CN100411725C - Ion liquid microcapsule and its preparation method - Google Patents
Ion liquid microcapsule and its preparation method Download PDFInfo
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- CN100411725C CN100411725C CNB2005101262040A CN200510126204A CN100411725C CN 100411725 C CN100411725 C CN 100411725C CN B2005101262040 A CNB2005101262040 A CN B2005101262040A CN 200510126204 A CN200510126204 A CN 200510126204A CN 100411725 C CN100411725 C CN 100411725C
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Abstract
The present invention relates to an ionic liquid microcapsule and a preparation method thereof, which belongs to novel functional materials and the preparation technical field thereof. The ionic liquid microcapsule is composed of wall materials made of high polymers, such as polysulphone, polystyrene, etc., and core materials, wherein the exterior wall materials have the advantages of acid and alkali-resisting performance, solvent-resisting performance and stable chemical property and have heat-resisting performance, cold-resisting performance and high-temperature creep-resisting performance at the same time, the core materials are wrapped inside, and the core materials have good stability and various types and are suitable for being used as ionic liquid of various media, such as 1-butylhexafluorophosphate pyridine, etc. The particle diameter of the ionic liquid microcapsule made by the present invention through using micro-channel dispersal, namely a solvent volatilization method, can be controlled in a micron order or a millimetre order, the distribution of the particle diameter is uniform, the ionic liquid microcapsule has large contact area of mass transfer, and the disadvantage of high ionic liquid viscidity is solved while all advantages of ionic liquid are maintained. A liquid reaction and separation process is changed into a liquid solid contact process, the preparation of multifunctional materials is achieved, and the present invention has a wide application prospect in multiple fields, such as chemistry, chemical engineering, petrochemical industry, medicine, food, etc.
Description
Technical field
The present invention relates to a kind of new function material that is used for chemical industry catalysis, chemical separation process, particularly the preparation method of green solvent ion liquid microcapsule belongs to a kind of new function material technical field.
Background technology
Ionic liquid, claim again ionic liquid at room temperature (Room Temperature Ionic Liquid, RTILs) or the room temperature fuse salt.It is the liquid substance of being made up of ion fully under room temperature and contiguous temperature.It generally is made up of volume bigger organic cation and the less inorganic anion of volume.Ionic liquid is as green solvent, and it is minimum to have (1) vapour pressure, and at room temperature, the ionic liquid vapour pressure is almost nil; (2) inorganic and organic material are shown good dissolving ability; (3) non-volatile, not flammable, toxicity is little; (4) can be by changing zwitterion, adjustment of acidity and other physicochemical properties, orientable design special nature ionic liquid; (5) good conductivity has the advantages such as electrochemical window of broad, and as catalyst carrier or reactant solvents, or solvent in the separation process or release agent are subjected to paying close attention to widely in catalysis and synthetic reaction.Yet the general viscosity of ionic liquid is too high, some kind ionic liquid can be lost to especially in the aqueous solution and stability not enough.Ion liquid microcapsuleization not only can be kept the ionic liquid advantage but also can improve its stability, overcome the too big shortcoming of viscosity, be the effective means that realizes that ionic liquid is used in industry.
The objective of the invention is to propose a kind of preparation method of ion liquid microcapsule.
Summary of the invention
Ion liquid microcapsule is to coat ion liquid microcapsules, and it is made up of core two parts that outer wall material and the inside are coated.
The skin of microcapsules forms membranous wall by macromolecular material, and the wall material is to have acid and alkali-resistance, solvent resistance, and chemical property is stable, has hear resistance, cold resistance and high polymers such as high-temperature creep resistance such as polysulfones, polystyrene simultaneously.
Core is coated in the microcapsules has good stable, and kind is various, is suitable for doing the ionic liquid of various media.As 1-butyl-3-methyl hexafluorophosphate imidazoline drone, 1-butyl hexafluorophosphate pyridine.
This ion liquid microcapsule is the preparation method may further comprise the steps:
(1) macromolecule wall material and ionic liquid are dissolved in the organic solvent (as carrene) of high volatility, form the decentralized photo solution of homogeneous phase, wall material and ion liquid weight percent content are 5%～10%.
