CN113173751A - Phase-change gypsum and preparation method thereof - Google Patents
Phase-change gypsum and preparation method thereof Download PDFInfo
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- CN113173751A CN113173751A CN202010388845.8A CN202010388845A CN113173751A CN 113173751 A CN113173751 A CN 113173751A CN 202010388845 A CN202010388845 A CN 202010388845A CN 113173751 A CN113173751 A CN 113173751A
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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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
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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
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
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Abstract
The invention discloses a phase change gypsum and a preparation method thereof, wherein a natural inorganic porous material is used as a carrier to load a hydrated salt phase change material, a hydrated salt-porous carrier compound is prepared, then the hydrated salt-porous carrier compound is wrapped by water-soluble silicon or water glass, the hydrated salt-porous material compound type phase change energy storage material coated by the hydrogel is prepared after dehydration, the hydrated salt-porous material compound type phase change energy storage material coated by the hydrogel is mixed with gypsum to obtain phase change gypsum slurry, and the phase change gypsum slurry is compounded and molded with fiber filaments, grid cloth and the like to prepare the phase change gypsum. The phase-change gypsum realizes the isolation of the hydrated salt phase-change material from the gypsum, keeps the storage and storage thermal properties of the hydrated salt phase-change material, and the hydrogel multilayer coating avoids possible hydrated salt leakage and migration of the hydrated salt phase-change energy storage material in the mixing process with the gypsum and the application process of the phase-change gypsum, so that the hydrated salt phase-change energy storage material can be applied to the gypsum.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to phase gypsum and a preparation method thereof.
Background
The phase-change energy storage technology is an effective means for improving the utilization efficiency of energy by absorbing or releasing a large amount of heat energy in the phase-change process of materials so as to play a role in controlling temperature and storing energy, solving the contradiction that the energy supply and demand are unbalanced in time and space distribution. The phase-change energy storage material is the core of the phase-change energy storage technology. The phase change energy storage material is combined with the gypsum, so that the temperature change of the gypsum in the aging and heat release process tends to be stable, and the energy storage capacity and the energy-saving effect of a building can be effectively improved.
Most of the current phase change energy storage materials compounded with gypsum are organic phase change materials, and the main problems are that slow oxidative decomposition reaction can occur to organic matters in the long-term application process, so that the energy storage performance is reduced, and the decomposition products damage gypsum building materials; in addition, when a fire disaster occurs in a building, the organic phase-change material is subjected to low-temperature smoldering to form smoke.
The hydrated salt is used as an important phase-change material and has the advantages of rich varieties, high energy storage density, low price, easy obtainment and the like. However, when the hydrated salt is compounded with gypsum, once leakage occurs in the process of stirring and mixing the hydrated salt with the gypsum, the volume expansion caused by solid-liquid phase change of the hydrated salt can damage the integral structure of the gypsum building material and migrate to the surface of the gypsum building material to generate the phenomena of frosting and pulverization. Thus, the use of hydrated salt phase change materials in gypsum must meet stringent leakage prevention requirements during manufacture and use. The problems of high cost, capsule breakage and the like exist when the microcapsule technology is used for coating the hydrated salt phase-change material.
The porous material is adopted to load the hydrated salt, the hydrated salt and the porous material are compounded, so that the shaping of the phase change material can be realized to a certain extent, and the problems of molten state leakage and phase separation in the phase change process are solved. In addition, the outer wall of the porous material always has a small amount of hydrated salt which is not absorbed into the pores, and when the hydrated salt has strong water absorption and deliquescence capacities, the harm to the gypsum is obvious.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide phase change gypsum, which maintains the storage and heat preservation performance of a hydrous salt phase change material and avoids possible leakage and migration of hydrous salt during the mixing process of the hydrous salt phase change material and the application process of the phase change gypsum, so that the hydrous salt phase change material can be applied to the phase change gypsum.
Another object of the present invention is to provide a method for preparing phase change gypsum.
The invention is realized by the following technical scheme:
the phase change gypsum contains 10-40 wt% of phase change energy storage materials;
the phase change energy storage material is a hydrated salt-porous material composite type phase change energy storage material coated by hydrogel;
the hydrated salt comprises but is not limited to one or a mixture of more than one of hydrated magnesium chloride, hydrated calcium chloride, sodium sulfate decahydrate, sodium carbonate dodecahydrate, calcium nitrate hexahydrate, zinc nitrate tetrahydrate, dipotassium hydrogen phosphate tetrahydrate, potassium fluoride tetrahydrate, ferric bromide hexahydrate, lithium nitrate trihydrate, manganese nitrate hexahydrate and calcium nitrate tetrahydrate;
the porous material includes but is not limited to porous silicon, expanded vermiculite, expanded perlite, diatomite, palygorskite, zeolite, sepiolite and fly ash;
the hydrogel is silicon-containing gel; the hydrogel can generate silicate precipitates with the exposed hydrated salt at the open ends of the open pore channels of the porous material, and the silicate components have better affinity with concrete;
a precipitating agent is added into the hydrogel, and the precipitating agent comprises but is not limited to one or a mixture of more than one of sodium carbonate, sodium sulfate, sodium hydroxide, potassium carbonate and potassium hydroxide; the insoluble precipitate formed by the hydrated salt and the precipitant in the hydrogel includes but is not limited to one or more of magnesium carbonate, magnesium hydroxide, basic magnesium carbonate, basic magnesium hydroxide, calcium carbonate, calcium hydroxide, basic calcium carbonate, barium sulfate, calcium fluoride, calcium oxalate and magnesium oxalate.
