CN110699044B - Polypyrrole-based composite shaping phase-change material and preparation method thereof - Google Patents
Polypyrrole-based composite shaping phase-change material and preparation method thereof Download PDFInfo
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- 229920000128 polypyrrole Polymers 0.000 title claims abstract description 75
- 239000012782 phase change material Substances 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000007493 shaping process Methods 0.000 title claims description 9
- 239000004964 aerogel Substances 0.000 claims abstract description 36
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000017 hydrogel Substances 0.000 claims abstract description 18
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 15
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000005642 Oleic acid Substances 0.000 claims abstract description 15
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 15
- 239000012188 paraffin wax Substances 0.000 claims abstract description 12
- 238000001179 sorption measurement Methods 0.000 claims abstract description 10
- 239000011148 porous material Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 9
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000004513 sizing Methods 0.000 claims description 8
- 239000012074 organic phase Substances 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000012512 characterization method Methods 0.000 claims 1
- 239000004567 concrete Substances 0.000 abstract description 4
- 238000004108 freeze drying Methods 0.000 abstract description 4
- 238000003980 solgel method Methods 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000004146 energy storage Methods 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 238000004378 air conditioning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
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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
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
- E04B1/00—Constructions in general; Structures which are not restricted either to walls, e.g. partitions, or floors or ceilings or roofs
- E04B1/62—Insulation or other protection; Elements or use of specified material therefor
- E04B1/74—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls
- E04B1/76—Heat, sound or noise insulation, absorption, or reflection; Other building methods affording favourable thermal or acoustical conditions, e.g. accumulating of heat within walls specifically with respect to heat only
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04B—GENERAL BUILDING CONSTRUCTIONS; WALLS, e.g. PARTITIONS; ROOFS; FLOORS; CEILINGS; INSULATION OR OTHER PROTECTION OF BUILDINGS
- E04B2/00—Walls, e.g. partitions, for buildings; Wall construction with regard to insulation; Connections specially adapted to walls
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F15/00—Flooring
- E04F15/02—Flooring or floor layers composed of a number of similar elements
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F15/00—Flooring
- E04F15/18—Separately-laid insulating layers; Other additional insulating measures; Floating floors
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/0068—Ingredients with a function or property not provided for elsewhere in C04B2103/00
- C04B2103/0071—Phase-change materials, e.g. latent heat storage materials used in concrete compositions
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F2290/00—Specially adapted covering, lining or flooring elements not otherwise provided for
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Abstract
The invention relates to a polypyrrole-based composite shape-stabilized phase-change material and a preparation method thereof. The phase-change material is prepared from raw materials including pyrrole, oleic acid, ferric trichloride and paraffin by a sol-gel method to prepare polypyrrole aerogel and vacuum adsorption of the paraffin to prepare the composite shape-stabilized phase-change material. And selecting oleic acid (HLB is 1) as a surfactant in the process of preparing the polypyrrole hydrogel by a sol-gel method, and freeze-drying the polypyrrole hydrogel to prepare the loose, porous and high-porosity polypyrrole aerogel. Oleic acid can change the microscopic surface morphology of the polypyrrole aerogel, so that the prepared polypyrrole aerogel mostly has effective pores larger than 20 nm. The composite shaped phase-change material prepared by the invention fills the vacancy of the composite shaped phase-change material with the conductive property, can be applied to conductive composite phase-change material concrete, and fully exerts the latent heat performance of the composite shaped phase-change material.
Description
Field of the invention
The invention relates to a phase change energy storage material technology, and belongs to the technical field of phase change energy storage material preparation.
Background
At present, a large amount of energy is consumed in the world every year due to production and life, the reserve of energy serving as the life of economic society and the survival and development power of human society is limited, and the thermal efficiency of traditional non-renewable conventional energy sources such as petroleum, natural gas, coal and other petrochemical fuel energy sources is generally low in the using process. Therefore, it is important to develop efficient materials or devices for the storage of new energy sources. Because the supply and the demand of natural energy have stronger practicality, the phase change energy storage technology is utilized to effectively regulate the time of the natural energy, and the utilization efficiency of natural clean energy can be improved. Phase change materials as thermal functional materials capable of absorbing or releasing latent heat, capable of storing thermal energy in a process or for a period of time, and used or transferred to a different location at a later point in time, are thus in various energy storage floors, air conditioning thermal storage systems, and the like.
Phase change materials are often used as means in the field of buildings, and room temperature comfort can be obviously improved by adding the phase change materials into floors and building enclosures. The conductive concrete can generate heat when being electrified, the phase-change material can store the heat in time, the conductive material and the phase-change material are applied to the concrete together, and therefore the power station can supply power and heat in time, the electric power in the valley period can be converted into heat energy to be stored, the heat energy can be used in the peak period of supplying power for the city, the use of heating equipment such as an air conditioner is reduced, and the peak clipping and valley filling of the electric power are realized.
