CN113185218B - Phase-change microcapsule material, preparation method thereof and composite phase-change insulation board - Google Patents

Phase-change microcapsule material, preparation method thereof and composite phase-change insulation board Download PDF

Info

Publication number
CN113185218B
CN113185218B CN202110438327.7A CN202110438327A CN113185218B CN 113185218 B CN113185218 B CN 113185218B CN 202110438327 A CN202110438327 A CN 202110438327A CN 113185218 B CN113185218 B CN 113185218B
Authority
CN
China
Prior art keywords
phase
phase change
change
microcapsule
change microcapsule
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202110438327.7A
Other languages
Chinese (zh)
Other versions
CN113185218A (en
Inventor
刘晓丽
唐振中
李朗
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangdong Bozhilin Robot Co Ltd
Original Assignee
Guangdong Bozhilin Robot Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangdong Bozhilin Robot Co Ltd filed Critical Guangdong Bozhilin Robot Co Ltd
Priority to CN202110438327.7A priority Critical patent/CN113185218B/en
Publication of CN113185218A publication Critical patent/CN113185218A/en
Application granted granted Critical
Publication of CN113185218B publication Critical patent/CN113185218B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • 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
    • C04B28/06—Aluminous 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
    • 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
    • C04B28/24—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 alkyl, ammonium or metal silicates; containing silica sols
    • C04B28/26—Silicates of the alkali metals
    • 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
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/14—Thermal energy storage

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

The invention relates to the technical field of building materials, in particular to a phase change microcapsule material, a preparation method thereof and a composite phase change insulation board. The preparation method of the phase-change microcapsule material comprises the following steps: 1) taking a phase-change material, granulating and preparing phase-change material particles; 2) utilizing gas to enable the phase change material particles to be in a solid fluidized state, enabling the temperature to reach the phase change temperature of the phase change material, and introducing an inorganic gel material to enable the inorganic gel material to coat the phase change material particles to prepare a phase change microcapsule intermediate; 3) hydrating the phase change microcapsule intermediate. The invention creatively utilizes the fluidized bed to prepare the phase-change microcapsule material, and solves the problems that the types of the wall materials of the existing microcapsules are limited and the mechanical properties of the heat-insulation products are seriously deteriorated.

Description

Phase-change microcapsule material, preparation method thereof and composite phase-change insulation board
Technical Field
The invention relates to the technical field of building materials, in particular to a phase-change microcapsule material, a preparation method thereof and a composite phase-change insulation board.
Background
Phase Change Material-PCM (Phase Change Material-PCM) refers to a substance that changes form with temperature and can provide latent heat. The phase-change material can absorb heat to store the phase-change material in a phase-change latent heat mode when the temperature is high, and then releases the absorbed heat when the temperature is low, so that the energy can be transferred among different vacant positions, the contradiction between energy supply and demand can be relieved, and the energy consumption can be effectively reduced. While maintaining the temperature within a relatively stable temperature range. Therefore, the house built by the phase-change material can form a permanent constant-temperature air-conditioning room, can greatly reduce the energy consumption required by refrigeration/heating in the building, and has the energy-saving effect far superior to the traditional heat-insulating material. At present, the application of the phase-change material in the building field as a novel energy-saving material is rapidly developed. Thermal energy storage by means of phase change materials is an important research area.
General phase change insulation material is solid-liquid phase transition type, and its low price is easily obtained, the phase transition enthalpy is high, phase transition in-process volume change is little, but if not through cladding and direct application, can take place to reveal at the in-process of heat absorption phase transition, and most organic phase change material heat conductivity is low, and is flammable, and most inorganic phase change material has stronger corrosivity, can destroy the storage container. Therefore, phase change materials are not suitable for direct incorporation into building materials. Microencapsulation of phase change materials has been reported. The application problem of the phase-change material in the building material can be effectively solved through microencapsulation treatment. Traditionally, the phase change microcapsule material is mainly prepared by hydrolysis deposition of silicon dioxide or polymerization process of polymer wall material, so at present, the phase change microcapsule material using silicon dioxide and polymer material as shell is common. However, the phase-change microcapsule materials have the limitations that the types of wall materials are limited, and microcapsules of cement-based or other inorganic gel material wall materials cannot be prepared, and the phase-change microcapsule materials seriously deteriorate the mechanical properties of heat insulation products. There is therefore a continuing need to develop new phase change microcapsule materials.
