CN114751673A - Phase-change thermal insulation mortar for greenhouse wall and preparation method thereof - Google Patents

Phase-change thermal insulation mortar for greenhouse wall and preparation method thereof Download PDF

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Publication number
CN114751673A
CN114751673A CN202210683025.0A CN202210683025A CN114751673A CN 114751673 A CN114751673 A CN 114751673A CN 202210683025 A CN202210683025 A CN 202210683025A CN 114751673 A CN114751673 A CN 114751673A
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mixing
stirring
mixture
preparation
phase change
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CN114751673B (en
Inventor
田素波
胡永军
胡莹莹
杨晋
辛晓菲
王鲲霆
王付彬
邱常亮
亓烨
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National Vegetable Quality Standard Center
Shandong Shouguang Vegetable Industry Group Co Ltd
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National Vegetable Quality Standard Center
Shandong Shouguang Vegetable Industry Group Co Ltd
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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
    • C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028—Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039—Premixtures of ingredients
    • 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
    • C04B20/02—Treatment
    • C04B20/023—Chemical treatment
    • 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
    • C04B28/04—Portland cements
    • 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
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/0068—Ingredients with a function or property not provided for elsewhere in C04B2103/00
    • C04B2103/0071—Phase-change materials, e.g. latent heat storage materials used in concrete compositions
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]
    • Y02B30/90—Passive houses; Double facade technology

Abstract

The invention discloses phase change thermal insulation mortar for greenhouse walls and a preparation method thereof, belonging to the technical field of thermal insulation mortar, wherein the preparation method comprises the following steps: primary mixing, secondary mixing, tertiary mixing and post-treatment; the primary mixing method comprises the steps of mixing the microcapsule phase change material, the modifier, the sodium dodecyl benzene sulfonate, the polyethylene glycol 400 and the zinc oxide, adding the mixture into a reaction kettle, vacuumizing the reaction kettle to 200-300Pa, controlling the temperature of the reaction kettle to 40-45 ℃, and stirring for 30-35min to obtain a primary mixture; the invention can improve the durability and the thermal stability of the phase-change thermal insulation mortar and improve the strength and the heat storage and thermal insulation properties of the phase-change thermal insulation mortar.

Description

Phase-change thermal insulation mortar for greenhouse wall and preparation method thereof
Technical Field
The invention relates to the technical field of thermal insulation mortar, in particular to phase change thermal insulation mortar for greenhouse walls and a preparation method thereof.
Background
The phase-change thermal-insulation mortar is prepared by mixing a phase-change material with materials such as cement, lightweight aggregate and an additive according to a certain proportion, and has excellent energy-storage, temperature-regulation and energy-saving effects after the phase-change thermal-insulation mortar is prepared into a mortar coating.
The phase-change thermal insulation mortar is easy to construct and does not need to be additionally leveled; the construction process is simple, and the operation is easy to master; the grade of combustion performance is A grade, and the fire-resistant fireproof paint is non-combustible, so that the defects of poor fire resistance, harmful gas generation at high temperature, low aging resistance, large rebound elasticity in construction, easiness in insect bite and the like of organic materials such as polyphenyl and the like are overcome; the bonding strength and the surface impact strength are more excellent; the heat preservation principle of the barrier type and the energy storage type is integrated, the heat preservation effect is excellent, the latent heat value is high, and the heat storage and preservation performance is excellent; the water absorption rate is extremely low, and the house water seepage phenomenon is not easy to occur; therefore, the phase-change thermal mortar is widely applied to external thermal insulation plastering engineering and internal thermal insulation plastering engineering of walls such as reinforced concrete, aerated concrete, bricklaying, sintered brick, non-sintered brick and the like of multi-storey and high-rise buildings, and in recent years, along with the development of agriculture, the phase-change thermal mortar is widely applied to greenhouse wall construction.
However, the phase-change thermal insulation mortar used for the construction of the wall of the greenhouse has the following problems: the phase change thermal insulation mortar can cause the degradation of thermal physical properties in the circulating phase change process, thereby causing the poor durability of the phase change thermal insulation mortar; in order to solve the above problems, the most common method at present is to coat the phase change material with microcapsules, but the microcapsules have poor thermal stability, which leads to poor thermal stability of the phase change thermal mortar. At present, no method for improving the strength and the heat storage and preservation properties of the phase-change thermal insulation mortar while improving the durability and the thermal stability of the phase-change thermal insulation mortar exists.
