CN107722943A - A kind of preparation method of wax phase change microcapsules - Google Patents
A kind of preparation method of wax phase change microcapsules Download PDFInfo
- Publication number
- CN107722943A CN107722943A CN201711108499.8A CN201711108499A CN107722943A CN 107722943 A CN107722943 A CN 107722943A CN 201711108499 A CN201711108499 A CN 201711108499A CN 107722943 A CN107722943 A CN 107722943A
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- paraffin
- preparation
- phase change
- wax
- microcapsules
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/18—In situ polymerisation with all reactants being present in the same phase
- B01J13/185—In situ polymerisation with all reactants being present in the same phase in an organic phase
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The present invention is applied to phase-change accumulation energy field, there is provided a kind of preparation method of wax phase change microcapsules, including step：Prepare cyanurotriamide modified urea resin prepolymer solution；Paraffin, emulsifier solution are added in prepolymer solution paraffin wax emulsions are made；The pH value of paraffin wax emulsions is adjusted to 3, constant temperature stirring carries out home position polymerization reaction and obtains the wax phase change microcapsules using cyanurotriamide modified urea resin as wall material.Phase-change microcapsule prepared by the present invention has the advantages that particle diameter is small, phase transition performance is excellent, stability is good, may be directly applied to the fields such as building heat preservation, solar energy drying, weaving.
Description
Technical field
The present invention relates to phase-change accumulation energy field, specifically, is related to a kind of preparation method of wax phase change microcapsules.
Background technology：
Phase-change accumulation energy refers to that phase-change material occurs in phase transition process, and heat is absorbed or released in a manner of latent heat,
Stored in less temperature range or discharge substantial amounts of heat.It is stable paraffin can be changed using microcapsules technology cladding paraffin
Property poor, easily leakage, the problems such as easily permeating.
Paraffin because having a good thermal storage performance, and without supercooling, be separated, there is corrosivity, become conventional
Phase-changing energy storage material.But be but not easy to paraffin microcapsuleization, this is primarily due to system in microcapsules forming process
PH value be difficult to control.PH value is excessive, can make the microcapsules softgel shell low intensity to be formed；PH value is too small, cyst wall formed it is too fast, can not
Cladding paraffin completely；Both of these case can all cause the clad ratio of microcapsules to reduce.And in the prior art, the paraffin being prepared
Core is that low melt point paraffin, wall material are mostly Lauxite mostly in microcapsules, therefore it is wall to prepare cyanurotriamide modified urea resin
The technology of the medium temperature paraffin microcapsule of material is still highly significant.
For Lauxite, the water resistance of cyanurotriamide modified urea resin is more preferable, can improve microcapsules capsule
The stability of shell；Simultaneously in microcapsules forming process, melamine is easier to react with formaldehyde compared with urea, it is easier to
Core surfaces form microcapsules softgel shell, so as to improve the clad ratio of microcapsules.
The stability of paraffin can be improved by preparing cyanurotriamide modified urea resin paraffin microcapsule, promote paraffin microcapsule
Application in phase-change accumulation energy field.
The content of the invention
The purpose of the present invention is to propose to it is a kind of can prepare have it is good with melamine modified urea compared with small particle, stability
Urea formaldehyde is the method for the wax phase change microcapsules of wall material, solves the problems, such as poor wax stability, easy leakage and existing paraffin
The technical problem of softgel shell poor water resistance in microcapsules technology.
The present invention is achieved in that the stone prepared by situ aggregation method using cyanurotriamide modified urea resin as wall material
The method of wax phase-change microcapsule, the preparation method of described wax phase change microcapsules include step：
Prepare cyanurotriamide modified urea resin performed polymer；
Paraffin, emulsifier solution are added in prepolymer solution, prepare paraffin wax emulsions；And
Paraffin wax emulsions pH value is adjusted to 3 or so, carry out home position polymerization reaction obtain using cyanurotriamide modified urea resin as
Wall material, paraffin are the phase-change microcapsule suspension of core.
The wax phase change provided by the invention prepared by situ aggregation method using cyanurotriamide modified urea resin as wall material
The method of microcapsules, gained microcapsules are applied to phase-change accumulation energy field.The present invention is using OP-10 as emulsifying agent.In microcapsules
In preparation process, OP-10 not with paraffin react, and formed emulsion-stabilizing, be not easy to be demulsified, it is ensured that gained microcapsules have
Higher clad ratio.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, the present invention is carried out further detailed
Explanation.It should be appreciated that specific embodiment described herein is not intended to limit the present invention only to explain the present invention.
