CN110862804A - Phase-change material microcapsule with internal heat channel and preparation method thereof - Google Patents
Phase-change material microcapsule with internal heat channel and preparation method thereof Download PDFInfo
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- CN110862804A CN110862804A CN201810990926.8A CN201810990926A CN110862804A CN 110862804 A CN110862804 A CN 110862804A CN 201810990926 A CN201810990926 A CN 201810990926A CN 110862804 A CN110862804 A CN 110862804A
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/04—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C08G12/10—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with acyclic compounds having the moiety X=C(—N<)2 in which X is O, S or —N
- C08G12/12—Ureas; Thioureas
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08G12/34—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds and acyclic or carbocyclic compounds
- C08G12/36—Ureas; Thioureas
- C08G12/38—Ureas; Thioureas and melamines
Abstract
Adding high-thermal-conductivity materials such as graphene, graphene oxide, carbon black and carbon nanotubes in the preparation process of the microcapsule wall material prepolymer to disperse the materials in the wall material of the microcapsule; simultaneously, mixing the high-thermal-conductivity nano material with the phase-change material to realize the dispersion of the high-thermal-conductivity material in the phase-change material microcapsule core material; and graphene oxide or modified graphene oxide is used as a dispersing agent to prepare an oil-in-water emulsion, and a continuous cross-linking heat conduction channel is formed in the phase change material microcapsule prepared by in-situ polymerization, so that the heat conductivity of the phase change material microcapsule is improved.
Description
Technical Field
The invention relates to the technical field of phase change material microcapsules, in particular to a phase change material microcapsule with an internal heat channel and a preparation method thereof.
Background
The phase-change energy storage material absorbs or releases a large amount of heat in the phase-change process, can realize the storage and utilization of energy and the control of temperature, is beneficial to improving the energy utilization efficiency, and can be widely applied to the fields of energy-saving energy storage, building materials, aerospace, thermal management and the like. The phase-change material microcapsule is an effective heat energy storage material and is prepared by taking a phase-change material as a core material and a film-forming material as a wall material. The phase-change material microcapsule effectively solves the problem of phase-change material leakage, prevents the reaction of a phase-change substance and the surrounding environment, improves the use efficiency of the phase-change material, increases the heat transfer surface area, is a material with high application value, and has low heat conductivity coefficient which is a key problem restricting the application of the material. The invention discloses a high-thermal-conductivity phase-change material microcapsule prepared by an in-situ polymerization method and a preparation method thereof.
At present, there are several patents that utilize the addition of highly heat conductive materials to enhance the thermal conductivity of phase change material microcapsules. Patent 201710220760.7 adds nano copper and nano graphene sheets in both wall material and core material; patent 201711097673.3 adds nano titanium dioxide, nano copper and nano alumina in the core material. In patent 201711101732.X, modified graphene oxide is coated outside a microcapsule to enhance the thermal conductivity of the microcapsule; patent 201710148400.0 discloses a phase-change material microcapsule with carbon nanotubes and graphene oxide doped in the wall material prepared by in-situ polymerization method using graphene oxide and carbon nanotubes as heat conductive filler; patent 20161045625x adding nanoparticles such as modified boron nitride, carbon nanotube or graphene oxide into wall material and core material of phase change material microcapsule; patent 201410006689.9 discloses that graphene oxide is used as a surfactant and wall material of thermal conductivity enhancing material to increase the thermal conductivity of the microcapsule.
The phase change material microcapsule is coated by graphene oxide in the above documents; or 2D nano materials such as graphene oxide and the like are taken as heat conducting fillers and added into the wall material and the core material; or adding heat conduction reinforcing materials into the wall materials and the core materials of the microcapsules; or the phase-change material microcapsule is prepared by using the graphene oxide as a surfactant and a heat conduction reinforcing material. According to the invention, the nano heat conduction material can be simultaneously added into the wall material and the core material of the phase-change material microcapsule, the amphiphilic graphene oxide is used as a surfactant to form a high heat conduction layer at the interface of the wall material and the core material, and a continuous cross-linking heat conduction channel is formed in the microcapsule, so that the heat conduction coefficient of the phase-change material microcapsule is further improved.
Disclosure of Invention
The invention provides a phase change material microcapsule with an internal heat channel and a preparation method thereof, aiming at the problem of low heat conductivity coefficient of the microcapsule in the prior art.
The invention utilizes an in-situ polymerization method to prepare the phase change material microcapsule with high thermal conductivity. Adding high-thermal-conductivity materials such as graphene, graphene oxide, carbon black and carbon nanotubes in the preparation process of the microcapsule wall material prepolymer, and dispersing the high-thermal-conductivity materials serving as the thermal-conductivity materials in the wall material of the microcapsule; simultaneously, high-thermal-conductivity nano materials such as graphene, graphene oxide, carbon black and carbon nano tubes are mixed with the phase-change material, so that the dispersion of the high-thermal-conductivity material in the phase-change material microcapsule core material is realized; and preparing the oil-in-water emulsion by using the graphene oxide or the modified graphene oxide as a dispersing agent. The prepared microcapsule realizes the continuity of the distribution of the high heat conduction material at the wall material, the core material and the interface, and forms a continuous cross-linking heat conduction channel in the microcapsule, thereby improving the heat conductivity of the microcapsule.