Disclosure of Invention
The technical problem is as follows: the invention aims to provide a novel polypyrrole-based composite shaped phase-change material and a preparation method thereof.
The technical scheme is as follows: in order to achieve the above purpose and other related purposes, the polypyrrole-based composite shape-stabilized phase change material adopts the following technical scheme:
polypyrrole aerogel with conductive property is used as a supporting material, and then paraffin is adsorbed to obtain the polypyrrole-based composite shaping phase-change material.
Wherein the content of the first and second substances,
the supporting material polypyrrole aerogel comprises pyrrole, ferric chloride hexahydrate and oleic acid, the molar mass ratio of the pyrrole to the ferric chloride hexahydrate is 1:3, Fe3+ can be guaranteed to fully participate in the polymerization reaction of the pyrrole, and the molar mass ratio of the pyrrole to the oleic acid is 1:5-1: 7.
The polypyrrole aerogel used as the support material has the average pore diameter larger than 20nm effective pores according to BET representation.
The support material polypyrrole aerogel has an adsorption rate of 69% -73% to the organic phase change material paraffin under the vacuum adsorption condition.
The phase-change temperature of the composite sizing phase-change material is 34.6 ℃, the phase-change enthalpy is 97.6J/g, and the electric conductivity is 0.0842S/cm.
The preparation method of the polypyrrole-based composite sizing phase-change material comprises the following steps:
step 1, mixing pyrrole and oleic acid with a molar ratio of 7:1 in deionized water; adding ferric chloride hexahydrate solution, wherein the molar ratio of Fe3+ to pyrrole is 1:1, and electromagnetically stirring until the solution becomes black to obtain polypyrrole hydrogel;
step 2, putting the polypyrrole hydrogel obtained in the step 1 into a vacuum freeze dryer, and carrying out vacuum drying for 48-72 hours to prepare polypyrrole aerogel;
and 3, adsorbing the polypyrrole aerogel prepared in the step 2 by using vacuum to obtain an organic phase change material paraffin to prepare the polypyrrole aerogel-based composite sizing phase change material.
Has the advantages that: according to the invention, the characteristic that the aerogel generally has higher porosity is utilized, the average pore diameter of the polypyrrole aerogel is changed by formulating the surfactant, and compared with the support material of the composite sizing phase-change material researched at present, the polypyrrole aerogel used as the support material has higher adsorption rate on the organic phase-change material, and the prepared polypyrrole aerogel-based composite sizing phase-change material has certain conductivity by utilizing the conductive property of the polypyrrole aerogel.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of a polypyrrole-based composite shape-stabilized phase-change material.
FIG. 2 is a diagram of a polypyrrole aerogel placed in a polystyrene board incubator.
Detailed Description
Example 1
0.89g (12.52mmol) of pyrrole monomer and 0.71g of oleic acid are put into a beaker and fully mixed with 4.00ml of deionized water, and the mixture is stirred for 60 seconds by an electromagnetic stirrer and is marked as solution A; 3.38g (12.52mol) of ferric chloride hexahydrate are weighed out and dissolved in 4.00ml of deionized water and designated as solution B. Slowly pouring the solution B into the solution A, keeping magnetic stirring, and immediately taking out magnetons after the solution becomes dark. The formation of polypyrrole hydrogel was observed by slowly tilting the beaker after waiting about 10 seconds.
The prepared polypyrrole hydrogel is cleaned by deionized water and absolute ethyl alcohol, placed in an ultralow temperature refrigerator at the temperature of 80 ℃ below zero, and kept stand for 24 hours. And taking out the polypyrrole hydrogel after 24 hours, putting the polypyrrole hydrogel into a vacuum freeze dryer, and freeze-drying for 60-72 hours to obtain the polypyrrole aerogel. And adsorbing the organic phase change material paraffin by polypyrrole aerogel in a vacuum adsorption mode to obtain the polypyrrole-based composite shaping phase change material.
Example 2: preparation of polypyrrole-based composite shaping phase-change material
0.89g (12.52mmol) of pyrrole monomer and 0.51g of oleic acid are taken to be mixed with 4.00ml of deionized water in a beaker, and stirred for 60 seconds by an electromagnetic stirrer to be marked as solution A; 3.38g (12.52mol) of ferric chloride hexahydrate are weighed out and dissolved in 4.00ml of deionized water and designated as solution B. Slowly pouring the solution B into the solution A, keeping magnetic stirring, and immediately taking out magnetons after the solution becomes dark. The formation of polypyrrole hydrogel was observed by slowly tilting the beaker after waiting about 10 seconds. The prepared polypyrrole hydrogel is cleaned by deionized water and absolute ethyl alcohol, placed in an ultralow temperature refrigerator at the temperature of 80 ℃ below zero, and kept stand for 24 hours. And taking out the polypyrrole hydrogel after 24 hours, placing the polypyrrole hydrogel in a vacuum freeze dryer, and freeze-drying for 72 hours to obtain the polypyrrole aerogel. And adsorbing the organic phase change material paraffin by polypyrrole aerogel in a vacuum adsorption mode to obtain the polypyrrole-based composite shaping phase change material.