Disclosure of Invention
Based on the above, the invention provides a preparation method of a phase change microcapsule material, which creatively utilizes a fluidized bed to prepare the phase change microcapsule material and solves the problems that the type of the existing microcapsule wall material is limited and the mechanical property of a heat insulation product is seriously deteriorated.
The preparation method of the phase-change microcapsule material comprises the following steps:
1) taking a phase-change material, granulating and preparing phase-change material particles;
2) utilizing gas to enable the phase change material particles to be in a solid fluidization state, enabling the temperature to reach the phase change temperature of the phase change material, and introducing an inorganic gel material to enable the inorganic gel material to coat the phase change material particles to prepare a phase change microcapsule intermediate;
3) hydrating the phase change microcapsule intermediate.
In one embodiment, the inorganic gel material is passed for a period of time ranging from 15min to 120 min. Ensuring that the inorganic gel material can fully and uniformly coat the phase change material particles, and if the time exceeds 120min, the phase change material particles can be completely melted to form a mixture instead of microcapsules.
In one embodiment, the method for hydrating the phase change microcapsule intermediate is as follows: and (3) utilizing water vapor to enable the phase change microcapsule intermediate to be in a solid fluidization state, enabling the temperature to be 1-5 ℃ lower than the phase change temperature of the phase change material, continuously introducing the water vapor, and hydrating for 10-70 min. Preferably, continuous convection is formed between the water vapor in the bin and the phase change microcapsule intermediate, so that the hydration and hardening of the wall material of the phase change microcapsule intermediate are completed.
In one embodiment, the volume ratio of the phase change material particles to the inorganic gel material is 1 (0.3-0.9). The wall thickness of the microcapsule can be controlled by controlling the volume ratio of the two, and the inorganic gel material can be ensured to completely coat the phase change material particles within the range, and the wall thickness is proper.
In one embodiment, the phase change material is selected from one or more of n-dodecane, n-pentadecane, n-hexadecane, n-octadecane, n-nonadecane, n-eicosane, n-docosane, paraffin, and natural cocoa fatty acid mixtures. The phase-change material of the phase-change material is generally between 10 and 90 ℃, and the phase-change temperature of the specific microcapsule can be designed according to the use requirement.
In one embodiment, the inorganic gelling material comprises one or a combination of cement-based gelling materials, admixtures and alkali-activated gelling materials.
In one embodiment, the cement-based gelling material is selected from one or a combination of portland cement, aluminate cement, sulphoaluminate cement, and pozzolanic cement.
In one embodiment, the admixture is selected from one or more of fly ash, water glass powder, mineral powder, silica fume and metakaolin.
In one embodiment, the inorganic gel material further comprises an additive.
In one embodiment, the admixture is selected from one or a combination of two of lignin glue powder and re-dispersible latex powder.
In one embodiment, the gas is hot air.
In one embodiment, the method further comprises the steps of wetting the phase change microcapsule intermediate after hydration, and then repeating the steps 2) and 3)1-3 times. The method can achieve the aims of increasing the compactness and the thickening of the microcapsule wall material and improving the strength of the microcapsule. The number of repetitions depends on the particular requirements.
In one embodiment, the method further comprises the step of drying to prepare the phase-change microcapsule.
The invention also provides a phase change microcapsule material prepared by the preparation method. Can have better compatibility with inorganic cementing materials such as concrete and the like.
The invention also provides a composite phase-change insulation board which comprises the phase-change microcapsule material. The phase change microcapsule material is used in the composite phase change insulation board, the indoor temperature can be regulated and controlled through phase change energy storage, and the shell layer strength of the phase change microcapsule prepared by the method is high, so that the prepared composite phase change insulation board has small influence on the strength of the composite phase change insulation board, has good mechanical property, and has the potential of realizing structure-insulation integration.
