CN111440596A - Phase-change energy-storage temperature-regulating slurry powder - Google Patents

Phase-change energy-storage temperature-regulating slurry powder Download PDF

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Publication number
CN111440596A
CN111440596A CN202010415451.7A CN202010415451A CN111440596A CN 111440596 A CN111440596 A CN 111440596A CN 202010415451 A CN202010415451 A CN 202010415451A CN 111440596 A CN111440596 A CN 111440596A
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parts
phase
slurry powder
change energy
temperature
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CN202010415451.7A
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周晶
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-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
    • C09K5/02Materials undergoing a change of physical state when used
    • C09K5/06Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
    • C09K5/063Materials absorbing or liberating heat during crystallisation; Heat storage materials

Abstract

The invention provides phase-change energy-storage temperature-regulating slurry powder which is prepared from the following components in parts by weight: 25-35 parts of microcrystalline wax, 15-25 parts of n-capric acid, 12-16 parts of flame retardant, 0.2-0.8 part of mildew preventive, 0.2-0.8 part of phase-change temperature regulator and 30-40 parts of vitrified micro bubbles; the phase transition temperature regulator is any one or any combination of sodium chloride, potassium chloride, ammonium chloride or ammonium sulfate; the vitrified micro bubbles are closed hole vitrified micro bubbles with the average grain size of 0.6-0.8 mm. The phase-change energy-storage temperature-regulating slurry powder prepared by the invention is non-toxic and odorless, and after the microcrystalline wax and the n-decanoic acid are added together, the thermal cycle stability of the phase-change energy-storage temperature-regulating slurry powder is improved; the addition of the vitrified micro bubbles improves the heat insulation, fire prevention, sound absorption and heat preservation performances of the phase-change energy-storage temperature-regulating slurry powder.

