CN1563251A - Water disperse liquid for capsule of organic phase change material and preparation method - Google Patents
Water disperse liquid for capsule of organic phase change material and preparation method Download PDFInfo
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- CN1563251A CN1563251A CN 200410017942 CN200410017942A CN1563251A CN 1563251 A CN1563251 A CN 1563251A CN 200410017942 CN200410017942 CN 200410017942 CN 200410017942 A CN200410017942 A CN 200410017942A CN 1563251 A CN1563251 A CN 1563251A
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Abstract
A capsule aqueous emulsion for organic phase transfer material consists of core layer which is C10-C28 paraffin with melting point at 10-80 deg.C and shell layer which is one or multitype of vinyl monomer or copolymer of multivinyl monomer. The preparing process includes forming fat solution by placing phase transfer material into vinyl monomer or multivinyl monomer, dissolving emulsifier in water for forming aqueous solution, mixing aqueous solution with fat solution to obtain fine emulsion, filling the fine emulsion into reactor, adding initiator to cause polymerization and cooling down slowly to room temperature for discharging product.
Description
Technical field
The present invention relates to a kind of organic phase transition material capsule aqueous dispersions and preparation method thereof.
Background technology
Phase change materials is a kind of important energy storage, energy-conservation, temperature control material, is widely used in various industry, civil area.Utilize material in the phase transition process, can store or discharge a large amount of latent heat, can carry out the storage and the utilization of heat energy efficiently.On the other hand, because in the phase transition process, temperature is invariable, so phase change materials still is a kind of intelligent material that can be temperature automatically controlled.For example, if system temperature surpasses the phase transition temperature of phase change materials, phase change materials just takes place to change mutually, and the energy of absorption system is kept the temperature-resistant of system; On the contrary, if system temperature is lower than the phase transition temperature of phase change materials, reverse transformation mutually just takes place in phase change materials, releases energy to system, keeps the temperature-resistant of system.If directly phase change materials is applied in various application systems, then there is caking, shortcoming such as component is separated, and burn into and system are incompatible, heat transfer surface area is limited.Thereby in many Application Areass, phase change materials must be made capsular form earlier and use.By optimizing the shell material, phase change materials can be adapted to various Application Areass better, increases the service life, and improves heat transfer area.In some Application Areass, hope can prepare phase change materials capsule aqueous dispersions, so that combine with other material better.Adopt common capsule technique, can prepare size at the capsule of micron to millimeter.Though these capsules can be dispersed in by the effect of emulsifying agent in the water, form dispersion liquid.This method not only exists processing step more, the difficult shortcoming of regulating of shell material, and because capsule size is excessive, dispersion liquid stable very poor.The present invention intends providing a kind of novel method for preparing organic phase transition material capsule aqueous dispersions, use this method can directly obtain organic phase transition material capsule water miscible liquid, capsule size is between 30nm～500nm, capsular shell material can be regulated according to service requirements, and this water miscible liquid has good stability simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of organic phase transition material capsule water miscible liquid and preparation method thereof.
Organic phase transition material capsule water miscible liquid has stratum nucleare and shell, and stratum nucleare is a fusing point at 10 ℃～80 ℃ C
10～C
28Alkane, shell is one or more vinyl monomers or multi-vinyl monomer multipolymer, capsule size is 30nm～500nm, the capsule stable dispersion is in water, solid content is 5wt%～55wt%.
A kind of preparation method of organic phase transition material capsule water miscible liquid is characterized in that: the step of method. for:
1) 10～50 parts phase change materials is added 10～200 parts of one or more vinyl monomers or multi-vinyl monomer mixes, form oil solution;
2) with 1 part of emulsifiers dissolve in 100～400 parts of water, form the aqueous solution; After oil solution and aqueous solution, after the high shear field effect, pulverize, make miniemulsion;
3) miniemulsion is moved in the reactor, add the aqueous solution of water soluble starter, initiated polymerization after polymerization is finished, slowly cools to discharging after the room temperature.