(2) preparation continuous phase solution, continuous phase solution is for containing the aqueous solution of dispersant (as gelatin), and the dispersant weight percent content is 0.1%～1%.
(3) microencapsulation: decentralized photo solution is pressed into passage from the decentralized photo feeder connection with the speed of 50～150 μ l/min, is that the continuous phase aqueous solution of 10～30ml/min is taken out of at other end place by the range of flow that enters from the continuous phase entrance, forms single drop in the continuous phase pipeline.After drop is taken out of the continuous phase pipeline, in coagulating bath, carry out solvent evaporates, make macromolecule wall material solidify, ionic liquid is formed coating, obtain the novel ion liquid microcapsules.
By changing the composition of decentralized photo solution, can obtain the microcapsules of different ionic liquid clad ratio.
Described passage internal diameter is 1-1000 μ m.The flow velocity of internal diameter, continuous phase and decentralized photo by changing passage, the ion liquid microcapsule particle diameter can be controlled in micron order or millimeter level, has the characteristics of big mass transfer contact area, and the particle diameter very homogeneous that distributes.
The present invention successfully utilizes microchannel dispersion-solvent evaporation method, makes macromolecule wall material and coats ion liquid microcapsules new function material.The present invention can be controlled at the ion liquid microcapsule particle diameter micron order or millimeter level, and particle diameter distribution ten minutes homogeneous, has the characteristics of big mass transfer contact area, is suitable for using.The ion liquid microcapsule that utilizes the present invention to make keeps the advantage of ionic liquid as green solvent, has solved the big shortcoming of viscosity of il simultaneously, has avoided the difficulty of disperseing, and reactive liquid solution, separation process are converted into liquid-solid contact process; Ionic liquid has good stability in microcapsules, be difficult for decomposing, and is difficult for running off.
The present invention can be applicable to various fields such as chemistry, chemical industry, petrochemical industry, medicine and food.The ion liquid microcapsule that utilizes the present invention to make can be used as the carrier of catalyst in catalysis and synthetic reaction, can be used as the function parting material simultaneously, is with a wide range of applications at aspects such as metal ion extraction, desulfurization, gas absorption.
Description of drawings
Fig. 1 prepares schematic diagram for ion liquid microcapsule, wherein, and 1-continuous phase fluid inlet tube, 2-dispersed phase fluid inlet tube, 3-continuous phase pipeline, 4-decentralized photo passage, 5-dispersant liquid drop, 6-coagulating bath container.
The specific embodiment
Below by embodiment the present invention is illustrated.
Fig. 1 prepares schematic diagram for ion liquid microcapsule, wherein, and 1-continuous phase fluid inlet tube, 2-dispersed phase fluid inlet tube, 3-continuous phase pipeline, 4-decentralized photo passage, 5-dispersant liquid drop, 6-coagulating bath container.
A kind of ion liquid microcapsule preparation method may further comprise the steps:
1, macromolecule wall material and ionic liquid are dissolved in the organic solvent (as carrene) of high volatility, form the decentralized photo solution of homogeneous phase, wall material and ion liquid weight percent content are 5%～10%.
2, preparation continuous phase solution, continuous phase solution is for containing the aqueous solution of dispersant (as gelatin), and the dispersant weight percent content is 0.1%～1%.
3, microencapsulation: decentralized photo solution is pressed into decentralized photo passage (4) from decentralized photo feeder connection (2) with the speed of 50～150 μ l/min, is that the continuous phase aqueous solution of 10～30ml/min is taken out of at the other end by the range of flow that enters from continuous phase entrance (1), forms single drop (5) in continuous phase pipeline (3).After drop is taken out of the continuous phase pipeline, in coagulating bath, carry out solvent evaporates, make macromolecule wall material solidify, ionic liquid is formed coating, obtain the novel ion liquid microcapsules.
The composition of these microcapsules: wall material: polysulfones; Ionic liquid: 1-butyl-3-methyl hexafluorophosphate imidazoline drone.
