CN113372671B - Phase-change heat storage film and preparation method thereof - Google Patents
Phase-change heat storage film and preparation method thereof Download PDFInfo
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- 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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- 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
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
Abstract
The invention discloses a phase-change heat storage film and a preparation method thereof, wherein the raw materials comprise a phase-change material and a high-molecular film-forming material, and the high-molecular film-forming material accounts for 30-70% and the phase-change material accounts for 30-70% by weight; the phase-change material comprises the following components in parts by weight: 200-700 parts of a porous adsorption material, 200-600 parts of an organic phase change material, 35-70 parts of an emulsifier, 300-600 parts of water, 200-500 parts of an emulsification auxiliary material and 2-10 parts of an interface stabilizer. The invention can effectively improve the content of the phase-change material in the film material, and the phase-change material can not volatilize to cause the phase-change material to lose efficacy when the film is formed at high temperature.
Description
Technical Field
The invention relates to the technical field of phase-change material production, in particular to a phase-change heat storage film and a preparation method thereof.
Background
With the development of electronic technology, the heat dissipation power and the heat dissipation density of an electronic chip are increasingly improved, and the requirement on the thermal control of the electronic chip is also increasingly higher. Phase change energy storage thermal control has become one of the most important passive thermal control means of electronic devices due to the advantages of high energy storage density, small temperature fluctuation, simple system, convenient operation and the like.
In order to prevent the phase-change material from leaking in a liquid state, the traditional phase-change heat storage film is manufactured by using a process for coating the phase-change material, such as microcapsules, but the production process of the microcapsules is complex, and the production is difficult, so the use cost is high. Although the problem of leakage of the phase-change material in the liquid state can be solved by using the porous adsorption material, the raw materials of the phase-change heat storage film are difficult to mix, the content of the phase-change material which can be added into the phase-change heat storage film is low, usually only about 10% -30%, and thus the energy storage density of the product is low. In addition, in the above-mentioned mode phase-change material film-forming process, if the film-forming temperature is too high, the phase-change material is still easy to volatilize, which can cause phase-change temperature runaway failure.
Disclosure of Invention
The invention aims to provide a phase-change heat storage film and a preparation method thereof, which can effectively improve the content of a phase-change material in a film material, and the phase-change material cannot volatilize to cause failure of the phase-change material during high-temperature film formation.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a phase-change heat storage film comprises raw materials and a heat storage layer, wherein the raw materials comprise a phase-change material and a high-molecular film-forming material, and the high-molecular film-forming material accounts for 30-70% and the phase-change material accounts for 30-70% by weight;
the phase-change material comprises the following components in parts by weight: 200-700 parts of a porous adsorption material, 200-600 parts of an organic phase change material, 35-70 parts of an emulsifier, 300-600 parts of water, 200-500 parts of an emulsification auxiliary material and 2-10 parts of an interface stabilizer.
In order to solve the problem of leakage of the phase-change material, the phase-change material is physically adsorbed by using the porous material, and basically, no leakage exists.
Usually, powder particles are directly mixed into a film-forming material, the content of the added phase-change material is very low, usually about 10-30 percent, in order to solve the problems of difficult mixing and low content of the traditional powder, the secondary emulsification process is utilized to ensure that the content of the phase-change material in the phase-change heat storage film can reach more than 80 percent.
The porous adsorption material is selected from one or more of silicon dioxide, activated carbon, expanded graphite, activated silica gel, alumina, molecular sieve, bentonite and bentonite.
The organic phase change material is selected from one or more of straight-chain alkane, branched-chain alkane, unsaturated alkane, silicone wax, alkene and alkyne.
The emulsifier is one or more selected from ceteareth-12, ceteareth-20, ceteareth-30, sorbitan fatty acid ester 80, and sorbitan monooleate polyoxyethylene ether.
The emulsification auxiliary material is selected from one or more saturated alkanes with less than 14 carbons.
The emulsification auxiliary material is n-tetradecane or n-dodecane.