In the above technical solution, the hydrated salt further comprises a nucleating agent. The nucleating agent can reduce the supercooling degree of the hydrated salt, is generally added in an amount of not more than 5% of the mass of the hydrated salt, is directly mixed with the hydrated salt, and can be uniformly dispersed in a system all the time. The nucleating agent used in the hydrated salt system is selected based on experience and experimental results.
A phase change gypsum, characterized by: the phase change gypsum comprises the following components in parts by weight: semi-hydrated gypsum: 350-1000 parts; water: 450-800 parts; phase change energy storage material: 350-1200 parts of; gelling material: 50-140 parts; filling agent: 40-300 parts; 3-50 parts of a chemical activator; the gelling material is any one of white cement, light aggregate and fly ash; the filler is any one of talcum powder, quicklime and ground calcium carbonate; the chemical activator is any one of ferrous sulfate, potassium sulfate, sodium sulfite, calcium chloride, sodium aluminate, calcium silicate, polyacrylate and cellulose ether; the filler has smaller particles than gypsum powder and mainly plays a role in filling small gaps
The phase change energy storage material is a hydrated salt-porous material composite type phase change energy storage material coated by hydrogel;
the hydrated salt comprises but is not limited to one or a mixture of more than one of hydrated magnesium chloride, hydrated calcium chloride, sodium sulfate decahydrate, sodium carbonate dodecahydrate, calcium nitrate hexahydrate, zinc nitrate tetrahydrate, dipotassium hydrogen phosphate tetrahydrate, potassium fluoride tetrahydrate, ferric bromide hexahydrate, lithium nitrate trihydrate, manganese nitrate hexahydrate and calcium nitrate tetrahydrate;
the porous material includes but is not limited to porous silicon, expanded vermiculite, expanded perlite, diatomite, palygorskite and the like, zeolite, sepiolite and fly ash;
the hydrogel is silicon-containing gel; the hydrogel can generate silicate precipitates with the exposed hydrated salt at the open ends of the open pore channels of the porous material, and the silicate components have better affinity with concrete;
the gelling agent of the hydrogel comprises an inorganic gelling agent and/or an organic gelling agent, the inorganic gelling agent is one or a mixture of more than one of montmorillonite, bentonite and kaolin, and the organic gelling agent is one or a mixture of more than one of polyacrylic acid, starch, polyvinyl alcohol, carboxyl cellulose, sodium carboxyl cellulose, agar, polysaccharide, xanthan gum, gelatin, chitose, cellulose ether, sodium alginate, polyurethane, k2 type carrageenan and carbopol; the sol formed by the organic gelling agent can better keep elasticity and stability after dehydration, and the colloidal particles aggregated after the sol formed by the inorganic gelling agent is dehydrated have better plugging performance for micron-sized pores;
a precipitating agent is added into the hydrogel, and the precipitating agent comprises but is not limited to one or a mixture of more than one of sodium carbonate, sodium sulfate, sodium hydroxide, potassium carbonate and potassium hydroxide; the insoluble precipitate formed by the hydrated salt and the precipitant in the hydrogel includes but is not limited to one or more of magnesium carbonate, magnesium hydroxide, basic magnesium carbonate, basic magnesium hydroxide, calcium carbonate, calcium hydroxide, basic calcium carbonate, barium sulfate, calcium fluoride, calcium oxalate and magnesium oxalate. The reaction between the hydrated salt and the precipitant is relatively fast and preferential, the reaction with the hydrogel is relatively slow, and the precipitates generated by the two reactions complement each other to play a better role in blocking the open ports of the porous material.
In the above technical scheme, the phase change gypsum further comprises hydroxypropyl cellulose: 0-1.5 parts of hydroxypropyl cellulose, wherein the hydroxypropyl cellulose can increase the bonding strength of the phase change gypsum, has a thickening effect and improves the initial strength of the phase change gypsum in the construction process. .
In the technical scheme, the hydrated salt also comprises a nucleating agent, the nucleating agent can reduce the supercooling degree of the hydrated salt, the addition amount of the nucleating agent is not more than 5% of the mass of the hydrated salt, and the nucleating agent is directly mixed with the hydrated salt and can be uniformly dispersed in a system preferably all the time. The nucleating agent used in the hydrated salt system is selected based on experience and experimental results.
