CN111961228A - Composite phase-change cold storage material hydrogel and preparation method and application thereof - Google Patents
Composite phase-change cold storage material hydrogel and preparation method and application thereof Download PDFInfo
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 73
- 239000011232 storage material Substances 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000008859 change Effects 0.000 claims abstract description 40
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 38
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910021538 borax Inorganic materials 0.000 claims abstract description 19
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 19
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 19
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 18
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 16
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- 239000002562 thickening agent Substances 0.000 claims abstract description 10
- 239000001103 potassium chloride Substances 0.000 claims abstract description 9
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000004321 preservation Methods 0.000 claims abstract description 6
- 238000004132 cross linking Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 13
- 238000010257 thawing Methods 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- IPGANOYOHAODGA-UHFFFAOYSA-N dilithium;dimagnesium;dioxido(oxo)silane Chemical group [Li+].[Li+].[Mg+2].[Mg+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O IPGANOYOHAODGA-UHFFFAOYSA-N 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- -1 phosphate ester Chemical class 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
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- 239000003431 cross linking reagent Substances 0.000 claims description 3
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/002—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches with controlled internal environment
- A41D13/005—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches with controlled internal environment with controlled temperature
- A41D13/0053—Cooled garments
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
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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
- C09K5/066—Cooling mixtures; De-icing compositions
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D2500/00—Materials for garments
- A41D2500/50—Synthetic resins or rubbers
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D2600/00—Uses of garments specially adapted for specific purposes
- A41D2600/20—Uses of garments specially adapted for specific purposes for working activities
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- C08J2329/00—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 at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
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- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
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Abstract
The invention discloses a composite phase change cold storage material hydrogel and a preparation method and application thereof. The anti-foaming agent comprises, by mass, 20-30 parts of polyvinyl alcohol, 2-3 parts of a water-based defoaming agent, 1-2 parts of a thickening agent, 8-15 parts of 8-15% potassium chloride solution, 80-120 parts of 8-12% sodium tetraborate solution and 400-600 parts of water. The preparation method comprises the following steps: respectively adding a water-based defoaming agent, a thickening agent and a potassium chloride solution into a polyvinyl alcohol solution, stirring until the mixture is fully and uniformly mixed, then adding a sodium tetraborate solution, quickly stirring for 30-60 seconds at 90-100 ℃ until the mixture is fully chemically crosslinked to obtain a polyvinyl alcohol hydrogel, carrying out water bath heat preservation to remove bubbles, repeatedly freezing and unfreezing for 1-3 times, and carrying out physical crosslinking to obtain the composite phase change cold storage material hydrogel. The product has no pollution and corrosiveness, the gel can be repeatedly utilized for many times, the supercooling degree is low, obvious phase separation is avoided, the latent heat of phase change is large, the cold insulation time is long, and the clothing is comfortable to wear when being used for cooling clothing.
Description
Technical Field
The invention belongs to the technical field of cold storage materials, and particularly relates to a composite phase change cold storage material hydrogel and a preparation method and application thereof.
Background
Since the 20 th century and the 30 th century, particularly under the influence of the energy crisis of the 80 th century, the basic theory and application technology research of phase change heat storage ((LTES) rapidly rises and develops in developed countries (such as America, Canada, Japan, Germany) because with the rapid development of scientific technology, energy gradually becomes the basis for human survival, but the supply and demand of energy have strong timeliness, and in order to improve the energy utilization efficiency, protect the environment and solve the contradiction between the mismatch of heat energy supply and demand, the phase change energy storage technology has been widely applied in solar energy utilization, peak shifting and valley filling of electric power, waste heat recycling and energy saving of buildings and air conditioners, and is currently the hot point of research in the world.
Phase change materials pcm (phase change materials) is a chemical material that uses latent heat of phase change to store and release energy. The phase change energy storage material is a substance which can automatically absorb or release latent heat to the environment by utilizing the phase state or structural change of the material within a certain temperature range, and maintain the state that the temperature of the material is kept unchanged, so as to regulate and control the temperature of the environment.