Example 3: practical application effect of polypyrrole-based composite shaping phase-change material
The prepared polypyrrole-based composite sizing phase-change material is filled in a polystyrene board incubator, the device diagram is shown in figure 2, and a box body without the phase-change material is arranged for comparison. The temperature of the comparison box is basically stabilized at about 30 ℃ at the temperature of 40 ℃ for 80 minutes, the temperature is stabilized at about 34 ℃ at the temperature of 130 minutes, and the final stable temperature of the experiment box is 3-4 ℃ lower than the temperature of the comparison box by comparing the temperature curves of the experiment box and the comparison box at all environmental temperatures. Test results show that the polypyrrole-based composite sizing phase-change material prepared by the invention has an obvious temperature control effect.
And selecting oleic acid (HLB is 1) as a surfactant in the process of preparing the polypyrrole hydrogel by a sol-gel method, and freeze-drying the polypyrrole hydrogel to prepare the loose, porous and high-porosity polypyrrole aerogel. Oleic acid can change the microscopic surface morphology of the polypyrrole aerogel, so that the prepared polypyrrole aerogel mostly has effective pores larger than 20 nm. The polypyrrole aerogel modified by the oleic acid has high adsorption rate to paraffin under the vacuum adsorption condition, and hardly generates quality loss after multiple melting and freezing cycles. Meanwhile, the polypyrrole aerogel is characterized by a porous structure in terms of microscopic morphology, and paraffin can be well adsorbed into pores of the polypyrrole aerogel. The composite shaped phase-change material prepared by the invention fills the vacancy of the composite shaped phase-change material with the conductive property, can be applied to conductive composite phase-change material concrete, and fully exerts the latent heat performance of the composite shaped phase-change material.
Claims (5)
1. A polypyrrole-based composite shaping phase-change material is characterized in that polypyrrole aerogel with conductive property is used as a supporting material, and paraffin is adsorbed to obtain the polypyrrole-based composite shaping phase-change material;
the supporting material polypyrrole aerogel comprises pyrrole, ferric chloride hexahydrate and oleic acid, wherein the molar mass ratio of the pyrrole to the ferric chloride hexahydrate is 1:1, and the molar mass ratio of the pyrrole to the oleic acid is 5: 1-7: 1;
wherein, the preparation of polypyrrole aerogel is: mixing pyrrole and oleic acid with the molar mass ratio of 5: 1-7: 1 in deionized water; adding ferric chloride hexahydrate solution, wherein Fe3+The molar ratio of the polypyrrole to the pyrrole is 1:1, and the solution is electromagnetically stirred until the solution becomes black to obtain polypyrrole hydrogel; and then putting the obtained polypyrrole hydrogel into a vacuum freeze dryer, and carrying out vacuum drying for 48-72 hours to prepare the polypyrrole aerogel.
2. The polypyrrole-based composite shape-stabilized phase-change material according to claim 1, wherein the polypyrrole aerogel used as the support material has an average pore diameter greater than 20nm as an effective pore according to BET characterization.
3. The polypyrrole-based composite shape-stabilized phase-change material according to claim 1, wherein the polypyrrole aerogel as the supporting material has an adsorption rate of 69% -73% to the organic phase-change material paraffin under a vacuum adsorption condition.
4. The polypyrrole-based composite shape-stabilized phase-change material according to claim 1, wherein the phase-change temperature of the composite shape-stabilized phase-change material is 34.6 ℃, the enthalpy of phase change is 97.6J/g, and the electric conductivity is 0.0842S/cm.
5. A method for preparing the polypyrrole based composite shaped phase change material according to the claim 1, 2, 3 or 4, characterized in that the preparation method comprises the following steps:
step 1, mixing pyrrole and oleic acid with a molar mass ratio of 7:1 in deionized water; adding ferric chloride hexahydrate solution, wherein Fe3+The molar ratio of the polypyrrole to the pyrrole is 1:1, and the solution is electromagnetically stirred until the solution becomes black to obtain polypyrrole hydrogel;
step 2, putting the polypyrrole hydrogel obtained in the step 1 into a vacuum freeze dryer, and carrying out vacuum drying for 48-72 hours to prepare polypyrrole aerogel;
and 3, adsorbing the polypyrrole aerogel prepared in the step 2 by using vacuum to obtain an organic phase change material paraffin to prepare the polypyrrole aerogel-based composite sizing phase change material.
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CN101203467A (en) * | 2005-07-26 | 2008-06-18 | 波音公司 | Composite materials of aerogel and phase change material |
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CN108689412A (en) * | 2017-04-12 | 2018-10-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of aeroge micro mist and preparation method thereof |
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