In the technical scheme, the hydrogel is obtained by dehydrating and drying hydrosol;
the hydrosol is a water-soluble silicon solution, a water glass solution, a water-soluble silicon solution added with an inorganic gelling agent and/or an organic gelling agent or a water glass solution added with an inorganic gelling agent and/or an organic gelling agent; the hydrosol is formed by dispersing nano-scale or micron-scale particles in a water phase, and has fluidity, wherein the colloid particles of the hydrosol lose charges, or a solvent layer coated on the outer ring of the colloid particles is damaged, the colloid particles polymerize, the sol is solidified, and the gel is formed after the fluidity is lost. The hydrogel is formed by connecting colloidal particles or macromolecules under a certain condition to form a space network structure, water solution is filled in structural gaps, and the water solution is enclosed in grids and cannot flow freely.
In the technical scheme, the mass content of the hydrogel in the hydrogel-coated hydrous salt-porous material composite type phase change energy storage material is 10-15%.
In the technical scheme, the hydrogel-coated hydrous salt-porous material composite type phase change energy storage material is prepared by the following method, and comprises the following steps:
step 1, uniformly mixing hydrated salt and a porous material, melting the hydrated salt at 30-50 ℃ to enable the hydrated salt to be absorbed by the porous material, and cooling to room temperature or below 20 ℃ to obtain a hydrated salt-porous material composite, wherein the porous material accounts for 15% -30% of the total mass of the hydrated salt-porous material composite;
step 2, preparing hydrosol containing a precipitator, a gelling agent and water-soluble silicon or water glass, wherein the mass content of the precipitator in the hydrosol is 1-3%, and the mass content of the gelling agent is 3-6%;
and 3, weighing the hydrated salt-porous material composite and the hydrosol according to the mass ratio (5-9): 1, uniformly mixing, and dehydrating to obtain the hydrogel-hydrated salt-porous material composite phase change energy storage material.
In the technical scheme, the particle size of the porous material is 200-400 meshes.
In the technical scheme, the organic gelling agent in the hydrogel is not more than 1 wt%.
In the above technical solution, the mixing of the hydrated salt-porous material composite and the hydrosol comprises the following steps: spraying the hydrosol on the surface of the hydrated salt-porous material compound, and dehydrating and granulating; after the hydrated salt-porous material compound is soaked in hydrosol, dehydration granulation is carried out.
In the technical scheme, the precipitating agent accounts for not more than 3% of the mass ratio of the hydrogel.
A preparation method of phase change gypsum comprises the following steps:
step 1, uniformly mixing hydrated salt and a porous material, melting the hydrated salt at 30-50 ℃ to enable the hydrated salt to be absorbed by the porous material, and cooling to room temperature or below 20 ℃ to obtain a hydrated salt-porous material composite, wherein the porous material accounts for 15% -30% of the total mass of the hydrated salt-porous material composite;
step 2, preparing hydrosol containing a precipitator, a gelling agent and water-soluble silicon or water glass, wherein the mass content of the precipitator in the hydrosol is 1-3%, and the mass content of the gelling agent is 3-6%;
step 3, weighing the hydrated salt-porous material composite and the hydrosol according to the mass ratio (5-9): 1, uniformly mixing, and dehydrating to obtain the hydrogel-hydrated salt-porous material composite phase change energy storage material;
and 4, step 4: uniformly mixing the hydrogel-hydrated salt-porous material phase change energy storage material with semi-hydrated gypsum, a gelling agent and a filling agent, adding water and a chemical activator, and uniformly mixing to obtain the phase change gypsum slurry, wherein the mass fraction of the hydrogel-hydrated salt-porous material phase change energy storage material in the phase change gypsum slurry is 10-40%, and the phase change gypsum slurry is compounded and formed with fiber yarns, grid cloth and the like to obtain the phase change gypsum.
In the technical scheme, the water and the chemical activator are added in the step 4, and the hydroxypropyl cellulose is also added at the same time, and the mixture is uniformly mixed.
The invention has the advantages and beneficial effects that:
the invention discloses a phase change gypsum and a preparation method thereof, wherein the used natural inorganic porous material, water-soluble silicon or water glass and other raw materials capable of forming hydrogel are all common additives for gypsum, and have good affinity with gypsum. The in-situ generated precipitate realizes the isolation of the hydrated salt and the hydrogel in the pore canal of the porous material, avoids the salting-out effect of the hydrated salt on the hydrogel, and ensures that the hydrated salt can fully exert the heat storage and release properties in the phase change process; the unadsorbed hydrated salt on the outer wall of the porous material reacts with the precipitator dissolved in the water-soluble silicon or the water glass to be consumed, so that the adverse effect of the residual salt on the outer wall of the porous material on the gypsum can be effectively reduced. The gel multi-layer coating formed by the water glass and the hydrosol avoids possible leakage and migration of the hydrated salt phase-change material in the mixing process of the hydrated salt phase-change material and the gypsum and possible leakage and migration of the hydrated salt in the application process of the phase-change gypsum, so that the hydrated salt phase-change material can be applied to the gypsum.
In addition, the hydrogel and the precipitator dissolved in the hydrogel can repair a new open port formed by the damage of the original coating layer at any time to form a new coating layer and a new blocking structure, and the coating and blocking effects on the opening end of the channel are long-term sustainable. And the hydrogel formed by the water-soluble silicon or the water glass has certain elasticity and lubricity due to the addition of the montmorillonite material, has buffering capacity on friction, impact and the like of particles in the gypsum, avoids damage of a hydrogel coating, and further reduces the possibility of leakage of hydrated salt. When a fire disaster occurs, the phase-change gypsum can absorb heat energy by utilizing solid-liquid phase change, and the thermal decomposition of the hydrated salt can also absorb the heat energy, the thermal decomposition products of the hydrated salt are mostly metal oxides, and the metal oxides are combined with the porous carrier to form an effective heat insulation layer to prevent the fire disaster from spreading.
