CN107641104A - The preparation method of the methylimidazole villaumite ionic liquid of 1 ethyl 3 - Google Patents
The preparation method of the methylimidazole villaumite ionic liquid of 1 ethyl 3 Download PDFInfo
- Publication number
- CN107641104A CN107641104A CN201711190354.7A CN201711190354A CN107641104A CN 107641104 A CN107641104 A CN 107641104A CN 201711190354 A CN201711190354 A CN 201711190354A CN 107641104 A CN107641104 A CN 107641104A
- Authority
- CN
- China
- Prior art keywords
- sealing
- water
- reactor
- ethyl
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Cosmetics (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention belongs to ionic liquid preparing technical field, is related to a kind of preparation method of the methylimidazole villaumite ionic liquid of 1 ethyl 3, comprises the following steps：N methylimidazoles are first added into sealing reactor, then sealing reactor is alternately vacuumized, inflated with nitrogen, vacuumized, are repeated 2 ~ 3 times, it is negative pressure to make sealing reacting kettle inner pressure；Chloroethanes is added into sealing reactor, is stirred, it is first that the hot water that water temperature is 60 DEG C is passed through into water-bath interlayer, it is changed to be passed through the hot water that water temperature is 75 DEG C into water-bath interlayer after 3h, the control of sealing reacting kettle inner pressure is in below 5MPa, reaction 24h；After reaction terminates, pressure release, ethyl acetate is injected into sealing reactor, is cooled to room temperature, centrifuges, obtains the methylimidazole villaumite ionic liquid of 1 ethyl 3, be immediately placed in aluminium foil bag, sealing preserves.The preparation method of the present invention effectively prevent the influence of air in reactor, improves the purity of yield and product, has ensured safety in production.
Description
Technical field
The invention belongs to ionic liquid preparing technical field, is related to a kind of 1- ethyl-3-methylimidazoles chloride salt ions liquid
Preparation method.
Background technology
The material being made up of ion being in a liquid state at a temperature of room temperature or near room temperature, referred to as ionic liquid at room temperature, abbreviation
Ionic liquid.Ionic liquid can be divided into according to the difference of organic cation by four classes, be imidazole salt, pyridine salt, season respectively
Ammonium salt class and quaternary phosphonium salt.
1- ethyl-3-methylimidazole villaumites（1-Ethyl-3-methylimidazolium Chloride）It is a kind of imidazoles
Salt, outward appearance are as follows for white or faint yellow solid, its structural formula：, it is soluble in water, two
Chloromethanes, ethanol, acetonitrile etc., insoluble in ethyl acetate, ether and alkane etc., it is mainly used in dissolving cellulose, electrolyte adds
Add agent etc..
1- ethyl-3-methylimidazoles villaumite is typically anti-in a suitable solvent by N- alkyl imidazoles and alkyl salt or halogenated hydrocarbons
Direct one-step synthesis is answered to obtain.But it is usually the temperature-pressure reaction that directly feeds, or lead to an inert gas and protected
Production, the so presence due to air in reactor may result in material oxidation jaundice, temperature shakiness, and products obtained therefrom moisture is inclined
Height, purity are relatively low, do not meet requirement.In addition, reactor is heated up using oil bath heating, easily make temperature in the kettle not easily-controllable
Make and produce temperature runaway phenomenon, cause that temperature of charge is too high, hypertonia in kettle, and then influence product quality or bring generation uneasy
Total factor.
The content of the invention
It is an object of the invention to provide a kind of preparation method of 1- ethyl-3-methylimidazoles chloride salt ions liquid, effectively
The influence of air in reactor is avoided, improves the purity of yield and product, has ensured safety in production.
To achieve the above object, the present invention uses following technical scheme：
The present invention provides a kind of preparation method of 1- ethyl-3-methylimidazoles chloride salt ions liquid, comprises the following steps：
Step 1：First to sealing reactor in add N- methylimidazoles, then to sealing reactor alternately vacuumize, inflated with nitrogen,
Vacuumize, repeat 2 ~ 3 times, it is negative pressure to make sealing reacting kettle inner pressure；Water-bath interlayer is provided with the outside of the sealing reactor；
Step 2：Chloroethanes is added into sealing reactor, is stirred, the hot water that water temperature is 60 DEG C, 3h are first passed through into water-bath interlayer
It is changed to be passed through the hot water that water temperature is 75 DEG C into water-bath interlayer afterwards, the control of sealing reacting kettle inner pressure is in below 5MPa, reaction
24h；The mass ratio of the N- methylimidazoles and chloroethanes is 1：1；
Step 3：After reaction terminates, pressure release, inject ethyl acetate into sealing reactor, slow cooling to room temperature, be transferred to from
Scheming centrifuges 5 ~ 10min in 500r/min, obtains the methylimidazole villaumite ionic liquid of 1- ethyls -3, is immediately placed in aluminium foil bag, seals
Mouth preserves.
