CN113174157B - Wall surface phase change putty and preparation method thereof - Google Patents
Wall surface phase change putty and preparation method thereof Download PDFInfo
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- CN113174157B CN113174157B CN202010388853.2A CN202010388853A CN113174157B CN 113174157 B CN113174157 B CN 113174157B CN 202010388853 A CN202010388853 A CN 202010388853A CN 113174157 B CN113174157 B CN 113174157B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/34—Filling pastes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
Abstract
The invention discloses phase change putty and a preparation method thereof, wherein a natural inorganic porous material is used as a carrier to load a hydrated salt phase change energy storage material to prepare a hydrated salt-porous carrier compound, then water-soluble silicon or water glass is used for wrapping the hydrated salt-porous carrier compound, and the hydrated salt-porous material compound type phase change energy storage material coated by hydrogel is prepared after dehydration. The phase change putty realizes the isolation of the hydrous salt phase change material and the putty, keeps the storage and storage thermal properties of the 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 putty by the multi-layer coating of the hydrogel, so that the hydrous salt phase change material can be applied to the putty.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to phase putty 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 putty, so that the temperature change of the putty 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.
The phase change energy storage materials compounded with the putty at present are mostly organic phase change materials, and the main problems are that the organic matters can generate slow oxidative decomposition reaction in the long-term application process, so that the energy storage performance is reduced, and the decomposition products damage the putty layer; in addition, the organic phase change material cannot improve the fire resistance of a building when the building is in fire.
The hydrated salt is used as an important phase change energy storage material and has the advantages of rich varieties, high energy storage density, low price, easy obtainment and the like. However, the problem of compounding the hydrated salt with the putty is that once leakage occurs in the process of stirring and mixing the hydrated salt with the putty or in the process of long-term application, the volume expansion caused by solid-liquid phase change of the hydrated salt can damage the integral structure of the putty and can migrate to the surface of the putty to generate the phenomena of bulging and liquid seepage. Therefore, the hydrous salt phase-change material used for the putty must meet the strict requirements of leakage prevention in the preparation and application processes. 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 composite material is obvious.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the phase change putty, which maintains the storage and storage thermal properties of the 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 putty, so that the hydrous salt phase change material can be applied to the putty.
The invention also aims to provide a preparation method of the phase change putty.
The invention is realized by the following technical scheme:
the wall surface phase change putty contains 10-30 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 one or more of hydrated magnesium chloride, hydrated calcium chloride, sodium sulfate decahydrate, sodium carbonate dodecahydrate, calcium nitrate hexahydrate, zinc nitrate tetrahydrate, potassium fluoride 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;
the hydrogel is added with a precipitating agent, the precipitating agent comprises but is not limited to one or more of sodium carbonate, sodium sulfate, sodium hydroxide, potassium carbonate and potassium hydroxide, and the insoluble precipitate formed by the hydrated salt and the precipitating agent in the hydrogel comprises 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 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.
The phase change putty for the wall surface comprises the following components in parts by weight: black/white cement: 300-400 parts; filling agent: 400-500 parts; phase change energy storage material: 110-450 parts; ash calcium powder: 100-200 parts; anti-cracking agent: 4-30 parts of a solvent; rubber powder: 8-30 parts of a solvent; wherein the specific form of the filler is any one or a mixture of a plurality of heavy calcium carbonate, double flying powder and quartz powder; the anti-cracking agent is any one or a mixture of more of polypropylene short fibers, wood fibers, hemp cut, hydroxypropyl methyl cellulose and pregelatinized starch;
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 one or more of hydrated magnesium chloride, hydrated calcium chloride, sodium sulfate decahydrate, sodium carbonate dodecahydrate, calcium nitrate hexahydrate, zinc nitrate tetrahydrate, potassium fluoride 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;
the gelling agent in 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, chitosan, 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;
the hydrogel is added with a precipitating agent, the precipitating agent comprises but is not limited to one or more of sodium carbonate, sodium sulfate, sodium hydroxide, potassium carbonate and potassium hydroxide, and the insoluble precipitate formed by the hydrated salt and the precipitating agent in the hydrogel comprises 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 technical scheme, the wall surface phase change putty further comprises hydroxypropyl cellulose: 0-2 parts of hydroxypropyl cellulose, wherein the hydroxypropyl cellulose can increase the bonding strength of the phase change putty, has a thickening effect, enhances the adhesive force of the putty, and reduces the sagging phenomenon in construction.