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Detailed Description
In order to make the technical solution of the present invention better understood, the technical solution of the present invention is further described below with reference to specific examples.
Example 1
A preparation method of phase change gypsum comprises the following steps:
step 1, weighing a manganese nitrate hexahydrate phase-change material (hydrated salt), a nucleating agent (manganese chloride tetrahydrate) and expanded vermiculite (porous material) according to a weight ratio of 77:3:20, wherein the granularity of the expanded vermiculite is 150 meshes, uniformly mixing, melting the manganese nitrate hexahydrate phase-change material at 40 ℃ to ensure that the manganese nitrate hexahydrate phase-change material is uniformly and fully absorbed by the expanded vermiculite, and cooling to room temperature to obtain a manganese nitrate hexahydrate-expanded vermiculite compound;
step 2, preparing hydrosol containing 1 wt% of sodium hydroxide (precipitator), 5 wt% of sodium montmorillonite (inorganic gelling agent), 1 wt% of sodium carboxymethylcellulose (organic gelling agent) and the balance of water-soluble silicon;
step 3, uniformly spraying the obtained hydrosol on the surface of the manganese nitrate hexahydrate-expanded vermiculite compound according to the mass ratio of 3:17, performing multiple circulation operations of spraying, dewatering and spraying, drying and granulating to realize complete coating of compound particles, preparing the hydrogel-manganese nitrate hexahydrate-expanded vermiculite composite phase change energy storage material, and sealing for later use;
and 4, weighing 1000 parts of semi-hydrated gypsum powder, 50 parts of white cement, 50 parts of talcum powder and 565 parts of hydrogel-manganese nitrate hexahydrate-expanded vermiculite composite phase change energy storage material according to the parts by weight, uniformly mixing, adding 800 parts of water and 30 parts of active calcium silicate micro powder, and uniformly mixing to obtain phase change gypsum slurry, wherein the mass fraction of the hydrogel-manganese nitrate hexahydrate-expanded vermiculite composite phase change energy storage material in the phase change gypsum slurry is 10%. And compounding and molding the phase-change gypsum slurry, fiber yarns, grid cloth and the like to obtain the phase-change gypsum board.
Through determination, the melting point of the phase change gypsum is 25 ℃, the phase change enthalpy is 30J/g, the phase change enthalpy is attenuated by 0.5% after 1000 times of circulation, and the service life of the phase change gypsum is 60 years. The phase change gypsum can be used as a decorative gypsum strip for the wall corner inside a house, a gypsum board for a suspended ceiling and the like, and has no bearing requirement. According to the testing method of the building industry standard GB/T9775-once 2008, after the phase-change gypsum is made into a water-resistant gypsum plaster board with the thickness of 12mm, the paper surface and the board core are both subjected to waterproof treatment, and after 300 days, the surface water absorption rate is about 140g/m2Less than 160g/m specified in the standard2And meets the standard.
Comparative example 1
Weighing a manganese nitrate hexahydrate phase-change material (hydrated salt), a nucleating agent (manganese chloride tetrahydrate) and expanded vermiculite (porous material) according to a weight ratio of 77:3:20, wherein the granularity of the expanded vermiculite is 150 meshes, uniformly mixing, melting the manganese nitrate hexahydrate phase-change material at 40 ℃ to ensure that the manganese nitrate hexahydrate phase-change material is uniformly and fully absorbed by the expanded vermiculite, and cooling to room temperature to obtain a manganese nitrate hexahydrate-expanded vermiculite compound;
weighing 1000 parts of semi-hydrated gypsum powder, 50 parts of white cement, 50 parts of talcum powder and 565 parts of manganese nitrate hexahydrate-expanded vermiculite compound according to the parts by weight, uniformly mixing, adding 800 parts of water and 30 parts of active calcium silicate micro powder, uniformly mixing to obtain phase change gypsum slurry, wherein the mass fraction of the manganese nitrate hexahydrate-expanded vermiculite compound in the phase change gypsum slurry is 10%, and compounding and forming the phase change gypsum slurry, cellosilk, mesh cloth and the like to obtain the phase change gypsum board.
Through determination, the melting point of the phase change gypsum is 25 ℃, the phase change enthalpy is 33J/g, the phase change enthalpy is attenuated by 40% after 1000 times of circulation, and the service life of the phase change gypsum is 9 years. According to the testing method of the building industry standard GB/T9775-once 2008, after the phase-change gypsum is made into a water-resistant gypsum plaster board with the thickness of 12mm, both the paper surface and the board core are subjected to waterproof treatment, and after 300 days, the surface water absorption rate is about 180g/m2Greater than 160g/m specified in the standard2And the product is unqualified.