Chinese patent CN1264776C discloses a paraffin phase-change thermal-insulation mortar powder and a preparation method thereof, comprising 35-75% of cement, 5-40% of lightweight aggregate and 0.5-10% of fiber, wherein 5-40% of paraffin is contained in the mixture ratio, and part of cement can be replaced by fly ash, slaked lime, gypsum or silica powder. When in preparation, the paraffin is heated to be molten and fully stirred to be uniformly dispersed, or the paraffin is prepared into microcrystal powder; then evenly mixing the melted and dispersed paraffin or paraffin microcrystal powder with other materials to prepare paraffin glue powder, adding the paraffin glue powder into water, stirring into paste, adding the lightweight aggregate, and fully stirring. The patent solves the technical problems of high water absorption, poor waterproofness, low softening coefficient and water intolerance of the existing heat-insulating mortar, but the prepared phase-change heat-insulating mortar powder has poor durability.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides phase-change thermal insulation mortar for greenhouse walls and a preparation method thereof, which can improve the durability and the thermal stability of the phase-change thermal insulation mortar and simultaneously improve the strength and the heat storage and insulation properties of the phase-change thermal insulation mortar.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
A preparation method of phase change thermal insulation mortar for greenhouse walls comprises the following steps: primary mixing, secondary mixing, tertiary mixing and post-treatment.
The primary mixing method comprises the steps of mixing the microcapsule phase change material, the modifier, the sodium dodecyl benzene sulfonate, the polyethylene glycol 400 and the zinc oxide, adding the mixture into a reaction kettle, vacuumizing the reaction kettle to 200-300Pa, controlling the temperature of the reaction kettle to 40-45 ℃, controlling the stirring speed to 200-250rpm, and stirring for 30-35min to obtain a primary mixture;
in the primary mixing, the weight ratio of the microcapsule phase change material, the modifier, the sodium dodecyl benzene sulfonate, the polyethylene glycol 400 and the zinc oxide is 70-75:5-7:4-6:8-10: 5-7;
in the primary mixing, the preparation method of the microcapsule phase change material comprises the steps of mixing the high-density polyethylene and the paraffin uniformly, heating to 140-142 ℃ at a heating rate of 2.5-3 ℃/min, standing at 140-, then adding stearic acid and zinc stearate, continuing stirring at the stirring speed of 280-300rpm for 20-25min, then cooling to 80-85 ℃ at a cooling rate of 3-4 ℃/min, standing at 80-85 deg.C for 30-35min, cooling to room temperature at a rate of 3-4 deg.C/min, carrying out solidification molding at room temperature, adding the mixture into a crusher after solidification molding, and crushing the mixture to a particle size of 150-200 mu m to obtain a microcapsule phase change material;
In the primary mixing, in the preparation of the microcapsule phase change material, the weight ratio of the high-density polyethylene to the paraffin wax to the stearic acid to the zinc stearate is 30-32:18-20:3-5: 1-3;
in the primary mixing, in the preparation of the microcapsule phase change material, the density of the high-density polyethylene is 0.941-0.960g/cm3。
In the primary mixing, the preparation method of the modifier comprises the steps of placing the sucrose, the xanthan gum, the re-dispersible emulsion powder and the polyvinyl alcohol 2488 into a ball mill for ball milling, controlling the ball-material ratio during ball milling to be 10-15:1, the temperature to be 45-50 ℃, the rotating speed to be 300-350rpm and the time to be 40-45min, and obtaining the modifier after the ball milling is finished;
in the primary mixing, in the preparation of the modifier, the weight ratio of the sucrose to the xanthan gum to the re-dispersible latex powder to the polyvinyl alcohol 2488 is 2-4:10-12:15-18: 5-8.
The secondary mixing method comprises the steps of adding the primary mixture, the expanded perlite, the nano boron nitride, the modified fly ash and the calcium stearate into a stirring kettle, controlling the rotating speed of the stirring kettle to be 180-year 200rpm, and stirring for 40-45min to obtain a secondary mixture;
in the secondary mixing, the weight ratio of the primary mixture, the expanded perlite, the nano boron nitride, the modified fly ash and the calcium stearate is 100-45: 1-2:8-10: 2-4;
In the secondary mixing, the bulk density of the expanded perlite is 45-50kg/m3The average grain diameter is 2.5-3 mm;
in the secondary mixing, the particle size of the nanometer boron nitride is 200-400 nm;
in the secondary mixing, the preparation method of the modified fly ash comprises the following steps: adding the fly ash, barium stearate and sodium hexametaphosphate into a reaction kettle, vacuumizing the reaction kettle until the vacuum degree is 100-150Pa, introducing mixed gas into the reaction kettle until the gas pressure is 0.12-0.15MPa, controlling the temperature of the reaction kettle to 150-160 ℃, starting stirring, controlling the stirring speed to 150-200rpm, and stirring for 40-50min to obtain modified fly ash;
in the secondary mixing, in the preparation of the modified fly ash, the weight ratio of the fly ash, the barium stearate and the sodium hexametaphosphate is 35-40:4-6: 2-5;
in the secondary mixing, the mixed gas is the mixed gas of ammonia and nitrogen, wherein the volume ratio of the ammonia to the nitrogen is 3: 4-5.