Description

Phase-change energy-storage temperature-regulating slurry powder
Technical Field
The invention relates to a synthesis method of an organic compound, in particular to phase-change energy-storage temperature-regulating slurry powder.
Background
In a building, the heat loss of the outer protective structure is large, and the wall body in the outer protective structure accounts for a large part. Therefore, the reformation of building wall bodies and the development of wall body energy-saving technology are the most important links of the building energy-saving technology, and the development of external wall heat-insulating technology and energy-saving materials are the main realization modes of building energy conservation. Among them, foamed plastic heat insulating materials such as EPS boards, XPS boards, foamed polyurethane boards, and the like have drawn attention because of their excellent comprehensive properties.
However, the existing external wall heat-insulating energy-saving materials have the defects of easy cracking and no high temperature resistance, and the heat storage capacity of the materials needs to be further improved.
Disclosure of Invention
The invention aims to provide phase-change energy-storage temperature-regulating slurry powder which is not easy to crack, resistant to high temperature and strong in heat storage capacity.
The invention is realized by the following technical scheme.
A phase-change energy-storage temperature-regulating slurry powder is prepared from the following components in parts by weight: 25-35 parts of microcrystalline wax, 15-25 parts of n-capric acid, 12-16 parts of flame retardant, 0.2-0.8 part of mildew preventive, 0.2-0.8 part of phase-change temperature regulator and 30-40 parts of vitrified micro bubbles;
the phase transition temperature regulator is any one or any combination of sodium chloride, potassium chloride, ammonium chloride or ammonium sulfate;
the vitrified micro bubbles are closed hole vitrified micro bubbles with the average grain size of 0.6-0.8 mm.
Preferably, the phase-change energy-storage temperature-regulating slurry powder is prepared from the following components in parts by weight: 28-32 parts of microcrystalline wax, 18-22 parts of n-decanoic acid, 13-15 parts of flame retardant, 0.4-0.6 part of mildew preventive, 0.4-0.6 part of phase change temperature regulator and 33-37 parts of vitrified micro bubbles.
Preferably, the phase-change energy-storage temperature-regulating slurry powder is prepared from the following components in parts by weight: 30 parts of microcrystalline wax, 20 parts of n-capric acid, 14 parts of flame retardant, 0.5 part of mildew preventive, 0.5 part of phase-change temperature regulator and 35 parts of vitrified micro bubbles.
Specifically, the flame retardant is prepared from active magnesium hydroxide, microcapsule red phosphorus, antimony trioxide and zinc borate according to the mass ratio of 50 (8-12) to (6-10) to (3-6).
Specifically, the mildew preventive is prepared from sorbic acid and benzoic acid according to the mass ratio of 4-6: 1.
The invention also provides a preparation method of the phase-change energy-storage temperature-regulating slurry powder, which comprises the following operation steps: mixing microcrystalline wax and n-capric acid, heating to 185 ℃, sequentially adding a flame retardant, a mildew preventive and a phase change temperature regulator while continuously stirring, continuously stirring for reaction for 2-3 hours, adding vitrified micro bubbles, continuously stirring for 6-8 hours, heating to 335 ℃, keeping the temperature, continuously stirring for 10-15 minutes, naturally cooling to the coating temperature, and coating to obtain the phase change energy storage temperature regulation slurry powder.
Specifically, the coating temperature is 45-50 ℃.
According to the technical scheme, the beneficial effects of the invention are as follows:
1) the phase-change energy-storage temperature-adjusting slurry powder prepared by the invention is pressed on the surface of a plate to prepare a heat-insulating layer, so that the heat resistance of the plate can be effectively improved, and the heat-insulating layer is not easy to crack in the using process;
2) the phase-change energy-storage temperature-regulating slurry powder prepared by the invention has excellent mildew-proof and moisture-proof performances and long service life;
3) the phase-change energy-storage temperature-regulating slurry powder prepared by the invention is non-toxic and odorless, and after the microcrystalline wax and the n-decanoic acid are added together, the thermal cycle stability of the phase-change energy-storage temperature-regulating slurry powder is improved;
4) the addition of the vitrified micro bubbles improves the heat insulation, fire prevention, sound absorption and heat preservation performances of the phase-change energy-storage temperature-regulating slurry powder.
Drawings
FIG. 1 is a diagram showing the state of the snow cake in the experiment of heat release in cold.
FIG. 2 is a diagram showing the state of the refrigerator body in the cooling heat release function experiment.
FIG. 3 is a diagram showing the state of ice cream after 4 hours of freezing in a box body in a cold exposure heat release function experiment.
Fig. 4 is a state diagram of the snow cake placed in the box body in the flame-retardant heat-insulation effect experiment.
FIG. 5 is a diagram showing the heating state of the box body in the experiment of flame-retardant and heat-insulating effects.
FIG. 6 is a diagram showing the state of the ice cream bar after the box body is heated in the experiment of the flame-retardant and heat-insulating effect.
FIG. 7 is a diagram of the experimental process of high-temperature spray combustion of the energy-storage thermal-insulation wall panel in the high-temperature explosion-proof real man experiment.
FIG. 8 is a diagram of the energy-storage thermal-insulation wall panel after high-temperature spray combustion in the high-temperature explosion-proof real man experiment.
Fig. 9-11 are schematic views of the fire-fighting comprehensive test process.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
A phase-change energy-storage temperature-regulating slurry powder is prepared from the following components in parts by weight: 25 parts of microcrystalline wax, 15 parts of n-capric acid, 12 parts of flame retardant, 0.2 part of mildew preventive, 0.2 part of sodium chloride and 30 parts of closed-cell vitrified micro-beads with the average particle size of 0.6 mm;
