CN108587573A - A kind of synthetic method of phase-changing energy storage material - Google Patents
A kind of synthetic method of phase-changing energy storage material Download PDFInfo
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- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
Abstract
The present invention relates to a kind of synthetic methods of phase-changing energy storage material.Include the following steps:Water phase is formed with deionized water, polyvinyl alcohol, tricalcium phosphate and methylene blue;Organic phase is formed with styrene, crosslinking agent and initiator;After paraffin is mixed with water conjunction uniformly, it is slowly added to organic phase, under stirring, 6 7h are reacted in 80 85 DEG C, product filtering is washed, dry, obtains phase-changing energy storage material.The present invention prepares phase-changing energy storage material by suspension polymerization, and method is easy to operate, and the phase-changing energy storage material of acquisition has the advantages that encapsulating solid, physics and chemical property stabilization, being convenient for storage and transport.
Description
Technical field
The present invention relates to energy storage environment-friendly materials field, especially one kind preparing phase-changing energy storage material by suspension polymerization
Method.
Background technology
Since 21 century, with the high speed development of modern science and technology and industry, people are growing day by day to the demand of the energy, entirely
Ball energy shortage problem getting worse.As the heat source of one of main energy sources, storage and utilization have become research and development
Hot spot.Phase-changing energy storage material (PCMs) is a kind of material with high fusion heat, when the temperature of material is more than or experience phase transformation
When temperature, they can absorb or discharge latent heat, it is possible to be used for heat accumulation or cold-storage.Therefore, energy can be effectively realized
Storage and utilization.Phase-changing energy storage material all has an application value in many fields, including Solar use, power peak regulation, useless
Heat utilization, cross-season heat-storing and Chu Leng, food fresh-keeping, building heat insulation, electronic device Thermal protection, textile garment, agricultural etc.
Deng.Compared with other PCM, paraffin has higher heat storage capacity, is easily obtained, and cheap, different according to paraffin
Chemical composition, paraffin have wider transition temperature range.But need the shell that a physics and chemical property are stablized by its
It is encapsulated, storage or release for carrying out heat when in need.Microcapsules technology is a kind of by solid or liquid
Got up to form the technology of fine particle with filmogen cladding.In recent years, extensive technology has been developed to prepare PCM
Microcapsules, such as the methods of spray drying, misting cooling, emulsification, interfacial polycondensation, cohesion, in-situ polymerization and suspension polymerisation.Traditional
Inorganic phase change energy storage material needs to solve encapsulation and corrosion problems, and it is smaller by encapsulation to be limited utilization scope.
Invention content
In order to solve problem above, the present invention provides a kind of method preparing phase-changing energy storage material by suspension polymerization.
The method of the present invention is easy to operate, and the phase-changing energy storage material of acquisition, which has, encapsulates solid, physics and chemical property stabilization, convenient for storage
The advantages that depositing and transporting.
The technical solution adopted by the present invention is:A kind of synthetic method of phase-changing energy storage material, includes the following steps:With go from
Sub- water, polyvinyl alcohol, tricalcium phosphate and methylene blue form water phase;It is formed with styrene (St), crosslinking agent and initiator organic
Phase;After paraffin is mixed with water conjunction uniformly, it is slowly added to organic phase, under stirring, 6-7h is reacted in 80-85 DEG C, product filtering is washed
It washs, it is dry, obtain phase-changing energy storage material.
The synthetic method of above-mentioned a kind of phase-changing energy storage material, with 220mL deionized waters, 50mL polyvinyl alcohol containing 0.48g
Aqueous solution, 0.96g tricalcium phosphates and 0.8mL methylene blues form water phase;With 10-16g styrene (St), 4-30g crosslinking agents
Organic phase is formed with 0.5g initiators;After 5-20g paraffin is mixed with water conjunction uniformly, it is slowly added to organic phase, under stirring, in
80-85 DEG C of reaction 6-7h, product filtering are washed, dry, obtain phase-changing energy storage material.