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 ensure that the hydrated salt is uniformly and fully 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 of (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 400-600 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 wall surface phase change putty comprises the following steps:
step 1, uniformly mixing hydrated salt and a porous material, melting the hydrated salt at 30-50 ℃ to ensure that the hydrated salt is uniformly and fully 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 composite phase change energy storage material with black/white cement, a filler, ash calcium powder, an anti-cracking agent, rubber powder and hydroxypropyl cellulose to obtain the wall surface phase change putty, wherein the mass fraction of the hydrogel-hydrated salt-porous material composite phase change energy storage material in the wall surface phase change putty is 10-30%.
In the technical scheme, hydroxypropyl cellulose is also added in the step 4 and is uniformly mixed.
The invention has the advantages and beneficial effects that:
the invention discloses a wall phase-change putty 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 common additives for putty, and have good affinity with the putty. 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 putty on the outer wall of the porous material can be effectively reduced. The gel multilayer coating formed by the water glass and the hydrosol avoids possible leakage and migration of the hydrated salt in the mixing process of the hydrated salt phase-change material and the putty and the application process of the phase-change putty, so that the hydrated salt phase-change material can be applied to the putty.
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 putty, avoids damage of a hydrogel coating layer, and further reduces the possibility of leakage of hydrated salt. When a fire disaster happens, the wall putty synthesized by the invention not only can utilize solid-liquid phase change to absorb heat energy, but also can absorb heat energy by virtue of hydrated salt pyrolysis, most of hydrated salt pyrolysis products are metal oxides, and the metal oxides are combined with a porous carrier to form an effective heat insulation layer so as 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 wall surface phase change putty 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 50 ℃ to ensure that the manganese nitrate hexahydrate phase-change material is uniformly and fully absorbed by the expanded vermiculite, and cooling to below 20 ℃ to obtain a manganese nitrate hexahydrate-expanded vermiculite compound;
step 2, preparing hydrosol containing 1wt% of sodium hydroxide (precipitator), 5 wt% of sodium montmorillonite (inorganic gelling agent), 1wt% 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 1:5, 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;
step 4, weighing 400 parts of white cement, 500 parts of ground limestone, 100 parts of ash calcium powder, 2 parts of wood fiber, 2 parts of polypropylene short fiber, 2 parts of hydroxypropyl cellulose, 8 parts of rubber powder and 435 parts of hydrogel-manganese nitrate hexahydrate-expanded vermiculite composite phase change energy storage material according to parts by weight, and uniformly mixing to obtain the phase change putty, wherein the mass fraction of the hydrogel-manganese nitrate hexahydrate-expanded vermiculite composite phase change energy storage material in the phase change putty is 30%.
Through determination, the melting point of the phase change putty 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 putty is 60 years. The phase change putty is mainly used for leveling the surfaces of inner and outer wallboards and top boards of buildings. According to a sample preparation and test method of 'putty for building interior' JG/T298-plus 2010 in the building industry standard, phase-change putty is respectively coated on a cement slab and a mortar block base material, the phase-change putty is subjected to water-resistant treatment, after 300 days, a putty layer coated on the cement slab base material has no foaming, cracking and powder falling phenomena, and the bonding strength of the putty layer coated on the mortar block base material is 0.53MPa (standard state) and 0.34MPa (after being soaked in water).
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 50 ℃ to ensure that the manganese nitrate hexahydrate phase-change material is uniformly and fully absorbed by the expanded vermiculite, and cooling to below 20 ℃ to obtain a manganese nitrate hexahydrate-expanded vermiculite compound;
weighing 400 parts of white cement, 500 parts of ground calcium carbonate, 100 parts of ash calcium powder, 2 parts of wood fiber, 2 parts of polypropylene short fiber, 2 parts of hydroxypropyl cellulose, 8 parts of rubber powder and 435 parts of manganese nitrate hexahydrate-expanded vermiculite compound according to parts by weight, and uniformly mixing to obtain the phase change putty, wherein the mass fraction of the manganese nitrate hexahydrate-expanded vermiculite compound in the phase change putty is 30%.
Through determination, the melting point of the phase change putty is 25 ℃, the phase change enthalpy is 33J/g, the phase change enthalpy is attenuated by 38% after 1000 times of circulation, and the service life of the phase change putty is 9 years. According to a sample preparation and test method of 'putty for building interior' JG/T298-plus 2010 in the building industry standard, phase-change putty is respectively coated on a cement slab and a mortar block base material, the phase-change putty and the mortar block base material are subjected to water-resistant treatment, after 300 days, a putty layer coated on the cement slab base material has a foaming phenomenon, the bonding strength of the putty layer coated on the mortar block base material is respectively 0.22MPa (standard state) and 0.15MPa (after water immersion), and the phase-change putty which is not subjected to gel treatment does not have qualified application performance.