wherein the flame retardant is prepared from active magnesium hydroxide, microcapsule red phosphorus, antimony trioxide and zinc borate according to the mass ratio of 50:8:6: 3; the mildew preventive is prepared from sorbic acid and benzoic acid according to the mass ratio of 4: 1.
Example 2
A phase-change energy-storage temperature-regulating slurry powder is prepared from the following components in parts by weight: 25-35 parts of microcrystalline wax, 15-25 parts of n-capric acid, 12-16 parts of flame retardant, 0.2-0.8 part of mildew preventive, 0.2-0.8 part of potassium chloride and 35 parts of closed-pore vitrified micro-beads with the average particle size of 0.7 mm;
wherein the flame retardant is prepared from active magnesium hydroxide, microcapsule red phosphorus, antimony trioxide and zinc borate according to the mass ratio of 50:10:8: 5; the mildew preventive is prepared from sorbic acid and benzoic acid according to the mass ratio of 5: 1.
Example 3
A phase-change energy-storage temperature-regulating slurry powder is prepared from the following components in parts by weight: 35 parts of microcrystalline wax, 25 parts of n-capric acid, 16 parts of flame retardant, 0.8 part of mildew preventive, 0.8 part of ammonium sulfate and 40 parts of closed-pore vitrified micro-beads with the average particle size of 0.8 mm;
wherein the flame retardant is prepared from active magnesium hydroxide, microcapsule red phosphorus, antimony trioxide and zinc borate according to the mass ratio of 50:12:10: 6; the mildew preventive is prepared from sorbic acid and benzoic acid according to the mass ratio of 6: 1.
Example 4
A preparation method of phase-change energy-storage temperature-regulating slurry powder comprises the following operation steps: mixing microcrystalline wax and n-capric acid, heating to 185 ℃, sequentially adding a flame retardant, a mildew preventive and a phase change temperature regulator while continuously stirring, continuously stirring for reaction for 2-3 hours, adding vitrified micro bubbles, continuously stirring for 6-8 hours, heating to 335 ℃, keeping the temperature, continuously stirring for 10-15 minutes, naturally cooling to the coating temperature, and coating to obtain the phase change energy storage temperature regulation slurry powder.
Specifically, the coating temperature is 45-50 ℃.
Comparative example 1
The n-decanoic acid was replaced with an equal amount of microcrystalline wax and the remaining ingredients were exactly the same as in example 1.
Comparative example 2
The composition was the same as in example 2 except that no vitrified small balls were added.
According to the components of the examples 1-3 and the comparative examples 1-2, the phase-change energy-storage temperature-regulating slurry powder is prepared by the method of the example 4, and then the various performances of the prepared phase-change energy-storage temperature-regulating slurry powder are tested, and the test results are shown in the table 1:
TABLE 1 phase-change energy-storage temp. -regulating slurry powder properties
Item Phase change latent heat value after 200 times of circulation, J/g Compared with the percent pre-cycle decay%
Example 1 298 1.3
Comparative example 1 231 7.6
Example 2 302 1.2
Comparative example 2 291 1.4
Example 3 301 1.2
As can be seen from the data of the example 1 and the comparative example 1 in the table 1, after the microcrystalline wax and the n-decanoic acid are added together, the thermal cycle stability of the phase-change energy-storage temperature-regulating slurry powder is effectively improved.
The phase-change energy-storage temperature-regulating slurry powder prepared in the embodiment 1 is adopted to prepare the energy-storage heat-preservation wallboard, and then the performance of the energy-storage heat-preservation wallboard is tested.
Test 1
And (3) a cold heat release function experiment: the energy-storage heat-insulation wall plate is manufactured into a box body, the box body is irradiated by sunlight for 4 hours for heat storage, three ice creams are placed in the box body after the heat storage is completed, the box body is sealed and placed in a freezer for freezing for 4 hours, and then the box body is taken out and opened to check the melting state of the ice creams.
As shown in the figures 1-3, the ice cream in the energy-storage thermal-insulation wall board prepared by the invention has a larger melting area, and the phase-change energy-storage temperature-adjusting slurry powder prepared by the invention has super-strong heat storage and cold insulation functions.
Test 2
Flame-retardant and heat-insulating effect experiment: the energy-storage heat-insulation wall plate is made into a box body, three ice creams are placed in the box body, the box body is sealed and placed on a liquefied gas stove to burn for 10 minutes by big fire, and the melting state of the ice creams is checked after the box body is opened. As can be seen from the figures 4-6, the ice cream in the energy-storage heat-insulation wall board prepared by the invention has no melting phenomenon after the energy-storage heat-insulation wall board is heated at high temperature, and the phase-change energy-storage temperature-regulating slurry powder prepared by the invention has super strong fireproof and heat-insulation functions.
Test 3
High-temperature explosion-proof human experiment: the energy storage heat preservation wallboard is sprayed to one surface of the energy storage heat preservation wallboard by an acetylene welding gun with the use temperature of 1200 ℃, and a laboratory technician manually arranges the other surface of the energy storage heat preservation wallboard and checks the state of the energy storage heat preservation wallboard after lasting for one minute. As can be seen from the graphs of FIGS. 7 to 8, the phase-change energy-storage temperature-adjusting slurry powder prepared by the invention is not broken, cracked or exploded after being heated at ultrahigh temperature, and has super-strong fireproof, flame-retardant and heat-insulating properties.
Test 4
Fire-fighting comprehensive test: in a room made of the energy storage and heat preservation wallboard, workers can be seen through doors and windows on the front side, diesel oil combustion materials are used for burning on five wall surfaces of a room body for 20 minutes with big fire, instruments for temperature and humidity in the room show no change, the workers are safe and innoxious, and the experimental process is shown in figures 9-11.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.

