WO2022257340A1 - Produit de matériau de construction à changement de phase présentant une performance de régulation de température et son procédé de préparation - Google Patents

Produit de matériau de construction à changement de phase présentant une performance de régulation de température et son procédé de préparation Download PDF

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WO2022257340A1
WO2022257340A1 PCT/CN2021/127552 CN2021127552W WO2022257340A1 WO 2022257340 A1 WO2022257340 A1 WO 2022257340A1 CN 2021127552 W CN2021127552 W CN 2021127552W WO 2022257340 A1 WO2022257340 A1 WO 2022257340A1
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phase
change
days
temperature
microcapsules
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PCT/CN2021/127552
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English (en)
Chinese (zh)
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王兵
杨正波
李帆
陈红霞
张赫
丛宇
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中建材创新科技研究院有限公司
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Publication of WO2022257340A1 publication Critical patent/WO2022257340A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B17/00—Details of, or accessories for, apparatus for shaping the material; Auxiliary measures taken in connection with such shaping
    • B28B17/02—Conditioning the material prior to shaping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00—Producing shaped prefabricated articles from the material
    • B28B1/008—Producing shaped prefabricated articles from the material made from two or more materials having different characteristics or properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B28—WORKING CEMENT, CLAY, OR STONE
    • B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B17/00—Details of, or accessories for, apparatus for shaping the material; Auxiliary measures taken in connection with such shaping
    • B28B17/0036—Cutting means, e.g. water jets
    • 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
    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/0008—Materials specified by a shape not covered by C04B20/0016 - C04B20/0056, e.g. nanotubes
    • 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
    • C04B28/14—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 calcium sulfate cements
    • C04B28/145—Calcium sulfate hemi-hydrate with a specific crystal form
    • 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
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00612—Uses not provided for elsewhere in C04B2111/00 as one or more layers of a layered structure
    • C04B2111/0062—Gypsum-paper board like materials
    • 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
    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