The preparation method provided by the invention comprises the following steps:
1) preparing a microcapsule wall material prepolymer: weighing urea and 37% of formaldehyde solution, mixing in deionized water, adjusting the pH value of the solution to 8.5-9, heating to 70 ℃, mixing at a stirring speed of 200rpm, reacting for 1 hour, adding a nano heat-conducting filler with the mass of 0.1-10% of that of a wall material, and performing ultrasonic dispersion to prepare a prepolymer solution for later use;
2) preparing a high-thermal-conductivity paraffin wax core material: melting paraffin, adding heat conduction materials such as graphene/graphene oxide/carbon black/carbon nano tubes and the like with the mass of 0.1-10% of the paraffin, and ultrasonically dispersing uniformly to form a nano heat conduction reinforced phase change material;
3) preparation of oil-in-water emulsion: mixing the graphene oxide dispersion liquid with the graphene-paraffin phase-change material prepared in the step (2), and stirring for 10min at a stirring speed of 7000rpm in a constant-temperature water bath at 70 ℃ to prepare an oil-in-water emulsion;
4) preparing microcapsules: and (3) adding the prepolymer solution prepared in the step (1) into the oil-in-water emulsion prepared in the step (3), reducing the pH value to 3-4, and reacting for 4 hours at a stirring speed of 500rpm and a temperature of 70 ℃. And filtering the microcapsule obtained by the reaction, and drying to obtain the phase-change material microcapsule.
Preferably, in the step (1), urea and a 37% formaldehyde solution are used as reaction monomers, or melamine and a 37% formaldehyde solution, urea-melamine-formaldehyde copolycondensation resin and the like are used as reaction monomers.
Preferably, the heat conductive filler in step (1) is one or more of carbon nanotubes, carbon black, graphene oxide, nano graphite, and the like.
Preferably, in the step (2), graphene oxide, graphene, carbon nanotubes and the like are used as core materials of the heat-conducting filling material.
Preferably, in the step (3), graphene oxide is used as a dispersion liquid or modified graphene oxide is used as a dispersion liquid.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a photomicrograph of a graphene oxide coated paraffin-carbon black oil-in-water dispersion.
Fig. 2 is a photograph of a phase change material microcapsule.
In the figure: 1. an oil-water interface with dispersed graphene oxide, 2, paraffin, 3 and carbon black.
Detailed Description
The invention is further described with reference to the following figures and specific examples.
Example 1:
the phase-change material microcapsule is prepared by the following steps:
step one, preparing a microcapsule wall material prepolymer solution: weighing 1.5g of urea and 3.2g of 37% formaldehyde solution, mixing in deionized water, adjusting the pH value of the solution to 8.5-9, heating to 70 ℃, reacting for 1 hour at a stirring speed of 200rpm, then adding carbon nanotube dry powder with the mass of 1% of the wall material, and performing ultrasonic dispersion to prepare a prepolymer solution for later use.
Step two, preparing a carbon black/paraffin wax core material: melting 10g of paraffin, adding carbon black accounting for 10% of the mass of the paraffin, and ultrasonically dispersing uniformly to prepare the carbon black-paraffin phase-change material for later use.
Step three, preparing an oil-in-water emulsion: the prepared carbon black-paraffin phase-change material is added into a beaker with the temperature of 70 ℃, 2ml of 5mg/ml graphene oxide dispersion liquid is added after the core material is melted, and the mixture is stirred for 10 minutes at the stirring speed of 7000rpm, so that an oil-in-water emulsion is prepared, as shown in figure 1.
Step four, microcapsule preparation: pouring the solution of the prepolymer into an oil-in-water emulsion, reducing the pH value to 3-4, reacting for 4 hours at a stirring speed of 500rpm and a temperature of 70 ℃, filtering and drying the microcapsule obtained by the reaction to obtain the phase-change material microcapsule, as shown in figure 2.
Example 2:
step one, preparing a microcapsule wall material prepolymer solution: weighing 1.5g of urea and 3.2g of 37% formaldehyde solution, mixing in deionized water, adjusting the pH value of the solution to 8.5-9, heating to 70 ℃, reacting for 1 hour at a stirring speed of 200rpm, then adding graphene oxide dry powder with the mass of 0.1% of that of the wall material, and performing ultrasonic dispersion to prepare a prepolymer solution for later use.
Step two, preparing a graphene/paraffin core material: melting 10g of paraffin, adding graphene with the mass of 0.1% of that of the paraffin, and performing ultrasonic dispersion uniformly to form the graphene-paraffin phase-change material for later use.
Step three, utilizing KH550 modified graphene oxide: 12.5mg of KH550 solution was weighed, 5ml of absolute ethanol was added, the beaker was gently shaken for 1min, and 50g of deionized water and 10ml of graphene oxide dispersion (5 mg/ml) were added. And heating the mixed solution to 90 ℃, and stirring for reacting for 6 hours to obtain the modified graphene oxide solution.
