CN104028163A - Method for synthesizing cardanol quaternary ammonium surfactant - Google Patents
Method for synthesizing cardanol quaternary ammonium surfactant Download PDFInfo
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- CN104028163A CN104028163A CN201410284316.8A CN201410284316A CN104028163A CN 104028163 A CN104028163 A CN 104028163A CN 201410284316 A CN201410284316 A CN 201410284316A CN 104028163 A CN104028163 A CN 104028163A
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- cardanol
- anacardol
- quaternary ammonium
- formula ratio
- gta
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Abstract
The invention discloses a method for synthesizing a cardanol quaternary ammonium surfactant. According to the technical scheme, the method comprises the following steps: introducing trimethylamine gas into epoxy chloropropane in a formula amount for reacting, immediately performing suction filtration after the reaction is ended, and washing products through acetone, wherein white crystal epoxypropyl trimethyl ammonium chloride subjected to vacuum drying is called GTA for short; by taking ethanol as a solvent, adding cardanol and GTA into a three-necked flask, heating, stirring for reacting, and performing rotary evaporation to remove the solvent ethanol after the reaction is ended, thereby obtaining a coarse product of the cardanol quaternary ammonium surfactant; and washing the coarse product for several times by acetone, removing raw materials which are not completely reacted, recrystallizing by petroleum ether, and drying in a vacuum drying box, thereby obtaining a faint yellow solid, namely the pure cardanol quaternary ammonium surfactant. The method has the beneficial effects that cardanol serving as a main raw material is a readily available and low-price renewable resource, and the cardanol quaternary ammonium surfactant is safe, green, high in functionality, high in chemical stability and particularly high in surface activity.
Description
Technical field
The present invention relates to technical field of surfactant, relate in particular to the synthetic method of anacardol quaternary surfactant.
Background technology
Surfactant, as an important class of fine chemicals industry, is widely used in the filed of daily-use chemical industry such as washing agent, cosmetics.Soap is to use one of surfactant the earliest, and soap runs into hard water can produce precipitation, and unstable in acid solution.Chilli oil is castor oil sulfating product, be first synthetic surfactant, in succession occurred afterwards various synthetic surfactants, especially along with the development of petrochemical industry, add the synthetic detergent of various auxiliary agents and improvement production technology, start application in producing and living in a large number.From development trend, surfactant more and more tends to the product of ecological safety, non-environmental-pollution, biodegradation safety.
Summary of the invention
The object of this invention is to provide the synthetic method of a kind of green non-pollution, with low cost, the good anacardol quaternary surfactant of surface-active.
To achieve these goals, technical scheme of the present invention is achieved in that the synthetic method of anacardol quaternary surfactant, and mole component and the production operation step of its each composition of filling a prescription are as follows:
Title molar constituent
Epoxychloropropane 5-20 part
Trimethylamine 2-4 part
Ethanol 29-70 part
Anacardol 6-34 part
Benzinum 5-20 part.
1, the described epoxychloropropane that takes formula ratio is put into 200ml and is placed in the there-necked flask of ice-water bath, under magnetic agitation, pass into the trimethylamine gas of formula ratio, time is controlled at 1.5-2h, continue to react the water-bath of 30min recession deicing in ice-water bath, then at 20 DEG C, continue to stir 4h, suction filtration immediately after reaction finishes, and with acetone washed product, vacuum drying white crystal epoxypropyltrimethylchloride chloride, is called for short GTA;
2, the described ethanol that measures formula ratio is solvent, taking the anacardol of formula ratio and above-mentioned steps 1 gained GTA adds and in there-necked flask, is warming up to 65-80 DEG C, constant temperature stirring reaction 5-7h, after reaction finishes, revolve to steam and remove etoh solvent, obtain brownish red thick liquid, be the crude product of anacardol quaternary surfactant;
3, by above-mentioned crude product through acetone washing for several times, remove unreacted raw material completely, then with benzinum recrystallization, be placed in vacuum drying chamber dry, obtain faint yellow solid, be anacardol quaternary surfactant sterling.
The present invention has following beneficial effect: primary raw material of the present invention adopts anacardol---a kind of abundant, cheap renewable resource, finished product safe green, functional strong, chemical stability is good, especially surface-active is better.