The third mixing method comprises the steps of adding the secondary mixture, fine sand, steel slag powder, ordinary portland cement, vitrified micro bubbles, sodium lignin sulfonate and sodium alginate into a stirring kettle, controlling the rotating speed of the stirring kettle to be 200-220rpm, and stirring for 50-55min to obtain a third mixture;
In the third mixing, the weight ratio of the secondary mixture, the fine sand, the steel slag powder, the ordinary portland cement, the vitrified micro bubbles, the sodium lignin sulfonate and the sodium alginate is 60-65:15-20:7-9:25-30:8-10:2-4: 3-5;
in the third mixing, the common portland cement is P.O42.5 portland cement.
Adding the tertiary mixture into a reaction kettle, fumigating the tertiary mixture by using steam of a mixed solution, namely steam generated under saturated steam pressure, drying at 40-45 ℃ after the fumigation is finished to obtain dry sand, and adding water into the dry sand and uniformly mixing to obtain the heat-insulating mortar for the wall of the greenhouse;
in the post-treatment, the mixed solution is a mixed solution of absolute ethyl alcohol and dichloromethane, wherein the weight ratio of the absolute ethyl alcohol to the dichloromethane is 1: 2-3;
in the post-treatment, the weight ratio of the third mixture to the mixed solution is 10: 1-1.2;
in the post-treatment, the weight ratio of the dry sand to the water is 100: 40-45.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the preparation method of the phase-change thermal insulation mortar for the greenhouse wall, disclosed by the invention, the modifier is added in the primary mixing step, and the modified fly ash is used in the secondary mixing step, so that the phase separation phenomenon can be avoided, the energy storage density of the phase-change thermal insulation mortar is improved, and the thermal storage and insulation properties are improved, wherein the phase-change temperature of the prepared phase-change thermal insulation mortar for the greenhouse wall is 41.5-42.1 ℃, the phase-change latent heat is 142.3-143.5kJ/kg, and the specific heat capacity is 1.28-1.32 kJ/(kg.K);
(2) According to the preparation method of the phase-change thermal insulation mortar for the greenhouse wall, the three-time mixture is subjected to fumigation treatment, the surface treatment can be performed on the mortar, the compactness of the surface of the mortar and the cohesiveness among the mortar are improved, and therefore the strength of the phase-change thermal insulation mortar is improved, the 7d flexural strength of the prepared phase-change thermal insulation mortar for the greenhouse wall is 10.2-10.7MPa, the 7d compressive strength is 28.7-29.4MPa, the 28d flexural strength is 17.2-17.8MPa, the 28d compressive strength is 47.8-48.4MPa, and the seepage pressure is 0.82-0.85 MPa;
(3) according to the preparation method of the phase change thermal insulation mortar for the greenhouse wall, the modifier is added in the primary mixing step, so that the surface modification can be performed on the microcapsule phase change material, the aging resistance of the microcapsule phase change material is improved, the cohesiveness of the microcapsule phase change material with expanded perlite, modified fly ash, fine sand and ordinary portland cement is improved, and the strength of the phase change thermal insulation mortar is improved; the surface compactness of the microcapsule phase change material can be further improved by fumigating the tertiary mixture, so that the durability of the microcapsule phase change material is improved, and after 50 times of repeated freeze thawing cycles, the prepared phase change heat preservation mortar for the greenhouse wall has the phase change temperature of 41.0-41.7 ℃, the 7d flexural strength of 9.8-10.4MPa, the 7d compressive strength of 28.4-29.0MPa, the 28d flexural strength of 16.7-17.1MPa, the 28d compressive strength of 47.2-48.0MPa and the seepage pressure of 0.79-0.82 MPa;
(4) According to the preparation method of the phase change thermal insulation mortar for the greenhouse wall, the modifier is added in the primary mixing step, so that the surface modification can be performed on the microcapsule phase change material, the surface strength of the microcapsule phase change material is improved, and the microcapsule phase change material is prevented from leaking at high temperature; and after standing the prepared phase-change thermal insulation mortar for the greenhouse wall at 60 ℃ for 10 hours, the phase-change temperature is 41.2-42.0 ℃, the 7d compressive strength is 10.0-10.5MPa, the 7d compressive strength is 28.4-29.2MPa, the 28d compressive strength is 17.0-17.5MPa, the 28d compressive strength is 47.5-48.1MPa, and the impervious pressure is 0.80-0.84 MPa.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.
