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Preparation method of sodium p-styrene sulfonate

A technology of sodium styrene sulfonate and bromophenylethane sulfonic acid is applied in the field of preparation of sodium p-styrene sulfonate, can solve the problems of high impurity content in the product, restricting the scope of use and product performance, etc., and achieves short reaction time, Sulfonation has good para-position and the effect of preventing pollution

Inactive Publication Date: 2017-07-14
XZL BIO TECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the limitations of the process, the product has high impurity content, including a large amount of sodium m-styrene sulfonate, sodium o-styrene sulfonate, sodium β-bromostyrene sulfonate, sodium bromide, sodium sulfate, dichloroethane and untreated Sulfonated bromophenylethane, etc., restrict the scope of use and product performance of the product

Method used

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  • Preparation method of sodium p-styrene sulfonate
  • Preparation method of sodium p-styrene sulfonate
  • Preparation method of sodium p-styrene sulfonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The bromophenylethane is quantitatively and continuously delivered to the head of the composite sulfonation reactor at a rate of 25 kg per hour by the bromophenylethane metering pump, and according to the molar ratio of 1:1.05, continuously and uniformly feed the trioxide with a mass content of 8% sulfur trioxide. Sulfur / air 142kg / hour, continuous sulfonation reaction occurs in the vertical tubular reactor in the composite sulfonation reactor, the temperature is controlled at 85°C, after preliminary sulfonation, it enters the aging homogeneous separation tank, and the tail gas is emptied after treatment Obtain 35.7kg of bromophenylethane sulfonic acid per hour, after testing: 0.2% of unsulfonated substance, 0.25% of sulfuric acid content; Uniformly add sodium hydroxide mass content 48% liquid caustic soda 23.65kg / hour, material neutralization temperature control 45-55 ℃, quickly heat up to 110 ℃ through heat exchanger to remove bromine, obtain liquid sodium p-styrene sul...

Embodiment 2

[0043] The bromophenylethane is quantitatively and continuously delivered to the head of the compound sulfonation reactor at a rate of 25 kg per hour by the bromophenylethane metering pump, and according to the molar ratio of 1:1.08, continuously and uniformly feed the trioxide with a mass content of 10% sulfur trioxide. Sulfur / air 116.7kg / hour, continuous sulfonation reaction occurs in the vertical tubular reactor in the composite sulfonation reactor, the temperature is controlled at 95°C, after preliminary sulfonation, it enters the aging homogeneous separation tank, and the tail gas is discharged after treatment Empty; obtain bromophenylethane sulfonic acid 35.8kg / hour, after testing: non-sulfonated matter 0.22%, sulfuric acid content 0.27%; Continuously and evenly add 23.65kg / hour of liquid caustic soda with a mass content of 48% of sodium hydroxide, control the neutralization temperature of the material at 45-55°C, and quickly raise the temperature to 110°C through a heat...

Embodiment 3

[0048]The bromophenylethane is quantitatively and continuously delivered to the head of the composite sulfonation reactor by the bromophenylethane metering pump at a rate of 25 kg per hour, and according to the molar ratio of 1:1.1, the trioxide with a mass content of sulfur trioxide of 10% is continuously and uniformly fed. Sulfur / air 118.9kg / hour, continuous sulfonation reaction occurs in the vertical tubular reactor in the composite sulfonation reactor, the temperature is controlled at 105°C, after preliminary sulfonation, it enters the aging homogeneous separation tank, and the tail gas is discharged after treatment Empty; obtain bromophenylethanesulfonic acid 35.9kg / hour, after testing: non-sulfonated substance 0.17%, sulfuric acid content 0.29%; Continuously and evenly add 23.65kg / hour of liquid caustic soda with a mass content of 48% of sodium hydroxide, control the neutralization temperature of the material at 45-55°C, and quickly raise the temperature to 110°C through...

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Abstract

The invention belongs to the technical field of chemical synthesis and in particular relates to a preparation method of sodium p-styrene sulfonate. The preparation method comprises the following steps of: preheating bromophenylethane and continuously conveying the bromophenylethane to a sulfonating reactor; adding dry gas into gas sulfur trioxide and mixing to obtain mixed gas; continuously conveying the mixed gas to a compound sulfonating reactor, wherein bromophenylethane and the mixed gas are continuously sulfonated in the compound sulfonating reactor to generate bromophenylethane sulfonic acid; continuously adding bromophenylethane sulfonic acid and liquid alkali into a high-speed homogeneous pump for neutralization, controlling the temperature, and raising the temperature to remove bromine to generate liquid sodium p-styrenesulfonate; and performing cooling crystallization, centrifugalization and drying to obtain the dried sodium p-styrenesulfonate. As no solvent is used, the cost can be greatly lowered, the product quality is improved and pollution of the solvent volatilization to air is avoided. No hazardous chemical substance is used, so that the safety risk is reduced, safety accidents are reduced or even avoided, and the essential safety requirement is met.

Description

Technical field [0001] The invention belongs to the technical field of chemical synthesis, and specifically relates to a preparation method of sodium p-styrenesulfonate. Background technique [0002] Sodium p-styrenesulfonate is a polymer monomer with unique functions. It is used in reactive emulsifiers, dyeing auxiliaries, water treatment agents (dispersants, flocculants), photo chemicals (diaphragms), and electrification prevention. Agents, semiconductors, imaging films, thermal conductive products, etc.; mainly used as the third monomer in the dry production of acrylic fiber; in the conventional process, after bromophenyl ethane is mixed with dichloroethane and other solvents, trioxide is introduced into the reaction kettle Sulfurization generates a mixture of bromophenyl ethane sulfonic acid and dichloroethane. After extracting dichloroethane, the sulfonic acid is neutralized by adding liquid alkali in the reaction kettle, bromine is removed, crystallization is centrifug...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/32C07C309/30
CPCC07C303/32C07C303/06C07C309/30C07C309/39
Inventor 汪会宝孙文玲聂怀军王立堂邓新基刘景亮王超张梅
Owner XZL BIO TECHNOLOGY CO LTD
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