CN1857767A - Multifunctional reactor for preparing ionic liquid - Google Patents
Multifunctional reactor for preparing ionic liquid Download PDFInfo
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- CN1857767A CN1857767A CN 200510086759 CN200510086759A CN1857767A CN 1857767 A CN1857767 A CN 1857767A CN 200510086759 CN200510086759 CN 200510086759 CN 200510086759 A CN200510086759 A CN 200510086759A CN 1857767 A CN1857767 A CN 1857767A
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Abstract
The present invention belongs to the field of ionic liquid preparing reactor, and is especially one multifunctional ionic liquid preparing reactor. The reactor is one kettle type or one horizontal reactor, which has a sandwiched reactor body with medium inlet and outlet, gaseous material inlet pipe, liquid material inlet pipe, vacuum pipe, vacuum suction filtering pipe, slurry stirring motor, temperature sensor, pressure sensor, sight glass, condensate return pipe, solid material outlet, bottom sampling port, etc. The present invention makes it possible to complete multiphase reaction or homogeneous reaction and subsequent product separation and purification, and has high reaction conversion rate, high equipment utilizing rate, less material conveying links and less impurity introduction.
Description
Technical field
The invention belongs to the ion liquid reactor of preparation field, particularly synthesize and prepare ion liquid multifunctional reactor.
Background technology
(Room Temperature Ionic Liquids RTILs) by organic cation and inorganic or organic anion constitutes, be the salt of liquid condition under near temperature room temperature or the room temperature, is called for short ionic liquid to ionic liquid at room temperature.Good characteristic such as because of having fusing point low (in room temperature often for liquid condition), steam, it forces down, not volatile, has extraordinary prospects for commercial application, application more and more widely relates to processes such as organic synthesis, extract and separate, electrochemistry, living things catalysis.
Ionic liquid all is under lab to carry out small-scale synthetic and purification, raw material costliness, complicated operation mostly at present, the cost of material height, solvent and raw material recycling poor, seriously polluted, conversion ratio low (being about 80%) therefore, has greatly limited ion liquid promotion and application.
General chemical reactor has comprised above one or several function, if any the centrifugal solid-liquid separator of special use, after crystallization is finished, transfers in the separator again and separates.Patent " multifunctional chemical reactor ", Granted publication number: the patent of CN22678564, relate to a kind of chemical experiment reactor, but can't realize direct Separation of Solid and Liquid operation at this reactor, be not exclusively used in ion liquid synthetic and preparation.
Summary of the invention
The object of the present invention is to provide the ion liquid multifunctional reactor of a kind of scale preparation, a plurality of operating in the same reactor finished, simplify technological process and operating process, improve reaction conversion ratio, raw material and energy consumption have been reduced, reduce preparation cost, solve the synthetic key issue of ionic liquid scale, for ion liquid industrial applications provides safeguard.
The ion liquid multifunctional reactor of preparation of the present invention can carry out homogeneous phase or heterogeneous phase chemical reaction, the multi-functional operation of realization response in a reactor, stirring, separatory, crystallization, washing, suction filtration, drying, be distributed with on the reactor: the outlet of solid material, the chuck medium is imported and exported, chuck, elevating lever, vacuum tube, vacuum filters pipe, the liquid feed inlet and outlet, the gas feed pipe, buncher, temperature sensor, pressure sensor, visor, the condensate liquid return duct, filter screen, stirring arm, sample tap, separatory is looked pipe; It is characterized in that:
Described reactor is still formula or horizontal reactor, and its tank body is the jacket type tank body, has the import of chuck medium on the top of chuck, and the bottom has the chuck media outlet; Top at tank body has liquid inlet opening, and vacuum tube, vacuum filtration pipe, the buncher that has stirring arm, temperature sensor, pressure sensor, visor, condensate liquid return duct are installed; Have the outlet of solid material in the bottom of tank body; Bottom at tank body has sample tap, and a separatory that has liquid outlet opening is looked pipe and is installed in the sample tap place; Be separately installed with elevating lever on the corresponding tank wall of tank body the inside, a filter screen is fixed on the elevating lever;
Gas feed pipe in the one insertion material is installed in top, middle part or the bottom of tank body.
