CN103724236A - Method for compounding sulphonate surface active agent by fluorocarbon alcohol - Google Patents
Method for compounding sulphonate surface active agent by fluorocarbon alcohol Download PDFInfo
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- CN103724236A CN103724236A CN201310655650.5A CN201310655650A CN103724236A CN 103724236 A CN103724236 A CN 103724236A CN 201310655650 A CN201310655650 A CN 201310655650A CN 103724236 A CN103724236 A CN 103724236A
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- fluorocarbon alcohol
- maleic anhydride
- sulfonate surfactant
- active agent
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Abstract
The invention discloses a method for compounding a sulphonate surface active agent by fluorocarbon alcohol. The method comprises the following steps: (1) putting fluorocarbon alcohol, maleic anhydride and a catalyst into a reaction still; pumping in N2 as a shielding gas; raising temperature to 70-100 DEG C; reacting for 3-7 hours; stopping reaction when the esterification rate remains unchanged to obtain maleic anhydride monoester; (2) putting sodium sulfite into the maleic anhydride monoester in step (1) for sulfonation; keeping the temperature in the still at 60-100 DEG C and reacting for a period; sampling to test the sulfonation rate; stopping reaction when the sulfonation rate remains unchanged; cooling down and discharging the materials. As fluorocarbon alcohol is adopted to compound the sulphonate surface active agent, the surface active agent has the characteristics of high surface activity, high thermal stability, high chemical stability, hydrophobicity, lipophobicity, relatively low price, and high economic benefit.
Description
Technical field
The present invention relates to a kind of preparation method of sulfonated salts tensio-active agent, especially a kind of method of synthetic fluorocarbon alcohol sulfonate surfactant.
Background technology
Fluorocarbon surfactant is a kind of novel tensio-active agent, is the highest a kind of tensio-active agent of surfactivity so far, is widely used in chemical industry, machinery, electronics, oil, weaving, papermaking, photograph, ink, household supplies and other field.Fluorocarbon surfactant not only has the performance of general hc-surfactant, also there is the special performance of " three high two hate ", be high surface, high heat-resistant stability and high chemical stability, not only hydrophobic but also hate oil of its fluorine-containing alkyl, has good compound property in addition.
Due to fluorocarbon surfactant synthesis technique complexity, expensive, limited to a certain extent its development.
Summary of the invention
The present invention produces synthetic fluorocarbon alcohol sulfosalt surfactant with telomerization method, when solving by-product utilized problem, obtain more cheap high performance fluorine carbon surface active agent, be applied in composite material pole tower, there is weather-proof resistance to soiling, have good economic benefit and use value, concrete steps are as follows:
1) fluorocarbon alcohol, maleic anhydride, catalyzer are put in reactor, passed into N
2make protection gas, be warmed up to 70～100 ℃, reaction 3～7h, stopped reaction after esterification yield remains unchanged, obtains maleic anhydride monoesters;
2) S-WAT is added to above-mentioned steps 1) carry out sulfonation in described maleic anhydride monoesters, keep the sampling after 60～100 ℃ of reaction for some time of still temperature to survey sulphonation rate, until sulphonation rate keep constant after stopped reaction, cooling discharging.
Further, the mass ratio of described fluorocarbon alcohol and maleic anhydride is (20～60): (20～60).
Further, the mass ratio of described maleic anhydride and S-WAT is (40～60): (40～60).
Further, the hydroxyl value scope of described fluorocarbon alcohol is 50～400mg KOH/g.
Further, described catalyzer is tosic acid, and accounts for 0.05～0.3% of all raw material total masses.
Further, described S-WAT is that massfraction is 40～60% sodium sulfite aqueous solution.
Adopt such scheme, obtained a kind of fluorocarbon alcohol sulfonate surfactant.Fluorocarbon alcohol synthesising sulfonate tensio-active agent for the present invention, has the special performance of high surface, high thermal stability, high chemical stability, hydrophobic nature, oil repellency, and its price is cheaper, has good economic benefit.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.
Embodiment 1:
1): pass into N
2make protection gas and keep not interrupting, by 20kg fluorocarbon alcohol (hydroxyl value 242KOH/g), 7.68kg maleic anhydride, the disposable reactor of putting into of 27.7g tosic acid, heat to 85 ℃, keep after for some time, esterification yield is surveyed in sampling, treats the constant maleic anhydride monoesters that obtains of esterification yield;
2): in the maleic anhydride monoesters obtaining above, add 19.97kg50% sodium sulfite aqueous solution, be warmed up to 80 ℃, keep after for some time, sulphonation rate is surveyed in sampling, stopped reaction after sulphonation rate keeps stablizing, obtains final fluorocarbon alcohol sulfonate surfactant.
Embodiment 2:
1): pass into N
2make protection gas and keep not interrupting, by 20kg fluorocarbon alcohol (hydroxyl value 169KOH/g), 5.62kg maleic anhydride, the disposable reactor of putting into of 51.2g tosic acid, heat to 85 ℃, keep after for some time, esterification yield is surveyed in sampling, treats the constant maleic anhydride monoesters that obtains of esterification yield;
2): in the maleic anhydride monoesters obtaining above, add 14.44kg50% sodium sulfite aqueous solution, be warmed up to 80 ℃, keep after for some time, sulphonation rate is surveyed in sampling, stopped reaction after sulphonation rate keeps stablizing, obtains final fluorocarbon alcohol sulfonate surfactant.