A kind of synthetic method of above-mentioned phase-changing energy storage material, the crosslinking agent are divinylbenzene (DVB).
A kind of synthetic method of above-mentioned phase-changing energy storage material, the initiator are azodiisobutyronitrile (AIBN).
A kind of synthetic method of above-mentioned phase-changing energy storage material, the stirring, mixing speed 200-600rpm.It is preferred that
, mixing speed 400rpm.
A kind of synthetic method of above-mentioned phase-changing energy storage material, it is preferred that by weight, paraffin:Styrene=1:1.
A kind of synthetic method of above-mentioned phase-changing energy storage material, it is preferred that by weight, styrene:Crosslinking agent=1:(1-
3).It is furthermore preferred that styrene:Crosslinking agent=1:1.
The beneficial effects of the invention are as follows:Phase-changing energy storage material prepared by method using the present invention, which has, encapsulates solid, object
It manages and chemical property is stablized, the advantages that convenient for storage and transport.The method of the present invention is simple.
Description of the drawings
Fig. 1 is that different paraffin doping low whipping speeds are 250rpm, St:DVB is 4:Microscope figure under conditions of 1;
Wherein, (a) is the microscope figure of phase-changing energy storage material prepared by 5g paraffin, and (b) (c) is phase prepared by 10g paraffin
The microscope figure of change energy-storage material, (d) (e) (f) is the microscope figure of phase-changing energy storage material prepared by 15g paraffin, and (g) (h) is
The microscope figure of phase-changing energy storage material prepared by 20g paraffin.
Fig. 2 a are the calorimetric curve graph of phase-changing energy storage material prepared by 5g paraffin.
Fig. 2 b are the calorimetric curve graph of phase-changing energy storage material prepared by 20g paraffin.
Fig. 3 is 10g paraffin, St:DVB is 1:1, the item of low whipping speed 200rpm, 300rpm, 400rpm, 600rpm
Microscope figure under part;
Wherein, (a) is the photo under 200rpm, and (b) (c) is the microscope figure of microballoon under 300rpm, and (d) (e) is
The microscope figure of microballoon under 400rpm is (f) microscope figure of microballoon under 600rpm.
Fig. 4 a are St:DVB is 1:The calorimetric curve graph of 1 phase-changing energy storage material.
Fig. 4 b are St:DVB is 1:The calorimetric curve graph of 2 phase-changing energy storage material.
Fig. 4 c are St:DVB is 1:The calorimetric curve graph of 3 phase-changing energy storage material.
Fig. 5 is 5g paraffin, St:DVB is 4:1, the phase-changing energy storage material prepared under the mixing speed of 250rpm is in not equality of temperature
Microscope figure under degree;
Wherein, (a) is microscope figure at room temperature, (b) is dried under 60 DEG C of baking ovens for phase-changing energy storage material micro- after 1h
Mirror figure, (c) be phase-changing energy storage material dries the microscope figure photo after 1h under 80 DEG C of baking ovens, (d) be phase-changing energy storage material 100
The microscope figure after 1h is dried under DEG C baking oven.
(a)-(d) is DVB in Fig. 6:Paraffin is 1:1 phase-changing energy storage material is respectively in 20-50 mesh, 50-80 mesh, 80-100
Microscope figure under the conditions of mesh and 100-170 mesh.(e)-(i) is DVB:Paraffin is 2:1 phase-changing energy storage material is respectively in 20-50
Microscope figure under the conditions of mesh, 50-80 mesh, 80-100 mesh, 100-170 mesh and 170-300 mesh.(j)-(m) is DVB:Paraffin is
3:1 phase-changing energy storage material microscope figure under the conditions of 50-80 mesh, 80-100 mesh, 100-170 mesh and 170-300 mesh respectively.
(n)-(q) is DVB:Paraffin is 4:1 phase-changing energy storage material is respectively in 50-80 mesh, 80-100 mesh, 100-170 mesh and 170-300
Microscope figure under the conditions of mesh.
