CN114058335A - Preparation and application of natural environment-friendly shape-stabilized phase change material - Google Patents
Preparation and application of natural environment-friendly shape-stabilized phase change material Download PDFInfo
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- CN114058335A CN114058335A CN202010771331.0A CN202010771331A CN114058335A CN 114058335 A CN114058335 A CN 114058335A CN 202010771331 A CN202010771331 A CN 202010771331A CN 114058335 A CN114058335 A CN 114058335A
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- phase change
- change material
- acid
- silkworm cocoons
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- 239000012782 phase change material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 241000255789 Bombyx mori Species 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 6
- 238000005470 impregnation Methods 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 14
- 238000010306 acid treatment Methods 0.000 claims description 12
- 238000003763 carbonization Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 235000010355 mannitol Nutrition 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 230000007704 transition Effects 0.000 claims description 3
- 239000004386 Erythritol Substances 0.000 claims description 2
- UNXHWFMMPAWVPI-UHFFFAOYSA-N Erythritol Natural products OCC(O)C(O)CO UNXHWFMMPAWVPI-UHFFFAOYSA-N 0.000 claims description 2
- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 claims description 2
- 235000019414 erythritol Nutrition 0.000 claims description 2
- 229940009714 erythritol Drugs 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000003860 storage Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 2
- 150000005846 sugar alcohols Chemical class 0.000 abstract description 2
- 239000000969 carrier Substances 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229930195725 Mannitol Natural products 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
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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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of a natural environment-friendly shape-stabilized phase change material. The method selects environment-friendly phase-change materials, uses acid-treated silkworm cocoons as supporting carriers, and synthesizes the materials by a vacuum impregnation method. The natural environment-friendly shape-stabilized phase change material synthesized by the method can prevent leakage of sugar alcohol during phase change, the raw materials are natural and environment-friendly, and the enthalpy value of a plurality of environment-friendly phase change materials is higher, so that the material has wide application prospect.
Description
Technical Field
The invention relates to a preparation method of a shape-stabilized phase-change material, in particular to a preparation method of a natural environment-friendly shape-stabilized phase-change material.
Background
The phase-change material is a novel energy material and is a research hotspot of current new energy. Among them, there are many kinds of environment-friendly materials with high phase change enthalpy value, and the material has wide application prospect.
However, the phase change material faces the leakage problem in application, and the application range of the phase change material can be expanded by shaping the phase change material. The silkworm cocoon is used as a natural environment-friendly material which is cheap and easy to obtain, has a large application space as a supporting material, and can be processed to enable the pore structure of the silkworm cocoon to be used for loading a phase change material so as to prepare the environment-friendly phase change material. The novel natural environment-friendly shape-stabilized phase change material has wide application prospect due to convenience, easy obtainment, nature and environment protection.
Disclosure of Invention
The invention aims to provide a novel natural environment-friendly shape-stabilized phase change material and a preparation method thereof, so as to solve the problems in the background technology.
The synthetic natural environment-friendly shape-stabilized phase change material comprises the following steps:
firstly, natural silkworm cocoons are put into a tubular furnace for high-temperature carbonization treatment, then products are ground into powder and put into a container, then concentrated acid is added to immerse the powder, the powder is subjected to acid treatment in an oil bath, inorganic matters in holes of the silkworm cocoons are completely removed, then the silkworm cocoons are poured out for suction filtration, the silkworm cocoons after the acid treatment are dried, then the silkworm cocoons and phase change materials are mixed according to a proportion and added into a beaker, the beaker is put into a vacuum oven for vacuum impregnation, and the obtained sample is the natural shape-stabilized phase change material.
Further, the carbonization temperature of the silkworm cocoons in the step is 800-; the time required for the carbonization of the silkworm cocoons is 10-12h, and the optimal time is 12 h.
Further, the concentrated acid subjected to acid treatment in the step is one or more of concentrated nitric acid (mass fraction of 65-68%), concentrated hydrochloric acid (mass fraction of 35-38%) and concentrated sulfuric acid (mass fraction of 95-98%).
Further, the acid treatment temperature is 50-60 ℃, preferably 50 ℃; the acid treatment is frequently carried out for 1 to 2 hours, preferably for 2 hours.
Further, drying the silkworm cocoons subjected to acid treatment in the step by using a common oven at the temperature of 80-100 ℃, and optimally selecting the temperature of 80 ℃; the drying time is 6-8h, and the optimal drying time is 8 h.
Further, the phase change material selected in the step can be one or more of erythritol, D-mannitol, paraffin, eicosane and the like; the mass ratio of the silkworm cocoon to the phase change material is 10-30:70-90, preferably 10: 85.
Further, the vacuum impregnation temperature in the step is 120-130 ℃, and the time is 3-4h, optimally 4 h; the vacuum degree is between-0.1 MPa and 0.1MPa, preferably-0.1 MPa.
Further, the product obtained in the step needs to be subjected to a leakage experiment, and the specific process is that filter paper is placed in a culture dish, the product is placed on the filter paper, and then the culture dish is placed in an oven to be heated at a temperature 10-20 ℃ higher than the phase transition temperature of the selected phase transition material until no liquid trace exists on the filter paper, namely the leakage experiment is completed.
The novel natural environment-friendly shape-stabilized phase change material synthesized by the method can prevent leakage of sugar alcohol during phase change, the raw materials are natural and environment-friendly, and the enthalpy value of a plurality of environment-friendly phase change materials is higher, so that the novel material has wide application prospect.