The interface stabilizer is sodium carboxymethyl cellulose.
The polymer film-forming material is selected from one or more of polyurethane emulsion, styrene-acrylic emulsion and acrylic emulsion. The solid content of the polymer film-forming material is 30-50%.
The preparation method of the phase-change heat storage film comprises the following steps:
(1) treating the porous adsorption material in a muffle furnace at a set temperature of 600-700 ℃ for 1-2 hours; this step is intended to remove impurities; (2) heating an organic phase change material to 70-75 ℃, adding the organic phase change material into the porous adsorption material treated in the step (1), uniformly stirring, putting the mixture into a vacuum oven at 100-105 ℃, and drying for 22-28 hours; the vacuum drying in the step aims to improve the adsorption capacity of the porous material to the organic phase-change material;
(3) washing the porous material loaded with the organic phase change material in the step (2) by using an organic solvent, and drying the porous material in an oven at the temperature of 80-85 ℃ for 10-14 hours to obtain phase change powder;
(4) adding part of water into the emulsification auxiliary material, heating to 80-85 ℃, adding part of emulsifier, stirring and uniformly mixing to prepare an emulsion A;
(5) stirring and mixing the interface stabilizer and the balance of water at 30-35 ℃ for 30-35 min, adding the phase change powder under the condition of maintaining the temperature and stirring, and mixing for 2-3 hours to prepare a prefabricated product B;
(6) heating the emulsified product A to 80-85 ℃, adding the rest of the emulsifier at the rotation speed of 400-600 rpm, then slowly dripping the prefabricated product B, and after finishing dripping, increasing the rotation speed to 2000-2500 rpm, and shearing and emulsifying for 25-35 minutes to prepare an emulsified product C; (7) and uniformly mixing the emulsified product C and the high-molecular film forming material, coating the mixture into a film with the thickness of 0.3-0.8 mm by using a film coating machine, and drying and forming at 90-95 ℃.
In the step (4), the using amount of the water accounts for 50-70% of the total using amount of the water, and the using amount of the emulsifier accounts for 40-55% of the total using amount of the emulsifier.
The invention has the beneficial effects that:
1. the traditional inorganic powder and organic material and liquid materials such as water and the like have large density difference, and the inorganic powder with large density is always settled at the bottom and is difficult to disperse uniformly, so the traditional emulsion preparation method is difficult to have good emulsification effect. According to the invention, an inorganic material adsorbs an organic phase-change material to form phase-change powder, and then the phase-change powder is prepared into high-content emulsion by a secondary emulsification method, so that the problem of compatibility of the powder material and other film materials can be effectively solved, and the content of the phase-change material in the film material can be effectively improved.
2. The invention can effectively solve the problem of high temperature resistance of the phase change material, and a protective film is formed on the surface of the phase change material after high-temperature demulsification through a secondary emulsification process, so that the phase change material cannot volatilize to cause failure of the phase change material during high-temperature film formation.
3. The invention can effectively solve the problem of phase change material leakage by utilizing physical adsorption, and the problems of poor heat-conducting property, low flame retardance and the like can be effectively improved by adding the inorganic adsorption material.
Detailed Description
The technical solution of the present invention will be further specifically described below by way of specific examples.
In the present invention, the raw materials and equipment used are commercially available or commonly used in the art, unless otherwise specified. The methods in the following examples are conventional in the art unless otherwise specified.
General implementation:
the phase-change heat storage film comprises raw materials of 30-70 wt% of a phase-change material and 30-70 wt% of a polymer film-forming material;
the phase-change material comprises the following components in parts by weight: 200-700 parts of a porous adsorption material, 200-600 parts of an organic phase change material, 35-70 parts of an emulsifier, 300-600 parts of water, 200-500 parts of an emulsification auxiliary material and 2-10 parts of an interface stabilizer.