Example 2
A preparation method of wall surface phase change putty 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 and 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 ensure that the calcium nitrate tetrahydrate-zinc nitrate phase-change material is 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 2 wt% of oxalic acid dihydrate (precipitator), 2 wt% of laponite (inorganic gelling agent) and 1wt% of 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;
step 4, weighing 400 parts of white cement, 200 parts of calcium carbonate powder, 200 parts of ash calcium powder, 200 parts of quartz powder, 30 parts of rubber powder, 30 parts of pregelatinized starch, 265 parts of hydrogel-calcium nitrate tetrahydrate-zinc nitrate hexahydrate-expanded perlite and uniformly mixing to obtain the phase change putty, wherein the mass fraction of the hydrogel-manganese nitrate hexahydrate-expanded vermiculite composite phase change energy storage material in the phase change putty is 20%.
Through determination, the melting point of the phase change putty is 24 ℃, the phase change enthalpy is 18J/g, the phase change enthalpy is attenuated by 0.5% after 1000 times of circulation, and the service life of the phase change putty is 50 years. The phase change putty is mainly used for leveling the surfaces of inner and outer wallboards and top boards of buildings. According to a sample preparation and test method of 'putty for building interior' JG/T298-plus 2010 in the building industry standard, phase-change putty is respectively coated on a cement slab and a mortar block base material, the phase-change putty is subjected to water-resistant treatment, after 300 days, a putty layer coated on the cement slab base material has no foaming, cracking and powder falling phenomena, and the bonding strength of the putty layer coated on the mortar block base material is 0.56MPa (standard state) and 0.37MPa (after being soaked in water).
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 and 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 ensure that the calcium nitrate tetrahydrate-zinc nitrate hexahydrate phase-change material is 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 400 parts of white cement, 200 parts of calcium carbonate powder, 200 parts of ash calcium powder, 200 parts of quartz powder, 30 parts of rubber powder, 30 parts of pregelatinized starch and 265 parts of calcium nitrate tetrahydrate-zinc nitrate hexahydrate-expanded perlite compound according to the parts by weight, and uniformly mixing to obtain the phase change putty, wherein the mass fraction of the calcium nitrate tetrahydrate-zinc nitrate hexahydrate-expanded perlite compound in the phase change putty is 20%.
Through determination, the melting point of the phase change putty is 24 ℃, the phase change enthalpy is 21J/g, the phase change enthalpy is attenuated by 50% after 1000 times of circulation, and the service life of the phase change putty is 6 years. According to a sample preparation and test method of 'putty for building interior' JG/T298-plus 2010 in the building industry standard, phase-change putty is respectively coated on a cement slab and a mortar block base material, the phase-change putty and the mortar block base material are subjected to water-resistant treatment, after 300 days, a putty layer coated on the cement slab base material has a foaming phenomenon, the bonding strength of the putty layer coated on the mortar block base material is respectively 0.35MPa (standard state) and 0.20MPa (after water immersion), and the phase-change putty which is not subjected to gel treatment does not have qualified application performance.
Example 3
A preparation method of wall surface phase change putty comprises the following steps:
step 1, mixing the components in a weight ratio of 83:1: weighing a potassium fluoride tetrahydrate phase-change material (hydrated salt), a nucleating agent (stannous fluoride, sodium dihydrogen phosphate dodecahydrate) and porous silicon (porous material), wherein the granularity of the porous silicon is 400 meshes, uniformly mixing, melting the potassium fluoride tetrahydrate phase-change material at 30 ℃ to ensure that the potassium fluoride tetrahydrate phase-change material is uniformly and fully absorbed by the porous silicon, and cooling to room temperature to obtain a potassium fluoride tetrahydrate-porous silicon composite;
step 2, preparing hydrosol (organic gelling agent) containing 3 wt% of calcium hydroxide (precipitant), 3 wt% of bentonite (inorganic gelling agent) and 1wt% of xanthan gum;
step 3, soaking the potassium fluoride tetrahydrate-porous silicon composite in the obtained hydrosol according to the mass ratio of 9:1, performing ultrasonic exhaust, taking out the composite, dehydrating, drying and granulating to realize complete coating of composite particles, preparing the hydrogel-potassium fluoride tetrahydrate-porous silicon composite phase change energy storage material, and sealing for later use;
and 4, weighing 300 parts of black cement, 300 parts of calcium carbonate powder, 200 parts of ash calcium powder, 200 parts of quartz powder, 22 parts of rubber powder, 30 parts of hydroxypropyl methyl cellulose and 117 parts of hydrogel-potassium fluoride tetrahydrate-porous silicon composite phase change energy storage material according to parts by weight, and uniformly mixing to obtain the phase change putty, wherein the mass fraction of the hydrogel-potassium fluoride tetrahydrate-porous silicon composite phase change energy storage material in the phase change putty is 10%.