The preparation method of another kind of organic phase transition material capsule water miscible liquid, it is characterized in that: the step of method is:
1) miscellany, the oil-soluble initiator with 10～50 parts phase change materials, 10～200 parts of one or more vinyl monomers or two (many) vinyl monomers mixes, and forms oil solution; 1 part of emulsifiers dissolve in 100～400 parts of water, is formed the aqueous solution;
2) with after oil solution and the aqueous solution, after the high shear field effect, pulverize, make miniemulsion;
3) miniemulsion is moved in the reactor, the rising reactor temperature carries out polymerization, after polymerization is finished, slowly cools to discharging after the room temperature.
Advantage of the present invention: adopt fine emulsion polymerization to prepare organic phase transition material capsule water miscible liquid, technology is simple, and the capsule size that makes is little, and latex stability is good, can be applied directly to fabric fibre, easy and various material of construction blending.
Embodiment
The preparation method of organic phase transition material capsule water miscible liquid: a certain amount of phase change materials is mixed the formation homogeneous solution with vinyl monomer, common monomer, linking agent, add emulsifier aqueous solution then, stir after 10 minutes, ultrasonication 15 minutes makes miniemulsion.Miniemulsion is moved into one mechanical stirring, prolong, N are housed
2In inlet device and the charging opening reactor, heating in water bath remains on temperature of reaction.Logical N
2After the deoxygenation, add initiator, initiated polymerization.After polymerization is finished, slowly cool to discharging after the room temperature.
Embodiment 1
With adding the mixture of 15 gram methyl methacrylates, 0.2 gram Ethylene glycol dimethacrylate, 0.2 gram methacrylic acid after paraffin wax (phase change materials) heating and melting of 5 grams, under magnetic agitation, mix, form oil solution; 0.2 gram sodium lauryl sulphate is dissolved in the 70 gram water, forms the aqueous solution; With oil solution and aqueous solution, stir after 10 minutes, give birth to KS-600 ultrasonic cell disruptor ultrasonication 15 minutes (70% output rating) with Ningbo section, make miniemulsion.Miniemulsion is moved into one mechanical stirring, prolong, N are housed
2In the reactor of inlet device and charging opening, reactor is placed water-bath, bath temperature remains on about 68 ℃.Logical N
2After the deoxygenation 0.5 hour, add the aqueous solution (0.3 gram Potassium Persulphate is dissolved in 10 gram water) of Potassium Persulphate, initiated polymerization.After polymerization is finished, slowly cool to discharging after the room temperature.
Embodiment 2
With adding the mixture of 15 gram vinylbenzene, 0.2 gram methacrylic acid after section Octadecane (phase change materials) heating and melting of 5 grams, under magnetic agitation, mix, form oil solution; 0.2 gram sodium lauryl sulphate is dissolved in the 70 gram water, forms the aqueous solution; With oil solution and aqueous solution, stir after 10 minutes, give birth to KS-600 ultrasonic cell disruptor ultrasonication 15 minutes (70% output rating) with Ningbo section, make miniemulsion.Miniemulsion is moved into one mechanical stirring, prolong, N are housed
2In the reactor of inlet device and charging opening, reactor is placed water-bath, bath temperature remains on about 68 ℃.Logical N
2After the deoxygenation 0.5 hour, add the aqueous solution (0.3 gram Potassium Persulphate is dissolved in 10 gram water) of Potassium Persulphate, initiated polymerization.After polymerization is finished, slowly cool to discharging after the room temperature.
Embodiment 3
With adding the mixture of 10 gram vinylbenzene, 0.2 gram Ethylene glycol dimethacrylate, 0.2 gram methacrylic acid after paraffin wax (phase change materials) heating and melting of 10 grams, under magnetic agitation, mix, form oil solution; 0.2 gram sodium lauryl sulphate is dissolved in the 70 gram water, forms the aqueous solution; With oil solution and aqueous solution, stir after 10 minutes, give birth to KS-600 ultrasonic cell disruptor ultrasonication 15 minutes (70% output rating) with Ningbo section, make miniemulsion.Miniemulsion is moved into one mechanical stirring, prolong, N are housed
2In the reactor of inlet device and charging opening, reactor is placed water-bath, bath temperature remains on about 68 ℃.Logical N
2After the deoxygenation 0.5 hour, add the aqueous solution (0.3 gram Potassium Persulphate is dissolved in 10 gram water) of Potassium Persulphate, initiated polymerization.After polymerization is finished, slowly cool to discharging after the room temperature.