Example 1
A preparation method of phase change thermal insulation mortar for greenhouse walls comprises the following steps:
1. primary mixing: mixing a microcapsule phase change material, a modifier, sodium dodecyl benzene sulfonate, polyethylene glycol 400 and zinc oxide, adding into a reaction kettle, vacuumizing the reaction kettle to 200Pa, controlling the temperature of the reaction kettle to 40 ℃, controlling the stirring speed to 200rpm, and stirring for 30min to obtain a primary mixture;
Wherein the weight ratio of the microcapsule phase change material to the modifier to the sodium dodecyl benzene sulfonate to the polyethylene glycol 400 to the zinc oxide is 70:5:4:8: 5;
the preparation method of the microcapsule phase change material comprises the following steps: uniformly mixing high-density polyethylene and paraffin, heating to 140 ℃ at a heating rate of 2.5 ℃/min, keeping the temperature and standing at 140 ℃ for 30min, stirring at a stirring speed of 280rpm for 10min, adding stearic acid and zinc stearate, continuously stirring at a stirring speed of 280rpm for 20min, cooling to 80 ℃ at a cooling rate of 3 ℃/min, keeping the temperature and standing at 80 ℃ for 30min, cooling to room temperature at a cooling rate of 3 ℃/min, carrying out solidification molding at room temperature, and after solidification molding, adding the mixture into a pulverizer and pulverizing to a particle size of 150 mu m to obtain a microcapsule phase change material;
wherein the weight ratio of the high-density polyethylene to the paraffin wax to the stearic acid to the zinc stearate is 30:18:3: 1;
the density of the high-density polyethylene is 0.941g/cm3。
The preparation method of the modifier comprises the following steps: placing sucrose, xanthan gum, re-dispersible latex powder and polyvinyl alcohol 2488 into a ball mill for ball milling, controlling the ball-material ratio during ball milling to be 10:1, the temperature to be 45 ℃, the rotating speed to be 300rpm, and the time to be 40min, and obtaining the modifier after ball milling;
Wherein the weight ratio of the sucrose to the xanthan gum to the re-dispersible latex powder to the polyvinyl alcohol 2488 is 2:10:15: 5.
2. And (3) secondary mixing: adding the primary mixture, expanded perlite, nano boron nitride, modified fly ash and calcium stearate into a stirring kettle, controlling the rotating speed of the stirring kettle to be 180rpm, and stirring for 40min to obtain a secondary mixture;
wherein the weight ratio of the primary mixture to the expanded perlite to the nano boron nitride to the modified fly ash to the calcium stearate is 100:40:1:8: 2;
the bulk density of the expanded perlite is 45kg/m3The average grain diameter is 2.5 mm;
the particle size of the nano boron nitride is 200 nm;
the preparation method of the modified fly ash comprises the following steps: adding fly ash, barium stearate and sodium hexametaphosphate into a reaction kettle, vacuumizing the reaction kettle until the vacuum degree is 100Pa, introducing mixed gas into the reaction kettle until the gas pressure is 0.12MPa, controlling the temperature of the reaction kettle to be 150 ℃, starting stirring, controlling the stirring speed to be 150rpm, and stirring for 40min to obtain modified fly ash;
wherein the weight ratio of the fly ash, the barium stearate and the sodium hexametaphosphate is 35:4: 2;
the mixed gas is a mixed gas of ammonia gas and nitrogen gas, wherein the volume ratio of the ammonia gas to the nitrogen gas is 3: 4.
3. Mixing for three times: adding the secondary mixture, fine sand, steel slag powder, ordinary portland cement, vitrified micro bubbles, sodium lignin sulfonate and sodium alginate into a stirring kettle, controlling the rotating speed of the stirring kettle to be 200rpm, and stirring for 50min to obtain a tertiary mixture;
wherein the weight ratio of the secondary mixture, the fine sand, the steel slag powder, the ordinary portland cement, the vitrified micro bubbles, the sodium lignin sulfonate and the sodium alginate is 60:15:7:25:8:2: 3;
the ordinary portland cement is P.O42.5 portland cement.
4. And (3) post-treatment: adding the tertiary mixture into a reaction kettle, fumigating the tertiary mixture by using steam of a mixed solution, namely steam generated under saturated steam pressure, drying at 40 ℃ after the fumigation is finished to obtain dry sand, adding water into the dry sand, and uniformly mixing to obtain the greenhouse wall heat-preservation mortar;
the mixed solution is a mixed solution of absolute ethyl alcohol and dichloromethane, wherein the weight ratio of the absolute ethyl alcohol to the dichloromethane is 1: 2;
the weight ratio of the third mixture to the mixed solution is 10: 1;
the weight ratio of the dry sand to the water is 100: 40.