The preparation method: it is that 5% polysulfones and 1-butyl-3-methyl hexafluorophosphate imidazoline drone ionic liquid (1-Butyl-3-methylimidazol ium hexafluorophosphate) of 5% are dissolved in the methylene chloride that decentralized photo adopts percentage by weight, and continuous phase is 0.1% aqueous gelatin solution.Passage No. 6 syringe needles of standard, the decentralized photo flow is 150 μ l/min, the continuous phase flow is 10ml/min.The microcapsules average grain diameter is 600 μ m.
The composition of these microcapsules: wall material: polysulfones; Ionic liquid: 1-butyl-3-methyl hexafluorophosphate imidazoline drone.
The preparation method: it is that 10% polysulfones and 1-butyl-3-methyl hexafluorophosphate imidazoline drone ionic liquid of 10% are dissolved in the methylene chloride that decentralized photo adopts percentage by weight, and continuous phase is 1.0% aqueous gelatin solution.Microchannel No. 6 syringe needles of standard, the decentralized photo flow is 50 μ l/min, the continuous phase flow is 30ml/min.The microcapsules average grain diameter is about 400 μ m.
The composition of these microcapsules: wall material: polystyrene; Ionic liquid: 1-butyl-3-methyl hexafluorophosphate imidazoline drone.
The preparation method: it is that 10% polystyrene and 1-butyl-3-methyl hexafluorophosphate imidazoline drone ionic liquid of 5% are dissolved in the methylene chloride that decentralized photo adopts percentage by weight, and continuous phase is 0.3% aqueous gelatin solution.Microchannel No. 6 syringe needles of standard, the decentralized photo flow is 50 μ l/min, the continuous phase flow is 20ml/min.The microcapsules average grain diameter is about 440 μ m.
The composition of these microcapsules: wall material: polysulfones; Ionic liquid: 1-butyl hexafluorophosphate pyridine.
The preparation method: it is that 10% polysulfones and 5% 1-butyl hexafluorophosphate pyridine ion liquid are dissolved in the methylene chloride that decentralized photo adopts percentage by weight, and continuous phase is 0.1% aqueous gelatin solution.Microchannel No. 6 syringe needles of standard, the decentralized photo flow is 50 μ l/min, the continuous phase flow is 10ml/min.The microcapsules average grain diameter is about 650 μ m.
The composition of these microcapsules: wall material: polystyrene; Ionic liquid: 1-butyl hexafluorophosphate pyridine.
The preparation method: it is that 5% polystyrene and 5% 1-butyl hexafluorophosphate pyridine ion liquid are dissolved in the methylene chloride that decentralized photo adopts percentage by weight, and continuous phase is 1.0% aqueous gelatin solution.Microchannel No. 6 syringe needles of standard, the decentralized photo flow is 100 μ l/min, the continuous phase flow is 30ml/min.The microcapsules average grain diameter is about 350 μ m.
Claims (6)
1. the ion liquid microcapsule preparation method is characterized in that, this preparation method may further comprise the steps:
(1) macromolecule wall material and ionic liquid are dissolved in the organic solvent of high volatility, form the decentralized photo solution of homogeneous phase, wall material and ion liquid weight percent content are 5%～10%;
(2) preparation continuous phase solution, continuous phase solution is the aqueous solution that contains dispersant, the dispersant weight percent content is 0.1%～1%;
(3) microencapsulation: decentralized photo solution is pressed into passage from the decentralized photo feeder connection with the speed of 50～150 μ l/min, taken out of with the continuous phase aqueous solution that 10～30ml/min speed enters from the continuous phase entrance at the other end, in the continuous phase pipeline, formed single drop; After drop is taken out of the continuous phase pipeline, in coagulating bath, carry out solvent evaporates, make macromolecule wall material solidify, ionic liquid is formed coating, obtain ion liquid microcapsule.
2. according to the described ion liquid microcapsule preparation method of claim 1, it is characterized in that described macromolecule wall material is polysulfones or polystyrene.
3. according to the described ion liquid microcapsule preparation method of claim 1, it is characterized in that, described ionic liquid be 1-butyl-3-methyl hexafluorophosphate imidazoline drone or 1-butyl hexafluorophosphate pyridine.
4. according to the described ion liquid microcapsule preparation method of claim 1, it is characterized in that described organic solvent is a carrene.