Embodiment 3:
1): pass into N
2make protection gas and keep not interrupting, by 20kg fluorocarbon alcohol (hydroxyl value 56KOH/g), 2.15kg maleic anhydride, the disposable reactor of putting into of 4.43g tosic acid, heat to 85 ℃, keep after for some time, esterification yield is surveyed in sampling, treats the constant maleic anhydride monoesters that obtains of esterification yield;
2): in the maleic anhydride monoesters obtaining above, add 4.6kg60% sodium sulfite aqueous solution, be warmed up to 80 ℃, keep after for some time, sulphonation rate is surveyed in sampling, stopped reaction after sulphonation rate keeps stablizing, obtains final fluorocarbon alcohol sulfonate surfactant.
Embodiment 4:
1): pass into N
2make protection gas and keep not interrupting, by 20kg fluorocarbon alcohol (hydroxyl value 334KOH/g), 12.84kg maleic anhydride, the disposable reactor of putting into of 32.8g tosic acid, heat to 85 ℃, keep after for some time, esterification yield is surveyed in sampling, treats the constant maleic anhydride monoesters that obtains of esterification yield;
2): in the maleic anhydride monoesters obtaining above, add 34.64kg50% sodium sulfite aqueous solution, be warmed up to 80 ℃, keep after for some time, sulphonation rate is surveyed in sampling, stopped reaction after sulphonation rate keeps stablizing, obtains final fluorocarbon alcohol sulfonate surfactant.
Claims (6)
1. a method for synthetic fluorocarbon alcohol sulfonate surfactant, is characterized in that, comprises the following steps:
1) fluorocarbon alcohol, maleic anhydride, catalyzer are put in reactor, passed into N
2make protection gas, be warmed up to 70～100 ℃, reaction 3～7h, stopped reaction after esterification yield remains unchanged, obtains maleic anhydride monoesters;
2) S-WAT is added to above-mentioned steps 1) carry out sulfonation in described maleic anhydride monoesters, keep the sampling after 60～100 ℃ of reaction for some time of still temperature to survey sulphonation rate, until sulphonation rate keep constant after stopped reaction, cooling discharging.
2. the method for a kind of synthetic fluorocarbon alcohol sulfonate surfactant according to claim 1, is characterized in that, described fluorocarbon alcohol and the mass ratio of maleic anhydride are (20～60): (20～60).
3. the method for a kind of synthetic fluorocarbon alcohol sulfonate surfactant according to claim 1, is characterized in that, described maleic anhydride and the mass ratio of S-WAT are (40～60): (40～60).
4. the method for a kind of synthetic fluorocarbon alcohol sulfonate surfactant according to claim 1, is characterized in that, the hydroxyl value scope of described fluorocarbon alcohol is 50～400mg KOH/g.
5. the method for a kind of synthetic fluorocarbon alcohol sulfonate surfactant according to claim 1, is characterized in that, described catalyzer is tosic acid, and accounts for 0.05～0.3% of all raw material total masses.
6. the method for a kind of synthetic fluorocarbon alcohol sulfonate surfactant according to claim 1, is characterized in that, described S-WAT is that massfraction is 40～60% sodium sulfite aqueous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310655650.5A CN103724236A (en) | 2013-12-06 | 2013-12-06 | Method for compounding sulphonate surface active agent by fluorocarbon alcohol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310655650.5A CN103724236A (en) | 2013-12-06 | 2013-12-06 | Method for compounding sulphonate surface active agent by fluorocarbon alcohol |
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| CN103724236A true CN103724236A (en) | 2014-04-16 |
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| CN201310655650.5A Pending CN103724236A (en) | 2013-12-06 | 2013-12-06 | Method for compounding sulphonate surface active agent by fluorocarbon alcohol |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104212652A (en) * | 2014-09-05 | 2014-12-17 | 东莞市长安东阳光铝业研发有限公司 | Glass cleaning agent |
| CN112759537A (en) * | 2020-12-18 | 2021-05-07 | 广东方中高新材料有限公司 | Novel synthesis method of fluorosulfonate surfactant |
-
2013
- 2013-12-06 CN CN201310655650.5A patent/CN103724236A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 姚志钢等: "双子表面活性剂———二元醇双琥珀酸双酯磺酸钠（FMI-01）的合成与性能研究", 《精细化工》 * |
| 邹祥龙等: "异辛基正丁基琥珀酸双酯磺酸钠的合成", 《化学试剂》 * |
| 陈银丰等: "氟碳阴离子表面活性剂的合成与性能", 《应用化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104212652A (en) * | 2014-09-05 | 2014-12-17 | 东莞市长安东阳光铝业研发有限公司 | Glass cleaning agent |
| CN112759537A (en) * | 2020-12-18 | 2021-05-07 | 广东方中高新材料有限公司 | Novel synthesis method of fluorosulfonate surfactant |
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Application publication date: 20140416 |