Definitions

  • This article relates to but not limited to the field of building material products, especially relates to but not limited to a phase change building material product with temperature control performance and its preparation method.
  • phase change energy storage wall can not only improve the thermal insulation performance of the wall, but also improve the heat storage and heat storage performance of the wall, and improve the indoor thermal environment of the building, but the phase change energy storage
  • the material is encapsulated in the building material product, and it should be ensured that the phase change building material product does not leak out of the phase change energy storage material during use, so as to realize the application of the phase change energy storage material in the field of building materials.
  • Common building material products in the field of building materials include, but are not limited to, gypsum boards, gypsum blocks, plastering gypsum, self-leveling mortar, gypsum battens, and concrete.
  • phase change energy storage gypsum board can be divided into three types: impregnation method, direct mixing method, and encapsulation method.
  • impregnation method and the direct mixing method are simple in preparation process, phase change materials are prone to exudation, so they are rarely used in actual production.
  • Encapsulation methods include micro-encapsulation and macro-encapsulation. Macro-encapsulation affects the breathing performance of gypsum boards. If the encapsulation is not perfect, flammable damage will occur and the scene of leakage.
  • micro-encapsulation is generally in the form of microcapsules, although microcapsules
  • the phase change material has been encapsulated, but when the phase change microcapsules are mixed with gypsum and water, friction or shear force will be generated, and the physical action will also damage the phase change microcapsules, resulting in leakage of the phase change material.
  • phase change building material product containing no leakage of the phase change material and a preparation method thereof.
  • the application provides a phase change building material product with temperature control performance and a preparation method thereof.
  • the phase-change building material product with temperature control performance of the present application can adjust the indoor temperature and the phase-change material does not leak, ensuring the safety of the phase-change building material product;
  • the advanced preparation process enables building material products to obtain higher strength.
  • a method for preparing a phase-change building material product with temperature-controlling properties comprising phase-change microcapsules before and after preparing the phase-change building material product with temperature-controlling properties
  • the phase change microcapsule or phase change microcapsule solution is in an environment lower than the phase change temperature, so that the phase change material is in a solid state.
  • the phase change microcapsules are placed in an environment lower than the phase change temperature for a period of time to ensure that the phase change material is in a solid state; And wherein the storage time is 5h to one month; the storage time can be 29 days to 10 days; the storage time can be 25 days to 9 days; the storage time can be 20 days to 8 days; the storage time It can be 15 days to 8 days; the storage time can be 10 days to 5 days; the storage time can be 5 days to 1 day; the storage time can be 3 days to 23h; the storage time can be 2 day to 12h; and the temperature of the environment lower than the phase transition temperature may be lower than the phase transition temperature by more than 5°C.
  • the storage time can be one month, 29 days, 28 days, 27 days, 26 days, 25 days, 24 days, 23 days, 22 days, 21 days, 20 days, 19 days, 18 days, 17 days, 16 days, 15 days, 14 days, 13 days, 12 days, 11 days, 10 days, 9 days, 8 days, 7 days, 6 days, 5 days, 4 days, 3 days, 2 days , 24h, 23h, 22h, 21h, 20h, 19h, 18h, 17h, 16h, 15h, 14h, 13h, 12h, 11h, 10h, 9h, 8h, 7h, 6h, 5h or any range between two values or value.
  • the phase-change microcapsules are in solid powder form; or the phase-change microcapsules are in liquid form.
  • phase-change microcapsules when the phase-change microcapsules are solid powders, the phase-change microcapsules in the form of solid powder in an environment lower than the phase transition temperature are mixed with water to make the phase-change microcapsules in the form of solid powder
  • the phase change microcapsules are evenly distributed in water to form a phase change microcapsule solution; the temperature of the water used in the phase change microcapsule solution is lower than the phase change temperature; when the phase change microcapsules are in liquid form, the phase change microcapsules in liquid form
  • the microcapsules are in an environment lower than the phase change temperature to ensure that the phase change material in the phase change microcapsules is in a solid state; and preserve the phase change microcapsules, the water used to prepare the phase change microcapsule solution or preserve the
  • the temperature of the phase change microcapsules in liquid form can be lower than the phase change temperature by more than 5°C.
  • the phase change microcapsules have an enthalpy retention rate of 60% to 99%, an enthalpy value of 50J/g to 200J/g, and an average particle size of 0.1 ⁇ m to 20 ⁇ m, or the average The particle size is 0.1 ⁇ m to 10 ⁇ m, and the phase transition temperature is 15°C to 30°C.
  • the solid content of the phase-change microcapsule solution is 20% to 60%, so as to ensure that the solution has better fluidity.
  • the solid content of the phase change microcapsules is 10% to 70%.
  • the solid content of the phase change microcapsules is 20% to 60%.
  • the solid content of the phase change microcapsules is 25% to 60%.
  • the solid content of the phase change microcapsules is 30% to 60%.
  • the solid content of the phase change microcapsules is 35% to 60%.
  • the solid content of the phase change microcapsules is 40% to 60%.
  • the solid content of the phase change microcapsules is 45% to 60%.
  • the solid content is the mass percentage of the remaining part of the emulsion or coating after drying under specified conditions.
  • the phase-change microcapsules include a core material and a wall material; and wherein the core material and the wall material are any one or both of inorganic substances and organic substances.
  • the core material is any one or more of alcohol compounds, organic acid compounds, ester compounds and alkane compounds.
  • the core material is any one or more of paraffin, capric acid, caprylic acid, butyl stearate, polyethylene glycol, lauryl alcohol and n-octane.
  • phase-change building material products with temperature control properties prepared by the above preparation method