Example 2
A preparation method of phase change gypsum comprises the following steps:
step 1, weighing calcium nitrate tetrahydrate and zinc nitrate hexahydrate according to a weight ratio of 45:55 to prepare a calcium nitrate tetrahydrate-zinc nitrate hexahydrate phase-change material, weighing the calcium nitrate tetrahydrate-zinc nitrate hexahydrate phase-change material (hydrated salt), a nucleating agent (sodium chloride) and expanded perlite (porous material) according to a weight ratio of 69:1:30, wherein the particle size of the expanded perlite is 250 meshes, uniformly mixing, melting the calcium nitrate tetrahydrate-zinc nitrate hexahydrate phase-change material at 40 ℃ to enable the calcium nitrate tetrahydrate-zinc nitrate hexahydrate phase-change material to be uniformly and fully absorbed by the expanded perlite, and cooling to below 20 ℃ to obtain a calcium nitrate tetrahydrate-zinc nitrate hexahydrate-expanded perlite compound;
step 2, preparing hydrosol containing 3 wt% oxalic acid dihydrate (precipitator), 2 wt% laponite (inorganic gelling agent) and 1 wt% polyacrylic acid (organic gelling agent);
step 3, uniformly spraying the obtained hydrosol on the surface of the calcium nitrate tetrahydrate-zinc nitrate hexahydrate-expanded perlite compound according to the mass ratio of 1:7, performing multiple cyclic operations of spraying, dewatering and spraying, drying and granulating to completely coat the compound particles to prepare the hydrogel-calcium nitrate tetrahydrate-zinc nitrate hexahydrate-expanded perlite compound phase change energy storage material, and sealing for later use;
and 4, weighing 380 parts of semi-hydrated gypsum powder, 140 parts of light aggregate, 40 parts of quick lime, 360 parts of hydrogel-calcium nitrate tetrahydrate-zinc nitrate hexahydrate-expanded perlite composite phase change energy storage material according to parts by weight, uniformly mixing, adding 470 parts of water and 50 parts of cellulose ether, uniformly mixing to obtain phase change gypsum slurry, wherein the mass fraction of the hydrogel-calcium nitrate tetrahydrate-zinc nitrate hexahydrate-expanded perlite composite phase change energy storage material in the phase change gypsum slurry is 25%, and compounding and molding the phase change gypsum slurry, fiber filaments, grid cloth and the like to obtain the phase change gypsum board.
Through determination, the melting point of the phase change gypsum is 24 ℃, the phase change enthalpy is 22J/g, the phase change enthalpy is attenuated by 0.5% after 1000 times of circulation, and the service life of the phase change gypsum is 50 years. The phase change gypsum can be used as a decorative gypsum strip for the wall corner inside a house, a gypsum board for a suspended ceiling and the like, and has no bearing requirement. According to the testing method of the building industry standard GB/T9775-once 2008, after the phase-change gypsum is made into a water-resistant gypsum plaster board with the thickness of 12mm, both the paper surface and the board core are subjected to waterproof treatment, and after 300 days, the surface water absorption rate is about 155g/m2Less than 160g/m specified in the standard2And meets the standard.
Comparative example 2
Weighing calcium nitrate tetrahydrate and zinc nitrate hexahydrate according to a weight ratio of 45:55 to prepare a calcium nitrate tetrahydrate-zinc nitrate hexahydrate phase-change material, weighing a calcium nitrate tetrahydrate-zinc nitrate hexahydrate phase-change material (hydrated salt), a nucleating agent (sodium chloride) and expanded perlite (porous material) according to a weight ratio of 69:1:30, wherein the particle size of the expanded perlite is 250 meshes, uniformly mixing, melting the calcium nitrate tetrahydrate-zinc nitrate hexahydrate phase-change material at 40 ℃ to enable the calcium nitrate tetrahydrate-zinc nitrate phase-change material to be uniformly and fully absorbed by the expanded perlite, and cooling to below 20 ℃ to obtain a calcium nitrate tetrahydrate-zinc nitrate hexahydrate-expanded perlite compound;
weighing 380 parts of semi-hydrated gypsum powder, 140 parts of light aggregate, 40 parts of quick lime and 360 parts of calcium nitrate tetrahydrate-zinc nitrate hexahydrate-expanded perlite compound according to parts by weight, uniformly mixing, adding 470 parts of water and 50 parts of cellulose ether, uniformly mixing to obtain phase change gypsum slurry, wherein the mass fraction of the calcium nitrate tetrahydrate-zinc nitrate hexahydrate-expanded perlite compound in the phase change gypsum slurry is 25%, and compounding and molding the phase change gypsum slurry, fiber filaments, grid cloth and the like to obtain the phase change gypsum board.
Through determination, the melting point of the phase change gypsum is 24 ℃, the phase change enthalpy is 23J/g, the phase change enthalpy is attenuated by 48% after 1000 times of circulation, and the service life of the phase change gypsum is 6 years. According to the building industry Standard "thistle Board" GB/T9775-2008. after the phase change gypsum is made into a water-resistant paper-surface gypsum board with the thickness of 12mm, both paper surface and board core are subjected to waterproof treatment, and after 300 days, the surface water absorption rate is about 200g/m2Greater than 160g/m specified in the standard2And the product is unqualified.