Detailed description of the invention
Embodiment 1:
The synthetic method of the present embodiment anacardol quaternary surfactant, mole component and the production operation step of its each composition of filling a prescription are as follows:
Title molar constituent
20 parts of epoxychloropropane
4 parts of trimethylamines
65 parts of ethanol
6 parts of anacardols
5 parts of benzinums.
1, the described epoxychloropropane that takes formula ratio is put into 200ml and is placed in the there-necked flask of ice-water bath, under magnetic agitation, pass into the trimethylamine gas of formula ratio, time is controlled at 1.5h, continue to react the water-bath of 30min recession deicing in ice-water bath, then at 20 DEG C, continue to stir 4h, suction filtration immediately after reaction finishes, and with acetone washed product, vacuum drying white crystal epoxypropyltrimethylchloride chloride, is called for short GTA;
2, the described ethanol that measures formula ratio is solvent, taking the anacardol of formula ratio and above-mentioned steps 1 gained GTA adds in there-necked flask and is warming up to 65 DEG C, constant temperature stirring reaction 5h, after reaction finishes, revolve to steam and remove etoh solvent, obtain brownish red thick liquid, be the crude product of anacardol quaternary surfactant;
3, by above-mentioned crude product through acetone washing for several times, remove unreacted raw material completely, then with benzinum recrystallization, be placed in vacuum drying chamber dry, obtain faint yellow solid, be anacardol quaternary surfactant sterling.
Embodiment 2:
The synthetic method of anacardol quaternary surfactant, mole component and the production operation step of its each composition of filling a prescription are as follows:
Title molar constituent
5 parts of epoxychloropropane
2 parts of trimethylamines
70 parts of ethanol
6 parts of anacardols
17 parts of benzinums.
1, the described epoxychloropropane that takes formula ratio is put into 200ml and is placed in the there-necked flask of ice-water bath, under magnetic agitation, pass into the trimethylamine gas of formula ratio, time is controlled at 2h, continue to react the water-bath of 30min recession deicing in ice-water bath, then at 20 DEG C, continue to stir 4h, suction filtration immediately after reaction finishes, and with acetone washed product, vacuum drying white crystal epoxypropyltrimethylchloride chloride, is called for short GTA;
2, the described ethanol that measures formula ratio is solvent, taking the anacardol of formula ratio and above-mentioned steps 1 gained GTA adds in there-necked flask and is warming up to 70 DEG C, constant temperature stirring reaction 6h, after reaction finishes, revolve to steam and remove etoh solvent, obtain brownish red thick liquid, be the crude product of anacardol quaternary surfactant;
3, by above-mentioned crude product through acetone washing for several times, remove unreacted raw material completely, then with benzinum recrystallization, be placed in vacuum drying chamber dry, obtain faint yellow solid, be anacardol quaternary surfactant sterling.
Embodiment 3:
The synthetic method of anacardol quaternary surfactant, mole component and the production operation step of its each composition of filling a prescription are as follows:
Title molar constituent
10 parts of epoxychloropropane
4 parts of trimethylamines
46 parts of ethanol
30 parts of anacardols
10 parts of benzinums.
1, the described epoxychloropropane that takes formula ratio is put into 200ml and is placed in the there-necked flask of ice-water bath, under magnetic agitation, pass into the trimethylamine gas of formula ratio, time is controlled at 2h, continue to react the water-bath of 30min recession deicing in ice-water bath, then at 20 DEG C, continue to stir 4h, suction filtration immediately after reaction finishes, and with acetone washed product, vacuum drying white crystal epoxypropyltrimethylchloride chloride, is called for short GTA;
2, the described ethanol that measures formula ratio is solvent, taking the anacardol of formula ratio and above-mentioned steps 1 gained GTA adds in there-necked flask and is warming up to 80 DEG C, constant temperature stirring reaction 7h, after reaction finishes, revolve to steam and remove etoh solvent, obtain brownish red thick liquid, be the crude product of anacardol quaternary surfactant;
3, by above-mentioned crude product through acetone washing for several times, remove unreacted raw material completely, then with benzinum recrystallization, be placed in vacuum drying chamber dry, obtain faint yellow solid, be anacardol quaternary surfactant sterling.
Finally explanation is, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, other amendments that those of ordinary skill in the art make technical scheme of the present invention or be equal to replacement, only otherwise depart from the spirit and scope of technical solution of the present invention, all should be encompassed in the middle of claim scope of the present invention.
