CN107252660A - A kind of preparation method of imidazoles surfactant - Google Patents
A kind of preparation method of imidazoles surfactant Download PDFInfo
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- CN107252660A CN107252660A CN201710475394.XA CN201710475394A CN107252660A CN 107252660 A CN107252660 A CN 107252660A CN 201710475394 A CN201710475394 A CN 201710475394A CN 107252660 A CN107252660 A CN 107252660A
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- imidazoles
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Abstract
This application discloses a kind of preparation method of imidazoles surfactant, comprise the following steps:Imidazoles, chloroform, dimethyl sulfoxide (DMSO) are added in a kettle., stirred using high speed machine agitator, add KOH solution, water is divided to be back to anhydrous generation, temperature of reaction kettle is promoted to 105 DEG C, stirs while add dibromobutane, filtrate is placed in and is stored at room temperature, white crystal is obtained, it is standby；White crystal is put into ethanol,aldehyde free, is added dropwise after butanone, magnetic agitation and stands under the protection of inert gas, after after slurries completely gelatinization, addition NaCl solution cyclic washing is removed and dried under butanone, vacuum condition, that is, the imidazoles surfactant is made.Thus, the method synthesis step is few, and product characterizes structure by proton nmr spectra, and poisonous acrylonitrile is used while being avoided in building-up process, environmental safety is improved, and environment-friendly type of the imidazoles surfactant in fields such as oilfield chemicals, which expands application, also has certain reference.
Description
Technical field
The present invention relates to a kind of preparation method of surfactant, more particularly to a kind of preparation side of imidazoles surfactant
Method.
Background technology
Surfactant refers to add the material that the interface state of its solution system can be made to occur significant change on a small quantity.Have
Fixed hydrophilic lipophilic group, can be aligned on the surface of solution.The molecular structure of surfactant has amphipathic：One end
For hydrophilic radical, the other end is hydrophobic grouping；Hydrophilic radical is often polar group, such as carboxylic acid, sulfonic acid, sulfuric acid, amino or amido
And its salt, hydroxyl, amide groups, ehter bond etc. can also be used as polar hydrophilic group；And hydrophobic grouping is often nonpolar hydrocarbon chain, such as 8
Carbon atom above hydrocarbon chain.Surfactant is divided into ionic surfactant, nonionic surface active agent, amophoteric surface active
Agent, compound surfactant, other surfaces activating agent etc..
The content of the invention
It is an object of the invention to provide a kind of preparation method of surfactant, comprise the following steps:
Step one：In a kettle. add imidazoles, chloroform, dimethyl sulfoxide (DMSO), using high speed machine agitator with
3000r/min speed stirs 10-15m, adds 65% KOH solution, and point water is back to anhydrous generation, by temperature of reaction kettle
105 DEG C are promoted to, stirs while add dibromobutane, dimethyl sulfoxide (DMSO) is distilled off, filtrate is placed in and is stored at room temperature 13-
15h, obtains white crystal, standby.
Step 2：By in obtained white crystal input ethanol,aldehyde free in step one, inert gas is subsequently passed, in inertia
It is added dropwise after completion of dropping in butanone, 1.5h, magnetic agitation 8m and stands under the protection of gas, after after slurries completely gelatinization, adds
NaCl solution cyclic washing removes and dries 5-7h under butanone, vacuum condition, that is, the imidazoles surfactant is made.
In one embodiment：Temperature is not above 110 DEG C when dibromobutane stirring is added in the step one.
In one embodiment：White solid need to be recrystallized three times in the step one.
In one embodiment：Inert gas is one kind in helium, neon or argon gas in the step 2.
A kind of preparation method of imidazoles surfactant of the present invention, the method synthesis step is few, and product is common by nuclear-magnetism
The hydrogen stave that shakes levies structure, while being avoided in building-up process using poisonous acrylonitrile, environmental safety is improved, imidazoles
Environment-friendly type of the surfactant in fields such as oilfield chemicals, which expands application, also has certain reference.