Example 2
A preparation method of phase change thermal insulation mortar for greenhouse walls comprises the following steps:
1. Primary mixing: mixing a microcapsule phase change material, a modifier, sodium dodecyl benzene sulfonate, polyethylene glycol 400 and zinc oxide, adding into a reaction kettle, vacuumizing the reaction kettle to 250Pa, controlling the temperature of the reaction kettle to 42 ℃, controlling the stirring speed to 220rpm, and stirring for 32min to obtain a primary mixture;
wherein the weight ratio of the microcapsule phase change material to the modifier to the sodium dodecyl benzene sulfonate to the polyethylene glycol 400 to the zinc oxide is 72:6:5:9: 6;
the preparation method of the microcapsule phase change material comprises the following steps: uniformly mixing high-density polyethylene and paraffin, heating to 141 ℃ at a heating rate of 2.7 ℃/min, keeping the temperature at 141 ℃, standing for 32min, stirring for 12min at a stirring speed of 290rpm, adding stearic acid and zinc stearate, continuously stirring for 22min at a stirring speed of 290rpm, cooling to 82 ℃ at a cooling rate of 3.5 ℃/min, keeping the temperature, standing for 32min at 82 ℃, cooling to room temperature at a cooling rate of 3.5 ℃/min, solidifying and forming at room temperature, after solidification and forming, adding the mixture into a crusher, and crushing to a particle size of 170 mu m to obtain a microcapsule phase change material;
wherein the weight ratio of the high-density polyethylene to the paraffin to the stearic acid to the zinc stearate is 31:19:4: 2;
The density of the high-density polyethylene is 0.950g/cm3。
The preparation method of the modifier comprises the following steps: placing sucrose, xanthan gum, re-dispersible latex powder and polyvinyl alcohol 2488 into a ball mill for ball milling, controlling the ball-material ratio in the ball milling process to be 12:1, the temperature to be 47 ℃, the rotating speed to be 320rpm, and the time to be 42min, and obtaining the modifier after the ball milling is finished;
wherein the weight ratio of the sucrose to the xanthan gum to the re-dispersible latex powder to the polyvinyl alcohol 2488 is 3:11:16: 6.
2. And (3) secondary mixing: adding the primary mixture, expanded perlite, nano boron nitride, modified fly ash and calcium stearate into a stirring kettle, controlling the rotating speed of the stirring kettle to be 190rpm, and stirring for 42min to obtain a secondary mixture;
wherein the weight ratio of the primary mixture to the expanded perlite to the nano boron nitride to the modified fly ash to the calcium stearate is 105:42:1.1:9: 3;
the bulk density of the expanded perlite is 47kg/m3The average grain diameter is 2.7 mm;
the particle size of the nano boron nitride is 300 nm;
the preparation method of the modified fly ash comprises the following steps: adding the fly ash, barium stearate and sodium hexametaphosphate into a reaction kettle, vacuumizing the reaction kettle until the vacuum degree is 120Pa, introducing mixed gas into the reaction kettle until the gas pressure is 0.13MPa, controlling the temperature of the reaction kettle to 155 ℃, starting stirring, controlling the stirring speed to 170rpm, and stirring for 45min to obtain modified fly ash;
Wherein the weight ratio of the fly ash, the barium stearate and the sodium hexametaphosphate is 37:5: 3;
the mixed gas is a mixed gas of ammonia gas and nitrogen gas, wherein the volume ratio of the ammonia gas to the nitrogen gas is 3: 4.5.
3. Mixing for three times: adding the secondary mixture, fine sand, steel slag powder, ordinary portland cement, vitrified micro bubbles, sodium lignin sulfonate and sodium alginate into a stirring kettle, controlling the rotating speed of the stirring kettle to be 210rpm, and stirring for 52min to obtain a tertiary mixture;
wherein the weight ratio of the secondary mixture, the fine sand, the steel slag powder, the ordinary portland cement, the vitrified micro bubbles, the sodium lignin sulfonate and the sodium alginate is 62:17:8:27:9:3: 4;
the ordinary portland cement is P.O42.5 portland cement.
4. And (3) post-treatment: adding the tertiary mixture into a reaction kettle, fumigating the tertiary mixture by using steam of a mixed solution, namely steam generated under saturated steam pressure, drying at 42 ℃ after the fumigation is finished to obtain dry sand, adding water into the dry sand, and uniformly mixing to obtain the greenhouse wall heat-preservation mortar;
the mixed solution is a mixed solution of absolute ethyl alcohol and dichloromethane, wherein the weight ratio of the absolute ethyl alcohol to the dichloromethane is 1: 2.5;
The weight ratio of the third mixture to the mixed solution is 10: 1.1;
the weight ratio of the dry sand to the water is 100: 42.