Step four, preparing an oil-in-water emulsion: adding the prepared graphene-paraffin phase-change material into a beaker at the temperature of 70 ℃, adding 2ml of 5mg/ml graphene oxide dispersion liquid after melting a core material, and stirring at the stirring speed of 7000rpm for 10 minutes to prepare the oil-in-water emulsion.
Step five, microcapsule preparation: and pouring the solution of the prepolymer into an oil-in-water emulsion, reducing the pH value to 4, keeping the solution at the stirring speed of 500rpm and the temperature of 70 ℃ for 4 hours, and filtering and drying the microcapsules obtained by reaction to obtain the phase-change material microcapsules.
Example 3:
step one, preparing a microcapsule wall material prepolymer solution: weighing 2g of melamine and 3.2g of 37% formaldehyde solution, mixing in deionized water, adjusting the pH value of the solution to 8.5-9, heating to 70 ℃, mixing at a stirring speed of 200rpm until the suspension becomes transparent, adding carbon black with the mass of 1% of the wall material, and performing ultrasonic dispersion to prepare a prepolymer solution for later use.
Step two, preparing a carbon nano tube/paraffin wax core material: melting 10g of paraffin, adding carbon nano tubes with the mass of 1% of the paraffin, and performing ultrasonic dispersion uniformly to form the carbon nano tube-paraffin phase-change material.
Step three, preparing an oil-in-water emulsion: adding the prepared carbon nano tube-paraffin phase-change material into a beaker at the temperature of 70 ℃, adding 2ml of 5mg/ml graphene oxide dispersion liquid after melting a core material, and stirring at the stirring speed of 7000rpm for 10 minutes to prepare the oil-in-water emulsion.
Step four, microcapsule preparation: and pouring the solution of the prepolymer into an oil-in-water emulsion, reducing the pH value to 3, reacting for 4 hours at the stirring speed of 500rpm and the temperature of 70 ℃, and filtering and drying the suspension obtained by the reaction to obtain the phase-change material microcapsule.
In addition to the technical features described in the specification, the technology is known to those skilled in the art.
Claims (4)
1. A method of making a phase change material microcapsule having an internal thermal pathway, the method comprising the steps of:
(1) preparing a microcapsule wall material prepolymer composite high-heat-conductivity material: adding high heat conduction material with the wall material mass of 0.1-10% into the prepared microcapsule wall material polymer, and preparing a composite prepolymer solution for later use;
(2) preparing a high-thermal-conductivity paraffin wax core material: melting paraffin, adding high heat conduction material with the mass of 0.1-10% of the paraffin, and uniformly dispersing by ultrasonic to form a nano heat conduction reinforced phase change material;
(3) melting the nano heat conduction reinforced phase change material prepared in the step (2), adding a proper amount of water and an amphiphilic nano material, and performing high-speed dispersion to prepare an oil-in-water emulsion;
(4) and (2) adding the prepolymer prepared in the step (1) into the oil-in-water emulsion prepared in the step (3), reducing the pH value to 3-4, and reacting for 4 hours at a stirring speed of 500rpm and a temperature of 70 ℃ to prepare the phase-change material microcapsule.
2. The method for preparing a phase change material microcapsule with high thermal conductivity according to claim 1, wherein the prepolymer in the step (1) is urea-formaldehyde resin prepolymer, melamine-formaldehyde resin prepolymer or urea-melamine-formaldehyde resin prepolymer.
3. The method for preparing the phase change material microcapsule with high thermal conductivity according to claim 1, wherein the high thermal conductivity material in steps (1) and (2) is one or more combinations of graphene, graphene oxide, carbon black, carbon nanotubes, nano graphite, and the like.
4. The method for preparing a phase change material microcapsule with high thermal conductivity according to claim 1, wherein the amphiphilic nanomaterial in step (3) is graphene oxide or modified graphene oxide.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111518522A (en) * | 2020-06-09 | 2020-08-11 | 长沙理工大学 | Preparation method of graphite modified phase-change microcapsule |
| CN112121738A (en) * | 2020-09-28 | 2020-12-25 | 杭州应星新材料有限公司 | Preparation method of functionalized microcapsule and functionalized microcapsule prepared by preparation method |
| CN113429632A (en) * | 2021-07-19 | 2021-09-24 | 青岛科技大学 | High-thermal-conductivity expandable graphite microcapsule and preparation method and application thereof |
| CN114029009A (en) * | 2021-11-22 | 2022-02-11 | 哈尔滨工业大学 | Preparation method of high-efficiency and environment-friendly graphene-paraffin phase-change microcapsule material |
| CN114716983A (en) * | 2022-04-11 | 2022-07-08 | 安徽陆海石油助剂科技有限公司 | Composite emulsifier for oil-based drilling fluid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114029009A (en) * | 2021-11-22 | 2022-02-11 | 哈尔滨工业大学 | Preparation method of high-efficiency and environment-friendly graphene-paraffin phase-change microcapsule material |
| CN114716983A (en) * | 2022-04-11 | 2022-07-08 | 安徽陆海石油助剂科技有限公司 | Composite emulsifier for oil-based drilling fluid |
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Application publication date: 20200306 |