Example 3
A preparation method of phase change gypsum comprises the following steps:
step 1, weighing magnesium chloride hexahydrate and calcium chloride hexahydrate according to a weight ratio of 50:50 to prepare a magnesium chloride hexahydrate-calcium chloride hexahydrate phase-change material, weighing the magnesium chloride hexahydrate-calcium chloride hexahydrate phase-change material (hydrated salt), a nucleating agent (barium hydroxide octahydrate) and porous silicon (porous material) according to a weight ratio of 83.3:1.7:15, wherein the particle size of the porous silicon is 400 meshes, uniformly mixing, melting the magnesium chloride hexahydrate-calcium chloride hexahydrate phase-change material at 30 ℃ to enable the phase-change material to be uniformly and fully absorbed by the porous silicon, and cooling to below 20 ℃ to obtain a magnesium chloride hexahydrate-calcium chloride hexahydrate-porous silicon composite;
step 2, preparing an aqueous sol containing 2 wt% of sodium carbonate (precipitant), 3 wt% of bentonite (inorganic gelling agent) and 0.5 wt% of xanthan gum (organic gelling agent);
step 3, soaking the magnesium chloride hexahydrate-calcium chloride hexahydrate-porous silicon composite in the hydrosol according to the mass ratio of 9:1, performing ultrasonic exhausting, taking out the composite, dehydrating, drying and granulating to completely coat composite particles, preparing the hydrogel-magnesium chloride hexahydrate-calcium chloride hexahydrate-porous silicon composite phase change energy storage material, and sealing for later use;
and 4, weighing 700 parts of semi-hydrated gypsum powder, 120 parts of fly ash, 300 parts of heavy calcium carbonate, 1123 parts of hydrogel-magnesium chloride hexahydrate-calcium chloride hexahydrate-porous silicon composite phase change energy storage material according to parts by weight, uniformly mixing, adding 560 parts of water, 3 parts of polyacrylate and 1.5 parts of hydroxypropyl cellulose, uniformly mixing to obtain phase change gypsum slurry, wherein the mass fraction of the hydrogel-magnesium chloride hexahydrate-calcium chloride hexahydrate-porous silicon composite phase change energy storage material in the phase change gypsum slurry is 40%, and compounding and forming the phase change gypsum slurry, fiber yarns, grid cloth and the like to obtain the phase change gypsum board.
The melting point of the phase-change gypsum is 22 ℃ through measurement, and the phase-change enthalpy is15J/g, the phase change enthalpy is attenuated by 0.5 percent after 1000 times of circulation, and the service life of the phase change gypsum is 45 years. The phase change gypsum can be used as a decorative gypsum strip for the wall corner inside a house, a gypsum board for a suspended ceiling and the like, and has no bearing requirement. According to the testing method of the building industry standard GB/T9775-once 2008, after the phase-change gypsum is made into a water-resistant gypsum plaster board with the thickness of 12mm, the paper surface and the board core are both subjected to waterproof treatment, and after 300 days, the surface water absorption rate is about 150g/m2Less than 160g/m specified in the standard2And meets the standard.
Comparative example 3
Weighing magnesium chloride hexahydrate and calcium chloride hexahydrate according to a weight ratio of 50:50 to prepare a magnesium chloride hexahydrate-calcium chloride hexahydrate phase-change material, weighing the magnesium chloride hexahydrate-calcium chloride hexahydrate phase-change material (hydrated salt), a nucleating agent (barium hydroxide octahydrate) and porous silicon (porous material) according to a weight ratio of 83.3:1.7:15, wherein the granularity of the porous silicon is 400 meshes, uniformly mixing, melting the magnesium chloride hexahydrate-calcium chloride hexahydrate phase-change material at 30 ℃ to ensure that the magnesium chloride hexahydrate-calcium chloride hexahydrate phase-change material is uniformly and fully absorbed by the porous silicon, and cooling to below 20 ℃ to obtain a magnesium chloride hexahydrate-calcium chloride hexahydrate-porous silicon composite;
weighing 700 parts of semi-hydrated gypsum powder, 120 parts of fly ash, 300 parts of heavy calcium carbonate and 1123 parts of magnesium chloride hexahydrate-calcium chloride hexahydrate-porous silicon compound according to parts by weight, uniformly mixing, adding 560 parts of water, 3 parts of polyacrylate and 1.5 parts of hydroxypropyl cellulose, uniformly mixing to obtain phase-change gypsum slurry, wherein the mass fraction of the magnesium chloride hexahydrate-calcium chloride hexahydrate-porous silicon compound in the phase-change gypsum slurry is 40%, and compounding and forming the phase-change gypsum slurry, fiber filaments, grid cloth and the like to obtain the phase-change gypsum board.