Further, cold water is passed through into water-bath interlayer described in step 2 makes sealing reactor temperature be no more than 80 DEG C.
Further, the methylimidazole villaumite ion of 1- ethyls -3 is washed while centrifugation described in step 3 with ethyl acetate
Liquid.
Compared with prior art, the beneficial effects of the present invention are：
1. the present invention preparation method before raw material chloroethanes is added, to seal reactor alternately vacuumize, inflated with nitrogen,
Vacuumize, air in reactor is eliminated, adds unstrpped gas, so as to effectively prevent the influence of air in reactor, carry
The high purity of yield and product.
2. the present invention has made oil bath heating of the prior art into heating water bath, water bath heating temperature holds temperature in the kettle
It is easy to control, also can be fast by being passed through the method for cold water or the logical hot water of pause to water-bath interlayer if temperature runaway phenomenon occurs in reactor
Speed cools to reactor, in addition, the maximum pressure in course of reaction is reduced to below 5MPa, improves safety coefficient, ensures
Safety in production.
Embodiment
Following examples are used to illustrate the present invention, but are not used to limit protection scope of the present invention.It is unless otherwise specified, real
Apply the conventional meanses that technological means used is well known to those skilled in the art in example.Test method in following embodiments, such as
It is conventional method without special instruction.
Embodiment 1
A kind of preparation method of 1- ethyl-3-methylimidazoles chloride salt ions liquid, comprises the following steps：
Step 1：15kg N- methylimidazoles are first added into sealing reactor, then sealing reactor is alternately vacuumized,
Inflated with nitrogen, vacuumize, repeat 2 ~ 3 times, sealing reacting kettle inner pressure is reached below -0.08MPa when vacuumizing, make during inflated with nitrogen
Sealing reacting kettle inner pressure is 0MPa, and it is negative pressure that sealing reacting kettle inner pressure is made when vacuumizing for the last time；The sealing reaction
Water-bath interlayer is provided with the outside of kettle.
Step 2：15kg chloroethanes is added into sealing reactor, starts to stir, being first passed through water temperature into water-bath interlayer is
60 DEG C of hot water, it is changed to after 3h be passed through the hot water that water temperature is 75 DEG C into water-bath interlayer.If sealing reactor temperature rose
It hurry up, logical hot water can be suspended or cold water cooling is passed through into water-bath interlayer, sealing reactor temperature is no more than 80 DEG C, sealing is anti-
Stress control is answered in kettle to react 24h in 3.6MPa.
Step 3：After reaction terminates, pressure release, the injection 12kg ethyl acetate into sealing reactor, slow cooling to room temperature,
It is transferred to centrifuge and washs the methylimidazole of 1- ethyls -3 with 5kg ethyl acetate while 500r/min 5 ~ 10min of centrifugation, centrifugation
Chloride salt ions liquid, 1- ethyl-3-methylimidazole chloride salt ions liquid is finally given, be immediately placed in aluminium foil bag, sealing preserves.
The yield of gained 1- ethyl-3-methylimidazole chloride salt ions liquid is 90.4%, and product purity reaches more than 99%.
Embodiment 2
A kind of preparation method of 1- ethyl-3-methylimidazoles chloride salt ions liquid, comprises the following steps：
Step 1：15kg N- methylimidazoles are first added into sealing reactor, then sealing reactor is alternately vacuumized,
Inflated with nitrogen, vacuumize, repeat 2 ~ 3 times, sealing reacting kettle inner pressure is reached below -0.08MPa when vacuumizing, make during inflated with nitrogen
Sealing reacting kettle inner pressure is 0MPa, and it is negative pressure that sealing reacting kettle inner pressure is made when vacuumizing for the last time；The sealing reaction
Water-bath interlayer is provided with the outside of kettle.