Claims (7)

1. The phase-change energy-storage temperature-regulating slurry powder is characterized by being prepared from the following components in parts by weight: 25-35 parts of microcrystalline wax, 15-25 parts of n-capric acid, 12-16 parts of flame retardant, 0.2-0.8 part of mildew preventive, 0.2-0.8 part of phase-change temperature regulator and 30-40 parts of vitrified micro bubbles;
the phase transition temperature regulator is any one or any combination of sodium chloride, potassium chloride, ammonium chloride or ammonium sulfate;
the vitrified micro bubbles are closed hole vitrified micro bubbles with the average grain size of 0.6-0.8 mm.
2. The phase-change energy-storage temperature-regulating slurry powder as claimed in claim 1, which is prepared from the following components in parts by weight: 28-32 parts of microcrystalline wax, 18-22 parts of n-decanoic acid, 13-15 parts of flame retardant, 0.4-0.6 part of mildew preventive, 0.4-0.6 part of phase change temperature regulator and 33-37 parts of vitrified micro bubbles.
3. The phase-change energy-storage temperature-regulating slurry powder as claimed in claim 1, which is prepared from the following components in parts by weight: 30 parts of microcrystalline wax, 20 parts of n-capric acid, 14 parts of flame retardant, 0.5 part of mildew preventive, 0.5 part of phase-change temperature regulator and 35 parts of vitrified micro bubbles.
4. The phase-change energy-storage temperature-regulating slurry powder as claimed in any one of claims 1 to 3, wherein the flame retardant is prepared from active magnesium hydroxide, microcapsule red phosphorus, antimony trioxide and zinc borate according to the mass ratio of 50 (8-12) to (6-10) to (3-6).
5. The phase-change energy-storage temperature-regulating slurry powder as claimed in claim 1, wherein the mildew preventive is prepared from sorbic acid and benzoic acid in a mass ratio of 4-6: 1.
6. The preparation method of the phase-change energy-storage temperature-regulating slurry powder is characterized by comprising the following operation steps of: mixing microcrystalline wax and n-capric acid, heating to 185 ℃, sequentially adding a flame retardant, a mildew preventive and a phase change temperature regulator while continuously stirring, continuously stirring for reaction for 2-3 hours, adding vitrified micro bubbles, continuously stirring for 6-8 hours, heating to 335 ℃, keeping the temperature, continuously stirring for 10-15 minutes, naturally cooling to the coating temperature, and coating to obtain the phase change energy storage temperature regulation slurry powder.
7. A phase change energy storing tempering slurry powder of claim 6 wherein said coating temperature is 45-50 ℃.
CN202010415451.7A 2020-05-15 2020-05-15 Phase-change energy-storage temperature-regulating slurry powder Pending CN111440596A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101613592A (en) * 2009-07-21 2009-12-30 刘磊 Phase-change thermal-storage material and production method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101613592A (en) * 2009-07-21 2009-12-30 刘磊 Phase-change thermal-storage material and production method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
庞维强等译: "《化学火箭推进用新型含能材料》", 31 May 2019, 国防工业出版社 *
董发勤等: "《生态功能基元材料及其复合建材集成技术》", 31 October 2008, 电子科技大学出版社 *
赵浩峰等: "《物理功能复合材料及其性能》", 31 October 2010, 冶金工业出版社 *

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