Fig. 7 a are DVB:Paraffin is 1:The calorimetric curve graph of 1 phase-changing energy storage material.
Fig. 7 b are DVB:Paraffin is 2:The calorimetric curve graph of 1 phase-changing energy storage material.
Fig. 7 c are DVB:Paraffin is 3:The calorimetric curve graph of 1 phase-changing energy storage material.
Fig. 7 d are DVB:Paraffin is 4:The calorimetric curve graph of 1 phase-changing energy storage material.
Specific implementation mode
A kind of synthetic method preparing phase-changing energy storage material by suspension polymerization, method include the following steps:
First, the preparation of decentralized medium poly-vinyl alcohol solution, by the polyvinyl alcohol (PVA) for the 0.48g that alcoholysis degree is 88%
It is added while stirring with glass bar in the clean beaker equipped with 50mL deionized waters.Then beaker is placed in supersonic wave cleaning machine
Interior progress ultrasound 30min or so, until solid all dissolves in solution.The solution for standby that will have been configured.
At room temperature, 220mL distilled water, the prepared water containing 0.48g polyvinyl alcohol of 50mL are added in round-bottomed flask
Solution, 0.96g tricalcium phosphates, 0.8mL methylene blues form water phase.
Secondly, the preparation of organic phase:4-30g divinylbenzenes (DVB) are poured into the burning for filling 10-16g styrene (St)
In cup, beaker is put on magnetic stirring apparatus and stirs 10min, is allowed to after being sufficiently mixed fall 0.5g azodiisobutyronitriles (AIBN)
Enter and be stirred for 10min in beaker, until there is no solid and solution to be uniformly mixed in solution, obtains organic phase.
Round-bottomed flask equipped with water phase is placed in oil bath by third, opens the heater switch of mechanical agitator and oil bath, will
Temperature setting is 80 DEG C.When temperature is raised to 60 DEG C, 5-20g solid paraffins are added in water phase, wait for that granular paraffin is complete
After thawing, it is slowly added to organic phase, under 200-600rpm stirrings, reacts 6h at being 80 DEG C in oil bath.After reaction, filtering point
It washs from and with methanol, is then dried at room temperature for repeatedly.Finally dried microballoon is sieved, by particle size difference
Separately bottling.
Embodiment 1
Influence of the different paraffin dopings to heat storage capacity, preparation method include the following steps:
1) prepared by water phase:In 500mL three neck round bottom flask, be added 220mL deionized waters, 50mL it is prepared containing
The aqueous solution of 0.48g polyvinyl alcohol, 0.96g tricalcium phosphates, 0.8mL methylene blues form water phase.
2) 4g divinylbenzenes (DVB) are poured into the beaker for filling 16g styrene (St), beaker is put into magnetic agitation
10min is stirred on device, is allowed to after being sufficiently mixed, and 0.5g azodiisobutyronitriles (AIBN) are poured into and are stirred for 10min in beaker, directly
To there is no solid and solution to be uniformly mixed in solution, organic phase is obtained.
3) the 500mL three neck round bottom flask equipped with water phase is placed in oil bath, opens the heating of mechanical agitator and oil bath
Temperature setting is 80 DEG C by switch.When temperature is raised to 60 DEG C, it is separately added into 5g, 10g, 15g, 20g paraffin, after mixing
Organic phase, low whipping speed 250rpm is added, oil bath is 80 DEG C, and reaction 6h is separated by filtration and anti-with methanol after reaction
After backwashing is washed, and is then dried at room temperature for, and phase-changing energy storage material is obtained.As a result such as Fig. 1, table 1, Fig. 2 a and Fig. 2 b.
As seen from Figure 1, (a) can be seen that the microsphere surface smoother prepared by 5g paraffin in Fig. 1, occur in figure
Two kinds of microballoons, white is phase-changing energy storage material, black is polystyrene microsphere.From Fig. 1 (b) (c) and (d) (e) (f)
It can be seen that there is the phenomenon that adhesion in the larger particle of phase-changing energy storage material prepared by 10g and 15g paraffin, and smaller particle
There is more regular spherical shape, it may be possible to since mixing speed is relatively slow caused.And from Fig. 1 (g) (h) it can be seen that by
Microballoon prepared by 20g paraffin does not occur apparent spherical, it may be possible to be encapsulated into the limit.