The air inlet of described vacuum filtration pipe is more than filter screen.
Described buncher is mounted in the top of tank body, and stirring arm is below filter screen.
The bottom of described tank body further has manhole or hand hole.
Described filter screen is to be fixed on the elevating lever by clamp.
The outlet of described manhole or hand hole and solid material can be a mouth, and also opening is in addition decided on tank body size and operation requirement.
Chuck medium of the present invention can add conduction oil, steam, heat (cold) water, various freezing liquids etc. according to reaction or separation requirement, to satisfy the needs of heating, cooling.
Reactor of the present invention can pressurize, normal pressure and vacuumizing, is used for all kinds of ion liquid syntheticly,, need carry out under normal pressure during synthetic reaction in building-up process as BmimCl, then needs decompression operation when drying.Vacuum tube is installed on the reactor, can reduces pressure and pressurized operation, to satisfy reaction and the different requirements that separate; Stirring arm is loaded in the reacting tank body, is driven by buncher, and according to the viscosity and the technological requirement of material, stirring arm can adopt slurry formula, cabinet type, anchor formula or turbine type etc.; The separatory operation can be looked pipe by the transparent separatory in liquid outlet opening below and realize; In order to reach the purpose of Separation of Solid and Liquid, elevating lever is housed in the reacting tank body, the clamp that can regulate upper-lower position is housed on the bar, the filter screen of unlike material is fixed on the clamp, can regulate screen location according to the amount of solid material.
Reactor material of the present invention can be the carbon steel tank body of carbon steel, stainless steel, enamel, pottery or inner liner polytetrafluoroethylene lining.
The present invention can finish heterogeneous or homogeneous reaction in a reactor according to the particularity of ion liquid building-up process, and the separation of subsequent products and purification.Be mainly used in all kinds of ion liquid synthetic, separation, purifying; Multiple modes of operation that reactor of the present invention is integrated, comprise: pressurization, decompression, heating, cooling, stir, separatory, crystallization, suction filtration, dry, the Separation of Solid and Liquid operation, the conversion ratio and the usage ratio of equipment of reaction have been improved, reaction conversion ratio can reach more than 90%, reduced the conveying process of material, avoided the introducing of other impurity, raw material and energy consumption have been reduced, equipment investment and operating cost have been saved, reduced cost, reduced environmental pollution, solved the key issue of ionic liquid scale preparation, also provide guarantee for ion liquid industrial applications.
The solid-liquid separation that the present invention is special and liquid-liquid separating apparatus and pre-existing reactors relatively are easier to operation, and applicability is stronger, is particularly suitable for producing the ion liquid needs of many kinds.
Description of drawings
Fig. 1. the present invention prepares the structural representation of ion liquid multifunctional universal reactor.
Reference numeral
1. reative cell 2. manholes or hand hole 3. solid material outlet
4. chuck media outlet 5. chucks 6. elevating levers
7. chuck medium import 8. vacuum tubes 9. vacuum filter pipe
10. liquid inlet opening 11. gas feed pipes 12. bunchers
13. temperature sensor 14. pressure sensors 15. visors
16. condensate liquid return duct 17. filter screens 18. clamps
19. stirring arm 20. sample taps 21. separatory are looked pipe
22. liquid outlet opening
The specific embodiment
See also Fig. 1.One tank reactor, its tank body are the jacket type tank body, and the cavity of tank body is a reative cell 1, and the hollow sandwich that double-deck tank wall constitutes is a chuck 5; On chuck 5, have chuck medium import 7, the chuck bottom has chuck media outlet 4, have liquid inlet opening 10 on tank body top, and vacuum tube 8, vacuum filtration pipe 9 be installed, and the air inlet of vacuum filtration pipe more than filter screen, gas feed pipe 11, and the gas outlet of gas feed pipe within the material below the filter screen, temperature sensor 13, pressure sensor 14, visor 15, condensate liquid return duct 16; One buncher 12 that has stirring arm 19 is installed in the top of tank body, and stirring arm is below filter screen; Have manhole or hand hole 2, solid material outlet 3 in the bottom of tank body; Have separatory that sample tap 20, has a liquid outlet opening 22 looks pipe 21 and is installed in sample tap 20 places in the bottom of tank body; Being separately installed with elevating lever 6, one filter screens 17 on the corresponding tank wall of tank body the inside is fixed on the elevating lever 6 by clamp.