Embodiment 4
With adding the mixture of 10 gram vinylbenzene, 0.2 gram Ethylene glycol dimethacrylate, 0.2 gram methacrylic acid after liquid n-Hexadecane (phase change materials) heating and melting of 10 grams, under magnetic agitation, mix, form oil solution; 0.2 gram sodium lauryl sulphate is dissolved in the 70 gram water, forms the aqueous solution; With oil solution and aqueous solution, stir after 10 minutes, give birth to KS-600 ultrasonic cell disruptor ultrasonication 15 minutes (70% output rating) with Ningbo section, make miniemulsion.Miniemulsion is moved into one mechanical stirring, prolong, N are housed
2In the reactor of inlet device and charging opening, reactor is placed water-bath, bath temperature remains on about 68 ℃.Logical N
2After the deoxygenation 0.5 hour, add the aqueous solution (0.3 gram Potassium Persulphate is dissolved in 10 gram water) of Potassium Persulphate, initiated polymerization.After polymerization is finished, slowly cool to discharging after the room temperature.
Embodiment 5
With adding the mixture of 10 gram vinylbenzene, 0.2 gram Ethylene glycol dimethacrylate, 0.2 gram methacrylic acid after section eicosane (phase change materials) heating and melting of 10 grams, under magnetic agitation, mix, form oil solution; 0.2 gram sodium lauryl sulphate and 1 gram Triton X-100 are dissolved in the 70 gram water, form the aqueous solution; With oil solution and aqueous solution, stir after 10 minutes, give birth to KS-600 ultrasonic cell disruptor ultrasonication 15 minutes (70% output rating) with Ningbo section, make miniemulsion.Miniemulsion is moved into one mechanical stirring, prolong, N are housed
2In the reactor of inlet device and charging opening, reactor is placed water-bath, bath temperature remains on about 68 ℃.Logical N
2After the deoxygenation 0.5 hour, add the aqueous solution (0.3 gram Potassium Persulphate is dissolved in 10 gram water) of Potassium Persulphate, initiated polymerization.After polymerization is finished, slowly cool to discharging after the room temperature.
Embodiment 6
With adding the mixture of 10 gram vinyl-acetic esters, 0.2 gram Ethylene glycol dimethacrylate, 0.2 gram methacrylic acid after section nonadecane (phase change materials) heating and melting of 10 grams, under magnetic agitation, mix, form oil solution; 0.2 gram sodium lauryl sulphate and 5 gram Triton X-100s are dissolved in the 70 gram water, form the aqueous solution; With oil solution and aqueous solution, stir after 10 minutes, give birth to KS-600 ultrasonic cell disruptor ultrasonication 15 minutes (70% output rating) with Ningbo section, make miniemulsion.Miniemulsion is moved into one mechanical stirring, prolong, N are housed
2In the reactor of inlet device and charging opening, reactor is placed water-bath, bath temperature remains on about 68 ℃.Logical N
2After the deoxygenation 0.5 hour, add the aqueous solution (0.3 gram Potassium Persulphate is dissolved in 10 gram water) of Potassium Persulphate, initiated polymerization.After polymerization is finished, slowly cool to discharging after the room temperature.
Embodiment 7
With adding the mixture of 15 gram vinylbenzene, 0.2 gram Ethylene glycol dimethacrylate, 0.2 gram methacrylic acid after section nonadecane (phase change materials) heating and melting of 5 grams, under magnetic agitation, mix, form oil solution; 0.2 gram sodium lauryl sulphate and 2 gram CO-890 (emulsifying agent, lark waffle learn a skill company limited) are dissolved in the 70 gram water, form the aqueous solution; With oil solution and aqueous solution, stir after 10 minutes, give birth to KS-600 ultrasonic cell disruptor ultrasonication 15 minutes (70% output rating) with Ningbo section, make miniemulsion.Miniemulsion is moved into one mechanical stirring, prolong, N are housed
2In the reactor of inlet device and charging opening, reactor is placed water-bath, bath temperature remains on about 68 ℃.Logical N
2After the deoxygenation 0.5 hour, add the aqueous solution (0.3 gram Potassium Persulphate is dissolved in 10 gram water) of Potassium Persulphate, initiated polymerization.After polymerization is finished, slowly cool to discharging after the room temperature.
