CN101851208A - Multifunctional ion liquid preparation device - Google Patents
Multifunctional ion liquid preparation device Download PDFInfo
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- CN101851208A CN101851208A CN 201010194313 CN201010194313A CN101851208A CN 101851208 A CN101851208 A CN 101851208A CN 201010194313 CN201010194313 CN 201010194313 CN 201010194313 A CN201010194313 A CN 201010194313A CN 101851208 A CN101851208 A CN 101851208A
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- ion liquid
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Abstract
The invention relates to the field of the synthesized ion liquid preparation device, in particular to a multifunctional ion liquid preparation device which can perform the large-scale continuous synthesis, purification and purity analysis, so the procedures such as the synthesis, separation purification and analysis of the ion liquid can be continuously completed, and the automatic control of the entire flow can be realized. The multifunctional ion liquid preparation device comprises a micro-channel reaction device part, a washing separation device part, a falling-film evaporation drying purification device part and a purity analysis device part, and can carry out the homogeneous chemical reaction and separation purification of the ion liquid. In the preparation device, the operations such as reaction, liquid separation, washing, crystallization, film falling purification, purity analysis and the like can be realized. The device not only is applicable to the production of different ion liquids, but also is applicable to other organic chemical reaction and product separation purification.
Description
Technical field
The invention belongs to synthetic ion liquid device preparation field, particularly relate to synthetic ion liquid microchannel reaction device part, washing separation device part, the dry purification devices part of falling film evaporation and purity check device part; This device can programme controlled continous way production, separate the purification ionic liquid and carry out its purity check.This device also can be used for other organic chemical reactions and organic separation is purified.
Background technology
Ionic liquid at room temperature (Room Temperature Ionic Liquids, RTILs) be by organic cation and organic or inorganic negatively charged ion constitute and room temperature and near be the salt of liquid body under the temperature, be called for short ionic liquid.Ionic liquid has LMP (great majority still can keep liquid state in the time of 300 ℃), low-steam pressure (volatilization hardly, nonflammable, non-explosive), wide electrochemical stability potential window, good good characteristics such as dissolution characteristics, and can regulate its physics and chemical property according to the variation of zwitterion, therefore, it is a kind of programmable that ionic liquid is considered to, the green solvent that has the novel environmental close friend of broad prospect of application in green in the synthetic and cleaner production, be widely used in every field such as catalyzed reaction and electrochemistry, promoted the development of chemical industry.
Yet present ion liquid preparation all is under lab to carry out small-scale synthetic and purification mostly, and complicated operation is wasted time and energy, and has limited ion liquid large-scale application greatly.
General chemical reactor can comprise one or more functions, " prepare ion liquid multifunctional reactor " as patent, patent publication No. is: CN1857767A relate to the ion liquid synthetic reactor that is located away from one, but this reactor needs manual operation and long reaction time.The ion liquid synthetic separating and purifying method variation that reaches as crystallization, extraction etc., still unitizes the ion liquid synthetic separating and purifying method that reaches at present, and realizes being exclusively used in ionic liquid and synthesize and separate the whole process control device of purifying.
Summary of the invention
The object of the present invention is to provide the multifunctional ion liquid preparation device that a kind of mass-producing is synthetic continuously, separate purification and purity check, steps such as ion liquid preparation, separation purification and purity check are finished continuously, and realized full-range automatic control.The invention of this device unitizes the synthetic separation method that reaches of ion liquid difference, realizes simultaneously producing with disjoint set being integral, and has reduced the production preparation cost, has solved ionic liquid mass-producing synthetic key issue.This complete equipment only needs manually raw material to be positioned over storage tank, and the setting program parameter can be got ionic liquid after the time of setting, need not manual operation, saves manpower, for ion liquid scale preparation provides foundation.
Multifunctional ion liquid preparation device of the present invention comprises microchannel reaction device part, washing separation device part, the dry purification devices of falling film evaporation and purity check device part, can carry out ion liquid homogeneous chemical reaction and separates and purify.In this preparation facilities, but operations such as realization response, separatory, washing, crystallization, falling liquid film purifying, purity check.Microchannel reaction synthesizer partly comprises charging crossing current pump, well heater, reactant preheater, micro passage reaction, reaction time delay unit, magnetic valve, temperature and pressure tester etc.; The dry purification devices of washing separation device and falling film evaporation partly comprises washing knockout tower, outer falling-film evaporator, heating or water cooler, vacuum pump, water cooler, solenoid electric valve, liquid circulation crossing current pump etc.; The purity check device partly comprises electrochemical workstation.