Compared with the prior art, the invention has the following beneficial effects:
generally, a fluidized bed is mainly used for drying and granulating products such as medicines, fertilizers and the like, the invention utilizes the fluidized bed technology to enable phase change material particles to be in a solid fluidized state and reach the phase change temperature of the phase change material, then inorganic gel materials are introduced to complete coating, and then hydration is carried out, so that the preparation of phase change microcapsules of cement-based or other inorganic gel material wall materials can be realized, and the problem that the types of the existing microcapsule wall materials are limited is solved. In addition, the method can also effectively control the particle size and the particle size distribution of the microcapsule, prepare the microcapsule with higher shell hardness, and ensure that the microcapsule prepared by the method has better compatibility with inorganic cementing materials such as concrete and the like.
The phase-change microcapsule material prepared by the method is used in a heat-insulation product, the indoor temperature can be regulated and controlled through phase-change energy storage, and the shell layer of the phase-change microcapsule prepared by the method has high strength, so that the prepared heat-insulation product has small influence on the strength of the heat-insulation product, has good mechanical property and has the potential of realizing integration of structure and heat insulation.
Drawings
FIG. 1 is a schematic view of a process for preparing a phase-change microcapsule material;
FIG. 2 is a schematic view of each bin of a fluidized bed reactor.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Generally speaking, fluidized beds are mostly used for drying and granulating products such as medicines, chemical fertilizers and the like, and the invention prepares the phase-change microcapsule material by utilizing the fluidized bed technology.
Referring to fig. 1, a schematic flow chart of the preparation of the phase-change microcapsule material is shown. In the step 1), the phase-change material is granulated to prepare the phase-change material particles, understandably, the granulation process can be carried out in a bin of a fluidized bed reactor, as shown in fig. 2, the phase-change material is added into a fluidized bed granulation bin 1 and granulated by a spray gun, and the cooling temperature is-5 ℃ to 10 ℃ to prepare the phase-change material particles.
Preferably, the phase change material is selected from one or more of n-dodecane, n-pentadecane, n-hexadecane, n-octadecane, n-nonadecane, n-eicosane, n-docosane, paraffin and natural cocoa fatty acid mixture.
The phase-change material of the phase-change material is generally between 10 and 90 ℃, and the phase-change temperature of the specific microcapsule can be designed according to the use requirement.
It will be appreciated that after granulation, the phase change material granules may also be screened, preferably with phase change material particles less than 106 microns in size, for the next step.
Step 2) can also be carried out in a bin of a fluidized bed reactor, the phase-change material particles prepared in step 1) are sent into a fluidized bed particle coating bin 2, preferably, dry hot air is introduced to enable the phase-change material particles to be in a solid fluidized state, the temperature is enabled to reach the phase-change temperature of the phase-change material, and an inorganic gel material is introduced to enable the phase-change material particles to be coated by the inorganic gel material, so that the phase-change microcapsule intermediate is prepared.
It is understood that both the phase change material particles prepared in step 1) and the inorganic gel material can be fed into the bin 2 by the airflow. The gas flow may be generated by a blowing device on the fluidized bed.
Preferably, the flowing direction of the inorganic gel material is perpendicular to the flowing direction of the phase change material particles.
Preferably, the time for introducing the inorganic gel material is 15min to 120min, so that the inorganic gel material can sufficiently and uniformly coat the phase change material particles, and if the time exceeds 120min, the phase change material particles can be completely melted to form a mixture instead of microcapsules.
Preferably, the volume ratio of the phase change material particles to the inorganic gel material is 1 (0.3-0.9). The wall thickness of the microcapsule can be controlled by controlling the volume ratio of the two, and the inorganic gel material can be ensured to completely coat the phase change material particles within the range, and the wall thickness is proper.
Preferably, the inorganic gel material comprises one or more of a cement-based gel material, an admixture and an alkali-activated gel material.
Preferably, the cement-based gelling material is selected from one or a combination of more of portland cement, aluminate cement, sulphoaluminate cement and pozzolan cement.
