CN100471552C - Sodium lauryl polyoxyethylene (7) octyl sulfosuccinate and its preparing process - Google Patents
Sodium lauryl polyoxyethylene (7) octyl sulfosuccinate and its preparing process Download PDFInfo
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- CN100471552C CN100471552C CNB2006101616923A CN200610161692A CN100471552C CN 100471552 C CN100471552 C CN 100471552C CN B2006101616923 A CNB2006101616923 A CN B2006101616923A CN 200610161692 A CN200610161692 A CN 200610161692A CN 100471552 C CN100471552 C CN 100471552C
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Abstract
The invention discloses a lauryl alcohol polyvinyl ether (7) octyl sulfo succinic mixed diester sodium and relative preparation, comprising that processing monoester reaction between maleic anhydride and lauryl alcohol polyvinyl ether (7), and processing diester reaction between the reaction product of monoester reaction and octanol, and processing conjugate addition reaction between the reaction product of diester reaction and sodium bisulfite to obtain final product. The invention has high-quality property and simple process.
Description
Technical field:
The present invention relates to a kind of surfactant.
Background technology:
Existing butanedioic acid dibasic acid esters sulfonate series of surfactants generally adopts alcohol excess to carry out esterification, again to the esterification products washing that neutralizes, adds the sulfonation phase transfer catalyst again after the dehydration depickling, carries out adding to depress in closed system.Complex procedures, properties of product are not very good yet.
Summary of the invention:
The object of the present invention is to provide that a kind of performance is good, the simple ethoxylated dodecyl alcohol of synthetic method (7) octyl sulfosuccinate sodium and preparation method.
Technical solution of the present invention is:
A kind of ethoxylated dodecyl alcohol (7) octyl sulfosuccinate sodium, it is characterized in that: structural formula is:
The preparation method of a kind of ethoxylated dodecyl alcohol (7) octyl sulfosuccinate sodium is characterized in that: comprise the following steps: successively
(1) maleic anhydride and ethoxylated dodecyl alcohol (7) are carried out single-esterification:
(2) above-mentioned single-esterification product and octanol are carried out double esterification reaction:
(3) above-mentioned double esterification reaction product and sodium hydrogensulfite are carried out conjugate addition reaction:
The preparation method of described ethoxylated dodecyl alcohol (7) octyl sulfosuccinate sodium, it is characterized in that: concrete steps are: in the four-hole boiling flask of being furnished with agitator, thermometer and reflux condenser by laruyl alcohol APEO (7): the amount of cis-butenedioic anhydride=1.00:1.10 adds ethoxylated dodecyl alcohol (7), cis-butenedioic anhydride after water treatment successively than (mol ratio), and adding accounts for the alkyl sulfonic acid catalyst of cis-butenedioic anhydride quality 1%, feed nitrogen, stir in 10～30 minutes and be warming up to 140 ℃ of temperature; Keep this temperature and timing, temperature retention time 150min, on same reaction unit, connect water knockout drum, and add octanol by the amount of octanol: cis-butenedioic anhydride=4.0:1.0 than (mol ratio) and carry out double esterification reaction, be heated 200 ℃ of temperature and timing, the insulation dehydration by the method for above-mentioned single-esterification, temperature retention time is 300min, cooling, neutralization are cooled to 20～60 ℃ of temperature, and the pH value that neutralizes is 7 ± 0.5; Above-mentioned neutralized reaction product is added the sulfonating agent sodium hydrogensulfite; the mol ratio of neutralized reaction product and the contained sulfur dioxide of sulfonating agent is 1.00:1.10; this sulfonating reaction is under the atmosphere protection that nitrogen is arranged; be warmed up to 103 ± 3 ℃; time 10～30min; sulfonating reaction finishes sulfonated tail gas SO through the 300min reaction under 100～110 ℃ of temperature
2Absorb with alkali lye, and return for sulfonating reaction, static layering under the maturation products room temperature obtains ethoxylated dodecyl alcohol (7) octyl sulfosuccinate sodium, and the waste water that is produced returns for sulfonating reaction and uses.