Emulsion property
| Embodiment | Median size (nm) | Nucleocapsid structure | Stability in storage |
| ????1 | ????250.9 | Complete | Good |
| ????2 | ????121.5 | Complete | Good |
| ????3 | ????104.5 | Complete | Good |
| ????4 | ????89.6 | Complete | Good |
| ????5 | ????80.6 | Complete | Good |
| ????6 | ????86.4 | Complete | Good |
| ????7 | ????97.3 | Complete | Good |
Wherein: nucleocapsid structure is by transmission electron microscope observing, stability in storage: GB-6753.3-86
Claims (10)
1. organic phase transition material capsule water miscible liquid, it is characterized in that: it has stratum nucleare and shell, and stratum nucleare is a fusing point at 10 ℃～80 ℃ C
10～C
28Alkane, shell is one or more vinyl monomers or multi-vinyl monomer multipolymer, capsule size is 30nm～500nm, the capsule stable dispersion is in water, solid content is 5wt%～55wt%.
2. the preparation method of an organic phase transition material capsule water miscible liquid, it is characterized in that: the step of method is:
1) 10～50 parts phase change materials is added 10～200 parts of one or more vinyl monomers or multi-vinyl monomer mixes, form oil solution;
2) with 1 part of emulsifiers dissolve in 100～400 parts of water, form the aqueous solution; After oil solution and aqueous solution, after the high shear field effect, pulverize, make miniemulsion;
3) miniemulsion is moved in the reactor, add the aqueous solution of water soluble starter, initiated polymerization after polymerization is finished, slowly cools to discharging after the room temperature.
3. the preparation method of a kind of organic phase transition material capsule water miscible liquid according to claim 2, it is characterized in that: described phase change materials is: C
10～C
28Alkane or its mixture.
4. the preparation method of a kind of organic phase transition material capsule water miscible liquid according to claim 2, it is characterized in that: described vinyl monomer is: vinylformic acid, methacrylic acid, vinyl-acetic ester, methyl acrylate, ethyl propenoate, n-butyl acrylate, the special butyl ester of vinylformic acid, methyl methacrylate, methacrylic. acetoacetic ester, butyl methacrylate, Hydroxyethyl acrylate, Propylene glycol monoacrylate, hydroxyethyl methylacrylate, dodecylacrylate, alpha-methyl styrene, vinyl cyanide, methacrylonitrile, vinylbenzene, Vinyl toluene, t-butyl styrene or vinyl pyrrolidone; Described multi-vinyl monomer is meant and contains two or more carbon-carbon double bond compounds, i.e. Vinylstyrene, Ethylene glycol dimethacrylate in the molecule.
5. the preparation method of a kind of organic phase transition material capsule water miscible liquid according to claim 2, it is characterized in that: described high shear field effect is by strong shearing liquid-liquid dispersing apparatus, and promptly ultrasonic grinding machine, high-pressure homogenizer, super gravity field generating unit provide;
6. the preparation method of an organic phase transition material capsule water miscible liquid, it is characterized in that: the step of method is:
1) miscellany, the oil-soluble initiator with 10～50 parts phase change materials, 10～200 parts of one or more vinyl monomers or two (many) vinyl monomers mixes, and forms oil solution; 1 part of emulsifiers dissolve in 100～400 parts of water, is formed the aqueous solution;
2) with after oil solution and the aqueous solution, after the high shear field effect, pulverize, make miniemulsion;
3) miniemulsion is moved in the reactor, the rising reactor temperature carries out polymerization, after polymerization is finished, slowly cools to discharging after the room temperature.
7. the preparation method of a kind of organic phase transition material capsule water miscible liquid according to claim 6 is characterized in that: described phase change materials is C
10～C
28Alkane or its mixture.