Utilize reactor made BmimCl of the present invention.
The raw material of synthetic BmimCl is methylimidazole and chlorobutane, with methylimidazole and chlorobutane (mol ratio 1: 1～1.7) batching by a certain percentage, add the reactor respectively from liquid inlet opening, in chuck, feed hot water as heat medium, keep the temperature of reactor to be controlled at 75～80 ℃, open buncher, feed small amount of N
2Protection refluxes and stirred 24～48 hours.After reaction was finished, the insulation standing demix was looked pipe by separatory product is separated with upper strata unreacted material, obtains the crude product of BmimCl.In thick BmimCl product, add a certain amount of ethyl acetate or other solvent as the crystallizing and washing agent, added thermal agitation 2～4 hours, in chuck, feed refrigerant in afterwards, make system temperature remain on-10 ℃～0 ℃, make the product crystallization.Regulate elevating lever, filter screen is placed correct position, clear liquid is separated by the suction filtration pipe.Cool off so repeatedly and the operation that is recrystallized, impurity content is reduced to standard in product.Open vacuum tube, under 100 ℃ of conditions, product is carried out vacuum distillation, remove a small amount of solvent, unreacting material and moisture once more, reach 99% purity requirement until product B mimCl.
Claims (7)
1. one kind can be carried out homogeneous phase or heterogeneous phase chemical reaction, and realization response, stirring, separatory, crystallization, washing, suction filtration, drying process prepare ion liquid multifunctional reactor, comprises the outlet of solid material, the chuck medium is imported and exported, chuck, elevating lever, vacuum tube, vacuum filters pipe, liquid feed inlet and outlet, gas feed pipe, buncher, temperature sensor, pressure sensor, visor, condensate liquid return duct, filter screen, stirring arm, sample tap, separatory is looked pipe; It is characterized in that:
Described reactor is still formula or horizontal reactor, and its tank body is the jacket type tank body, has the import of chuck medium on the top of chuck, and the bottom has the chuck media outlet; Top at tank body has liquid inlet opening, and vacuum tube, vacuum filtration pipe, the buncher that has stirring arm, temperature sensor, pressure sensor, visor, condensate liquid return duct are installed; Have the outlet of solid material in the bottom of tank body; Bottom at tank body has sample tap, and a separatory that has liquid outlet opening is looked pipe and is installed in the sample tap place; Be separately installed with elevating lever on the corresponding tank wall of tank body the inside, a filter screen is fixed on the elevating lever;
Gas feed pipe in the one insertion material is installed in top, middle part or the bottom of tank body.
2. reactor according to claim 1 is characterized in that: the air inlet of described vacuum filtration pipe is more than filter screen.
3. reactor according to claim 1 is characterized in that: described buncher is mounted in the top of tank body, and stirring arm is below filter screen.
4. reactor according to claim 1 is characterized in that: the bottom of described tank body has manhole or hand hole.
5. reactor according to claim 1 is characterized in that: described filter screen is to be fixed on the elevating lever by clamp.
6. reactor according to claim 1 is characterized in that: described stirring arm adopts slurry formula, cabinet type, anchor formula or turbine type.