Multifunctional ion liquid preparation device of the present invention mainly uses the crossing current pump with the liquid form continuously feeding, in micro passage reaction, fully react, can pressurize in the micro passage reaction, normal pressure and vacuum operating, microchannel reaction raising transformation efficiency of reactant and the production rate of product, the transformation efficiency of reactant can reach more than 95%, and the reaction times is short, has reduced energy consumption.Used washing separation device is the washing tower that has the stirring arm of adjustable rotating speed, stirring arm is driven by buncher, and computer program control is arranged, according to viscosity and other requirement of reaction after product, different rotating speeds can be set, and stirring arm can be slurry formula, turbine type or anchor formula in program.The separatory operation can realize by the conductivitimeter and the magnetic valve of washing separation device below, need not to look the pipe manual operation by separatory; If after the product crystallization, in order to reach the purpose of solid-liquid separation, the liquid of top can be taken away by vacuum pump, condensation in water cooler then.The drying of product is purified mainly by falling film evaporation device part, and by the crossing current pump, product is continuable to carry out falling film evaporation, and the speed of falling film evaporation can be controlled by the flow of crossing current pump, and solvent is taken away in water cooler by vacuum pump and cooled off.
Heating of the present invention and cooling medium can be air, steam, hot water, silicone oil, cold water, ethanol according to reaction and isolating heating or cooling requirement, preferred air.
The pipeline of ion liquid preparation device of the present invention and the material of equipment can be stainless steel, enamel, pottery or inner liner polytetrafluoroethylene.
The temperature of microchannel reaction synthesizer part, washing separation device part, the dry purification devices of falling film evaporation and the purity check device part of multifunctional ion liquid preparation device of the present invention is controlled respectively, is beneficial to continuous reaction and isolating carrying out.
The working routine of multifunctional ion liquid preparation device of the present invention is by computer controlled automatic, and in computer, can call different programs arbitrarily according to different sepn processes, as ion liquid recrystallization and ion liquid washing separation etc., time in the program and input speed can freely be provided with by the operator.
The continuable synthetic different ionic liquid of the multi-functional preparation facilities of ionic liquid of the present invention, can be glyoxaline ion liquid, pyridines ionic liquid, guanidine class ionic liquid, amino functional ionic liquid, Lewis acidic ion liquid,
Acidic ion liquid, chirality function ionic liquid, hydroxyl functional ionic liquid, ester group functionalized ion liquid, thioether functionalized ion liquid, SULPHURYL CHLORIDE functionalized ion liquid, difunctionalization ionic liquid etc.
This device is not only applicable to produce different types of ionic liquid, for other organic chemical reactions and all adaptations of product separation purification.
The present invention compared with prior art, its remarkable advantage is: (1) is synthetic and separation method unitized with ion liquid difference, makes ion liquid batch production be integrated into continous way production; (2) micro passage reaction is used for ion liquid production, has improved ion liquid purity, and make the reaction times shorten to several hours, saved the time by tens hours; (3) ion liquid production and separation are integrated in one, have realized that whole process controls automatically, need not manual operation, save manpower, help large-scale industrial production.
Description of drawings
Fig. 1 is the structure flow chart that the present invention prepares ion liquid multifunctional ion liquid preparation device
Reference numeral
1-2. raw material storage tank; 3-4. washing composition storage tank; 5-6. intermediate storage tank;
7. product storage tank 8. water coolers; 9-12. crossing current pump;
13,15. heating units; 14. heating or refrigerating unit; 16,17. feed preheaters;
18. micro passage reaction; 19. reaction time delay unit; 20. washing separator;
21. outer falling-film evaporator; 22. vacuum pump; 23. electrochemical workstation;
24-26. temperature test point; 27. pressure test point 28-32. two way solenoid valve;
33-37. three-way solenoid valve;
Embodiment
See also Fig. 1, the present invention is described in further detail below in conjunction with accompanying drawing.
In conjunction with the accompanying drawings, the ion liquid synthetic and separating and purifying method of multifunctional ion liquid preparation device of the present invention adopts continuous processing, raw material A and B or corresponding aqueous solution importing raw material storage tank 1 and 2 with synthetic target product, (regulate the speed of charging according to the speed of reaction by reinforced crossing current pump 9 and 10 with the speed of setting, slow especially for reaction then with the low discharge charging) enter microchannel reaction device, regulate temperature in the device in advance, raw material is through preheating, little reaction, the time-delay reaction, enter washing separation device by T-valve 33 then, by two three-way electromagnetic valves 28 and crossing current pump 11, washing composition 1 enters washing separation device and washs separation, ionic liquid, washing composition, the aqueous solution is divided into organic ion liquid level and water layer, (or ionic liquid recrystallization in washing composition) ionic liquid organic layer below, water up, switch by automatic separatory of conductivitimeter and magnetic valve 34 imports storage tank 5 with lower floor's liquid, upper aqueous layer imports storage tank 6, if (ionic liquid recrystallization, then upper strata liquid is taken away by two three-way electromagnetic valves 30 and vacuum pump, cooling in water cooler 8), by by- pass valve control 28,32,34-36, crossing current pump 11-12, with washing composition 1 circulation cleaning several times, and then with the ionic liquid in the 2 backwash storage tanks 5 of the washing composition in the storage tank more than 4 times.Ionic liquid in the storage tank 5 and solvent 1 enter falling-film evaporator by crossing current pump 12 and carry out falling film evaporation except that desolvating 1, and ionic liquid enters the product bottle then, derives a spot of ionic liquid again and carries out the electrochemistry purity check.