Through determination, the melting point of the phase change putty is 18 ℃, the phase change enthalpy is 12J/g, the phase change enthalpy is attenuated by 0.3% after 1000 times of circulation, and the service life of the phase change putty is 45 years. The phase change putty is mainly used for leveling the surfaces of inner and outer wallboards and top boards of buildings. According to a sample preparation and test method of 'putty for building interior' JG/T298-plus 2010 in the building industry standard, phase-change putty is respectively coated on a cement slab and a mortar block base material, the phase-change putty is subjected to water-resistant treatment, after 300 days, a putty layer coated on the cement slab base material has no foaming, cracking and powder falling phenomena, and the bonding strength of the putty layer coated on the mortar block base material is 0.60MPa (standard state) and 0.38MPa (after being soaked in water).
Comparative example 3
According to the weight ratio of 83:1: weighing a potassium fluoride tetrahydrate phase-change material (hydrated salt), a nucleating agent (stannous fluoride, sodium dihydrogen phosphate dodecahydrate) and porous silicon (porous material), wherein the granularity of the porous silicon is 400 meshes, uniformly mixing, melting the potassium fluoride tetrahydrate phase-change material at 30 ℃ to ensure that the potassium fluoride tetrahydrate phase-change material is uniformly and fully absorbed by the porous silicon, and cooling to room temperature to obtain a potassium fluoride tetrahydrate-porous silicon composite;
weighing 300 parts of black cement, 300 parts of calcium carbonate powder, 200 parts of ash calcium powder, 200 parts of quartz powder, 22 parts of rubber powder, 30 parts of hydroxypropyl methyl cellulose and 117 parts of potassium fluoride tetrahydrate-porous silicon compound according to parts by weight, and uniformly mixing to obtain the phase change putty, wherein the mass fraction of the potassium fluoride tetrahydrate-porous silicon compound in the phase change putty is 10%.
Through determination, the melting point of the phase change putty is 18 ℃, the phase change enthalpy is 14J/g, the phase change enthalpy is attenuated by 64% after 1000 times of circulation, and the service life of the phase change putty is 5 years. According to a sample preparation and test method of 'putty for building interior' JG/T298-plus 2010 in the building industry standard, phase-change putty is respectively coated on a cement slab and a mortar block base material, the phase-change putty and the mortar block base material are subjected to water-resistant treatment, after 300 days, a putty layer coated on the cement slab base material has a foaming phenomenon, the bonding strength of the putty layer coated on the mortar block base material is respectively 0.41MPa (standard state) and 0.24MPa (after water immersion), and the phase-change putty which is not subjected to gel treatment does not have qualified application performance. .
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. The wall surface phase change putty is characterized in that: the wall surface phase change putty contains 10-30 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 carbonate dodecahydrate, calcium nitrate hexahydrate, zinc nitrate tetrahydrate, potassium fluoride tetrahydrate, ferric bromide hexahydrate, 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;
the hydrogel is added with a gelling agent, 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 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, chitosan, cellulose ether, sodium alginate, polyurethane and k2 type carrageenan;
the hydrogel is added with a precipitator, the precipitator is one or a mixture of more than one of sodium carbonate, sodium sulfate, sodium hydroxide, potassium carbonate, potassium hydroxide and calcium hydroxide, and insoluble precipitates formed by the hydrated salt and the precipitator in the hydrogel are one or a mixture of more than one of magnesium carbonate, magnesium hydroxide, basic magnesium carbonate, basic magnesium hydroxide, calcium carbonate, basic calcium carbonate and calcium fluoride.