7. reactor according to claim 1 is characterized in that: described reactor material is the carbon steel tank body of carbon steel, stainless steel, enamel, pottery or inner liner polytetrafluoroethylene lining.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100867597A CN100411727C (en) | 2005-11-02 | 2005-11-02 | Multifunctional reactor for preparing ionic liquid |
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| CNB2005100867597A CN100411727C (en) | 2005-11-02 | 2005-11-02 | Multifunctional reactor for preparing ionic liquid |
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| CN1857767A true CN1857767A (en) | 2006-11-08 |
| CN100411727C CN100411727C (en) | 2008-08-20 |
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Cited By (17)
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| CN101851208A (en) * | 2010-05-28 | 2010-10-06 | 中国科学院过程工程研究所 | Multifunctional ion liquid preparation device |
| CN102382139A (en) * | 2010-08-31 | 2012-03-21 | 中国石油化工股份有限公司 | Preparation method of organic phosphate polypropylene nucleating agent |
| CN102382135A (en) * | 2010-08-31 | 2012-03-21 | 中国石油化工股份有限公司 | Preparation method of organic phosphate polypropylene nucleating agent |
| CN102430538A (en) * | 2011-09-01 | 2012-05-02 | 无锡双雄通用机械有限公司 | Improved discharge port structure of washing kettle |
| CN103831072A (en) * | 2012-11-21 | 2014-06-04 | 虞文娟 | High-efficient reaction vessel |
| CN104587931A (en) * | 2015-01-15 | 2015-05-06 | 浙江工业大学 | Multi-microcapillary reactor used for continuously preparing carrier particles |
| CN105672000A (en) * | 2016-01-18 | 2016-06-15 | 海宁源远纺织助剂有限公司 | Mending agent and preparation method thereof |
| CN105709621A (en) * | 2014-12-04 | 2016-06-29 | 中国石油天然气股份有限公司 | Dissolving device for preventing reactants from subliming and method for operating by using same |
| CN106621513A (en) * | 2016-09-21 | 2017-05-10 | 北京化工大学 | Filter-element dispersed filtering device and method for preparing inorganic material |
| CN107126920A (en) * | 2017-07-19 | 2017-09-05 | 陈宗良 | A kind of stirred tank |
| CN109317070A (en) * | 2018-11-30 | 2019-02-12 | 西安科技大学 | A kind of mining ionic liquid retardant preparation facilities and preparation method |
| CN111001365A (en) * | 2019-12-23 | 2020-04-14 | 张小飞 | Fine chemical product purification equipment |
| CN111495311A (en) * | 2020-04-29 | 2020-08-07 | 沈阳工业大学 | Horizontal continuous precipitation reaction device |
| CN111821937A (en) * | 2020-07-27 | 2020-10-27 | 山东朗晖石油化学股份有限公司 | Be applicable to PVC paste resin safety in production equipment |
| CN112345669A (en) * | 2020-11-17 | 2021-02-09 | 海南卫康制药(潜山)有限公司 | Method for measuring ceftazidime polymer for injection |
| 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 |
| CN117029420A (en) * | 2023-08-22 | 2023-11-10 | 苏州贝茵佳智能科技有限公司 | Vacuum drying oven for microbial agent detection experiment and use method thereof |
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| KR101645472B1 (en) * | 2014-10-28 | 2016-08-04 | 손창민 | Multifunctional chemical equipment |
Family Cites Families (3)
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| CN2105485U (en) * | 1991-12-13 | 1992-05-27 | 王升全 | Causticizing reactor for preparing alkaline |
| CN2267856Y (en) * | 1996-06-14 | 1997-11-19 | 曹营军 | Multifunction chemical unit integrated reactor |