The present invention is owing to adopt the control esterification yield to determine raw material octanol consumption in the double esterification process, and consumption of raw material significantly reduces in the course of reaction; After reducing the octanol input amount, it is few to cross consumption, and esterification temperature reduces, and esterification time shortens, and it is few to enable depletion; Excessive octanol input amount has been saved esterification products washing, dehydration, dealcoholysis operation after reducing; Reduced reaction time and reduced reaction temperature, made esterification yield between 90～97%, the unreacted monoester salt that obtains through neutralization of monoesters has completely been avoided the influence of extra catalyst impurity as the non-phase transfer catalyst that adds, and has reduced the material consumption; Sulfonating reaction is carried out under normal pressure, and the nitrogen atmosphere that is aided with influence sulfonation process and product color to prevent air oxidation aggravation, by simple tail gas absorption, makes the SO that escapes simultaneously
2Become aqueous solution of sodium bisulfite, use, reduced requirement, solved tail gas pollution simultaneously equipment for sulfonating reaction; Sulfonation waste water returns for sulfonating reaction and uses, and the reaction time is shortened, and raw material availability further improves, and pollution-free, and technology is very compact.Product ethoxylated dodecyl alcohol (7) octyl sulfosuccinate sodium is the mixing dibasic acid esters sulfosuccinic acid sodium salt that has anion and non-ionic surface active agent duplex surface chemical property concurrently that has hydroxyl and ethyoxyl simultaneously, when both having kept the preferable wetting and permeance property of butanedioic acid symmetric double sulfonated ester, has the surfactant of good anti-hard water, dispersion and emulsifiability of the pure polyethers monoesters sulfonate of butanedioic acid fat again.Be widely used in daily-use chemical industry, agricultural chemicals, coating, printing and dyeing, mine, papermaking, leather and sensitization industry etc., can be used as emulsifying agent, wetting agent, bleeding agent, dispersant and glass antidimmer.
The invention will be further described below in conjunction with embodiment.
The specific embodiment:
In the four-hole boiling flask of being furnished with agitator, thermometer and reflux condenser, add ethoxylated dodecyl alcohol (7), cis-butenedioic anhydride after water treatment successively than (mol ratio) by the 1.00:1.10 amount, and adding accounts for the alkyl sulfonic acid catalyst of cis-butenedioic anhydride quality 1%, feed nitrogen, stir in 10～30 minutes (example 10,20,30 minutes) and be warming up to 140 ℃ of temperature; Keep this temperature and timing, temperature retention time 150min, on same reaction unit, connect water knockout drum, and add octanol by the amount of octanol: cis-butenedioic anhydride=4.0:1.0 than (mol ratio) and carry out double esterification reaction, be heated 200 ℃ of temperature and timing, the insulation dehydration by the method for above-mentioned single-esterification, temperature retention time is 300min, cooling, neutralization are cooled to 20～60 ℃ of temperature (20 ℃, 40 ℃, 60 ℃ of examples), and the pH value that neutralizes is 7 ± 0.5; Above-mentioned neutralized reaction product is added the sulfonating agent sodium hydrogensulfite; the mol ratio of neutralized reaction product and the contained sulfur dioxide of sulfonating agent is 1.00:1.10; this sulfonating reaction is under the atmosphere protection that nitrogen is arranged; be warmed up to 103 ± 3 ℃; time 10～30min (example 10,20,30 minutes); sulfonating reaction finishes sulfonated tail gas SO through the 300min reaction under 100～110 ℃ of (100 ℃, 105 ℃, 110 ℃ of examples) temperature
2Absorb with alkali lye (NaOH or sodium carbonate etc.), and return for sulfonating reaction, static layering under the maturation products room temperature obtains ethoxylated dodecyl alcohol (7) octyl sulfosuccinate sodium, and structural formula is:
The waste water that is produced returns for sulfonating reaction and uses.
