reaction; after the reaction product passes through the gas-liquid separator, the liquid part enters the aging kettle and is aged for 45 minutes at the sulfonation temperature to obtain 2-sec-butyl Phenolsulfonic acid; add process water to the neutralization kettle, add 2-sec-butylphenolsulfonic acid and ammonium hydroxide solution with a mass concentration of 28%, carry out neutralization reaction at 40°C, stir for 2 hours, and make the product pH Reach 7~9, obtain mass concentration and be 50% ammonium 2-sec-butylphenolsulfonate.

Embodiment 3

[0021] Embodiment 3: Preparation of p-tert-amylphenolsulfonic acid monoethanolamine salt

[0022] P-tert-amylphenol and SO 3 - The air mixture is metered separately into the membrane sulfonator, where the SO 3 The molar ratio to p-tert-amylphenol is 1.1:1, SO 3 - SO in the air mixture 3 The volume concentration is 5%; the sulfonation temperature is 50°C, and the sulfonation reaction is an instantaneous continuous reaction; after the reaction product passes through the gas-liquid separator, the liquid part enters the aging kettle and is aged at the sulfonation temperature for 1 hour to obtain p-tert-amyl Phenolsulfonic acid; add process water to the neutralization kettle, add p-tert-amylphenolsulfonic acid and monoethanolamine, carry out neutralization reaction at 50°C, stir for 2 hours, make the pH value of the product reach 7-9, and obtain the mass concentration It is 60% p-tert-amylphenol sulfonic acid monoethanolamine salt.

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Abstract

A method of using SO3-air mixture to produce alkylphenol sulfonic acid and salts thereof through sulfonating the alkylphenol via a film sulfonator belongs to sulphonate preparing technology field. The invention uses alkylphenol as raw material, and uses the SO3-air mixture to sulfonate the raw material via the film sulfonator to obtain alkylphenol sulfonic acid, and uses alkaline solution such as NaOH to neutralize thealkylphenol sulfonic acid to obtain alkylphenol sulphonate. The alkylphenol used is a alkylphenol containing one or two C1-C20 straight-chain or branched chain alkyl. The alkylphenol sulfonic acid and salt thereof prepared by the method has high sulphonation rate, low free oil content, low inorganic salt content and producing no spend acid, which is no corrosion to equipments and helpful for environmental protection.

Description

technical field [0001] The present invention relates to a kind of SO 3 -A method for producing alkylphenol sulfonic acid and its salt by sulfonating alkylphenol with air mixture through a membrane sulfonator, belonging to the technical field of sulfonate preparation. The sulfonic acid and its salts can be used as surfactants or important raw materials for producing surfactants, and can also be used as dyes and drug intermediates. technical background [0002] The process and technology of sulfonation reaction play an important role in the field of modern chemical industry. Sulfonic acid compounds and alkyl sulfate compounds are currently one of the most widely used anionic surfactants. [0003] At present, sulfonation production technology has been developed rapidly both at home and abroad. The industrially available sulfonation methods mainly include SO 3 Sulfonation method, concentrated sulfuric acid sulfonation method, oleum sulfonation method, chlorosulfonic acid sul...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/42C07C303/06C07C303/32B01J10/02
Inventor 方云何志强夏咏梅
Owner TAIXING LINGFEI CHEM TECH CO LTD
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