Preferably, the admixture is selected from one or more of fly ash, water glass powder, mineral powder, silica fume and metakaolin.
Preferably, the inorganic gel material further comprises an additive.
Preferably, the additive is selected from one or a combination of two of lignin glue powder and re-dispersible latex powder.
And 3) the step can also be carried out in a bin of a fluidized bed reactor, the phase change microcapsule intermediate prepared in the step 2) is sent into a fluidized bed wall material hydration bin 3, water vapor is utilized to enable the phase change microcapsule intermediate to be in a solid fluidized state, the temperature is 1-5 ℃ lower than the phase change temperature of the phase change material, the temperature range is the highest hydration temperature for ensuring that the phase change material is not molten, and the rapid hydration of the inorganic material can be ensured. And (3) continuously introducing the water vapor, hydrating for 10-70 min, preferably enabling the water vapor in the bin and the phase change microcapsule intermediate to form continuous convection, and completing hydration hardening of the phase change microcapsule intermediate wall material.
If further encapsulation is needed to make the microcapsule wall material more compact, step 4) can be executed, step 4) can be continuously carried out in the fluidized bed chamber 3 in step 3), and after the hydration step in step 3) is completed, water vapor is continuously introduced for 3min-10min to wet the hydrated phase-change microcapsule intermediate.
After the microcapsule is wetted, the step 2) and the step 3) are repeated for 1 to 3 times, so that the aims of increasing the compactness and the thickening of the wall material of the microcapsule are fulfilled, and the strength of the microcapsule is improved. The number of repetitions depends on the particular requirements.
After the steps are finished, drying the product obtained in the step 3) to prepare the phase-change microcapsule. The step can be carried out in a drying bin of the fluidized bed, and understandably, the drying temperature does not exceed the phase-change temperature of the phase-change material, and the dried phase-change material is subpackaged for standby.
The fluidized bed can be provided with a granulation bin, a particle coating bin and a wall material hydration bin which are relatively independent and continuous, all the steps can be realized on the fluidized bed, so that the microcapsules can be formed in the fluidized bed at one time.
The invention can realize the preparation of the phase-change microcapsule of the wall material of the cement-based or other inorganic gel materials by utilizing the fluidized bed technology, and solves the problem that the types of the wall materials of the existing microcapsule are limited. In addition, the method can also effectively control the particle size and the particle size distribution of the microcapsule, prepare the microcapsule with higher shell hardness, and ensure that the microcapsule prepared by the method has better compatibility with inorganic cementing materials such as concrete and the like.
A phase change microcapsule material is prepared by the preparation method of the phase change microcapsule material. Can have better compatibility with inorganic cementing materials such as concrete and the like.
A composite phase-change insulation board comprises the phase-change microcapsule material.
The phase change microcapsule material is used in the composite phase change insulation board, the indoor temperature can be regulated and controlled through phase change energy storage, and the shell layer strength of the phase change microcapsule prepared by the method is high, so that the prepared composite phase change insulation board has small influence on the strength of the composite phase change insulation board, has good mechanical property, and has the potential of realizing structure-insulation integration.
Preferably, the phase change microcapsule material accounts for 5-30% of the total mass of the composite phase change insulation board.
The heat-insulating composite phase-change heat-insulating plate is manufactured according to a conventional processing and manufacturing method, and can also be used in the forms of heat-insulating mortar containing phase-change microcapsule materials, heat-insulating coagulation and the like.
The following examples and comparative examples are further described below, and the starting materials used in the following examples can be commercially available, unless otherwise specified, and the equipment used therein can be commercially available, unless otherwise specified.
The commercially available vitrified microsphere inorganic thermal insulation mortar powder is purchased from Qingmei building materials and is high-strength vitrified microsphere inorganic thermal insulation mortar powder.