Nowadays, many special workers have to face high-temperature and hot-summer work, such as founders, steel makers, high-temperature welders, oil workers, firemen, duty traffic polices and the like, and the problem of cooling and heat dissipation is not negligible. As in the construction field, construction workers often need to be in contact with some high heat rebar and concrete for long periods of time. When the human body works and produces in high-temperature working environments such as high-temperature environment, hot summer open-air environment and the like, the human body is influenced by high temperature, not only physiological function tension related to body temperature regulation is caused, but also heat-induced diseases such as heatstroke and the like can be caused in serious cases. On the one hand, the high temperature of environment can lead to work efficiency's reduction, and on the other hand, in case ambient temperature is higher than the high temperature threshold that the human body can bear, can lead to human physiological safety problem. Therefore, when the high-temperature operation is carried out, the body of the high-temperature operation personnel is timely and effectively protected at high temperature and cooled, the working time can be prolonged, the working efficiency can be improved, and the physiological safety of the personnel can be greatly improved.
Through the analysis, under the high temperature environment, the change of the physiological function of the human body is compensatory reaction of the human body to high temperature labor within a certain range, once the heat stress exceeds the tolerance of the human body, the work efficiency is reduced, the judgment is influenced, sunstroke can be caused seriously, and more serious death can be caused. The use of cooling suits is essential for personnel working in high temperature environments without air conditioners or other refrigeration equipment. Therefore, it is necessary to research the phase change cool storage material in the cooling suit.
Different from liquid materials needing quick cold accumulation such as air conditioners, refrigerated cabinets and the like, the cooling waistcoats need to have strong cold accumulation aging, and most of cooling waistcoats made of the existing cold accumulation materials have the problems of insufficient cold accumulation, short cold accumulation time, poor economic benefit or poor human body comfort level and the like, so that the current-stage research is dedicated to improving the formula of the cold accumulation materials, optimizing the preparation process, increasing the cold accumulation amount, and improving the cold accumulation time and the close-fitting comfort level of the frozen products.
Disclosure of Invention
The invention aims to provide a composite phase change cold storage material hydrogel and a preparation method and application thereof.
In order to solve the technical problems, the invention provides the following technical scheme:
the composite phase change cold storage material hydrogel comprises the following components in parts by weight: 20-30 parts of polyvinyl alcohol, 2-3 parts of an aqueous defoaming agent, 1-2 parts of a thickening agent, 8-15 parts of a potassium chloride solution with the mass percentage concentration of 8-15%, 80-120 parts of a sodium tetraborate solution with the mass percentage concentration of 8-12% and 400-600 parts of water.
According to the scheme, the molecular weight of the polyvinyl alcohol is 1500-2000.
According to the scheme, the defoaming agent is a phosphate ester water-based defoaming agent.
According to the scheme, the thickening agent is the magnesium lithium silicate, and the effect of the thickening agent can improve the water retention performance of the hydrogel and reduce the phase separation phenomenon of the hydrogel.
The preparation method of the composite phase change cold storage material hydrogel comprises the following steps:
1) dissolving 20-30 parts of polyvinyl alcohol into 400-600 parts of water to obtain a polyvinyl alcohol solution;
2) respectively adding 2-3 parts of a water-based defoaming agent, 1-2 parts of a thickening agent and 8-15 parts of a potassium chloride solution with the mass percentage concentration of 8-15% into the polyvinyl alcohol solution obtained in the step 1), and stirring until the mixture is fully and uniformly mixed;
3) adding 80-120 parts of sodium tetraborate solution as a crosslinking agent with the mass percentage concentration of 8-12% into the mixed solution obtained in the step 2), wherein the temperature of the sodium tetraborate solution and the mixed solution is 90-100 ℃, and rapidly stirring for 30-60 s at the rotating speed of 1000-1200 r/min until full chemical crosslinking is achieved to obtain polyvinyl alcohol hydrogel;
4) placing the polyvinyl alcohol hydrogel obtained in the step 3) in a water bath at the temperature of 90-100 ℃ for heat preservation for 1-2 hours to remove bubbles in the hydrogel;
5) and (3) repeatedly freezing and unfreezing the hydrogel subjected to bubble removal in the step 4) for 1-3 times, and carrying out physical crosslinking to obtain the composite phase change cold storage material hydrogel.