Example 3
A preparation method of phase change thermal insulation mortar for greenhouse walls comprises the following steps:
1. primary mixing: mixing a microcapsule phase change material, a modifier, sodium dodecyl benzene sulfonate, polyethylene glycol 400 and zinc oxide, adding the mixture into a reaction kettle, vacuumizing the reaction kettle to 300Pa, controlling the temperature of the reaction kettle to 45 ℃, controlling the stirring speed to 250rpm, and stirring for 35min to obtain a primary mixture;
wherein the weight ratio of the microcapsule phase change material to the modifier to the sodium dodecyl benzene sulfonate to the polyethylene glycol 400 to the zinc oxide is 75:7:6:10: 7;
the preparation method of the microcapsule phase change material comprises the following steps: uniformly mixing high-density polyethylene and paraffin, heating to 142 ℃ at a heating rate of 3 ℃/min, keeping the temperature and standing at 142 ℃ for 35min, stirring at a stirring speed of 300rpm for 15min, adding stearic acid and zinc stearate, continuously stirring at a stirring speed of 300rpm for 25min, cooling to 85 ℃ at a cooling speed of 4 ℃/min, keeping the temperature and standing at 85 ℃ for 35min, cooling to room temperature at a cooling speed of 4 ℃/min, performing solidification molding at room temperature, and after solidification molding, adding into a pulverizer and pulverizing to a particle size of 200 mu m to obtain a microcapsule phase change material;
Wherein the weight ratio of the high-density polyethylene to the paraffin wax to the stearic acid to the zinc stearate is 32:20:5: 3;
the density of the high-density polyethylene is 0.960g/cm3。
The preparation method of the modifier comprises the following steps: placing sucrose, xanthan gum, re-dispersible latex powder and polyvinyl alcohol 2488 into a ball mill for ball milling, controlling the ball-material ratio during ball milling to be 15:1, the temperature to be 50 ℃, the rotating speed to be 350rpm, and the time to be 45min, and obtaining the modifier after ball milling;
wherein the weight ratio of the sucrose to the xanthan gum to the re-dispersible latex powder to the polyvinyl alcohol 2488 is 4:12:18: 8.
2. And (3) secondary mixing: adding the primary mixture, expanded perlite, nano boron nitride, modified fly ash and calcium stearate into a stirring kettle, controlling the rotating speed of the stirring kettle to be 200rpm, and stirring for 45min to obtain a secondary mixture;
wherein the weight ratio of the primary mixture to the expanded perlite to the nano boron nitride to the modified fly ash to the calcium stearate is 110:45:2:10: 4;
the bulk density of the expanded perlite is 50kg/m3The average grain diameter is 3 mm;
the particle size of the nano boron nitride is 400 nm;
the preparation method of the modified fly ash comprises the following steps: adding the fly ash, barium stearate and sodium hexametaphosphate into a reaction kettle, vacuumizing the reaction kettle until the vacuum degree is 150Pa, introducing mixed gas into the reaction kettle until the gas pressure is 0.15MPa, controlling the temperature of the reaction kettle to 160 ℃, starting stirring, controlling the stirring speed to 200rpm, and stirring for 50min to obtain modified fly ash;
Wherein the weight ratio of the fly ash to the barium stearate to the sodium hexametaphosphate is 40:6: 5;
the mixed gas is a mixed gas of ammonia gas and nitrogen gas, wherein the volume ratio of the ammonia gas to the nitrogen gas is 3: 5.
3. Mixing for three times: adding the secondary mixture, fine sand, steel slag powder, ordinary portland cement, vitrified micro bubbles, sodium lignin sulfonate and sodium alginate into a stirring kettle, controlling the rotating speed of the stirring kettle to be 220rpm, and stirring for 55min to obtain a tertiary mixture;
wherein the weight ratio of the secondary mixture, the fine sand, the steel slag powder, the ordinary portland cement, the vitrified micro bubbles, the sodium lignin sulfonate and the sodium alginate is 65:20:9:30:10:4: 5;
the ordinary portland cement is P.O42.5 portland cement.
4. And (3) post-treatment: adding the tertiary mixture into a reaction kettle, fumigating the tertiary mixture by using steam of a mixed solution, namely steam generated under saturated steam pressure, drying at 45 ℃ after the fumigation is finished to obtain dry sand, adding water into the dry sand, and uniformly mixing to obtain the greenhouse wall heat-preservation mortar;
the mixed solution is a mixed solution of absolute ethyl alcohol and dichloromethane, wherein the weight ratio of the absolute ethyl alcohol to the dichloromethane is 1: 3;
The weight ratio of the mixture obtained in the third step to the mixed solution is 10: 1.2;
the weight ratio of the dry sand to the water is 100: 45.
Comparative example 1
The preparation method of the phase-change thermal insulation mortar for greenhouse walls in the embodiment 1 is characterized by comprising the following steps: the addition of the modifier in the first mixing step of step 1 was omitted.
