CN101824306B - Method for preparing multi-phase change material coated with microcapsule - Google Patents
Method for preparing multi-phase change material coated with microcapsule Download PDFInfo
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- CN101824306B CN101824306B CN201010131608XA CN201010131608A CN101824306B CN 101824306 B CN101824306 B CN 101824306B CN 201010131608X A CN201010131608X A CN 201010131608XA CN 201010131608 A CN201010131608 A CN 201010131608A CN 101824306 B CN101824306 B CN 101824306B
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Abstract
The invention provides a method for preparing multi-phase change materials coated with microcapsules, which relates to a preparation method for optoelectronic materials. The method comprises the steps: taking materials as per the mass ratio of paraffin to styrene being 2:5; weighing methacrylate in 5 % of the total mass of paraffin and styrene, 0.5% to 2% of dodecanethiol, 2% to 5% of sodium dodecyl benzene sulfonate, and 2% to 10% of potassium persulfate; adding the styrene, methacrylate and the dodecanethiol into deionized water and stirring to obtain mixed solution; melting and adding the paraffin into the mixed solution; dissolving and heating the sodium dodecyl benzene sulfonate to 50 DGE C and then adding the sodium dodecyl benzene sulfonate into the mixed solution; ultrasonically emulsifying the mixed solution and then adding the solution into a four-port container; supplying nitrogen for 0.5 hour and heating the container with water bath to 70 DEG C; stirring the solution and then adding potassium persulfate solution for polymerization; cooling, filtering in vacuum and drying the product, thereby obtaining the sample. The method solves the problem of single type of coating material, improves the utility of phase change microcapsules, expands phase change temperature range and enlarges application scope of phase change microcapsules.
Description
Technical field
The present invention relates to a kind of preparation method of photoelectron material.Be applicable to heat exchange field, domain of control temperature and military field, like aerospace, material of construction, heat-accumulation temperature-adjustment textiles etc.
Background technology
Because solid-liquid phase change takes place in low-temperature phase-change material commonly used when work, directly use phase change material can bring inconvenience, therefore consider the phase change material encapsulation to be used with several different methods, wherein the microcapsule encapsulation is a focus of people's research in recent years.Microcapsulary is a kind ofly to be wrapped to form the fine particle technology of size in micron or millimeter scope to solid or liquid with film forming material.The polymeric membrane that coats one deck stable performance at the phase change material microparticle surfaces constitutes the NEW TYPE OF COMPOSITE phase change material with nucleocapsid structure.When the phase change material generation solid-liquid of kernel changed mutually, its outer shell remained solid-state, and general performance is solid-state, had realized the insulation purpose simultaneously again.
The research of present stage to phase-change material micro-capsule focuses mostly in a kind of phase change material; Or a kind of phase change material and other substance reactions generate the more excellent compound of performance as core; All be to coat single phase-change material micro-capsule in essence; Transformation temperature also has only one, has limited the application of microcapsule.
Summary of the invention
Technical problem to be solved by this invention is: the coating material kind is single, has limited the application of microcapsule.
Technical scheme of the present invention:
The preparation method of the multi-phase change material that a kind of microcapsule coat, this preparing method's step comprises:
Step 1, by paraffin: cinnamic mass ratio is to get material at 2: 5;
Step 2,5% of paraffin that takes by weighing in one set by step and vinylbenzene total mass takes by weighing methylacrylic acid, 0.5%～2% Dodecyl Mercaptan, 2%～5% X 2073,2%～10% Potassium Persulphate;
Step 3 joins the vinylbenzene that takes by weighing among step 1 and two, methylacrylic acid, Dodecyl Mercaptan in the deionized water, mixes, and stirring obtains solution.
Step 4 after the heating paraffin thawing that takes by weighing, joins in the solution of step 3 gained;
Step 5 joins the X 2073 that takes by weighing in the deionized water, is heated to 50 ℃;
Step 6 joins the X 2073 solution in the step 5 in the mixing solutions that step 3 obtains ultrasonic emulsification;
Step 7 joins the Potassium Persulphate that takes by weighing in the deionized water heating for dissolving;
Step 8 moves into a four-hole container that includes mechanical stirring, prolong, nitrogen inlet and charging opening with the mixture solution that obtains behind the step 6 ultrasonic emulsification;
Step 9, logical nitrogen deoxygenation be after 0.5 hour, heating in water bath to 70 ℃, and mechanical stirring slowly adds the resulting persulfate aqueous solution of step 7, initiated polymerization; Polymerization is cooled to room temperature after accomplishing, and obtains the multi-phase change material solution that microcapsule coat.