According to the scheme, the heating temperature in the step 1) is 90-100 ℃.
According to the scheme, in the step 5), the freezing and unfreezing conditions are as follows: and freezing the hydrogel at-15 to-20 ℃ for 12 to 24 hours, taking out the hydrogel, and completely thawing the hydrogel at 40 to 55 ℃.
Provides the application of the composite phase change cold storage material hydrogel in cooling clothes.
The invention has the beneficial effects that:
1. the composite phase change cold storage material hydrogel provided by the invention adopts nontoxic and easily-obtained polyvinyl alcohol and water as main raw materials, non-corrosive inorganic salt as a cooling agent, sodium tetraborate as a cross-linking agent, and a small amount of nontoxic and non-corrosive aqueous defoaming agent and thickening agent as auxiliary materials, so that the product is free of pollution and corrosion, the gel can be repeatedly utilized for many times, the supercooling degree is small, obvious phase separation is avoided, the phase change latent heat is large, and the cold retention time reaches 5-6 hours; when the gel is used for cooling clothes, the gel prepared by using polyvinyl alcohol as a main material has moderate softness, does not feel uncomfortable when contacting with a human body, and simultaneously has better cold insulation effect because the gel has better cold insulation effect, and can achieve better cold insulation effect only by loading a small amount of cold storage material, thereby reducing the burden of the human body.
2. In the preparation process, the addition of the defoaming agent can obviously reduce bubbles generated in the earlier stage polyvinyl alcohol dissolving process, and meanwhile, the addition of the borax solution in the later stage of high-temperature rapid stirring can greatly reduce bubbles generated in hydrogel in the crosslinking process, shorten the later stage water bath defoaming time, reduce the overall preparation time, improve the uniformity of the composite phase change cold storage material hydrogel system, and have the advantages of simple preparation process, cheap and easily available raw materials, low cost and industrial application prospect.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
The phase change latent heat value of the composite phase change cold storage material hydrogel obtained in the embodiment is determined as follows:
the phase change latent heat value is obtained by measuring a DSC curve of a sample, and the specific test conditions are as follows:
test range of temperature: -150 ℃ to +600 ℃; equipment sensitivity: 5 MuV/mW; linearity of baseline: 0.8 mW; heat range: +/-700 mW; temperature rise range: 10 to 50 ℃; the heating rate is as follows: 0.1 to 99.9K/min; cooling atmosphere: liquid nitrogen.
Example 1
The preparation method of the composite phase change cold storage material hydrogel comprises the following specific steps:
(1) 20g of polyvinyl alcohol (PVA1799) is added into 400g of deionized water, heated to 95 ℃ in a water bath and stirred for 10min until the polyvinyl alcohol is completely dissolved.
(2) After the materials are completely dissolved, 2.0g of phosphate ester aqueous defoaming agent, 12g of potassium chloride solution with the mass percentage concentration of 10% and 1.0g of magnesium lithium silicate are respectively added, and the materials are stirred for 10min until the materials are fully and uniformly mixed.
(3) And (3) adding 80g of 8% sodium tetraborate solution into the mixed solution obtained in the step (2), wherein the temperature of the sodium tetraborate solution and the temperature of the mixed solution are both 90 ℃, and the PVA hydrogel is obtained after the sodium tetraborate solution and the mixed solution are rapidly stirred for 30s at the rotating speed of 1000r/min until the PVA hydrogel is fully chemically crosslinked.