Through determination, the melting point of the phase change gypsum is 22 ℃, the phase change enthalpy is 16J/g, the phase change enthalpy is attenuated by 75% after 1000 times of circulation, and the service life of the phase change gypsum is 4 years. According to the testing method of the building industry standard GB/T9775-once 2008, after the phase-change gypsum is made into a water-resistant gypsum plaster board with the thickness of 12mm, the paper surface and the board core are both subjected to waterproof treatment, and after 300 days, the surface water absorption rate is about 220g/m2Greater than 160g/m specified in the standard2And the product is unqualified.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (14)
1. A phase change gypsum, characterized by: the phase change gypsum contains 10-40 wt% of phase change energy storage materials;
the phase change energy storage material is a hydrated salt-porous material composite type phase change energy storage material coated by hydrogel;
the hydrated salt is one or a mixture of more than one of hydrated magnesium chloride, hydrated calcium chloride, sodium sulfate decahydrate, sodium carbonate dodecahydrate, calcium nitrate hexahydrate, zinc nitrate tetrahydrate, dipotassium hydrogen phosphate tetrahydrate, potassium fluoride tetrahydrate, ferric bromide hexahydrate, lithium nitrate trihydrate, manganese nitrate hexahydrate and calcium nitrate tetrahydrate;
the porous material is porous silicon, expanded vermiculite, expanded perlite, diatomite, palygorskite, zeolite, sepiolite and fly ash;
the hydrogel is silicon-containing gel; the hydrogel can generate silicate precipitates with the exposed hydrated salt at the open ends of the open pores of the porous material;
a precipitator is added into the hydrogel and is one or a mixture of more than one of sodium carbonate, sodium sulfate, sodium hydroxide, potassium carbonate and potassium hydroxide; the insoluble precipitate formed by the hydrated salt and the precipitator in the hydrogel is one or a mixture of more than one of magnesium carbonate, magnesium hydroxide, basic magnesium carbonate, basic magnesium hydroxide, calcium carbonate, calcium hydroxide, basic calcium carbonate, barium sulfate, calcium fluoride, calcium oxalate and magnesium oxalate.
2. The phase change gypsum according to claim 1, wherein: the hydrated salt also comprises a nucleating agent, and the addition amount of the nucleating agent is not more than 5% of the mass of the hydrated salt.
3. A phase change gypsum, characterized by: the phase change gypsum comprises the following components in parts by weight: semi-hydrated gypsum: 350-1000 parts; water: 450-800 parts; phase change energy storage material: 350-1200 parts of; gelling material: 50-140 parts; filling agent: 40-300 parts; 3-50 parts of a chemical activator; the gelling material is any one of white cement, light aggregate and fly ash; the filler is any one of talcum powder, quicklime and ground calcium carbonate; the chemical activator is any one of ferrous sulfate, potassium sulfate, sodium sulfite, calcium chloride, sodium aluminate, calcium silicate, polyacrylate and cellulose ether;
the phase change energy storage material is a hydrated salt-porous material composite type phase change energy storage material coated by hydrogel;
the hydrated salt is one or a mixture of more than one of hydrated magnesium chloride, hydrated calcium chloride, sodium sulfate decahydrate, sodium carbonate dodecahydrate, calcium nitrate hexahydrate, zinc nitrate tetrahydrate, dipotassium hydrogen phosphate tetrahydrate, potassium fluoride tetrahydrate, ferric bromide hexahydrate, lithium nitrate trihydrate, manganese nitrate hexahydrate and calcium nitrate tetrahydrate;
the porous material is porous silicon, expanded vermiculite, expanded perlite, diatomite, palygorskite and the like, zeolite, sepiolite and fly ash;
the hydrogel is silicon-containing gel; the hydrogel can generate silicate precipitates with the exposed hydrated salt at the open ends of the open pores of the porous material;
the gelling agent of the hydrogel comprises an inorganic gelling agent and/or an organic gelling agent, the inorganic gelling agent is one or a mixture of more than one of montmorillonite, bentonite and kaolin, and the organic gelling agent is one or a mixture of more than one of polyacrylic acid, starch, polyvinyl alcohol, carboxyl cellulose, sodium carboxyl cellulose, agar, polysaccharide, xanthan gum, gelatin, chitose, cellulose ether, sodium alginate, polyurethane, k2 type carrageenan and carbopol;
a precipitator is added into the hydrogel and is one or a mixture of more than one of sodium carbonate, sodium sulfate, sodium hydroxide, potassium carbonate and potassium hydroxide; the insoluble precipitate formed by the hydrated salt and the precipitator in the hydrogel is one or a mixture of more than one of magnesium carbonate, magnesium hydroxide, basic magnesium carbonate, basic magnesium hydroxide, calcium carbonate, calcium hydroxide, basic calcium carbonate, barium sulfate, calcium fluoride, calcium oxalate and magnesium oxalate.
4. The phase change gypsum according to claim 3, wherein: the phase change gypsum further comprises hydroxypropyl cellulose: 0 to 1.5 portions.
5. The phase change gypsum according to claim 3, wherein: the hydrated salt also comprises a nucleating agent, and the addition amount of the nucleating agent is not more than 5% of the mass of the hydrated salt.
6. The phase change gypsum according to claim 3, wherein: the hydrogel is obtained by dehydrating and drying hydrosol.
7. The phase change gypsum according to claim 3, wherein: the mass content of hydrogel in the hydrogel-coated hydrous salt-porous material composite type phase-change energy storage material is 10-15%.