Describe the synthetic ionic liquid of multifunctional ion liquid preparation device continuous processing of the present invention in detail with specific embodiment below.
Utilize multifunctional ion liquid preparation device of the present invention to prepare BmimBr
Raw material N-Methylimidazole (82.0g with synthetic BmimBr, 1.0mol) and 1-n-butyl bromide (142.0g, 1.05mol) add respectively in raw material storage tank 1 and 2, enter microchannel reaction device with the speed of 5ml/min respectively by reinforced crossing current pump 9 and 10, temperature is controlled at 70 ℃ in the device, preheating, little reaction, the time-delay reaction, enter washing separation device by T-valve 33 then, washing device is chilled to about 0 ℃ in advance, BmimBr crystallization in this device, unreacted raw material is on the upper strata, open vacuum pump and open two-way valve 30, take upper strata liquid away, open two three-way electromagnetic valves 28 and crossing current pump 11, mixed solvent (acetonitrile/ethyl acetate) is imported washing tower, BmimBr recrystallization 3 times.Heated scrub device to 60 ℃, making BmimBr is liquid, opens two three-way electromagnetic valves 32 and three-way solenoid valve 34, making BmimBr is that liquid flows into storage tank 5 (116.0g 0.83mol), derives a spot of BmimBr ionic liquid then and carries out the electrochemistry purity check.
Utilize multifunctional ion liquid preparation device of the present invention to prepare ionic liquid BmimBF
4, this synthesis step calls another program that is different from ionic liquid BmimBr.
Raw material BmimBr (219.0g, 1.0mol) aqueous solution 300mL and NaBF with synthetic BmimBF4
4(121.0g, 1.1mol) aqueous solution 300mL adds in the raw material storage tank 1 and 2, enter microchannel reaction device with the speed of 10ml/min respectively by reinforced crossing current pump 9 and 10, temperature is controlled at 60 ℃ in the device, preheating, little reaction, time-delay reaction enter washing separation device by T-valve 33 then, open mechanical stirring device, open two three-way electromagnetic valves 28 and crossing current pump 11 simultaneously, the washing composition methylene dichloride enters washing separation device with the speed of 50ml/min and carries out BmimBF
4Washing separates, and methylene dichloride charging 6min behind the restir 10min, stops mechanical stirring, separatory 5min, methylene dichloride ionic liquid BmimBF
4The layer below, water and NaBr layer are opened magnetic valve 32 up, make liquid flow through conductivitimeter, enter storage tank 5 by the three-way solenoid valve of opening 34, when the value of conductivitimeter has sudden change, three-way solenoid valve 34 is closed, upper aqueous layer enters storage tank 6, by by- pass valve control 28,32, the switch of 34-36 and crossing current pump 11-12, with methylene dichloride circulation cleaning water layer several times, and then with the ionic liquid BmimBF in the detergent water backwash storage tank 5 in the storage tank 4
4Dichloromethane layer several times, making the Br ionic content in the dichloromethane layer is zero as far as possible.Ionic liquid in the storage tank 5 and methylene dichloride enter falling-film evaporator by crossing current pump 12 with the speed of 20ml/min to carry out falling film evaporation and removes methylene dichloride, temperature is controlled at 50 ℃ in the falling film evaporation device, methylene chloride is used cooled with liquid nitrogen in water cooler, last BmimBF
4Ionic liquid enters product bottle 7 under the effect of vacuum pump (190.2g 0.85mol), derives a spot of BmimBF again
4Ionic liquid carries out the electrochemistry purity check.
Utilize multifunctional ion liquid preparation device of the present invention to prepare ionic liquid BmimPF
6
The same BmimBF of synthesis step
4Ionic liquid, just after the reaction of microchannel, ionic liquid and water stratification need not to use washed with dichloromethane, only need wash separation with water and get final product.With raw material NaBF
4The aqueous solution is replaced by KPF
6The aqueous solution.Raw material BmimBr (219.0g, 1mol) aqueous solution 300mL and KPF
6(200.3g, 1.1mol) aqueous solution 300mL get BmimPF at last
6(204.9g, 0.9mol).