Step 10, vacuum filtration, drying obtain the powdered sample that microcapsule coat multi-phase change material.
Described paraffin comprises the alkane paraffin not of the same race that quality equates, is heated to 80 ℃, and making whole fusions is colourless transparent liquid, stirs thorough mixing.
Beneficial effect of the present invention:
The present invention coats multiple transformation temperature material different in microcapsule; When having kept original advantage of phase-change microcapsule; Strengthened the practicality of phase-change microcapsule, the transformation temperature scope is expanded and extended, and has enlarged the range of application of phase-change microcapsule.
Description of drawings
The structural representation of the multi-phase change material that Fig. 1 microcapsule coat.
The SEM figure of the multi-phase change material that Fig. 2 microcapsule coat.
The DSC figure of the multi-phase change material that Fig. 3 microcapsule coat.
Embodiment
Embodiment one
The preparing method's of the multi-phase change material that a kind of microcapsule coat step comprises:
Step 1 takes by weighing paraffin 6g, vinylbenzene 15g, methylacrylic acid 1.05g, Dodecyl Mercaptan 0.105g, X 2073 0.42g, Potassium Persulphate 0.42g;
Step 2 joins the vinylbenzene that takes by weighing, methylacrylic acid, Dodecyl Mercaptan in the 40g deionized water, mixes, and stirring obtains solution.
Step 3, the heating paraffin fusion that takes by weighing made uniform mixing after, join in the solution of step 2;
Step 4 joins the X 2073 that takes by weighing in the 20g deionized water, heating in water bath to 50 ℃;
Step 5 joins the X 2073 solution in the step 4 in the mixing solutions that step 2 obtains ultrasonic emulsification 5 minutes;
Step 6 joins the Potassium Persulphate that takes by weighing in the 20g deionized water heating for dissolving;
Step 7 has one of the mixing solutions immigration that obtains behind the step 5 ultrasonic emulsification in the four-hole boiling flask of mechanical stirring, prolong, nitrogen inlet and charging opening;
Step 8, logical nitrogen deoxygenation be after 0.5 hour, heating in water bath to 70 ℃, and 300 rev/mins of mechanical stirring slowly drip the persulfate aqueous solution that step 6 obtains, initiated polymerization; Polymerization is cooled to room temperature after accomplishing, and obtains the multi-phase change material solution that microcapsule coat.
Step 9, vacuum filtration, drying obtain the powdered sample that microcapsule coat multi-phase change material.
Employed paraffin is C
nH
2n+2, wherein, n
1=6, n
2=18, n
3=20; The mass ratio of its three kinds of paraffin 1: 1: 1 is heated to 80 ℃, and making whole fusions is colourless transparent liquid, stirs thorough mixing.
The structural representation of the multi-phase change material that microcapsule coat, as shown in Figure 1, its core is the mixture of different paraffin, its external shell material is the multipolymer of vinylbenzene and methylacrylic acid.
Embodiment two
The concrete steps of the heterogeneous height preparation methods that a kind of microcapsule coat:
Step 1 takes by weighing paraffin 6g, vinylbenzene 15g, methylacrylic acid 1.05g, Dodecyl Mercaptan 0.2g, X 2073 0.5g, Potassium Persulphate 1g;
Step 2 joins the vinylbenzene that takes by weighing, methylacrylic acid, Dodecyl Mercaptan in the 40g deionized water, mixes, and stirring obtains solution.