A kind of preparation method of wax phase change microcapsules includes step：
The first step, prepare cyanurotriamide modified urea resin performed polymer；
Second step, paraffin, emulsifier solution are added in prepolymer solution, prepare paraffin wax emulsions；And
3rd step, regulation paraffin wax emulsions pH value to 3 or so, carry out home position polymerization reaction and obtain with melamine modified urea-formaldehyde
Resin is wall material, and paraffin is the phase-change microcapsule suspension of core；
4th step, above-mentioned reaction product is stood, wash, filter, is dried to constant weight, obtain phase-change microcapsule powder.
In the first step, the formalin that urea, 12.6g melamines, 50g mass fractions that quality is 9g are 37% is mixed
Close, adjust pH value to 8 or so with triethanolamine, with electric blender under 700r/min rotating speeds, 70 DEG C of isothermal reaction 1h, obtain
Cyanurotriamide modified urea resin performed polymer；
In second step, the formalin of 80g paraffin, 6.4g mass fractions 50% is mixed to join in 40g performed polymers, instead
It is 1200r/min to answer rotating speed, and reaction temperature is 60 DEG C, emulsifies 30min, forms stable paraffin wax emulsions；
In the third step, reaction rotating speed is first reduced to 540r/min, and keeping temperature is 60 DEG C；Quality point is added dropwise thereto again
Number is 10% citric acid solution, and regulation pH value is warming up to 70 DEG C, insulation reaction 2h to 3 or so after insulation reaction 1h；
In the 4th step, cleaned, filtered with deionized water again after being cleaned twice with petroleum ether, baking oven is dried at 60 DEG C
Constant weight, obtain microscapsule powder.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement done within refreshing and principle etc., should be included in the scope of the protection.
Claims (6)
1. a kind of preparation method of wax phase change microcapsules, comprises the following steps：
The first step, prepare cyanurotriamide modified urea resin performed polymer；
Second step, paraffin, emulsifier solution are added in prepolymer solution, prepare paraffin wax emulsions；
3rd step, regulation paraffin wax emulsions pH value to 3 or so, carry out home position polymerization reaction and obtain with cyanurotriamide modified urea resin
For wall material, paraffin is the phase-change microcapsule suspension of core；
4th step, above-mentioned reaction product is stood, wash, filter, is dried to constant weight, obtain phase-change microcapsule powder.
2. the preparation method of wax phase change microcapsules as claimed in claim 1, it is characterised in that in the first step, will rub
You are than being 1：2：7 melamine, urea, formaldehyde mixing, add 100ml deionized waters, and pH value is adjusted to 8 left with triethanolamine
The right side, with 700r/min rotating speed, 70 DEG C of reaction 1h of constant temperature are kept, obtain cyanurotriamide modified urea resin performed polymer.
3. the preparation method of wax phase change microcapsules as claimed in claim 1, it is characterised in that in the second step, emulsification
Agent is OP-10 nonionic surface active agent, and the dosage of emulsifying agent is the 8% of Quality of Paraffin Waxes used, and the temperature of emulsion reaction is
60 DEG C, speed of agitator 1200r/min, emulsification times 30min.
4. the preparation method of wax phase change microcapsules as claimed in claim 1, it is characterised in that in the 3rd step, use
The citric acid solution that mass fraction is 10% adjusts pH value.
5. the preparation method of wax phase change microcapsules as claimed in claim 1, it is characterised in that in the 3rd step, first will
Reaction rotating speed is reduced to 540r/min, and temperature is 60 DEG C；Then it is 3 to adjust pH value, after insulation reaction 1h, then from 60 DEG C is increased to 70
DEG C, insulation reaction 2h.