The porous adsorption material is selected from one or more of silicon dioxide, activated carbon, expanded graphite, activated silica gel, alumina, molecular sieve, bentonite and bentonite. The organic phase change material is selected from one or more of straight-chain alkane, branched-chain alkane, unsaturated alkane, silicone wax, alkene and alkyne. The emulsifier is one or more selected from ceteareth-12, ceteareth-20, ceteareth-30, sorbitan fatty acid ester 80, and sorbitan monooleate polyoxyethylene ether. The emulsification auxiliary material is selected from one or more saturated alkanes with less than 14 carbons. The emulsification auxiliary material is n-tetradecane or n-dodecane. The interface stabilizer is sodium carboxymethyl cellulose. The polymer film-forming material is selected from one or more of polyurethane emulsion, styrene-acrylic emulsion and acrylic emulsion.
Example 1:
(1) 500g of silica was put into a muffle furnace, and the temperature was set at 600 ℃ for 2 hours.
(2) Heating 500g of n-docosane to 70 ℃, adding the treated silicon dioxide, uniformly stirring, putting into a vacuum oven with the temperature of 100 ℃, vacuumizing to the vacuum degree of-0.02 Mpa, and standing for 22 hours.
(3) The silica adsorbing n-docosane was washed with petroleum ether and dried in an oven at 80 ℃ for 14 hours to prepare a silica-based phase change powder.
(4) Adding 300g of n-tetradecane into 300g of water, heating to 80 ℃, adding 30g of ceteareth-12, and stirring at 600 rpm for 2 hours to obtain emulsion A.
(5) Adding 200g of water into 5g of sodium carboxymethylcellulose, stirring at 35 ℃ and 300 r/min for 30 min, slowly adding the phase change powder, and reacting for 2 h under the same conditions to obtain a preform B.
(6) Heating the emulsion A to 80 ℃, setting the rotation speed at 400 r/min, adding 30g of sorbitan fatty acid ester 80, slowly dripping into the pre-preparation B, and then shearing and emulsifying at 2000 r/min for 35 minutes to obtain emulsion C.
(7) 200g of the emulsion C was mixed with 200g of an acrylic emulsion (solid content: 40%, commercially available) under stirring, and the mixture was formed into a film having a thickness of 0.5mm by a film-coating machine, and dried at 90 ℃ to form a film.
The phase-change heat storage film prepared by the embodiment has the advantages that the phase-change temperature is 42-45 ℃, the enthalpy value is more than 150kj/kg, and the supercooling degree is lower than 3 ℃.
Comparative example 1:
the difference from example 1 is that steps (4) to (6) are eliminated, and the silica-based phase change powder and the acrylic emulsion are directly mixed without a secondary emulsification process, and the other steps are the same as example 1.
The temperature of the phase change heat storage film prepared in the comparative example 1 is 41-45 ℃, the enthalpy value is about 60kj/kg, and the supercooling degree is 3 ℃.
Example 2:
(1) 200g of silica were taken and placed in a muffle furnace, the temperature was set at 650 ℃ and the treatment was carried out for 1.5 hours.
(2) Heating 300g of n-eicosane to 70 ℃, adding the treated silicon dioxide, uniformly stirring, putting into a vacuum oven with the temperature of 100 ℃, vacuumizing to the vacuum degree of-0.03 MPa, and standing for 24 hours.
(3) And (3) washing the silicon dioxide adsorbing the n-eicosane by using petroleum ether, and then putting the silicon dioxide into an oven at 80 ℃ for drying for 12 hours to prepare silicon dioxide-based phase change powder.
(4) 200g of n-tetradecane is added with 200g of water, the temperature is raised to 80 ℃, 10g of ceteareth-12 and 10g of ceteareth-30 are added, and the mixture is stirred for 2 hours at a stirring speed of 600 revolutions per minute to prepare emulsion A.
(5) Adding 100g of water into 2g of sodium carboxymethylcellulose, stirring at 35 ℃ and 300 r/min for 30 min, slowly adding the phase change powder, and reacting for 2 h under the same conditions to obtain a preform B.