Step 2：15kg chloroethanes is added into sealing reactor, starts to stir, being first passed through water temperature into water-bath interlayer is
60 DEG C of hot water, it is changed to after 3h be passed through the hot water that water temperature is 75 DEG C into water-bath interlayer.If sealing reactor temperature rose
It hurry up, logical hot water can be suspended or cold water cooling is passed through into water-bath interlayer, sealing reactor temperature is no more than 80 DEG C, sealing is anti-
Stress control is answered in kettle to react 24h in 5MPa.
Step 3：After reaction terminates, pressure release, the injection 12kg ethyl acetate into sealing reactor, slow cooling to room temperature,
It is transferred to centrifuge and washs the methylimidazole of 1- ethyls -3 with 8kg ethyl acetate while 500r/min 5 ~ 10min of centrifugation, centrifugation
Chloride salt ions liquid, 1- ethyl-3-methylimidazole chloride salt ions liquid is finally given, be immediately placed in aluminium foil bag, sealing preserves.
The yield of gained 1- ethyl-3-methylimidazole chloride salt ions liquid is 91.5%, and product purity reaches more than 99%.
Embodiment described above, simply presently preferred embodiments of the present invention, only to explain the present invention, is not limited
The scope of the present invention processed, to those of ordinary skill in the art, certainly can be according to skill disclosed in this specification
Art content, make other embodiments easily by way of replacing or changing, thus it is all in principle and technique bar of the invention
Changes and improvements that part is done etc., it all should be included in scope of the present invention patent.
Claims (3)
1. a kind of preparation method of 1- ethyl-3-methylimidazoles chloride salt ions liquid, it is characterised in that comprise the following steps：
Step 1：First to sealing reactor in add N- methylimidazoles, then to sealing reactor alternately vacuumize, inflated with nitrogen,
Vacuumize, repeat 2 ~ 3 times, it is negative pressure to make sealing reacting kettle inner pressure；Water-bath interlayer is provided with the outside of the sealing reactor；
Step 2：Chloroethanes is added into sealing reactor, is stirred, the hot water that water temperature is 60 DEG C, 3h are first passed through into water-bath interlayer
It is changed to be passed through the hot water that water temperature is 75 DEG C into water-bath interlayer afterwards, the control of sealing reacting kettle inner pressure is in below 5MPa, reaction
24h；The mass ratio of the N- methylimidazoles and chloroethanes is 1：1；
Step 3：After reaction terminates, pressure release, inject ethyl acetate into sealing reactor, slow cooling to room temperature, be transferred to from
Scheming centrifuges 5 ~ 10min in 500r/min, obtains the methylimidazole villaumite ionic liquid of 1- ethyls -3, is immediately placed in aluminium foil bag, seals
Mouth preserves.
2. the preparation method of 1- ethyl-3-methylimidazoles chloride salt ions liquid according to claim 1, it is characterised in that
Cold water is passed through into water-bath interlayer described in step 2 makes sealing reactor temperature be no more than 80 DEG C.