Step 3, the heating paraffin fusion that takes by weighing made uniform mixing after, join in the solution of step 2;
Step 4 joins the X 2073 that takes by weighing in the 20g deionized water, heating in water bath to 50 ℃;
Step 5 joins the X 2073 solution in the step 4 in the mixing solutions that step 2 obtains ultrasonic emulsification 5 minutes;
Step 6 joins the Potassium Persulphate that takes by weighing in the 20g deionized water heating for dissolving;
Step 7 has one of the mixing solutions immigration that obtains behind the step 5 ultrasonic emulsification in the four-hole boiling flask of mechanical stirring, prolong, nitrogen inlet and charging opening;
Step 8, logical nitrogen deoxygenation be after 0.5 hour, heating in water bath to 70 ℃, and 300 rev/mins of mechanical stirring slowly drip the persulfate aqueous solution that step 6 obtains, initiated polymerization; Polymerization is cooled to room temperature after accomplishing, and obtains the multi-phase change material solution that microcapsule coat.
Step 9, vacuum filtration, drying obtain the powdered sample that microcapsule coat multi-phase change material, and its sem photograph (SEM) is like Fig. 2.
Employed three kinds of paraffin are C
nH
2n+2, wherein, n
1=16, n
2=20, n
3=28; The mass ratio of its three kinds of paraffin 1: 1: 1 is heated to 80 ℃, and making whole fusions is colourless transparent liquid, stirs thorough mixing.
The structure of the phase change material that microcapsule coat, its core is the mixture of different paraffin, its shell material is the multipolymer of vinylbenzene and methylacrylic acid.
Embodiment three
The concrete steps of the heterogeneous height preparation methods that a kind of microcapsule coat:
Step 1 takes by weighing paraffin 6g, vinylbenzene 15g, methylacrylic acid 1.05g, Dodecyl Mercaptan 0.42g, X 2073 1.05g, Potassium Persulphate 2.1g;
Step 2 joins the vinylbenzene that takes by weighing, methylacrylic acid, Dodecyl Mercaptan in the 40g deionized water, mixes, and stirring obtains solution.
Step 3, the heating paraffin fusion that takes by weighing made uniform mixing after, join in the solution of step 2;
Step 4 joins the X 2073 that takes by weighing in the 20g deionized water, heating in water bath to 50 ℃;
Step 5 joins the X 2073 solution in the step 4 in the mixing solutions that step 2 obtains ultrasonic emulsification 5 minutes;
Step 6 joins the Potassium Persulphate that takes by weighing in the 30g deionized water heating for dissolving;
Step 7 has one of the mixing solutions immigration that obtains behind the step 5 ultrasonic emulsification in the four-hole boiling flask of mechanical stirring, prolong, nitrogen inlet and charging opening;
Step 8, logical nitrogen deoxygenation be after 0.5 hour, heating in water bath to 70 ℃, and 300 rev/mins of mechanical stirring slowly drip the persulfate aqueous solution that step 6 obtains, initiated polymerization; Polymerization is cooled to room temperature after accomplishing, and obtains the multi-phase change material solution that microcapsule coat.
Step 9, vacuum filtration, drying obtain the powdered sample that microcapsule coat multi-phase change material.
Employed three kinds of paraffin are C in three embodiments
nH
2n+2, wherein, n
1=16, n
2=20, n
3=32; The mass ratio of its three kinds of paraffin 1: 1: 1 is heated to 80 ℃, and making whole fusions is colourless transparent liquid, stirs thorough mixing.
The structure of the phase change material that microcapsule coat, its core is the mixture of different paraffin, its shell material is the multipolymer of vinylbenzene and methylacrylic acid.
Fig. 3 is differential scanning calorimetric (DSC) figure of the multi-phase change material that microcapsule coat, and is to inhale what of (putting) heat at the situation reflection sample of constant temperature rise rate, and each peak value place of this figure is the different transformation temperatures of counter sample respectively.