  • the phase-change building material products include phase-change gypsum board, phase-change gypsum block, phase-change putty, phase-change self-leveling Mortar, phase change stone slats and phase change concrete.
  • the application provides a phase-change gypsum board with temperature-controlling properties prepared by the above-mentioned preparation method, with gypsum accounting for 100 parts by weight, phase-change microcapsules: binder: face-protecting paper: water The weight ratio is (5 to 50):(0.1 to 1):(0.05 to 0.1):(55 to 95).
  • the phase-change gypsum board also includes a reinforcing agent, and the weight ratio of the phase-change microcapsule: the binder: the reinforcing agent: the protective paper: the water is ( 5 to 50):(0.1 to 1):(0.05 to 5):(0.05 to 0.1):(55 to 95).
  • the phase-change gypsum board further includes a water-reducing agent, the phase-change microcapsule: the binder: the strengthening agent: the water-reducing agent: the face-protecting paper: the The weight ratio of said water is (5 to 50): (0.1 to 1): (0.05 to 5): (0.05 to 5): (0.05 to 0.1): (55 to 95).
  • the phase-change gypsum board also includes a surfactant
  • the phase-change microcapsule the binder: the reinforcing agent: the water reducing agent: the surfactant: the Said facial protection paper: the weight ratio of the water is (5 to 50): (0.1 to 1): (0.05 to 5): (0.05 to 5): (0.05 to 5): (0.05 to 0.1): (55 to 95).
  • the binder is any one or more of corn starch, modified corn starch, tapioca starch and pregelatinized starch; the viscosity of the above starch is 1000mPa ⁇ s to 5000mPa ⁇ s s.
  • the test method in the Chinese chemical industry standard HG/T 3932-2007 was adopted, the sample concentration was 5%, the temperature was 25°C, the rotor number was 3, and the speed was 6r/min.
  • the reinforcing agent is any one or more of glass fibers, carbon fibers, wollastonite and gypsum whiskers.
  • the water reducer is lignosulfonate-based water reducer, naphthalene-based high-efficiency water-reducer, melamine-based high-efficiency water-reducer, sulfamate-based high-efficiency water-reducer Any one or more of superplasticizers, fatty acid-based superplasticizers, and polycarboxylate-based superplasticizers.
  • the surfactant is any one or more of sodium linear alkylbenzene sulfonate, sodium fatty alcohol polyoxyethylene ether sulfate, and ammonium fatty alcohol polyoxyethylene ether sulfate.
  • the phase change gypsum board is obtained through the following steps:
  • phase-change microcapsules of solid powder as a phase-change microcapsule solution or preparing the phase-change microcapsules in liquid form as a phase-change microcapsule solution in a stand-by form;
  • phase change microcapsules are placed in an environment lower than the phase change temperature for a period of time to ensure that the phase change material is in a solid state;
  • the placement time is 5h to one month; the placement time can be 29 days to 10 days; the placement time can be 25 days to 9 days; the placement time can be 20 days to 8 days; the placement time can be It is 15 days to 8 days; the storage time can be 10 days to 5 days; the storage time can be 5 days to 1 day; the storage time can be 3 days to 23h; the storage time can be 2 days to 12h; and
  • the temperature of the environment lower than the phase transition temperature may be more than 5°C lower than the phase transition temperature
  • a binder and optionally a reinforcing agent may not be mixed into the plaster of paris in step (1); the binder and optionally a reinforcing agent are mixed in step (3).
  • the present application provides an application of a phase-change gypsum board with temperature control properties in room partition walls or suspended ceilings.
  • the application provides a phase-change gypsum block with temperature-controlling properties prepared by the above-mentioned preparation method.
  • the weight ratio of phase-change microcapsules: water is: (5 to 50 ): (55 to 95);
  • the phase-change gypsum block with temperature control performance can also include binder, reinforcing agent, water reducer, surfactant, etc., wherein phase-change microcapsules: water: binder :Strengthening agent:Water reducer:Surfactant
  • the weight ratio is (5 to 50):(55 to 95):(0.1 to 1):(0.05 to 5):(0.05 to 5):(0.05 to 5) .
  • the application provides phase-change plastering gypsum with temperature-controlling properties prepared by the above-mentioned preparation method, taking 100 parts by weight of plaster, phase-change microcapsules: cellulose ether: the weight ratio of water is ( 5 to 50): (0.01 to 0.5): (25 to 75); the phase change plastering gypsum with temperature control performance can also include retarder, cement, etc., wherein phase change microcapsules: cellulose ether: retarder Coagulant: cement: the weight of water is (5 to 50): (0.01 to 0.5): (0.01 to 1): (0.01 to 1): (25 to 75).
  • the application provides a phase-change self-leveling mortar with temperature control properties prepared by the above-mentioned preparation method, taking 100 parts by weight of plaster, phase-change microcapsules: rheology modifier: weight ratio of water It is (5 to 50): (0.01 to 0.5): (25 to 75); the phase change self-leveling mortar with temperature control performance can also include filler, cellulose ether, reinforcing agent, water reducer, surface Activator, defoamer etc., wherein, phase change microcapsule: rheology modifier: water: filler: cellulose ether: strengthening agent: water reducer: surfactant: the weight of defoamer is (5 to 50):(0.01 to 0.5):(25 to 75):(1:30):(0.1 to 5):(0.05 to 5):(0.05 to 5):(0.05 to 5):(0.05 to 5):(0.05 to 5) . ).
  • phase change microcapsules included in this application require storage and use below the phase change temperature.
  • the phase-change building material products prepared by this application fuse phase-change microcapsules with building materials, and the low-temperature preparation process enables the phase-change building material products to obtain higher strength, and the microscopic observation of the phase-change microcapsules does not leak, ensuring that the phase-change building material products are used safety.
  • Figure 1 is a photo of the color change on the surface of the gypsum board after the phase-change gypsum board prepared in Example 2 and the comparative example were placed in an oven at 45°C and baked for 24 hours.
  • the face paper of the gypsum board prepared by the embodiment is the natural color, while the face paper prepared by the comparative example has been impregnated with oil, indicating that the phase change microcapsules used in the preparation method of the comparative example have not played a sealing phase. Due to the role of the change material, the paraffin wax in the phase change microcapsules has leaked and migrated to the surface of the protective paper, which has the potential to volatilize and affect the quality of the gypsum board.