It can be obtained from table 1, Fig. 2 a and Fig. 2 b, the transformation temperature of the phase-changing energy storage material prepared by 5g and 20g paraffin differs
Less, respectively 58.66 DEG C and 59.58 DEG C, close to melting point of paraffin wax.And the heat storage capacity difference of two kinds of materials is larger, respectively
For 30.03J/g and 63.69J/g, illustrate when paraffin doping increases, the heat storage capacity enhancing of paraffin.
Table 1
Embodiment 2
Influence of the different mixing speeds to heat storage capacity, preparation method include the following steps:
1) prepared by water phase:In 500mL three neck round bottom flask, be added 220mL deionized waters, 50mL it is prepared containing
0.48g polyvinyl alcohol water solutions, 0.96g tricalcium phosphates, 0.8mL methylene blues form water phase.
2) 10g divinylbenzenes (DVB) are poured into the beaker for filling 10g styrene (St), beaker, which is put into magnetic force, to be stirred
It mixes and stirs 10min on device, be allowed to after being sufficiently mixed, 0.5g azodiisobutyronitriles (AIBN) are poured into and are stirred for 10min in beaker,
Until there is no solid and solution to be uniformly mixed in solution, organic phase is obtained.
3) the 500mL three neck round bottom flask equipped with water phase is placed in oil bath, opens the heating of mechanical agitator and oil bath
Temperature setting is 80 DEG C by switch.When temperature is raised to 60 DEG C, it is separately added into 10g paraffin, organic phase is added after mixing,
Low whipping speed is 200rpm, 300rpm, 400rpm, 600rpm respectively, and oil bath is 80 DEG C, reacts 6h, after reaction, filtering
It detaches and is washed repeatedly with methanol, be then dried at room temperature for, obtain phase-changing energy storage material.As a result such as Fig. 3.
From the figure 3, it may be seen that from Fig. 3 (a) it is found that when mixing speed be 200rpm when, product all forms bulk, cannot be very
It detaches well.(b) (c) finds out in Fig. 3, when mixing speed is 300rpm, occurs apparent spherical shape in figure, but has
Adhesion phenomenon exists, and when mixing speed is increased to 400rpm, (d) (e) finds out in Fig. 3, and microballoon detaches preferable, in figure
It can obviously see the presence of two kinds of microballoons.When mixing speed is 600rpm, (f) is as can be seen that there is broken ball to go out from Fig. 3
It is existing, microballoon may be caused broken since mixing speed is excessive.Therefore, best mixing speed is 400rpm.
Embodiment 3
Influence of the different DVB contents to heat storage capacity, preparation method include the following steps:
1) prepared by water phase:In 500mL three neck round bottom flask, be added 220mL deionized waters, 50mL it is prepared containing
0.48g polyvinyl alcohol water solutions, 0.96g tricalcium phosphates, 0.8mL methylene blues form water phase.
2) 10g, 20g, 30g divinylbenzene (DVB) are poured into respectively in the beaker for filling 10g styrene (St), will be burnt
Cup, which is put on magnetic stirring apparatus, stirs 10min, is allowed to after being sufficiently mixed, 0.5g azodiisobutyronitriles (AIBN) are poured into beaker
It is stirred for 10min, until not having solid and solution to be uniformly mixed in solution, obtains organic phase.
3) the 500mL three neck round bottom flask equipped with water phase is placed in oil bath, opens the heating of mechanical agitator and oil bath
Temperature setting is 80 DEG C by switch.When temperature is raised to 60 DEG C, 10g paraffin is added, organic phase is added after mixing, is stirring
It is 400rpm to mix speed, and oil bath is 80 DEG C, and reaction 6h is separated by filtration and is washed repeatedly with methanol, then in room after reaction
The lower drying of temperature, obtains phase-changing energy storage material.As a result such as table 2, Fig. 4 a-4c.