Claims (6)
1. multifunctional ion liquid preparation device is characterized in that: make ion liquid synthetic, separate and purify and the purity check step is finished continuously, and realize full-range automatic control; Multifunctional ion liquid preparation device comprises microchannel reaction device part, washing separation device part, the dry purification devices part of falling film evaporation and purity check device part, can carry out ion liquid homogeneous chemical reaction and separates and purify; In this preparation facilities, but realization response, separatory, washing, crystallization, falling liquid film purifying, purity check operation.
2. multifunctional ion liquid preparation device according to claim 1 is characterized in that: microchannel reaction device partly comprises fresh feed pump, well heater, reactant preheater, micro passage reaction, reaction time delay unit, solenoid electric valve, temperature and pressure tester; The dry purification devices of washing separation device and falling film evaporation partly comprises washing knockout tower, outer falling-film evaporator, heating or water cooler, vacuum pump, solenoid electric valve, liquid circulation crossing current pump; The purity check device partly comprises electrochemical workstation.
3. multifunctional ion liquid preparation device according to claim 1 is characterized in that: the temperature of microchannel reaction device part, washing separation device part and the dry purification devices part of falling film evaporation is controlled respectively, helps reaction and isolatingly carries out in order.
4. multifunctional ion liquid preparation device according to claim 1 is characterized in that: heating and cooling medium can be air, steam, hot water, silicone oil, cold water, ethanol according to reaction and isolating heating or cooling requirement, preferred air.
5. multifunctional ion liquid preparation device according to claim 1 is characterized in that: working routine is by computer controlled automatic, and can call different programs according to different sepn processes arbitrarily in computer.
6. multifunctional ion liquid preparation device according to claim 1 is characterized in that: micro passage reaction is used for ion liquid production, and the W-response time shortened to several hours by tens hours, had saved the time.
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| CN2010101943137A CN101851208B (en) | 2010-05-28 | 2010-05-28 | Multifunctional ion liquid preparation device |
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| CN2010101943137A CN101851208B (en) | 2010-05-28 | 2010-05-28 | Multifunctional ion liquid preparation device |
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| CN101851208B CN101851208B (en) | 2012-07-25 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432541A (en) * | 2011-08-31 | 2012-05-02 | 微楷化学（大连）有限公司 | Technology for synthesizing ionic liquid |
| CN103127897A (en) * | 2013-03-08 | 2013-06-05 | 南开大学 | Synthesizer of imidazolium ionic liquids and application thereof |
| CN112705260A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Production method and device of ionic liquid catalyst |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1857767A (en) * | 2005-11-02 | 2006-11-08 | 中国科学院过程工程研究所 | Multifunctional reactor for preparing ionic liquid |
| US20090043141A1 (en) * | 2007-05-30 | 2009-02-12 | Terry Mazanec | Oxidative coupling of methane |
-
2010
- 2010-05-28 CN CN2010101943137A patent/CN101851208B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1857767A (en) * | 2005-11-02 | 2006-11-08 | 中国科学院过程工程研究所 | Multifunctional reactor for preparing ionic liquid |
| US20090043141A1 (en) * | 2007-05-30 | 2009-02-12 | Terry Mazanec | Oxidative coupling of methane |
Non-Patent Citations (4)
| Title |
|---|
| 《Chemical Engineering and Processing》 20070615 A.Renken et al. Ionic liquid synthesis in a microstructured reactor for process intensification 第46卷, 2 * |
| 《Organic Process Research & Development》 20090617 Daniel Wilms et al. Ionic Liquids on Demand in Continuous Flow 第13卷, 第5期 2 * |
| 《Organic Process Research & Development》 20090702 Faysal Benaskar et al. Intensification of the Capillary-Based Kolbe-Schmitt Synthesis from Resorcinol by Reactive Ionic Liquids,Microwave Heating,or a Combination Thereof 第13卷, 第5期 2 * |
| 《中国科学 B辑：化学》 20091231 张锁江 等 离子液体的前沿、进展及应用 第39卷, 第10期 2 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432541A (en) * | 2011-08-31 | 2012-05-02 | 微楷化学（大连）有限公司 | Technology for synthesizing ionic liquid |
| CN102432541B (en) * | 2011-08-31 | 2015-03-18 | 大连微凯化学有限公司 | Technology for synthesizing ionic liquid |
| CN103127897A (en) * | 2013-03-08 | 2013-06-05 | 南开大学 | Synthesizer of imidazolium ionic liquids and application thereof |
| CN103127897B (en) * | 2013-03-08 | 2014-05-28 | 南开大学 | Synthesizer of imidazolium ionic liquids and application thereof |
| CN112705260A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Production method and device of ionic liquid catalyst |
| CN112705260B (en) * | 2019-10-25 | 2024-03-26 | 中国石油化工股份有限公司 | Production method and device of ionic liquid catalyst |
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| CN101851208B (en) | 2012-07-25 |
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