3. the preparation method of 1- ethyl-3-methylimidazoles chloride salt ions liquid according to claim 1, it is characterised in that
While centrifugation described in step 3 the methylimidazole villaumite ionic liquid of 1- ethyls -3 is washed with ethyl acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711190354.7A CN107641104A (en) | 2017-11-24 | 2017-11-24 | The preparation method of the methylimidazole villaumite ionic liquid of 1 ethyl 3 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711190354.7A CN107641104A (en) | 2017-11-24 | 2017-11-24 | The preparation method of the methylimidazole villaumite ionic liquid of 1 ethyl 3 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107641104A true CN107641104A (en) | 2018-01-30 |
Family
ID=61125918
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711190354.7A Pending CN107641104A (en) | 2017-11-24 | 2017-11-24 | The preparation method of the methylimidazole villaumite ionic liquid of 1 ethyl 3 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107641104A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112063544A (en) * | 2020-08-04 | 2020-12-11 | 陕西省西安植物园(陕西省植物研究所) | Ionic liquid-composite microbial inoculum system |
| CN115010668A (en) * | 2022-06-07 | 2022-09-06 | 林州市科能材料科技有限公司 | Preparation method of 1-ethyl-3-methylimidazole chloride salt |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092399A (en) * | 2007-04-11 | 2007-12-26 | 东华大学 | Method for preparing ionic liquid with anion being as ion in halogen family |
| CN101654438A (en) * | 2009-08-14 | 2010-02-24 | 河南利华制药有限公司 | Imidazole ionic liquid production technology |
| CN102351796A (en) * | 2011-08-23 | 2012-02-15 | 林州市科能材料科技有限公司 | Production process of imidazole ionic liquid |
-
2017
- 2017-11-24 CN CN201711190354.7A patent/CN107641104A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092399A (en) * | 2007-04-11 | 2007-12-26 | 东华大学 | Method for preparing ionic liquid with anion being as ion in halogen family |
| CN101654438A (en) * | 2009-08-14 | 2010-02-24 | 河南利华制药有限公司 | Imidazole ionic liquid production technology |
| CN102351796A (en) * | 2011-08-23 | 2012-02-15 | 林州市科能材料科技有限公司 | Production process of imidazole ionic liquid |
Non-Patent Citations (3)
| Title |
|---|
| 张俊: "《绿色络合催化》", 30 November 2009, 甘肃文化出版社 * |
| 张军良，郭燕文: "《有机合成实验方法》", 31 January 2011, 中国医药科技出版社 * |
| 汪多仁: "《绿色增塑剂》", 31 October 2011, 科学技术文献出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112063544A (en) * | 2020-08-04 | 2020-12-11 | 陕西省西安植物园(陕西省植物研究所) | Ionic liquid-composite microbial inoculum system |
| CN115010668A (en) * | 2022-06-07 | 2022-09-06 | 林州市科能材料科技有限公司 | Preparation method of 1-ethyl-3-methylimidazole chloride salt |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107641104A (en) | The preparation method of the methylimidazole villaumite ionic liquid of 1 ethyl 3 | |
| CN107697933B (en) | A kind of preparation method of lithium hexafluoro phosphate | |
| CN106882782B (en) | A kind of synthetic method of difluorophosphate | |
| CN113402437B (en) | Novel method for synthesizing dietary supplement melatonin | |
| CN102304139B (en) | Method for preparing 2 beta-methyl penicillanate benzhydryl dioxide | |
| CN104910178B (en) | A kind of preparation method of Piperacillin acid | |
| CN108026036A (en) | The method for preparing Guanoctine and s-triazine | |
| CN114655939B (en) | Preparation method of lithium bis (fluorosulfonyl) imide | |
| CN106632306B (en) | Unformed dextral-rabeprazole sodium and preparation method thereof | |
| CN105152976A (en) | Improved process of ethyl N-cyanoethanimideate preparation method | |
| WO2019219093A3 (en) | Preparation of zinc linoleate, and application thereof in preparing anti-helicobacter pylori drug | |
| CN107235967A (en) | The synthesis technique of antineoplastic Tegafur | |
| CN111592539A (en) | Preparation method of trifluoro-benzene pyrimidine | |
| CN102391186A (en) | Method for preparing ozagrel intermediate (E)-4-(methyl imidazolyl) methyl cinnamate | |
| CN107098855A (en) | A kind of method for preparing the quinolinone of 7 hydroxyl 2 | |
| CN106279118A (en) | One prepares the method for 2,4 diaminourea 6 [2 (2 methyl 1 imidazoles) ethyl] 1,3,5 triazines | |
| CN114835661A (en) | Industrial preparation method of a-acetyl-r-butyrolactone | |
| CN108727364A (en) | A kind of hydrobromic acid is unformed and preparation method thereof for Ge Lieting | |
| CN111217667B (en) | Synthetic method of tetrabromocyclooctane | |
| CN114181107A (en) | Synthesis method of benzyloxy amine hydrochloride | |
| CN105367391A (en) | 2-chlorine-1,1,1-trimethoxyethane preparing method | |
| CN104987300A (en) | Preparation process for cyanomethyl ester | |
| CN108546266B (en) | Synthesis method of 1,4,6, 7-tetrahydropyrane [4,3-C ] pyrazole-3-carboxylic acid | |
| CN104761500B (en) | (E) preparation method of 4 (1 imidazolmethyl) methyl cinnamates | |
| CN115010668A (en) | Preparation method of 1-ethyl-3-methylimidazole chloride salt |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180130 |
|
| RJ01 | Rejection of invention patent application after publication |