Claims (2)
1. the synthetic method of anacardol quaternary surfactant, is characterized in that, mole component and the production operation step of its each composition of filling a prescription are as follows:
Title molar constituent
Epoxychloropropane 5-20 part
Trimethylamine 2-4 part
Ethanol 29-70 part
Anacardol 6-34 part
Benzinum 5-20 part.
The described epoxychloropropane that 2.(1) takes formula ratio is put into 200ml and is placed in the there-necked flask of ice-water bath, under magnetic agitation, pass into the trimethylamine gas of formula ratio, time is controlled at 1.5-2h, continue to react the water-bath of 30min recession deicing in ice-water bath, then at 20 DEG C, continue to stir 4h, suction filtration immediately after reaction finishes, and with acetone washed product, vacuum drying white crystal epoxypropyltrimethylchloride chloride, is called for short GTA;
(2) the described ethanol that measures formula ratio is solvent, taking the anacardol of formula ratio and above-mentioned steps (1) gained GTA adds and in there-necked flask, is warming up to 65-80 DEG C, constant temperature stirring reaction 5-7h, after reaction finishes, revolve to steam and remove etoh solvent, obtain brownish red thick liquid, be the crude product of anacardol quaternary surfactant;
(3) by above-mentioned crude product through acetone washing for several times, remove unreacted raw material completely, then with benzinum recrystallization, be placed in vacuum drying chamber dry, obtain faint yellow solid, be anacardol quaternary surfactant sterling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410284316.8A CN104028163A (en) | 2014-06-24 | 2014-06-24 | Method for synthesizing cardanol quaternary ammonium surfactant |
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| CN201410284316.8A CN104028163A (en) | 2014-06-24 | 2014-06-24 | Method for synthesizing cardanol quaternary ammonium surfactant |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105817176A (en) * | 2016-03-25 | 2016-08-03 | 黑龙江幸福人生物合成树脂科技开发有限公司 | Quaternary ammonium salt surface active agent and preparation method thereof |
| CN111690476A (en) * | 2020-06-22 | 2020-09-22 | 王智勇 | Special cleaning agent for garbage can and preparation method thereof |
| CN114957648A (en) * | 2021-07-28 | 2022-08-30 | 上海物竞化工科技有限公司 | Preparation method and application of cardanol polyoxyethylene ammonium sulfonate surfactant |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2434613A1 (en) * | 2001-02-13 | 2002-08-22 | Schlumberger Canada Limited | Viscoelastic compositions |
| CN102824876A (en) * | 2012-09-11 | 2012-12-19 | 上海美东生物材料有限公司 | Anacardol cationic surface active agent and preparation method thereof |
-
2014
- 2014-06-24 CN CN201410284316.8A patent/CN104028163A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2434613A1 (en) * | 2001-02-13 | 2002-08-22 | Schlumberger Canada Limited | Viscoelastic compositions |
| CN102824876A (en) * | 2012-09-11 | 2012-12-19 | 上海美东生物材料有限公司 | Anacardol cationic surface active agent and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 卢珍仙: "季铵型高取代阳离子淀粉的合成", 《湖北化工》 * |
| 沈国鹏等: "新型腰果酚季铵盐型表面活性剂的合成及表面性能研究", 《林产化学与工业》 * |
| 沈国鹏等: "新型腰果酚季铵盐型表面活性剂的合成及表面性能研究", 《林产化学与工业》, vol. 33, no. 3, 30 June 2013 (2013-06-30), pages 13 - 16 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105817176A (en) * | 2016-03-25 | 2016-08-03 | 黑龙江幸福人生物合成树脂科技开发有限公司 | Quaternary ammonium salt surface active agent and preparation method thereof |
| CN105817176B (en) * | 2016-03-25 | 2017-06-16 | 黑龙江幸福人生物合成树脂科技开发有限公司 | Quaternary ammonium salt surface active agent and preparation method thereof |
| CN111690476A (en) * | 2020-06-22 | 2020-09-22 | 王智勇 | Special cleaning agent for garbage can and preparation method thereof |
| CN114957648A (en) * | 2021-07-28 | 2022-08-30 | 上海物竞化工科技有限公司 | Preparation method and application of cardanol polyoxyethylene ammonium sulfonate surfactant |
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Application publication date: 20140910 |