Example 1
The embodiment provides a phase change microcapsule material and a preparation method thereof, and a composite phase change insulation board and a preparation method thereof, wherein the preparation method comprises the following steps:
preparation of phase-change microcapsule material
And adding paraffin with the phase change temperature of 45 ℃ into a granulation bin of the fluidized bed, and granulating by cooling with a spray gun at the cooling temperature of 40 ℃ to prepare phase change material particles. Passing the phase change material particles through a 200-mesh screen, feeding the phase change material particles passing through the screen into a particle coating bin through air flow, introducing dry hot air into the particle coating bin to enable the phase change material particles to be in a solid fluidized state, controlling the temperature to be 45 ℃, feeding inorganic cementing material formed by mixing PO42.5 portland cement and redispersible rubber powder through air flow in a vertical direction, wherein the weight ratio of the PO42.5 cement to the redispersible rubber powder in the inorganic cementing material is 1: 0.005. the volume ratio of the phase-change material particles to the inorganic gelled material is 1: and (3) 0.6, wherein the microencapsulation time (namely the introduction time of the inorganic gel material) is 30 minutes, and the phase-change microcapsule intermediate is prepared. And (3) feeding the phase change microcapsule intermediate into a wall material hydration bin, wherein the temperature of water vapor in the bin is 40 ℃, the hydration time is 70 minutes, and after full hydration, drying to obtain the phase change microcapsule material.
Preparation of composite phase-change insulation board
Weighing 85% of commercial vitrified micro bubble inorganic thermal insulation mortar powder and 15% of the phase change microcapsule material according to the weight percentage, and mixing the powder and the phase change microcapsule material to obtain a dry material.
Mixing the dry materials with water 4: 1, and pouring to form the composite phase change insulation board.
Example 2
The embodiment provides a phase change microcapsule material and a preparation method thereof, and a composite phase change insulation board and a preparation method thereof, wherein the preparation method comprises the following steps:
preparation of phase-change microcapsule material
And adding paraffin with the phase change temperature of 35 ℃ into a granulation bin of the fluidized bed, and granulating by cooling with a spray gun at the cooling temperature of 30 ℃ to prepare phase change material particles. Passing the phase change material particles through a 150-mesh screen, feeding the phase change material particles passing through the screen into a particle coating bin through air flow, introducing dry hot air into the particle coating bin to enable the phase change material particles to be in a solid fluidization state, controlling the temperature to be 35 ℃, feeding an inorganic cementing material formed by mixing R.SAC42.5 sulphoaluminate cement and lignin rubber powder through air flow in a vertical direction, wherein the weight ratio of the R.SAC42.5 sulphoaluminate cement to the lignin rubber powder in the inorganic cementing material is 1: 0.01. the volume ratio of the phase-change material particles to the inorganic gelled material is 1: and (3) 0.8, wherein the microencapsulation time (namely the introduction time of the inorganic gel material) is 40 minutes, and the phase-change microcapsule intermediate is prepared. And (3) feeding the phase change microcapsule intermediate into a wall material hydration bin, wherein the temperature of water vapor in the bin is 30 ℃, the hydration time is 60 minutes, and after full hydration, drying to obtain the phase change microcapsule material.
Preparation of composite phase-change insulation board
Weighing 85% of commercial vitrified micro bubble inorganic thermal insulation mortar powder and 15% of the phase change microcapsule material according to the weight percentage, and mixing the powder and the phase change microcapsule material to obtain a dry material.
Mixing the dry materials with water 4: 1, and pouring to form the composite phase change insulation board.
Example 3
The embodiment provides a phase change microcapsule material and a preparation method thereof, and a composite phase change insulation board and a preparation method thereof, wherein the preparation method comprises the following steps:
preparation of phase-change microcapsule material
And adding paraffin with the phase change temperature of 45 ℃ into a granulation bin of the fluidized bed, and granulating by cooling with a spray gun at the cooling temperature of 40 ℃ to prepare phase change material particles. Passing the phase change material particles through a 150-mesh screen, feeding the phase change material particles passing through the screen into a particle coating bin through air flow, introducing dry hot air into the particle coating bin to enable the phase change material particles to be in a solid fluidized state, controlling the temperature to be 45 ℃, feeding an inorganic cementing material formed by mixing first-stage fly ash and water glass powder through air flow in a vertical direction, wherein the weight ratio of the first-stage fly ash to the water glass powder in the inorganic cementing material is 1: 0.6. the volume ratio of the phase-change material particles to the inorganic gelled material is 1: and (3) 0.9, wherein the microencapsulation time (namely the introduction time of the inorganic gel material) is 40 minutes, and the phase-change microcapsule intermediate is prepared. And (3) feeding the phase change microcapsule intermediate into a wall material hydration bin, wherein the temperature of water vapor in the bin is 40 ℃, the hydration time is 40 minutes, and after full hydration, drying to obtain the phase change microcapsule material.