8. The phase change gypsum according to claim 3, wherein: the hydrogel-coated hydrated salt-porous material composite type phase change energy storage material is prepared by the following method, and comprises the following steps:
step 1, uniformly mixing hydrated salt and a porous material, melting the hydrated salt at 30-50 ℃ to enable the hydrated salt to be absorbed by the porous material, and cooling to room temperature or below 20 ℃ to obtain a hydrated salt-porous material composite, wherein the porous material accounts for 15% -30% of the total mass of the hydrated salt-porous material composite;
step 2, preparing hydrosol containing a precipitator and a gelling agent, wherein the hydrosol is soluble glass or soluble silicon, the mass content of the precipitator in the hydrosol is 1-3%, and the mass content of the gelling agent is 3-6%;
and 3, weighing the hydrated salt-porous material composite and the hydrosol according to the mass ratio (5-9): 1, uniformly mixing, and dehydrating to obtain the hydrogel-hydrated salt-porous material composite phase change energy storage material.
9. The phase change gypsum of claim 8, wherein: the particle size of the porous material is 200-400 meshes.
10. The phase change gypsum of claim 8, wherein: the hydrogel contains no more than 1 wt% of organic gelling agent.
11. The phase change gypsum of claim 8, wherein: the mixing of the hydrated salt-porous material composite and the hydrosol comprises the following modes: spraying the hydrosol on the surface of the hydrated salt-porous material compound, and dehydrating and granulating; after the hydrated salt-porous material compound is soaked in hydrosol, dehydration granulation is carried out.
12. The phase change gypsum of claim 8, wherein: the precipitating agent accounts for not more than 3% of the mass ratio of the hydrogel.
13. The preparation method of the phase change gypsum is characterized by comprising the following steps:
step 1, uniformly mixing hydrated salt and a porous material, melting the hydrated salt at 30-50 ℃ to enable the hydrated salt to be absorbed by the porous material, and cooling to room temperature or below 20 ℃ to obtain a hydrated salt-porous material composite, wherein the porous material accounts for 15% -30% of the total mass of the hydrated salt-porous material composite;
step 2, preparing hydrosol containing a precipitator and a gelling agent, wherein the hydrosol is soluble glass or soluble silicon, the mass content of the precipitator in the hydrosol is 1-3%, and the mass content of the gelling agent is 3-6%;
step 3, weighing the hydrated salt-porous material composite and the hydrosol according to the mass ratio (5-9): 1, uniformly mixing, and dehydrating to obtain the hydrogel-hydrated salt-porous material composite phase change energy storage material;
and 4, step 4: uniformly mixing 350-1200 parts by weight of hydrogel-hydrated salt-porous material phase change energy storage material, 350-1000 parts by weight of semi-hydrated gypsum, 50-140 parts by weight of gelling material and 40-300 parts by weight of filler, adding 450-800 parts by weight of water and 3-50 parts by weight of chemical activator, and uniformly mixing to obtain phase change gypsum slurry, wherein the mass fraction of the hydrogel-hydrated salt-porous material phase change energy storage material in the phase change gypsum slurry is 10-40%, and the phase change gypsum slurry is compounded and formed with fiber filaments, grid cloth and the like to prepare phase change gypsum;
the hydrated salt is one or a mixture of more than one of hydrated magnesium chloride, hydrated calcium chloride, sodium sulfate decahydrate, sodium carbonate dodecahydrate, calcium nitrate hexahydrate, zinc nitrate tetrahydrate, dipotassium hydrogen phosphate tetrahydrate, potassium fluoride tetrahydrate, ferric bromide hexahydrate, lithium nitrate trihydrate, manganese nitrate hexahydrate and calcium nitrate tetrahydrate;
the porous material is porous silicon, expanded vermiculite, expanded perlite, diatomite, palygorskite and the like, zeolite, sepiolite and fly ash;
the gelling agent comprises an inorganic gelling agent and/or an organic gelling agent, the inorganic gelling agent is one or a mixture of more than one of montmorillonite, bentonite and kaolin, and the organic gelling agent is one or a mixture of more than one of polyacrylic acid, starch, polyvinyl alcohol, carboxyl cellulose, sodium carboxyl cellulose, agar, polysaccharide, xanthan gum, gelatin, chitose, cellulose ether, sodium alginate, polyurethane, k2 type carrageenan and carbopol;
the precipitator is one or a mixture of more than one of sodium carbonate, sodium sulfate, sodium hydroxide, potassium carbonate and potassium hydroxide; the insoluble precipitate formed by the hydrated salt and the precipitator in the hydrogel is one or a mixture of more than one of magnesium carbonate, magnesium hydroxide, basic magnesium carbonate, basic magnesium hydroxide, calcium carbonate, calcium hydroxide, basic calcium carbonate, barium sulfate, calcium fluoride, calcium oxalate and magnesium oxalate.
14. The method for preparing phase change gypsum according to claim 13, wherein 0-1.5 parts by weight of hydroxypropyl cellulose is added while adding water and a chemical activator in the step 4, and the mixture is uniformly mixed.
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