2. The wall surface phase change putty as claimed in claim 1, which is characterized in that: 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. The wall surface phase change putty is characterized in that: the wall surface phase change putty consists of the following components in parts by weight: black/white cement: 300-400 parts; filling agent: 400-500 parts; phase change energy storage material: 110-450 parts; ash calcium powder: 100-200 parts; anti-cracking agent: 4-30 parts of a solvent; rubber powder: 8-30 parts of a solvent; wherein the specific form of the filler is any one or a mixture of a plurality of heavy calcium carbonate, double flying powder and quartz powder; the anti-cracking agent is any one or a mixture of more of polypropylene short fibers, wood fibers, hemp cut, hydroxypropyl methyl cellulose and pregelatinized starch;
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 carbonate dodecahydrate, calcium nitrate hexahydrate, zinc nitrate tetrahydrate, potassium fluoride tetrahydrate, ferric bromide hexahydrate, 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;
the hydrogel is added with a gelling agent, 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 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, chitosan, cellulose ether, sodium alginate, polyurethane and k2 type carrageenan;
the hydrogel is added with a precipitator, the precipitator is one or a mixture of more than one of sodium carbonate, sodium sulfate, sodium hydroxide, potassium carbonate, potassium hydroxide and calcium hydroxide, and insoluble precipitates formed by the hydrated salt and the precipitator in the hydrogel are one or a mixture of more than one of magnesium carbonate, magnesium hydroxide, basic magnesium carbonate, basic magnesium hydroxide, calcium carbonate, basic calcium carbonate and calcium fluoride.
4. The wall surface phase change putty as claimed in claim 3, which is characterized in that: the wall surface phase change putty also comprises hydroxypropyl cellulose: 0-2 parts of.
5. The wall surface phase change putty as claimed in claim 3, which is characterized in that: 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 wall surface phase change putty as claimed in claim 3, which is characterized in that: the hydrogel is obtained by dehydrating and drying hydrosol.
7. The wall surface phase change putty as claimed in claim 3, which is characterized in that: the mass content of hydrogel in the hydrogel-coated hydrous salt-porous material composite phase change energy storage material is 10% -15%.
8. The wall surface phase change putty as claimed in claim 3, which is characterized in that: 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 ensure that the hydrated salt is uniformly and fully 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 water glass or water-soluble silicon, the mass content of the precipitator in the hydrosol containing the precipitator and the gelling agent is 1-3%, and the mass content of the gelling agent is 3-6%;
and 3, weighing the hydrated salt-porous material composite and hydrosol containing a precipitator and a gelling agent according to the mass ratio of (5-9): 1, uniformly mixing, and dehydrating to obtain the hydrated salt-porous material composite type phase change energy storage material coated by the hydrogel.
9. The wall surface phase change putty as claimed in claim 8, which is characterized in that: the particle size of the porous material is 400-600 meshes.
10. The wall surface phase change putty as claimed in claim 8, which is characterized in that: the organic gelling agent in the hydrogel does not exceed 1 wt%.
11. The wall surface phase change putty as claimed in claim 8, which is characterized in that: the mixing of the hydrated salt-porous material composite and the hydrosol containing the precipitant and the gelling agent comprises the following modes: spraying hydrosol containing precipitant and gelatinizer onto the surface of the hydrated salt-porous material composite, dewatering and pelletizing; the hydrated salt-porous material composite is soaked in hydrosol containing precipitant and colloid forming agent, and dewatered and granulated.
12. The wall surface phase change putty as claimed in claim 8, which is characterized in that: the precipitating agent accounts for not more than 3% of the mass ratio of the hydrogel.
13. The preparation method of the wall surface phase change putty as claimed in claim 3, which 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 ensure that the hydrated salt is uniformly and fully 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 water glass or water-soluble silicon, the mass content of the precipitator in the hydrosol containing the precipitator and the gelling agent is 1-3%, and the mass content of the gelling agent is 3-6%;
step 3, weighing the hydrated salt-porous material composite and hydrosol containing a precipitator and a gelling agent according to the mass ratio of (5-9): 1, uniformly mixing, and dehydrating to obtain the hydrated salt-porous material composite type phase change energy storage material coated by the hydrogel;
and 4, step 4: according to the weight parts, uniformly mixing 110-450 parts of hydrogel-coated hydrated salt-porous material composite type phase change energy storage material, 300-400 parts of black/white cement, 400-500 parts of filler, 100-200 parts of ash calcium powder, 4-30 parts of anti-cracking agent and 8-30 parts of rubber powder to obtain the wall surface phase change putty.
14. The preparation method of the wall surface phase change putty as claimed in claim 13, which is characterized in that: and 4, adding 0-2 parts by weight of hydroxypropyl cellulose in the step 4, and uniformly mixing.
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