Embodiment
The present invention is described in further detail below by embodiment.
Embodiment 1：
A kind of preparation method of imidazoles surfactant, comprises the following steps:
Step one：In a kettle. add imidazoles, chloroform, dimethyl sulfoxide (DMSO), using high speed machine agitator with
3000r/min speed stirs 35m, adds 65% KOH solution, and point water is back to anhydrous generation, and temperature of reaction kettle is carried
105 DEG C are risen to, stirs while add dibromobutane, dimethyl sulfoxide (DMSO) is distilled off, filtrate is placed in and is stored at room temperature 20h,
White crystal is obtained, it is standby.
Step 2：By in obtained white crystal input ethanol,aldehyde free in step one, inert gas is subsequently passed, in inertia
It is added dropwise after completion of dropping in butanone, 1.5h, magnetic agitation 8m and stands under the protection of gas, after after slurries completely gelatinization, adds
NaCl solution cyclic washing removes and dries 7h under butanone, vacuum condition, that is, the imidazoles surfactant is made.
Wherein, temperature is not above 110 DEG C when dibromobutane stirring is added in the step one.
Wherein：White solid need to be recrystallized three times in the step one.
Wherein：Inert gas is one kind in helium, neon or argon gas in the step 2.
Embodiment 2：
A kind of preparation method of imidazoles surfactant, comprises the following steps:
Step one：In a kettle. add imidazoles, chloroform, dimethyl sulfoxide (DMSO), using high speed machine agitator with
3000r/min speed stirs 55m, adds 65% KOH solution, and point water is back to anhydrous generation, and temperature of reaction kettle is carried
105 DEG C are risen to, stirs while add dibromobutane, dimethyl sulfoxide (DMSO) is distilled off, filtrate is placed in and is stored at room temperature 23h,
White crystal is obtained, it is standby.
Step 2：By in obtained white crystal input ethanol,aldehyde free in step one, inert gas is subsequently passed, in inertia
It is added dropwise after completion of dropping in butanone, 1.5h, magnetic agitation 8m and stands under the protection of gas, after after slurries completely gelatinization, adds
NaCl solution cyclic washing removes and dries 12h under butanone, vacuum condition, that is, the imidazoles surfactant is made.
Wherein, temperature is not above 110 DEG C when dibromobutane stirring is added in the step one.
Wherein：White solid need to be recrystallized three times in the step one.
Wherein：Inert gas is one kind in helium, neon or argon gas in the step 2.
Embodiment 3：
A kind of preparation method of imidazoles surfactant, comprises the following steps:
Step one：In a kettle. add imidazoles, chloroform, dimethyl sulfoxide (DMSO), using high speed machine agitator with
3000r/min speed stirs 60m, adds 65% KOH solution, and point water is back to anhydrous generation, and temperature of reaction kettle is carried
105 DEG C are risen to, stirs while add dibromobutane, dimethyl sulfoxide (DMSO) is distilled off, filtrate is placed in and is stored at room temperature 34h,
White crystal is obtained, it is standby.
Step 2：By in obtained white crystal input ethanol,aldehyde free in step one, inert gas is subsequently passed, in inertia
It is added dropwise after completion of dropping in butanone, 1.5h, magnetic agitation 12m and stands under the protection of gas, after after slurries completely gelatinization, adds
NaCl solution cyclic washing removes and dries 6h under butanone, vacuum condition, that is, the imidazoles surfactant is made.
Wherein, temperature is not above 110 DEG C when dibromobutane stirring is added in the step one.
Wherein：White solid need to be recrystallized three times in the step one.
Wherein：Inert gas is one kind in helium, neon or argon gas in the step 2.
Embodiment 4：
A kind of preparation method of imidazoles surfactant, comprises the following steps:
Step one：In a kettle. add imidazoles, chloroform, dimethyl sulfoxide (DMSO), using high speed machine agitator with
3000r/min speed stirs 29m, adds 65% KOH solution, and point water is back to anhydrous generation, and temperature of reaction kettle is carried
105 DEG C are risen to, stirs while add dibromobutane, dimethyl sulfoxide (DMSO) is distilled off, filtrate is placed in and is stored at room temperature 14h,
White crystal is obtained, it is standby.