It can be seen from table 2 and Fig. 4 a-4c the transformation temperature of three kinds of phase-changing energy storage materials be respectively 58.86 DEG C, 58.66 DEG C,
It is 57.55 DEG C, almost the same with the transformation temperature of paraffin.When DVB contents increase, under the heat storage capacity of phase-changing energy storage material is gradual
Drop.It is advantageous to, by weight, styrene:Crosslinking agent=1:1.
Table 2
Embodiment 4
1) prepared by water phase:In 500mL three neck round bottom flask, be added 220mL deionized waters, 50mL it is prepared containing
0.48g polyvinyl alcohol water solutions, 0.96g tricalcium phosphates, 0.8mL methylene blues form water phase.
2) 4g divinylbenzenes (DVB) are poured into the beaker for filling 16g styrene (St), beaker is put into magnetic agitation
10min is stirred on device, is allowed to after being sufficiently mixed, and 0.5g azodiisobutyronitriles (AIBN) are poured into and are stirred for 10min in beaker, directly
To there is no solid and solution to be uniformly mixed in solution, organic phase is obtained.
3) the 500mL three neck round bottom flask equipped with water phase is placed in oil bath, opens the heating of mechanical agitator and oil bath
Temperature setting is 80 DEG C by switch.When temperature is raised to 60 DEG C, 5g paraffin is added, water phase is added after mixing, in stirring speed
Degree is 250rpm, and oil bath is 80 DEG C, and reaction 6h is separated by filtration and is washed repeatedly with methanol, then at room temperature after reaction
It is dry, obtain phase-changing energy storage material.
Phase-changing energy storage material after drying is placed into 1h at 60 DEG C, 80 DEG C, 100 DEG C respectively, is then seen under the microscope
Examine its situation of change.As a result such as Fig. 5.
As can be seen that when the temperature increases, the variation of shape does not occur for microballoon from Fig. 5 (a) (b) (c) (d), encapsulating
Paraffin also without there is apparent leakage phenomenon, it was demonstrated that paraffin polystyrene (nucleocapsid) phase-changing energy storage material has resistance to well
Warm ability.
5 comparative example of embodiment
The amount of styrene St is 0g, and divinylbenzene DVB and paraffin total amount are 20g, and DVB:Paraffin is respectively 1-4:1
1) prepared by water phase:In 500mL three neck round bottom flask, be added 220mL deionized waters, 50mL it is prepared containing
0.48g polyvinyl alcohol water solutions, 0.96g tricalcium phosphates, 0.8mL methylene blues form water phase.
2) 0.5g azodiisobutyronitriles (AIBN) are poured into the beaker for filling divinylbenzene (DVB), beaker is put into
20min is stirred on magnetic stirring apparatus, until not having solid and solution to be uniformly mixed in solution, obtains organic phase.
3) the 500mL three neck round bottom flask equipped with water phase is placed in oil bath, opens the heating of mechanical agitator and oil bath
Temperature setting is 85 DEG C by switch.When temperature is raised to 60 DEG C, paraffin is added, organic phase is added after mixing, in stirring speed
Degree is 500rpm, and oil bath is 85 DEG C, and reaction 3h is separated by filtration and is washed repeatedly with methanol, then at room temperature after reaction
It is dry, obtain phase-changing energy storage material.As a result such as table 3, Fig. 6 and Fig. 7 a-7d.
There is the phenomenon that adhesion between 20-80 mesh from can be seen that microballoon in the microscope figure of different proportion in Fig. 6,
And occur spherical shape well between 80-300 mesh, and with the increase of ratio, microballoon is distributed evenly, and surfaces stick
The phenomenon that reduce, the transparent beads occurred from the microscope figure of 100-300 mesh may be DVB autohemagglutinations formed poly- divinyl
Benzene microballoon.It can be seen that the phase-changing energy storage material of the polydivinylbenezene packet paraffin microballoon of different proportion in conjunction with table 3 and Fig. 7 a-7d
Phase transition temperature be all 58 DEG C or so, and with the increase of ratio, the heat storage capacity of energy storage material is gradually reduced.In conjunction with calorimetric song
Line and microscope figure can prove that paraffin is encapsulated in the shell of polydivinylbenezene, and obtained energy storage material minimum is big
Generally it is distributed in tens microns.