8. the preparation method of a kind of organic phase transition material capsule water miscible liquid according to claim 6 is characterized in that: described vinyl monomer is a vinylformic acid, methacrylic acid, vinyl-acetic ester, methyl acrylate, ethyl propenoate, n-butyl acrylate, the special butyl ester of vinylformic acid, methyl methacrylate, Jia Jibingxisuanyizhi, butyl methacrylate, Hydroxyethyl acrylate, Propylene glycol monoacrylate, hydroxyethyl methylacrylate, dodecylacrylate, alpha-methyl styrene, vinyl cyanide, methacrylonitrile, vinylbenzene, Vinyl toluene, t-butyl styrene, vinyl pyrrolidone; Described multi-vinyl monomer is meant in the molecule and contains two or more carbon-carbon double bonds, i.e. Vinylstyrene, Ethylene glycol dimethacrylate.
9. the preparation method of a kind of organic phase transition material capsule water miscible liquid according to claim 6 is characterized in that: described high shear field effect is that ultrasonic grinding machine, high-pressure homogenizer, super gravity field generating unit provide by strong shearing liquid-liquid dispersing apparatus.
10. according to the preparation method of claim 2 or 6 described a kind of organic phase transition material capsule water miscible liquids, it is characterized in that: the ratio of described monomer and organic phase transition material is: 1: 5～10: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410017942 CN1256398C (en) | 2004-04-21 | 2004-04-21 | Water disperse liquid for capsule of organic phase change material and preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410017942 CN1256398C (en) | 2004-04-21 | 2004-04-21 | Water disperse liquid for capsule of organic phase change material and preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN1563251A true CN1563251A (en) | 2005-01-12 |
| CN1256398C CN1256398C (en) | 2006-05-17 |
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|---|---|---|---|
| CN 200410017942 Expired - Fee Related CN1256398C (en) | 2004-04-21 | 2004-04-21 | Water disperse liquid for capsule of organic phase change material and preparation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348625C (en) * | 2005-05-11 | 2007-11-14 | 浙江大学 | Process for preparing microcapsule by initiating active fine emulsion polymerization of water-soluble initiating agent |
| CN102030483A (en) * | 2010-10-29 | 2011-04-27 | 浙江大学 | Preparation method of porous antireflection film formed by nanopolymer hollow particles |
| CN102718906A (en) * | 2012-06-26 | 2012-10-10 | 华南理工大学 | Preparation method of spherical polyacrylonitrile latex nanoparticle based on oxidation reduction |
| CN102731704A (en) * | 2012-07-06 | 2012-10-17 | 浙江大学 | Method for preparing open-cell submicron porous polymer materials by miniemulsion template method |
| CN106693814A (en) * | 2016-12-20 | 2017-05-24 | 清华大学 | Method for preparing droplet emulsion by hypergravity technology |
-
2004
- 2004-04-21 CN CN 200410017942 patent/CN1256398C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348625C (en) * | 2005-05-11 | 2007-11-14 | 浙江大学 | Process for preparing microcapsule by initiating active fine emulsion polymerization of water-soluble initiating agent |
| CN102030483A (en) * | 2010-10-29 | 2011-04-27 | 浙江大学 | Preparation method of porous antireflection film formed by nanopolymer hollow particles |
| CN102030483B (en) * | 2010-10-29 | 2012-07-04 | 浙江大学 | Preparation method of porous antireflection film formed by nanopolymer hollow particles |
| CN102718906A (en) * | 2012-06-26 | 2012-10-10 | 华南理工大学 | Preparation method of spherical polyacrylonitrile latex nanoparticle based on oxidation reduction |
| CN102718906B (en) * | 2012-06-26 | 2014-07-02 | 华南理工大学 | Preparation method of spherical polyacrylonitrile latex nanoparticle based on oxidation reduction |
| CN102731704A (en) * | 2012-07-06 | 2012-10-17 | 浙江大学 | Method for preparing open-cell submicron porous polymer materials by miniemulsion template method |
| CN106693814A (en) * | 2016-12-20 | 2017-05-24 | 清华大学 | Method for preparing droplet emulsion by hypergravity technology |
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| Publication number | Publication date |
|---|---|
| CN1256398C (en) | 2006-05-17 |
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Granted publication date: 20060517 Termination date: 20110421 |