| FR2796310B1 (en) * | 1999-07-01 | 2001-10-19 | Rhodia Chimie Sa | MULTIFUNCTIONAL SYNTHESIS AND CRYSTALLIZATION PROCESS AND REACTOR |
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2005
- 2005-11-02 CN CNB2005100867597A patent/CN100411727C/en active Active
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101851208B (en) * | 2010-05-28 | 2012-07-25 | 中国科学院过程工程研究所 | Multifunctional ion liquid preparation device |
| CN101851208A (en) * | 2010-05-28 | 2010-10-06 | 中国科学院过程工程研究所 | Multifunctional ion liquid preparation device |
| CN102382139A (en) * | 2010-08-31 | 2012-03-21 | 中国石油化工股份有限公司 | Preparation method of organic phosphate polypropylene nucleating agent |
| CN102382135A (en) * | 2010-08-31 | 2012-03-21 | 中国石油化工股份有限公司 | Preparation method of organic phosphate polypropylene nucleating agent |
| CN102430538A (en) * | 2011-09-01 | 2012-05-02 | 无锡双雄通用机械有限公司 | Improved discharge port structure of washing kettle |
| CN103831072A (en) * | 2012-11-21 | 2014-06-04 | 虞文娟 | High-efficient reaction vessel |
| CN105709621A (en) * | 2014-12-04 | 2016-06-29 | 中国石油天然气股份有限公司 | Dissolving device for preventing reactants from subliming and method for operating by using same |
| CN105709621B (en) * | 2014-12-04 | 2019-01-18 | 中国石油天然气股份有限公司 | Dissolving device for preventing reactants from subliming and method for operating by using same |
| CN104587931A (en) * | 2015-01-15 | 2015-05-06 | 浙江工业大学 | Multi-microcapillary reactor used for continuously preparing carrier particles |
| CN104587931B (en) * | 2015-01-15 | 2016-04-13 | 浙江工业大学 | A kind of many microcapillaries reactor for continuous production carrier granular |
| CN105672000A (en) * | 2016-01-18 | 2016-06-15 | 海宁源远纺织助剂有限公司 | Mending agent and preparation method thereof |
| CN106621513A (en) * | 2016-09-21 | 2017-05-10 | 北京化工大学 | Filter-element dispersed filtering device and method for preparing inorganic material |
| CN107126920A (en) * | 2017-07-19 | 2017-09-05 | 陈宗良 | A kind of stirred tank |
| CN109317070A (en) * | 2018-11-30 | 2019-02-12 | 西安科技大学 | A kind of mining ionic liquid retardant preparation facilities and preparation method |
| CN109317070B (en) * | 2018-11-30 | 2023-08-08 | 西安科技大学 | Preparation device and preparation method of mining ionic liquid inhibitor |
| 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 |
| CN111001365B (en) * | 2019-12-23 | 2021-08-24 | 甘肃金川恒信高分子科技有限公司 | Fine chemical product purification equipment |
| CN111001365A (en) * | 2019-12-23 | 2020-04-14 | 张小飞 | Fine chemical product purification equipment |
| CN111495311A (en) * | 2020-04-29 | 2020-08-07 | 沈阳工业大学 | Horizontal continuous precipitation reaction device |
| CN111821937A (en) * | 2020-07-27 | 2020-10-27 | 山东朗晖石油化学股份有限公司 | Be applicable to PVC paste resin safety in production equipment |
| CN112345669A (en) * | 2020-11-17 | 2021-02-09 | 海南卫康制药(潜山)有限公司 | Method for measuring ceftazidime polymer for injection |
| CN117029420A (en) * | 2023-08-22 | 2023-11-10 | 苏州贝茵佳智能科技有限公司 | Vacuum drying oven for microbial agent detection experiment and use method thereof |
| CN117029420B (en) * | 2023-08-22 | 2024-02-13 | 苏州贝茵佳智能科技有限公司 | Vacuum drying oven for microbial agent detection experiment and use method thereof |
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| CN100411727C (en) | 2008-08-20 |
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