CN86105852A - The production method of heavy alkylbenzene sulfonic acid - Google Patents
The production method of heavy alkylbenzene sulfonic acid Download PDFInfo
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- CN86105852A CN86105852A CN 86105852 CN86105852A CN86105852A CN 86105852 A CN86105852 A CN 86105852A CN 86105852 CN86105852 CN 86105852 CN 86105852 A CN86105852 A CN 86105852A CN 86105852 A CN86105852 A CN 86105852A
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- sulfonation
- alkyl benzene
- sulphur trioxide
- heavy alkyl
- liquid sulphur
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Abstract
A kind of stable liquid sulphur trioxide Direct Sulfonation heavy alkyl benzene novel method.Be used in the nitrogen of cyclic drying or air stable liquid sulphur trioxide cohesion or be dispersed among nitrogen or the air and the heavy alkyl benzene Direct Sulfonation, promptly liquid-liquid phase is carried out sulfonation, synthesized heavy alkyl benzene sulfonic acid.And saving sulfuric acid is saved power and energy, has shortened operation, and the ability of enhanced reactor shortens the sulfonation reaction time, has eliminated the three wastes, has improved quality product.
Description
The invention belongs to the novel method of stablizing liquid sulphur trioxide Direct Sulfonation heavy alkylbenzene sulfonic acid
The method of general synthesized heavy alkyl benzene sulfonic acid has 20% oleum method of sulfonation, and gas Sulphurex process and employing liquid sulfur dioxide are made solvent attitude Sulphurex process.
Aforesaid method, oleum and heavy alkyl benzene intermingling, sulfonation temperature is 60 ℃ in tubular reactor.React under the normal pressure.Just the sulfonated sulfonated bodies is through overaging, and sedimentation and branch acid can obtain sulfonated products.This kind method, spent acid is many, long flow path.The gas Sulphurex process with refining sulphur, through fusion, changes into sulfurous gas and sulphur trioxide with atmospheric oxygen; This sulphur trioxide carries out sulfonation reaction with after dry air mixes with heavy alkyl benzene in film reactor.This method, flow process is tediously long, and waste gas is arranged, and is many with stainless steel, and investment is big.The liquid sulfur dioxide solvent method is with sulfur dioxide liquid and sulphur trioxide intermingling, carries out sulfonation reaction in 60 ℃ of temperature and heavy alkyl benzene, this method, and sulfur dioxide corrosion is big, troublesome poeration.
The object of the invention is to improve heavy alkyl benzene sulfonated transformation efficiency, improves the quality shortened process, the conservation and the energy, the novel method of the elimination three wastes.
Main points of the present invention are to use the nitrogen of cyclic drying or air stable liquid sulphur trioxide cohesion or be dispersed among nitrogen or the air and the heavy alkyl benzene Direct Sulfonation, and promptly liquid-liquid carries out sulfonation, synthesized heavy alkyl benzene sulfonic acid mutually.
In sulfonation reactor, add heavy alkyl benzene after, with material slowly be heated to 40-45 ℃ this moment temperature be the sulfonation optimum temps, treat temperature-stable after, begin to add stable liquid sulphur trioxide.The adding method is, the initial stage is slow, prevents the heavy alkyl benzene oxidation, and speed up mid-term, thus the time have under the situation that the part heavy alkylbenzene sulfonic acid generates, accelerate to stablize the speed of liquid sulphur trioxide, can shorten the reaction times, the ability of enhanced reactor.Later stage, a large amount of the dropping stablized liquid sulphur trioxide, its objective is the raising transformation efficiency, fast reaction speed.Question response finishes, and through sampling analysis, every index reaches standard, and heavy alkyl benzene sulfonation transformation efficiency reaches more than 99%.
Sulfonation condition: heavy alkyl benzene: stable state liquid sulphur trioxide=1: 1.0-1.2.Stablize liquid sulphur trioxide concentration expressed in percentage by weight 2-10% in exsiccant nitrogen or air, the speed of stablizing liquid sulphur trioxide adding sulfonation reactor is the 0.1-20 Grams Per Minute, and stablizing liquid sulphur trioxide maintenance temperature is 30-45 ℃.
Advantage of the present invention and effect, conservation sulfuric acid is saved the energy, and technical process is short, the elimination three wastes, non-corrosiveness, the few and sulfonated product quality advantages of higher of construction investment.Its effect is that sulphonating agent is to stablize sulphur trioxide, is carrier with the nitrogen or the air of cyclic drying.Can improve the quality of sulfonated products, heavy alkyl benzene sulfonation transformation efficiency can reach more than 99%.Sulfuric acid 60-70% can be saved as calculating, about 25,000,000 yuan of economic benefits can be saved about sulfuric acid 10,005 kilotons by producing ten thousand tons of washing composition every year.