(4) And (3) placing the polyvinyl alcohol hydrogel obtained in the step 3) in a water bath at 90 ℃ for heat preservation for 2h to remove bubbles in the hydrogel.
(5) And (3) freezing the hydrogel subjected to bubble removal in the step 4) in a refrigerator at the temperature of-18 ℃ for 24 hours, taking out the hydrogel from the refrigerator, putting the hydrogel in a constant-temperature drying oven at the temperature of 55 ℃ until the hydrogel is completely thawed, and repeatedly freezing and thawing for three times to obtain the physically crosslinked composite phase change cold storage material hydrogel.
The phase change latent heat of the hydrogel prepared under the condition is 267.89J/g through DSC detection calculation, the cold insulation time in a forced air drying oven at 35 ℃ is 6h, after 200 times of freeze thawing circulation, the phase change latent heat value is reduced by 7.8J/kg, the mass is reduced by 1.3%, and the prepared hydrogel is longer in cold insulation time and has no obvious reduction in performance effect after being used for many times.
Example 2
The preparation method of the composite phase change cold storage material hydrogel comprises the following specific steps:
(1) 25g of polyvinyl alcohol (PVA1799) is added into 500g of deionized water, heated to 95 ℃ in a water bath and stirred for 15min until the polyvinyl alcohol is completely dissolved.
(2) After the materials are completely dissolved, 2.5g of phosphate ester aqueous defoaming agent, 12g of potassium chloride solution with the mass percentage concentration of 10% and 1.5g of magnesium lithium silicate are respectively added, and the materials are stirred for 10min until the materials are fully and uniformly mixed.
(3) And (3) adding 100g of 10% sodium tetraborate solution into the mixed solution obtained in the step (2), wherein the temperatures of the sodium tetraborate solution and the mixed solution are both 95 ℃, and the PVA hydrogel is obtained after the sodium tetraborate solution and the mixed solution are rapidly stirred for 60s at the rotating speed of 1200r/min until the PVA hydrogel is fully chemically crosslinked.
(4) Placing the polyvinyl alcohol hydrogel obtained in the step 3) in a water bath at 95 ℃ for heat preservation for 2h to remove bubbles existing in the hydrogel;
(5) and (3) freezing the hydrogel subjected to bubble removal in the step 4) in a refrigerator at the temperature of-18 ℃ for 24 hours, taking out the hydrogel from the refrigerator, putting the hydrogel in a constant-temperature drying oven at the temperature of 55 ℃ until the hydrogel is completely thawed, and repeatedly freezing and thawing for three times to obtain the physically crosslinked composite phase change cold storage material hydrogel.
The phase change latent heat of the hydrogel prepared under the condition is 254.72J/g through DSC detection calculation, the cold insulation time in a forced air drying oven at 35 ℃ is 5h, after 200 times of freeze-thaw cycles, the phase change latent heat value is reduced by 6.84J/kg, the mass is reduced by 1.1%, and the prepared hydrogel is longer in cold insulation time and has no obvious reduction in performance effect after being used for many times.
Example 3
The preparation method of the composite phase change cold storage material hydrogel comprises the following specific steps:
(1) 20g of polyvinyl alcohol (PVA1799) is added into 400g of deionized water, heated to 95 ℃ in a water bath and stirred for 10min until the polyvinyl alcohol is completely dissolved.
(2) After the mixture is completely dissolved, 2.5g of phosphate ester aqueous defoaming agent, 12g of potassium chloride solution with the concentration of 10% and 2g of magnesium lithium silicate are respectively added, and the mixture is stirred for 10min until the mixture is fully and uniformly mixed.
(3) And (3) adding 80g of 10% sodium tetraborate solution into the mixed solution obtained in the step (2), wherein the temperature of the sodium tetraborate solution and the temperature of the mixed solution are both 100 ℃, and the polyvinyl alcohol hydrogel is obtained after the sodium tetraborate solution and the mixed solution are rapidly stirred for 60s at the rotating speed of 1200r/min until the chemical crosslinking is fully performed.