  • Fig. 2 is an electron microscope image of the morphology of phase-change gypsum boards prepared in Example 2 and Comparative Example.
  • phase-change microcapsules of Example 2 still completely exist between the gypsum crystals, and the gypsum crystals basically do not change greatly; while the phase-change microcapsules of the comparative example are damaged, and the gypsum crystals also undergo significant changes, and the crystals change Short and trivial with reduced intensity.
  • Figure 3 is an electron microscope image of gypsum hardened slurry prepared by slurrying gypsum board at 15°C and 40°C. It can be seen from the figure that the high temperature makes the crystals grow and become larger, and the overlap between the crystals is loose; but the low temperature makes the crystals compact, elongated and tightly clustered and strengthens the crystal strength.
  • FIG. 4 is a graph corresponding to the gypsum board of FIG. 3 .
  • A is the average Young's modulus-indentation depth curve of the gypsum board corresponding to FIG. 3 .
  • the ordinate is Young's modulus (GPa), and the abscissa is displacement (nm).
  • B is the average hardness-indentation depth graph of the gypsum board corresponding to FIG. 3 .
  • the ordinate is the hardness (GPa), and the abscissa is the displacement (nm).
  • HT high temperature (40°C).
  • LT low temperature (15°C).
  • Phase-change microcapsules prepared according to the method steps described in the examples of patent ZL200810103749.3;
  • Binder Shenyang Xuegong Adhesive Technology Co., Ltd., modified corn starch;
  • Naphthalene-based high-efficiency water reducer Laiwu Dongfuxiang Chemical Co., Ltd., the brand is FDN-A.
  • phase-change microcapsules are prepared according to the patent ZL200810103749.3 paragraphs [0009] to [0015] to prepare microcapsules of inorganic phase-change energy storage materials by the gel sol method; the difference is that the phase-change microcapsules prepared by the present application are Single-layer phase-change microcapsules; the phase-change microcapsules are a solution with a solid content of 35%; the enthalpy is about 120J/g; the average particle size is 5 ⁇ m;
  • phase change temperature of the phase change microcapsules is 20°C to 25°C, in an environment of 15°C;
  • the slurry is placed in the middle of the protective paper, cut and dried to form a phase-change gypsum board with temperature control performance.
  • phase-change microcapsules are prepared as microcapsules of organic phase-change energy storage materials according to paragraphs [0009] to [0015] of patent ZL200810103749.3; the difference is that the phase-change microcapsules prepared by the present application are single phase-change microcapsules layer; the phase-change microcapsules are a solution with a solid content of 35%; the enthalpy is about 120J/g; the average particle size is 5 ⁇ m;
  • phase change temperature of the phase change microcapsules is 20°C to 25°C, in an environment of 15°C;
  • the slurry is placed in the middle of the protective paper, cut and dried to form a phase-change gypsum board with temperature control performance.
  • phase change microcapsules are prepared by combining the in-situ polymerization method and the sol-gel method in Example 3 of the patent ZL200810103749.3 to prepare microcapsules with double-layer composite functional shells encapsulating organic phase change energy storage materials; the phase change microcapsules are powder , the enthalpy value is about 120J/g; the average particle size is 5 ⁇ m;
  • phase change temperature of the phase change microcapsules is 20°C to 25°C, in an environment of 15°C; mix the phase change microcapsules with 25 parts of water, and the water temperature is 15°C, so that the phase change materials are evenly distributed in the water to form phase change microcapsules solution;
  • the slurry is placed in the middle of the protective paper, cut and dried to form a phase-change gypsum board with temperature control performance.
  • phase change temperature of the phase change microcapsules is 20°C to 25°C, in an environment of 25°C; mix the phase change microcapsules with 25 parts of water, and the water temperature is 25°C, so that the phase change materials are evenly distributed in the water to form phase change microcapsules solution;
  • the slurry is placed in the middle of the protective paper, cut and dried to form a phase-change gypsum board with temperature control performance.
  • test block of the embodiment and the comparative example is to mix and stir the plaster of paris with water at 15°C and 40°C respectively, and pour it into a grinding tool after uniformity to prepare a test block of 160*40*40mm; then dry it at 45°C for 24 hours;
  • Table 2 The results of the flexural and compressive strength of the test block are shown in Table 2 below;
  • the phase-change gypsum board prepared by the examples of the present application has a flexural strength of 9.2/MPa and a compressive strength of 26.13/MPa; while the phase-change gypsum board prepared by the comparative example has a flexural strength of 8.63/MPa,
  • the compressive strength is 21.84/MPa; the flexural and compressive properties of the phase-change gypsum board prepared in the examples of the present application are much better than those of the comparative examples.
  • the face paper of the gypsum board prepared in the embodiment is the natural color, while the face paper prepared in the comparative example has been impregnated with oil, indicating that the phase change microcapsules used in the preparation method of the comparative example (not stored in an environment lower than the phase change temperature and the temperature of the water used is not lower than the phase change temperature) did not play the role of sealing the phase change material, the paraffin in the phase change microcapsules has leaked and migrated to the protective surface On the paper surface, there are hidden dangers of volatilization and affecting the quality of gypsum board.
  • phase-change microcapsules of the embodiment still completely exist between the gypsum crystals, and the gypsum crystals have not changed substantially; while the phase-change microcapsules of the comparative example are damaged, and the gypsum crystals have also undergone large changes. changes, the crystals become shorter and trivial and lose strength.
  • the nano-indentation test can obtain the nano-mechanical properties of gypsum materials; as can be seen from Table 3, the nano-mechanical properties of gypsum hardened slurry prepared at low temperature are greatly improved compared with those at high temperature, Young's modulus, the average value of Young's modulus of low-temperature samples It is 14.41GPa, which is 4 times of 3.62GPa of high-temperature sample; the hardness of low-temperature sample is 0.205GPa, which is 5 times of 0.041GPa of high-temperature sample.