Comparative example 2
The preparation method of the phase change thermal insulation mortar for the greenhouse wall in the embodiment 1 is adopted, and the difference is that: in the second mixing step of the step 2, fly ash is used for replacing modified fly ash.
Comparative example 3
The preparation method of the phase change thermal insulation mortar for the greenhouse wall in the embodiment 1 is adopted, and the difference is that: and (4) omitting the post-treatment step, namely directly taking the tertiary mixture as the phase-change thermal insulation mortar for the greenhouse wall.
Test example 1
The phase change temperature, the phase change latent heat and the specific heat capacity of the phase change thermal insulation mortar for the greenhouse walls prepared in the examples 1 to 3 and the comparative examples 1 to 3 are tested according to the JC/T2111 to 2012 standard, and the test results are as follows:
Figure 67623DEST_PATH_IMAGE001
test example 2
The phase change thermal insulation mortar for greenhouse walls prepared in examples 1-3 and comparative examples 1-3 is tested for 7d flexural strength, 7d compressive strength, 28d flexural strength, 28d compressive strength and impermeability strength according to JGJ/T70-2009, and the test results are as follows:
Figure 578239DEST_PATH_IMAGE002
Test example 3
The phase change thermal insulation mortar for greenhouse walls prepared in examples 1 to 3 and comparative examples 1 to 3 were subjected to a durability test, and the test method and results were as follows:
the phase change thermal insulation mortar for greenhouse walls prepared in examples 1-3 and comparative examples 1-3 are respectively subjected to freeze thawing circulation, specifically, after standing for 12h at-25 ℃, standing for 12h at 25 ℃, and then repeating the freeze thawing circulation for 50 times, phase change temperature, 7d flexural strength, 7d compressive strength, 28d flexural strength, 28d compressive strength and impermeability strength are tested, and the test results are as follows:
Figure 92397DEST_PATH_IMAGE003
test example 4
The phase change thermal insulation mortar for greenhouse walls prepared in examples 1 to 3 and comparative examples 1 to 3 was subjected to a thermal stability test, and the test method and results were as follows:
the phase change thermal insulation mortar for greenhouse walls prepared in examples 1 to 3 and comparative examples 1 to 3 is placed at 60 ℃ for standing for 10 hours, and tested for phase change temperature, 7d flexural strength, 7d compressive strength, 28d flexural strength, 28d compressive strength and impermeability, and the test results are as follows:
Figure 956448DEST_PATH_IMAGE004
all percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. The preparation method of the phase change thermal insulation mortar for the greenhouse wall is characterized by comprising the following steps: primary mixing, secondary mixing, tertiary mixing and post-treatment;
the primary mixing method comprises the steps of mixing the microcapsule phase change material, the modifier, the sodium dodecyl benzene sulfonate, the polyethylene glycol 400 and the zinc oxide, adding the mixture into a reaction kettle, vacuumizing the reaction kettle to 200-45 ℃ under the pressure of 300Pa, controlling the temperature of the reaction kettle to 40-45 ℃, controlling the stirring speed to 200-250rpm, and stirring for 30-35min to obtain a primary mixture;
in the primary mixing, the weight ratio of the microcapsule phase change material, the modifier, the sodium dodecyl benzene sulfonate, the polyethylene glycol 400 and the zinc oxide is 70-75:5-7:4-6:8-10: 5-7;
in the primary mixing, the preparation method of the microcapsule phase change material comprises the steps of mixing the high-density polyethylene and the paraffin uniformly, heating to 140-142 ℃ at a heating rate of 2.5-3 ℃/min, standing at 140-, then adding stearic acid and zinc stearate, continuing stirring at the stirring speed of 280-300rpm for 20-25min, then cooling to 80-85 ℃ at a cooling rate of 3-4 ℃/min, standing at 80-85 deg.C for 30-35min, cooling to room temperature at a rate of 3-4 deg.C/min, carrying out solidification molding at room temperature, adding the mixture into a crusher after solidification molding, and crushing the mixture to a particle size of 150-200 mu m to obtain a microcapsule phase change material;
In the primary mixing, in the preparation of the microcapsule phase change material, the weight ratio of the high-density polyethylene to the paraffin wax to the stearic acid to the zinc stearate is 30-32:18-20:3-5: 1-3;
in the primary mixing, the preparation method of the modifier comprises the steps of placing the sucrose, the xanthan gum, the re-dispersible emulsion powder and the polyvinyl alcohol 2488 into a ball mill for ball milling, controlling the ball-material ratio during ball milling to be 10-15:1, the temperature to be 45-50 ℃, the rotating speed to be 300-350rpm and the time to be 40-45min, and obtaining the modifier after the ball milling is finished;