6. the preparation method of wax phase change microcapsules as claimed in claim 1, it is characterised in that in the 4th step, use stone
Oily ether washs 2 times, it is therefore an objective to removes the paraffin residues that surface of microcapsule is not coated completely；Then it is washed with deionized and takes out
Filter, drying temperature are 60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711108499.8A CN107722943A (en) | 2017-11-09 | 2017-11-09 | A kind of preparation method of wax phase change microcapsules |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711108499.8A CN107722943A (en) | 2017-11-09 | 2017-11-09 | A kind of preparation method of wax phase change microcapsules |
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| Publication Number | Publication Date |
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| CN107722943A true CN107722943A (en) | 2018-02-23 |
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| CN201711108499.8A Pending CN107722943A (en) | 2017-11-09 | 2017-11-09 | A kind of preparation method of wax phase change microcapsules |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108300425A (en) * | 2018-03-01 | 2018-07-20 | 苏州维洛克电子科技有限公司 | The preparation method of polyester sheet containing accumulation energy microcapsule |
| CN108300428A (en) * | 2018-03-22 | 2018-07-20 | 云南省交通规划设计研究院 | It is a kind of to inhibit phase-change microcapsule and preparation method icy on road |
| CN109925985A (en) * | 2019-03-15 | 2019-06-25 | 湖州闪思新材料科技有限公司 | A kind of methods and applications of phase-change material micro-capsule cladding |
| CN110343511A (en) * | 2019-07-31 | 2019-10-18 | 北京林业大学 | A kind of nano-zirconium carbide modified paraffin phase-change microcapsule and preparation method thereof |
| CN111545142A (en) * | 2020-05-21 | 2020-08-18 | 中国石油大学(华东) | High-temperature phase-change constant-temperature microcapsule, active temperature-control high-temperature drilling fluid system, and preparation and application thereof |
| CN114277971A (en) * | 2021-12-27 | 2022-04-05 | 广东乾兴建设工程有限公司 | Building energy-saving structure and building energy-saving method |
| CN115287047A (en) * | 2022-08-30 | 2022-11-04 | 长安大学 | Phase-change microcapsule for pavement temperature control, high-temperature phase-change thermoregulation asphalt and preparation method thereof |
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| EP1382656A1 (en) * | 2002-07-15 | 2004-01-21 | Kun-Hsiang Huang | Heat-absorbing particle |
| CN101879426A (en) * | 2010-04-19 | 2010-11-10 | 天津大学 | Gelatin modified urea formaldehyde electrophoretic microcapsule and preparation method thereof |
| CN102268238A (en) * | 2011-06-10 | 2011-12-07 | 朴英奎 | Phase change energy storage material and production method for microcapsules |
| CN103102552A (en) * | 2013-03-12 | 2013-05-15 | 泰山体育产业集团有限公司 | Phase-changed heat insulation polyolefin foam material and preparation method thereof |
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| CN101879426A (en) * | 2010-04-19 | 2010-11-10 | 天津大学 | Gelatin modified urea formaldehyde electrophoretic microcapsule and preparation method thereof |
| CN102268238A (en) * | 2011-06-10 | 2011-12-07 | 朴英奎 | Phase change energy storage material and production method for microcapsules |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108300425A (en) * | 2018-03-01 | 2018-07-20 | 苏州维洛克电子科技有限公司 | The preparation method of polyester sheet containing accumulation energy microcapsule |
| CN108300428A (en) * | 2018-03-22 | 2018-07-20 | 云南省交通规划设计研究院 | It is a kind of to inhibit phase-change microcapsule and preparation method icy on road |
| CN108300428B (en) * | 2018-03-22 | 2020-11-03 | 云南省交通规划设计研究院 | Phase change microcapsule for inhibiting road icing and preparation method thereof |
| CN109925985A (en) * | 2019-03-15 | 2019-06-25 | 湖州闪思新材料科技有限公司 | A kind of methods and applications of phase-change material micro-capsule cladding |
| CN110343511A (en) * | 2019-07-31 | 2019-10-18 | 北京林业大学 | A kind of nano-zirconium carbide modified paraffin phase-change microcapsule and preparation method thereof |
| CN111545142A (en) * | 2020-05-21 | 2020-08-18 | 中国石油大学(华东) | High-temperature phase-change constant-temperature microcapsule, active temperature-control high-temperature drilling fluid system, and preparation and application thereof |
| CN114277971A (en) * | 2021-12-27 | 2022-04-05 | 广东乾兴建设工程有限公司 | Building energy-saving structure and building energy-saving method |
| CN115287047A (en) * | 2022-08-30 | 2022-11-04 | 长安大学 | Phase-change microcapsule for pavement temperature control, high-temperature phase-change thermoregulation asphalt and preparation method thereof |
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Application publication date: 20180223 |