Abstract

Produit de matériau de construction à changement de phase présentant une performance de régulation de température et son procédé de préparation. Selon le procédé de préparation, avant la préparation du produit de matériau de construction à changement de phase présentant la performance de régulation de température et pendant la préparation d'une solution de microcapsule à changement de phase, la microcapsule à changement de phase se trouve dans un environnement au-dessous de la température de changement de phase, de telle sorte qu'un matériau à changement de phase se trouve dans un état solide. Avant la préparation du produit de matériau de construction à changement de phase présentant la performance de régulation de température, la microcapsule à changement de phase est placée dans un environnement au-dessous de la température de changement de phase pendant une certaine période, de manière à s'assurer que le matériau à changement de phase se trouve dans un état solide, le temps pendant lequel cette dernière est placée étant de 5 heures à 1 mois ; le temps pendant lequel cette dernière est placée pouvant être de 8 jours à 20 jours, ou de 12 heures à 2 jours ; et la température de l'environnement au-dessous de la température de changement de phase pouvant être inférieure à la température de changement de phase à raison de 5 °C ou plus. Le procédé de préparation évite la fuite du matériau à changement de phase, de telle sorte que le produit de matériau de construction à changement de phase obtenu permet de régler la température intérieure et présente une résistance plus élevée.
PCT/CN2021/127552 2021-06-07 2021-10-29 Produit de matériau de construction à changement de phase présentant une performance de régulation de température et son procédé de préparation WO2022257340A1 (fr)

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CN117185706A (zh) * 2023-09-20 2023-12-08 重庆诺奖二维材料研究院有限公司 一种相变微胶囊储能保温离心玻璃棉板及其制备方法

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CN113414869A (zh) * 2021-06-07 2021-09-21 中建材创新科技研究院有限公司 一种具有控温性能的相变建材制品及其制备方法

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