(4) And (3) placing the polyvinyl alcohol hydrogel obtained in the step 3) in a water bath at 100 ℃ for heat preservation for 2h to remove bubbles in the hydrogel.
(5) And (3) freezing the hydrogel subjected to bubble removal in the step 4) in a refrigerator at the temperature of-18 ℃ for 24 hours, taking out the hydrogel from the refrigerator, putting the hydrogel in a constant-temperature drying oven at the temperature of 55 ℃ until the hydrogel is completely thawed, and repeatedly freezing and thawing for three times to obtain the physically crosslinked composite phase change cold storage material hydrogel.
The phase change latent heat of the hydrogel prepared under the condition is 281.23J/g through DSC detection calculation, the cold insulation time in a blast drying box at 35 ℃ is 6h, the phase change latent heat value is reduced by 9.1J/kg and the quality is reduced by 1.8% after 200 times of freeze-thaw cycles, which indicates that the prepared hydrogel has longer cold insulation time and the performance effect is not obviously reduced after multiple times of use.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents and are included in the scope of the present invention.
Claims (8)
1. The composite phase change cold storage material hydrogel is characterized by comprising the following components in parts by weight: 20-30 parts of polyvinyl alcohol, 2-3 parts of an aqueous defoaming agent, 1-2 parts of a thickening agent, 8-15 parts of a potassium chloride solution with the mass percentage concentration of 8-15%, 80-120 parts of a sodium tetraborate solution with the mass percentage concentration of 8-12% and 400-600 parts of water.
2. The composite phase change cold storage material hydrogel according to claim 1, wherein the molecular weight of the polyvinyl alcohol is 1500-2000.
3. The composite phase change cold storage material hydrogel according to claim 1, wherein the aqueous defoaming agent is a phosphate ester aqueous defoaming agent.
4. The composite phase-change cold storage material hydrogel according to claim 1, wherein the thickener is lithium magnesium silicate.
5. A preparation method of the composite phase change cold storage material hydrogel according to any one of claims 1 to 4, characterized by comprising the following steps:
1) dissolving 20-30 parts of polyvinyl alcohol into 400-600 parts of water to obtain a polyvinyl alcohol solution;
2) respectively adding 2-3 parts of a water-based defoaming agent, 1-2 parts of a thickening agent and 8-15 parts of a potassium chloride solution with the mass percentage concentration of 8-15% into the polyvinyl alcohol solution obtained in the step 1), and stirring until the mixture is fully and uniformly mixed;
3) adding 80-120 parts of sodium tetraborate solution as a crosslinking agent with the mass percentage concentration of 8-12% into the mixed solution obtained in the step 2), wherein the temperature of the sodium tetraborate solution and the mixed solution is 90-100 ℃, and rapidly stirring for 30-60 s at the rotating speed of 1000-1200 r/min until full chemical crosslinking is achieved to obtain polyvinyl alcohol hydrogel;
4) placing the polyvinyl alcohol hydrogel obtained in the step 3) in a water bath at the temperature of 90-100 ℃ for heat preservation for 1-2 hours to remove bubbles in the hydrogel;
5) and (3) repeatedly freezing and unfreezing the hydrogel subjected to bubble removal in the step 4) for 1-3 times, and carrying out physical crosslinking to obtain the composite phase change cold storage material hydrogel.
6. The method according to claim 5, wherein in the step 5), the freezing and thawing conditions are: and freezing the hydrogel at-15 to-20 ℃ for 12 to 24 hours, taking out the hydrogel, and completely thawing the hydrogel at 40 to 55 ℃.
7. The method according to claim 5, wherein in the step 1), the temperature of the polyvinyl alcohol dissolved in water in the step 1) is 90 to 100 ℃.
8. Use of the composite phase change cold storage material hydrogel according to any one of claims 1 to 4 in cooling clothes.
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