The reaction equation of above-mentioned reaction is:
(1)
(2)
(3)
Products obtained therefrom gets physicochemical property and sees the following form:
| Solid content % | Critical capsule concentration/mol/L | Critical surface tension mN/m | Dispersibility is (right 50g reduces blue)Product quality mark 2% | Wettability/s | Degreasing power % | Emulsifiability (0.1%)/s |
| 57.3 | 1×10 -4 | 31.5 | 92.2 | 3.5 | 100 | 180 |
Claims (1)
1, the preparation method of ethoxylated dodecyl alcohol (7) octyl sulfosuccinate sodium, it is characterized in that: concrete steps are:
In the four-hole boiling flask of being furnished with agitator, thermometer and reflux condenser by laruyl alcohol APEO (7): the amount of cis-butenedioic anhydride=1.00:1.10 adds ethoxylated dodecyl alcohol (7), cis-butenedioic anhydride after water treatment successively than (mol ratio), and adding accounts for the alkyl sulfonic acid catalyst of cis-butenedioic anhydride quality 1%, feed nitrogen, stir in 10～30 minutes and be warming up to 140 ℃ of temperature; Keep this temperature and timing, temperature retention time 150min, on same reaction unit, connect water knockout drum, and add octanol by the amount of octanol: cis-butenedioic anhydride=4.0:1.0 than (mol ratio) and carry out double esterification reaction, be heated 200 ℃ of temperature and timing, the insulation dehydration by the method for above-mentioned single-esterification, temperature retention time is 300min, cooling, neutralization are cooled to 20～60 ℃ of temperature, and the pH value that neutralizes is 7 ± 0.5; Above-mentioned neutralized reaction product is added the sulfonating agent sodium hydrogensulfite; the mol ratio of neutralized reaction product and the contained sulfur dioxide of sulfonating agent is 1.00:1.10; this sulfonating reaction is under the atmosphere protection that nitrogen is arranged; be warmed up to 103 ± 3 ℃; time 10～30min; sulfonating reaction finishes sulfonated tail gas SO through the 300min reaction under 100～110 ℃ of temperature
2Absorb with alkali lye, and return for sulfonating reaction, static layering under the maturation products room temperature obtains ethoxylated dodecyl alcohol (7) octyl sulfosuccinate sodium, and the waste water that is produced returns for sulfonating reaction and uses.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101616923A CN100471552C (en) | 2006-12-25 | 2006-12-25 | Sodium lauryl polyoxyethylene (7) octyl sulfosuccinate and its preparing process |
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| CNB2006101616923A CN100471552C (en) | 2006-12-25 | 2006-12-25 | Sodium lauryl polyoxyethylene (7) octyl sulfosuccinate and its preparing process |
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| CN101015779A CN101015779A (en) | 2007-08-15 |
| CN100471552C true CN100471552C (en) | 2009-03-25 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105503669A (en) * | 2016-02-17 | 2016-04-20 | 南通大学 | Preparation method for 1,4-butanediol polyoxyethylene ether (7) sec-sodium bi-sulfosuccinic diester surfactant |
| CN113277964A (en) * | 2021-04-19 | 2021-08-20 | 上海科沣新材料有限公司 | Sulfosuccinate surfactant and preparation method thereof |
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Non-Patent Citations (4)
| Title |
|---|
| 月桂醇聚氧乙烯醚（7）己基磺基琥珀酸混合双酯钠的合成与性能. 华平.精细化工，第21卷第2期. 2004 |
| 月桂醇聚氧乙烯醚（7）己基磺基琥珀酸混合双酯钠的合成与性能. 华平.精细化工，第21卷第2期. 2004 * |
| 月桂醇聚氧乙烯醚(7)已基磺基琥珀酸混合双酯钠的合成与性能. 华平.精细化工，第21卷第2期. 2002 |
| 月桂醇聚氧乙烯醚(7)已基磺基琥珀酸混合双酯钠的合成与性能. 华平.精细化工，第21卷第2期. 2002 * |
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