Table 3
Claims (9)
1. a kind of synthetic method of phase-changing energy storage material, which is characterized in that include the following steps:With deionized water, polyvinyl alcohol,
Tricalcium phosphate and methylene blue form water phase;Organic phase is formed with styrene, crosslinking agent and initiator;Paraffin is mixed with water conjunction
After uniformly, it is slowly added to organic phase, under stirring, 6-7h is reacted in 80-85 DEG C, product filtering is washed, dry, obtains phase-change accumulation energy
Material.
2. a kind of synthetic method of phase-changing energy storage material according to claim 1, which is characterized in that with 220mL deionizations
Water, the aqueous solution of 50mL polyvinyl alcohol containing 0.48g, 0.96g tricalcium phosphates and 0.8mL methylene blues form water phase;With 10-16g
Styrene, 4-30g crosslinking agents and 0.5g initiators form organic phase;After 5-20g paraffin is mixed with water conjunction uniformly, it is slowly added to
Under stirring, 6-7h is reacted in 80-85 DEG C for organic phase, and product filtering is washed, dry, obtains phase-changing energy storage material.
3. a kind of synthetic method of phase-changing energy storage material according to claim 1 or 2, which is characterized in that the crosslinking
Agent is divinylbenzene.
4. a kind of synthetic method of phase-changing energy storage material according to claim 1 or 2, which is characterized in that the initiation
Agent is azodiisobutyronitrile.
5. a kind of synthetic method of phase-changing energy storage material according to claim 1 or 2, which is characterized in that the stirring,
Mixing speed is 200-600rpm.
6. a kind of synthetic method of phase-changing energy storage material according to claim 5, which is characterized in that mixing speed is
400rpm。
7. a kind of synthetic method of phase-changing energy storage material according to claim 1 or 2, which is characterized in that by weight, stone
Wax:Styrene=1:1.
8. a kind of synthetic method of phase-changing energy storage material according to claim 1 or 2, which is characterized in that by weight, benzene
Ethylene:Crosslinking agent=1:(1-3).
9. a kind of synthetic method of phase-changing energy storage material according to claim 8, which is characterized in that styrene:Crosslinking agent
=1:1.
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CN109837068A (en) * | 2019-01-16 | 2019-06-04 | 浙江理工大学 | A kind of preparation method of cross-linking type phase-changing and temperature-regulating functional agent |
CN110317577A (en) * | 2019-06-13 | 2019-10-11 | 深圳诺必达节能环保有限公司 | A kind of phase-changing energy storage material and preparation method thereof |
CN113150201A (en) * | 2021-04-06 | 2021-07-23 | 辽宁大学 | Method for synthesizing phase-change energy-storage type polystyrene adsorbent |
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CN109837068A (en) * | 2019-01-16 | 2019-06-04 | 浙江理工大学 | A kind of preparation method of cross-linking type phase-changing and temperature-regulating functional agent |
CN110317577A (en) * | 2019-06-13 | 2019-10-11 | 深圳诺必达节能环保有限公司 | A kind of phase-changing energy storage material and preparation method thereof |
CN113150201A (en) * | 2021-04-06 | 2021-07-23 | 辽宁大学 | Method for synthesizing phase-change energy-storage type polystyrene adsorbent |
CN113929805A (en) * | 2021-11-22 | 2022-01-14 | 上海交通大学 | Preparation method of phase-change energy-storage polystyrene closed-cell foam |
CN113929805B (en) * | 2021-11-22 | 2022-06-28 | 上海交通大学 | Preparation method of phase-change energy-storage polystyrene closed-cell foam |
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