5. according to the described ion liquid microcapsule preparation method of claim 1, it is characterized in that described dispersant is a gelatin.
6. ion liquid microcapsule preparation method according to claim 1 is characterized in that, described decentralized photo passage internal diameter is 1～1000 μ m.
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| CN100411725C true CN100411725C (en) | 2008-08-20 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101239296B (en) * | 2008-03-07 | 2010-04-21 | 清华大学 | Method for preparing solvent microcapsule |
| CN103153466B (en) | 2010-07-22 | 2016-04-13 | 基因细胞生物系统有限公司 | Composite fluid pond |
| CN102008983B (en) * | 2010-11-01 | 2012-08-08 | 武汉大学 | Microfluidic chip suitable for producing microcapsules |
| JP2014520665A (en) * | 2011-06-29 | 2014-08-25 | ザ ユニバーシティ オブ アクロン | Method of encapsulation and immobilization |
| CN104812492A (en) | 2012-11-27 | 2015-07-29 | 基因细胞生物系统有限公司 | Handling liquid samples |
| WO2015120398A1 (en) | 2014-02-10 | 2015-08-13 | Gencell Biosystems Limited | Composite liquid cell (clc) mediated nucleic acid library preparation device, and methods for using the same |
| CN104193965A (en) * | 2014-08-21 | 2014-12-10 | 江汉大学 | Imidazole epoxy curing agent micro capsule and preparation method thereof |
| CN105254490B (en) * | 2015-10-28 | 2017-06-06 | 南京工业大学 | The technique that a kind of microcapsules extract succinic acid |
| US20190105606A1 (en) * | 2016-03-30 | 2019-04-11 | Osaka Gas Co., Ltd. | Gas Sorbent and Carbon Dioxide Separation and Recovery System and Method |
| CN110433740B (en) * | 2019-06-25 | 2021-12-07 | 浙江工业大学 | Preparation method of thermal expansibility microsphere wrapping ionic liquid |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87105291A (en) * | 1987-07-30 | 1988-06-08 | 浙江大学 | The method of coating solid alikali with organic high-molecule film |
| CN1385410A (en) * | 2002-04-10 | 2002-12-18 | 中国科学院兰州化学物理研究所 | Method for preparing phenol by directly hydrocylating benzene |
| KR20040031921A (en) * | 2002-10-07 | 2004-04-14 | 한국화학연구원 | A method for preparing ionic liquid supported liquid membrane |
| WO2004052340A1 (en) * | 2002-12-06 | 2004-06-24 | Novartis Ag | Microparticles prepared using an ionic liquid |
| CN1681878A (en) * | 2002-07-05 | 2005-10-12 | 德古萨公司 | Polymeric compositions containing polymers and ionic liquids |
| US6958085B1 (en) * | 2003-03-26 | 2005-10-25 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | High performance immobilized liquid membrane for carbon dioxide separations |
-
2005
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87105291A (en) * | 1987-07-30 | 1988-06-08 | 浙江大学 | The method of coating solid alikali with organic high-molecule film |
| CN1385410A (en) * | 2002-04-10 | 2002-12-18 | 中国科学院兰州化学物理研究所 | Method for preparing phenol by directly hydrocylating benzene |
| CN1681878A (en) * | 2002-07-05 | 2005-10-12 | 德古萨公司 | Polymeric compositions containing polymers and ionic liquids |
| KR20040031921A (en) * | 2002-10-07 | 2004-04-14 | 한국화학연구원 | A method for preparing ionic liquid supported liquid membrane |
| WO2004052340A1 (en) * | 2002-12-06 | 2004-06-24 | Novartis Ag | Microparticles prepared using an ionic liquid |
| US6958085B1 (en) * | 2003-03-26 | 2005-10-25 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | High performance immobilized liquid membrane for carbon dioxide separations |
Non-Patent Citations (2)
| Title |
|---|
| 离子液体简介. 胡德荣，张新位，赵景芝.首都师范大学学报（自然科学版），第26卷第2期. 2005 |
| 离子液体简介. 胡德荣，张新位，赵景芝.首都师范大学学报（自然科学版），第26卷第2期. 2005 * |
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