Step 2：By in obtained white crystal input ethanol,aldehyde free in step one, inert gas is subsequently passed, in inertia
It is added dropwise after completion of dropping in butanone, 1.5h, magnetic agitation 8m and stands under the protection of gas, after after slurries completely gelatinization, adds
NaCl solution cyclic washing removes and dries 10h under butanone, vacuum condition, that is, the imidazoles surfactant is made.
Wherein, temperature is not above 110 DEG C when dibromobutane stirring is added in the step one.
Wherein：White solid need to be recrystallized three times in the step one.
Wherein：Inert gas is one kind in helium, neon or argon gas in the step 2.
Described above is only one embodiment of the present invention, it is noted that to those skilled in the art,
Without departing from the concept of the premise of the invention, some similar modification and improvement can also be made, these also should be regarded as this
Within the protection domain of invention.
Claims (4)
1. a kind of preparation method of imidazoles surfactant, it is characterised in that comprise the following steps:
Step one：Imidazoles, chloroform, dimethyl sulfoxide (DMSO) are added in a kettle., using high speed machine agitator with 3000r/
Min speed stirs 25-70m, adds 65% KOH solution, and point water is back to anhydrous generation, and temperature of reaction kettle is promoted to
105 DEG C, stir while add dibromobutane, dimethyl sulfoxide (DMSO) is distilled off, filtrate is placed in and is stored at room temperature 13-46h, obtains
It is standby to white crystal.
Step 2：By in obtained white crystal input ethanol,aldehyde free in step one, inert gas is subsequently passed, in inert gas
Protection under be added dropwise after completion of dropping in butanone, 1.5h, magnetic agitation 8m stand, after slurries completely gelatinization after, add NaCl it is molten
Liquid cyclic washing removes and dries 5-13h under butanone, vacuum condition, that is, the imidazoles surfactant is made.
2. a kind of preparation method of imidazoles surfactant according to claim 1, it is characterised in that：In the step one
Temperature is not above 110 DEG C when adding dibromobutane stirring.
3. a kind of preparation method of imidazoles surfactant according to claim 1, it is characterised in that：In the step one
White solid need to be recrystallized three times.
4. a kind of preparation method of imidazoles surfactant according to claim 1, it is characterised in that：In the step 2
Inert gas is one kind in helium, neon or argon gas.
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| CN201710475394.XA CN107252660A (en) | 2017-06-21 | 2017-06-21 | A kind of preparation method of imidazoles surfactant |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102943086A (en) * | 2012-10-22 | 2013-02-27 | 山东大学 | Application of cationic imidazole Gemini surfactant [Cn-s-Cnim]Br2 in gene transfection |
| CN105669882A (en) * | 2014-11-18 | 2016-06-15 | 北京化工大学 | Azonium-ionized poly(styrene-b-isobutylene-b-styrene) triblock copolymer and preparation method thereof |
| US20170066717A1 (en) * | 2014-02-21 | 2017-03-09 | Inventiva | New phenylazetidinecarboxylate or -carboxamide compounds |
-
2017
- 2017-06-21 CN CN201710475394.XA patent/CN107252660A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102943086A (en) * | 2012-10-22 | 2013-02-27 | 山东大学 | Application of cationic imidazole Gemini surfactant [Cn-s-Cnim]Br2 in gene transfection |
| US20170066717A1 (en) * | 2014-02-21 | 2017-03-09 | Inventiva | New phenylazetidinecarboxylate or -carboxamide compounds |
| CN105669882A (en) * | 2014-11-18 | 2016-06-15 | 北京化工大学 | Azonium-ionized poly(styrene-b-isobutylene-b-styrene) triblock copolymer and preparation method thereof |
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Application publication date: 20171017 |
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