Embodiment 1
At first in sulfonation reactor, add 150 grammes per square metre alkylbenzenes, stirring velocity is 100-130 rev/min, 40-45 ℃ of temperature control, feed cyclic drying nitrogen or air stable liquid sulphur trioxide, with the 0.1-20 Grams Per Minute, concentration is 2-10%, is added in the sulfonation reactor to react 2-4 hour, and the analysis heavy alkyl benzene is sulfonation near tracer level and finishes.
Embodiment 2
Under the experiment condition of embodiment 1, to stablize liquid sulphur trioxide with the nitrogen of cyclic drying or air and be heated to 40 ℃-45 ℃, with feed rate 0.1-20 Grams Per Minute, suitable sulphur trioxide concentration expressed in percentage by weight 2-10%, join sulfonation reactor, sulfonation temperature is 40-60 ℃ of reaction 2-4 hour, analytical results: unsulfonated oil, the heavy alkyl benzene tracer level promptly finishes.
Claims (3)
1, a kind of production method that contains liquid sulphur trioxide and heavy alkyl benzene sulfonation synthesized heavy alkyl benzene sulfonic acid, it is characterized in that using stable liquid sulphur trioxide, nitrogen or air with cyclic drying are done carrier, the cohesion of stable liquid sulphur trioxide be dispersed in the nitrogen of cyclic drying or air among with the heavy alkyl benzene Direct Sulfonation.
2, as the production method of claim 1 described sulfonation synthesized heavy alkyl benzene sulfonic acid, it is characterized in that stable liquid sulphur trioxide and heavy alkyl benzene mol ratio of components are 1.0-1.2: 1.0, stablize liquid sulphur trioxide concentration expressed in percentage by weight 2-10% in exsiccant nitrogen or air, the speed of stablizing liquid sulphur trioxide adding sulfonation reactor is 10-100 ℃ of 0.1-20 Grams Per Minute sulfonation temperature, pressure 0-5 kilograms per centimeter
2, stirring revolution is 80-150 rev/min.
3, as the production method of claim 1,2 described sulfonation synthesized heavy alkyl benzene sulfonic acid: it is characterized in that best sulfonation temperature is 40-45 ℃, optimum pressure 0.2-0.5 kilograms per centimeter
2, optimum reacting time 2.5-3 hour, the best revolution that stirs was: 100-130 rev/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 86105852 CN86105852A (en) | 1986-07-14 | 1986-07-14 | The production method of heavy alkylbenzene sulfonic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 86105852 CN86105852A (en) | 1986-07-14 | 1986-07-14 | The production method of heavy alkylbenzene sulfonic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN86105852A true CN86105852A (en) | 1988-02-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 86105852 Pending CN86105852A (en) | 1986-07-14 | 1986-07-14 | The production method of heavy alkylbenzene sulfonic acid |
Country Status (1)
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| CN (1) | CN86105852A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101195593B (en) * | 2007-07-31 | 2010-12-08 | 浙江嘉化集团股份有限公司 | Industrial production method of alkylbenzene sulfonyl chloride |
| CN101947424A (en) * | 2010-09-30 | 2011-01-19 | 中国日用化学工业研究院 | Hybrid vaporizer and application thereof to preparation of sulfonated or sulfated product from liquid sulfur trioxide |
| CN101723858B (en) * | 2008-10-17 | 2012-07-18 | 南化集团研究院 | Method for preparing benzenesulfonic acid |
| CN109627195A (en) * | 2018-05-18 | 2019-04-16 | 南京科技职业学院 | A method of heavy alkylbenzene sulfonate is prepared using microreactor |
-
1986
- 1986-07-14 CN CN 86105852 patent/CN86105852A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101195593B (en) * | 2007-07-31 | 2010-12-08 | 浙江嘉化集团股份有限公司 | Industrial production method of alkylbenzene sulfonyl chloride |
| CN101723858B (en) * | 2008-10-17 | 2012-07-18 | 南化集团研究院 | Method for preparing benzenesulfonic acid |
| CN101947424A (en) * | 2010-09-30 | 2011-01-19 | 中国日用化学工业研究院 | Hybrid vaporizer and application thereof to preparation of sulfonated or sulfated product from liquid sulfur trioxide |
| CN109627195A (en) * | 2018-05-18 | 2019-04-16 | 南京科技职业学院 | A method of heavy alkylbenzene sulfonate is prepared using microreactor |
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