(6) Heating the emulsion A to 80 ℃, setting the rotation speed at 600 revolutions per minute, adding 20g of sorbitan monooleate polyoxyethylene ether, slowly dripping into the pre-product B, and then shearing and emulsifying for 30 minutes at 2000 revolutions per minute to obtain the emulsion C.
(7) 100g of the emulsion C was mixed with 100g of a polyurethane emulsion (solid content: 50%, commercially available) under stirring, and the mixture was formed into a film having a thickness of 0.5mm by a film-coating machine, and dried at 90 ℃.
The phase-change heat storage film provided by the embodiment has the advantages that the phase-change temperature is 35-37 ℃, the enthalpy value is more than 120kj/kg, and the supercooling degree is lower than 3 ℃.
Comparative example 2:
the difference from the example 2 is that the steps (4) to (6) are eliminated, the silica-based phase change powder is directly mixed with the polyurethane emulsion without a secondary emulsification process, and the other steps are the same as the example 2.
The temperature of the phase change heat storage film prepared in the comparative example 2 is 35-37 ℃, the enthalpy value is about 45kj/kg, and the supercooling degree is 3 ℃.
Example 3:
(1) 300g of activated carbon was taken and put into a muffle furnace, and the temperature was set at 700 ℃ for 1 hour.
(2) Heating 300g of n-eicosane to 75 ℃, adding the treated activated carbon, uniformly stirring, putting into a vacuum oven with the temperature of 105 ℃, and drying for 22 hours under the vacuum degree of-0.05 Mpa.
(3) And washing the activated carbon adsorbing the n-eicosane by using petroleum ether, and drying the washed activated carbon in an oven at 85 ℃ for 10 hours to prepare the activated carbon-based phase change powder.
(4) 200g of n-tetradecane is added with 200g of water, the temperature is raised to 85 ℃, 25g of ceteareth-20 is added, and the mixture is stirred for 2 hours at the stirring speed of 600 revolutions per minute to prepare the emulsion A.
(5) Adding 100g of water into 3g of sodium carboxymethylcellulose, stirring at 30 ℃ and at the rotating speed of 300 r/min for 35 minutes, slowly adding the phase change powder, and reacting for 3 hours under the same conditions to obtain a preform B.
(6) Heating the emulsion A to 85 deg.C, setting rotation speed at 600 rpm, adding 25g of sorbitan fatty acid ester 80, slowly dripping into the pre-preparation B, and shearing and emulsifying at 2500 rpm for 25 min to obtain emulsion C.
(7) 100g of the emulsion C was mixed with 100g of a polyurethane emulsion (solid content: 50%, commercially available) under stirring, and the mixture was formed into a film having a thickness of 0.5mm by a film-coating machine, and dried at 95 ℃.
The phase-change heat storage film provided by the embodiment has the advantages that the phase-change temperature is 35-37 ℃, the enthalpy value is more than 120kj/kg, and the supercooling degree is lower than 3 ℃.
Comparative example 3:
the difference from the example 3 is that the steps (4) to (6) are eliminated, the activated carbon-based phase change powder and the polyurethane emulsion are directly mixed without a secondary emulsification process, and the other steps are the same as the example 3.
The temperature of the phase change heat storage film prepared in the comparative example 3 is 35-37 ℃, the enthalpy value is about 50kj/kg, and the supercooling degree is 4 ℃.