Claims (3)
1. the preparation method of the multi-phase change material that coats of microcapsule is characterized in that this preparing method's step comprises:
Step 1, by paraffin: cinnamic mass ratio is to get material at 2: 5;
Step 2,5% of paraffin that takes by weighing in one set by step and vinylbenzene total mass takes by weighing methylacrylic acid, 0.5%～2% Dodecyl Mercaptan, 2%～5% X 2073,2%～10% Potassium Persulphate;
Step 3 joins the vinylbenzene that takes by weighing among step 1 and two, methylacrylic acid, Dodecyl Mercaptan in the deionized water, mixes, and stirring obtains solution;
Step 4 after the heating paraffin thawing that takes by weighing, joins in the solution of step 3 gained;
Step 5 joins the X 2073 that takes by weighing in the deionized water, is heated to 50 ℃;
Step 6 joins the X 2073 solution in the step 5 in the mixing solutions that step 3 obtains ultrasonic emulsification;
Step 7 joins the Potassium Persulphate that takes by weighing in the deionized water heating for dissolving;
Step 8 moves into a four-hole container that includes mechanical stirring, prolong, nitrogen inlet and charging opening with the mixture solution that obtains behind the step 6 ultrasonic emulsification;
Step 9, logical nitrogen deoxygenation be after 0.5 hour, heating in water bath to 70 ℃, and mechanical stirring slowly adds the resulting persulfate aqueous solution of step 7, initiated polymerization; Polymerization is cooled to room temperature after accomplishing, and obtains the multi-phase change material solution that microcapsule coat;
Step 10, vacuum filtration, drying obtain the powdered sample that microcapsule coat multi-phase change material.
2. the preparation method of the multi-phase change material that a kind of microcapsule according to claim 1 coat; It is characterized in that; Described paraffin total mass is 2/5 of a vinylbenzene quality, and paraffin is made up of quality such as alkane paraffin not of the same race, is heated to 80 ℃; Making whole fusions is colourless transparent liquid, stirs thorough mixing.
3. a kind of microcapsule according to claim 2 coat the preparation method of multi-phase change material, it is characterized in that the molecular formula of described alkane paraffin is C
nH
2n+2, wherein, 6≤n≤32, and paraffin uniform mixing not of the same race.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017208004A1 (en) | 2016-06-03 | 2017-12-07 | The University Of Nottingham | Encapsulated phase change materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592434A (en) * | 2014-12-29 | 2015-05-06 | 三棵树涂料股份有限公司 | High-solid content environment-friendly phase transition microcapsule and preparation method thereof |
| CN106758264B (en) * | 2016-11-15 | 2019-03-15 | 浙江英凡新材料科技有限公司 | A kind of production method of temperature-regulating fiber, temperature-regulating fiber and thermostat quilt |
| CN108129923A (en) * | 2017-12-30 | 2018-06-08 | 嘉力丰科技股份有限公司 | New-type phase change energy storage wall paper-based membrane and preparation method thereof and construction technology |
| CN115386344A (en) * | 2021-05-25 | 2022-11-25 | 中国石油天然气股份有限公司 | Paraffin-based composite phase change microcapsule and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1321182A1 (en) * | 2001-12-20 | 2003-06-25 | Basf Aktiengesellschaft | Microcapsules |
| WO2004092299A1 (en) * | 2003-04-17 | 2004-10-28 | Basf Aktiengesellschaft | Use of aqueous microcapsule dispersions as heat transfer liquids |
| CN1657587A (en) * | 2004-12-30 | 2005-08-24 | 北京巨龙博方科学技术研究院 | Preparation method of phase transformation material for microcapsult packing and forming |
| CN101306341A (en) * | 2008-07-02 | 2008-11-19 | 深圳先进技术研究院 | Phase-change accumulation energy microcapsule prepared by interfacial polymerization method and its method |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1321182A1 (en) * | 2001-12-20 | 2003-06-25 | Basf Aktiengesellschaft | Microcapsules |
| WO2004092299A1 (en) * | 2003-04-17 | 2004-10-28 | Basf Aktiengesellschaft | Use of aqueous microcapsule dispersions as heat transfer liquids |
| CN1774489A (en) * | 2003-04-17 | 2006-05-17 | 巴斯福股份公司 | Use of aqueous microcapsule dispersions as heat transfer liquids |
| CN1657587A (en) * | 2004-12-30 | 2005-08-24 | 北京巨龙博方科学技术研究院 | Preparation method of phase transformation material for microcapsult packing and forming |
| CN101306341A (en) * | 2008-07-02 | 2008-11-19 | 深圳先进技术研究院 | Phase-change accumulation energy microcapsule prepared by interfacial polymerization method and its method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017208004A1 (en) | 2016-06-03 | 2017-12-07 | The University Of Nottingham | Encapsulated phase change materials |
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