in the primary mixing, in the preparation of the modifier, the weight ratio of the sucrose to the xanthan gum to the re-dispersible latex powder to the polyvinyl alcohol 2488 is 2-4:10-12:15-18: 5-8;
the secondary mixing method comprises the steps of adding the primary mixture, the expanded perlite, the nano boron nitride, the modified fly ash and the calcium stearate into a stirring kettle, controlling the rotating speed of the stirring kettle to be 180-year 200rpm, and stirring for 40-45min to obtain a secondary mixture;
in the secondary mixing, the bulk density of the expanded perlite is 45-50kg/m3The average grain diameter is 2.5-3 mm;
in the secondary mixing, the weight ratio of the primary mixture, the expanded perlite, the nano boron nitride, the modified fly ash and the calcium stearate is 110:40-45:1-2:8-10: 2-4;
In the secondary mixing, the preparation method of the modified fly ash comprises the following steps: adding the fly ash, barium stearate and sodium hexametaphosphate into a reaction kettle, vacuumizing the reaction kettle until the vacuum degree is 100-150Pa, introducing mixed gas into the reaction kettle until the gas pressure is 0.12-0.15MPa, controlling the temperature of the reaction kettle to 150-160 ℃, starting stirring, controlling the stirring speed to 150-200rpm, and stirring for 40-50min to obtain modified fly ash;
in the secondary mixing, in the preparation of the modified fly ash, the weight ratio of the fly ash to the barium stearate to the sodium hexametaphosphate is 35-40:4-6: 2-5;
in the secondary mixing, the mixed gas is the mixed gas of ammonia and nitrogen, wherein the volume ratio of the ammonia to the nitrogen is 3: 4-5;
the third mixing method comprises the steps of adding the secondary mixture, fine sand, steel slag powder, ordinary portland cement, vitrified micro bubbles, sodium lignin sulfonate and sodium alginate into a stirring kettle, controlling the rotating speed of the stirring kettle to be 200-220rpm, and stirring for 50-55min to obtain a third mixture;
in the third mixing, the weight ratio of the secondary mixture, the fine sand, the steel slag powder, the ordinary portland cement, the vitrified micro bubbles, the sodium lignin sulfonate and the sodium alginate is 60-65:15-20:7-9:25-30:8-10:2-4: 3-5;
Adding the tertiary mixture into a reaction kettle, fumigating the tertiary mixture by using steam of mixed solution, wherein the steam of the mixed solution is generated under saturated steam pressure, drying at 40-45 ℃ after fumigating is finished to obtain dry sand, and adding water into the dry sand and uniformly mixing to obtain the thermal insulation mortar for the wall of the greenhouse;
in the post-treatment, the mixed solution is a mixed solution of absolute ethyl alcohol and dichloromethane, wherein the weight ratio of the absolute ethyl alcohol to the dichloromethane is 1: 2-3;
in the post-treatment, the weight ratio of the mixture obtained in the third step to the mixed solution is 10: 1-1.2;
in the post-treatment, the weight ratio of the dry sand to the water is 100: 40-45.
2. The method for preparing phase-change thermal mortar for greenhouse walls according to claim 1, wherein in the first mixing, the density of the high-density polyethylene in the preparation of the microcapsule phase-change material is 0.941 to 0.960g/cm3。
3. The preparation method of the phase-change thermal mortar for greenhouse walls as claimed in claim 1, wherein the particle size of the nano boron nitride in the secondary mixing is 200-400 nm.
4. The method for preparing the phase-change thermal mortar for greenhouse walls according to claim 1, wherein in the third mixing, the ordinary portland cement is p.o42.5 portland cement.
5. Phase change thermal insulation mortar for greenhouse walls, which is characterized by being prepared by the preparation method of the phase change thermal insulation mortar for greenhouse walls as claimed in any one of claims 1 to 4.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101838520A (en) * 2010-04-28 2010-09-22 清华大学深圳研究生院 Preparation method of composition containing phase-change and energy-storage micro-capsules
CN102070845A (en) * 2010-12-24 2011-05-25 金发科技股份有限公司 Phase change energy storage thermoplastic composite material and preparation method thereof
WO2012073258A2 (en) * 2010-11-30 2012-06-07 Pradeep Vasant Joshi A composition suitable for use in building construction

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101838520A (en) * 2010-04-28 2010-09-22 清华大学深圳研究生院 Preparation method of composition containing phase-change and energy-storage micro-capsules
WO2012073258A2 (en) * 2010-11-30 2012-06-07 Pradeep Vasant Joshi A composition suitable for use in building construction
CN102070845A (en) * 2010-12-24 2011-05-25 金发科技股份有限公司 Phase change energy storage thermoplastic composite material and preparation method thereof

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