Comparison of high temperature failure test results
The test method comprises the following steps: the phase change material was left at 100 ℃ for 4 hours, and the results are shown in table 1 below:
table 1:
the data in table 1 show that the invention can effectively solve the problem of high temperature resistance of the phase change material, and through the secondary emulsification process, a protective film is formed on the surface of the phase change material after high-temperature demulsification, so that the phase change material cannot volatilize during high-temperature film formation to cause the phase change material to lose efficacy.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (5)
1. A phase change heat storage film, characterized in that: the raw materials comprise 30-70 wt% of a phase-change material and 30-70 wt% of a polymer film-forming material;
the phase-change material comprises the following components in parts by weight: 200-700 parts of a porous adsorption material, 200-600 parts of an organic phase change material, 35-70 parts of an emulsifier, 300-600 parts of water, 200-500 parts of an emulsification auxiliary material and 2-10 parts of an interfacial stabilizer;
the porous adsorption material is selected from one or more of silicon dioxide, activated carbon, expanded graphite, activated silica gel, alumina, molecular sieve, bentonite and bentonite;
the organic phase change material is selected from one or more of n-docosane, n-eicosane and silicone wax;
the emulsification auxiliary material is selected from one or more saturated alkanes with less than 14 carbons or n-tetradecane; the interface stabilizer is sodium carboxymethyl cellulose;
the preparation method of the phase-change heat storage film comprises the following steps:
(1) treating the porous adsorption material in a muffle furnace at a set temperature of 600-700 ℃ for 1-2 hours;
(2) heating an organic phase change material to 70-75 ℃, adding the organic phase change material into the porous adsorption material treated in the step (1), uniformly stirring, putting the mixture into a vacuum oven at 100-105 ℃, and drying for 22-28 hours;
(3) washing the porous material loaded with the organic phase change material in the step (2) by using an organic solvent, and drying the porous material in an oven at the temperature of 80-85 ℃ for 10-14 hours to obtain phase change powder;
(4) adding part of water into the emulsification auxiliary material, heating to 80-85 ℃, adding part of emulsifier, stirring and uniformly mixing to prepare an emulsion A;
(5) stirring and mixing the interface stabilizer and the balance of water at 30-35 ℃ for 30-35 min, adding the phase change powder under the condition of maintaining the temperature and stirring, and mixing for 2-3 hours to prepare a prefabricated product B;
(6) heating the emulsified product A to 80-85 ℃, adding the rest of the emulsifier at the rotation speed of 400-600 rpm, then slowly dripping the prefabricated product B, and after finishing dripping, increasing the rotation speed to 2000-2500 rpm, and shearing and emulsifying for 25-35 minutes to prepare an emulsified product C;
(7) and uniformly mixing the emulsified product C and the high-molecular film forming material, coating the mixture into a film with the thickness of 0.3-0.8 mm by using a film coating machine, and drying and forming at 90-95 ℃.
2. The phase change heat storage film according to claim 1, wherein: the emulsifier is one or more selected from ceteareth-12, ceteareth-20, ceteareth-30, sorbitan fatty acid ester 80, and sorbitan monooleate polyoxyethylene ether.
3. The phase change heat storage film according to claim 1, wherein: the emulsification auxiliary material is n-tetradecane or n-dodecane.
4. The phase change heat storage film according to claim 1, wherein: the polymer film-forming material is selected from one or more of polyurethane emulsion, styrene-acrylic emulsion and acrylic emulsion.
5. The phase change heat storage film according to claim 1, wherein: in the step (4), the using amount of the water accounts for 50-70% of the total using amount of the water, and the using amount of the emulsifier accounts for 40-55% of the total using amount of the emulsifier.
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| US5106520A (en) * | 1985-11-22 | 1992-04-21 | The University Of Dayton | Dry powder mixes comprising phase change materials |
| CN1995264A (en) * | 2006-12-06 | 2007-07-11 | 清华大学深圳研究生院 | Silicon dioxde coated phase-change energy-storage material microcapsule preparation method |
| CN102504766A (en) * | 2011-10-09 | 2012-06-20 | 上海工程技术大学 | Phase-change energy-storage microcapsule, and preparation method and application thereof |
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| JP2013241499A (en) * | 2012-05-18 | 2013-12-05 | Kuraray Co Ltd | Composition for heat storage material, and heat storage material |
| CN111117159A (en) * | 2019-12-27 | 2020-05-08 | 杭州鲁尔新材料科技有限公司 | Phase change interface material for heat dissipation of electronic product |
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