Detailed Description
Example 1
(1) Placing natural silkworm cocoons into a tube furnace for carbonization treatment at 800 ℃ for 12h, taking out and grinding the natural silkworm cocoons into powder, placing 0.5g of the powder into a round bottom flask, adding 20ml of concentrated nitric acid (mass fraction is 68%) to immerse the powder, heating the powder in an oil bath at 50 ℃ for 1h, and removing inorganic substances in holes of the silkworm cocoons.
(2) Then pouring out the silkworm cocoon, carrying out suction filtration, drying the silkworm cocoon subjected to acid treatment for 2 hours at 100 ℃ for 8 hours, then respectively adding the dried silkworm cocoon and paraffin into a beaker according to the mass ratio of 10:90, and then putting the beaker into a vacuum oven (the vacuum degree is-0.1 MPa) for dipping for 4 hours at 120 ℃.
(3) And (3) placing the product in the step (2) in a culture dish with filter paper, placing the culture dish in an oven, and heating at 130 ℃ until no liquid trace exists on the filter paper, namely the leakage experiment is completed, and obtaining a sample, namely the pure natural shape-stabilized phase change material.
The novel natural environment-friendly shape-stabilized phase change material is black block-shaped, and the enthalpy value of the novel natural environment-friendly shape-stabilized phase change material is 102.32kJ/Kg measured by differential scanning calorimetry.
Example 2
(1) Placing natural silkworm cocoons into a tube furnace for carbonization treatment at 800 ℃ for 12h, taking out and grinding the natural silkworm cocoons into powder, placing 0.5g of the powder into a round bottom flask, adding 20ml of concentrated sulfuric acid (mass fraction is 98%) to immerse the powder, heating the powder in an oil bath at 60 ℃ for 1.5h, and removing inorganic substances in holes of the silkworm cocoons.
(2) Then pouring out and carrying out suction filtration, placing the silkworm cocoons which are subjected to acid treatment for 1.5h in a drying oven to be dried for 7h at 80 ℃, then respectively adding the dried silkworm cocoons and mannitol into a beaker according to the proportion of 15:85, and then placing the beaker into a vacuum drying oven (the vacuum degree is-0.1 MPa) to be soaked for 4h at 180 ℃.
(3) And (3) placing the product in the step (2) in a culture dish with filter paper, placing the culture dish in an oven, and heating at 180 ℃ until no liquid trace exists on the filter paper, namely the leakage experiment is completed, and obtaining a sample, namely the pure natural shape-stabilized phase change material.
The novel natural environment-friendly shape-stabilized phase change material is black block-shaped, and the enthalpy value of the novel natural environment-friendly shape-stabilized phase change material is 89.69kJ/Kg measured by differential scanning calorimetry.
Claims (10)
1. A preparation method of a natural environment-friendly shape-stabilized phase change material is characterized by comprising the following process steps:
firstly, natural silkworm cocoons are put into a tubular furnace for high-temperature carbonization treatment, then products are ground into powder and put into a container, then concentrated acid is added to immerse the powder, the powder is subjected to acid treatment in an oil bath, inorganic matters in holes of the silkworm cocoons are completely removed, then the silkworm cocoons are poured out for suction filtration, the silkworm cocoons after the acid treatment are dried, then the silkworm cocoons and phase change materials are mixed according to a proportion and added into a beaker, the beaker is put into a vacuum oven for vacuum impregnation, and the obtained sample is the natural shape-stabilized phase change material.
2. The method according to claim 1, wherein the cocoon carbonization temperature is 800-;
the time required for the carbonization of the silkworm cocoons is 10-12h, and the optimal time is 12 h.
3. The preparation method according to claim 1, wherein the concentrated acid is one or more of concentrated nitric acid (mass fraction of 65-68%), concentrated hydrochloric acid (mass fraction of 35-38%), and concentrated sulfuric acid (mass fraction of 95-98%).
4. The method of claim 1 or 3, wherein the acid treatment temperature is 50 to 60 ℃, preferably 50 ℃;
the acid treatment is frequently carried out for 1 to 2 hours, preferably for 2 hours.
5. The method of claim 1, wherein the acid-treated silkworm cocoon is dried in a common oven at 80-100 ℃, preferably 80 ℃;
the drying time is 6-8h, and the optimal drying time is 8 h.
6. The preparation method according to claim 1, wherein the selected phase change material is one or more of erythritol, D-mannitol, paraffin, eicosane, etc.;
the mass ratio of the dried silkworm cocoons to the phase change material is 10-30:70-90, preferably 10: 85.
7. The method as claimed in claim 1, wherein the vacuum impregnation temperature is 120-130 ℃, and the time is 3-4h, preferably 4 h;
the vacuum degree is between-0.1 MPa and 0.1MPa, preferably-0.1 MPa.
8. The method of claim 1, wherein the product is subjected to a leakage test by placing filter paper in a petri dish, placing the product on the filter paper, and placing the petri dish in an oven to heat at a temperature 10-20 ℃ higher than the phase transition temperature of the selected phase change material until no trace of liquid is on the filter paper.
9. A phase change material produced by the production method according to any one of claims 1 to 8.
10. Use of a phase change material according to claim 9, characterized in that: the phase-change material product can be used as a phase-change material for thermal energy conversion and storage.
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| CN202010771331.0A CN114058335A (en) | 2020-08-04 | 2020-08-04 | Preparation and application of natural environment-friendly shape-stabilized phase change material |
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| CN202010771331.0A CN114058335A (en) | 2020-08-04 | 2020-08-04 | Preparation and application of natural environment-friendly shape-stabilized phase change material |
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2020
- 2020-08-04 CN CN202010771331.0A patent/CN114058335A/en active Pending
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