Preparation of composite phase-change insulation board
Weighing 85% of commercial vitrified micro bubble inorganic thermal insulation mortar powder and 15% of the phase change microcapsule material according to the weight percentage, and mixing the powder and the phase change microcapsule material to obtain a dry material.
Mixing the dry materials with water 4: 1, and pouring to form the composite phase change insulation board.
Example 4
The embodiment provides a phase change microcapsule material and a preparation method thereof, and a composite phase change insulation board and a preparation method thereof, wherein the preparation method comprises the following steps:
preparation of phase-change microcapsule materials
And adding paraffin with the phase change temperature of 65 ℃ into a granulation bin of the fluidized bed, and granulating by cooling with a spray gun at the cooling temperature of 60 ℃ to prepare phase change material particles. Passing the phase change material particles through a 150-mesh screen, feeding the phase change material particles passing through the screen into a particle coating bin through air flow, introducing dry hot air into the particle coating bin to enable the phase change material particles to be in a solid fluidized state, controlling the temperature to be 65 ℃, feeding inorganic gelled material formed by mixing PO42.5 cement, first-stage fly ash and lignin rubber powder through air flow in a vertical direction, wherein the weight ratio of the PO42.5 cement to the first-stage fly ash to the lignin rubber powder in the inorganic gelled material is 1: 0.6: 0.01. the volume ratio of the phase-change material particles to the inorganic gelled material is 1: and (3) 0.5) microencapsulating time (namely the introduction time of the inorganic gel material) is 40 minutes, and preparing the phase-change microcapsule intermediate. Sending the phase change microcapsule intermediate into a wall material hydration bin, wherein the temperature of water vapor in the bin is 60 ℃, the hydration time is 100 minutes, after full hydration, continuously introducing water vapor for 5 minutes, wetting the surface of the hydrated phase change microcapsule intermediate, then sending the hydrated phase change microcapsule intermediate into a particle coating bin, introducing dry hot air into the particle coating bin to control the phase change material particles to be in a solid fluidization state, controlling the temperature to be 65 ℃, sending an inorganic cementing material formed by mixing PO42.5 cement, primary fly ash and lignin rubber powder through air flow in the vertical direction, wherein the weight ratio of the PO42.5 cement to the primary fly ash to the lignin rubber powder in the inorganic cementing material is 1: 0.6: 0.01. the volume ratio of the phase-change material particles to the inorganic gelled material is 1: 0.5, the micro-encapsulation time (namely the leading-in time of the inorganic gel material) is 40 minutes, and the secondary micro-encapsulation is completed. And (3) feeding the microcapsules into a wall material hydration bin, wherein the temperature of water vapor in the bin is 60 ℃, the hydration time is 100 minutes, and after the microcapsules are fully hydrated, drying the microcapsules to obtain the phase-change microcapsule material.
Preparation of composite phase-change insulation board
Weighing 85% of commercial vitrified micro bubble inorganic thermal insulation mortar powder and 15% of the phase change microcapsule material according to the weight percentage, and mixing the powder and the phase change microcapsule material to obtain a dry material.
Mixing the dry materials with water 4: 1, and pouring to form the composite phase change insulation board.
Comparative example 1
Mixing commercially available vitrified microbead inorganic thermal insulation mortar powder and water 4: 1, and pouring to form the composite phase change insulation board.
Comparative example 2
Preparing phase-change microcapsules:
weighing 10g of hexadecyl trimethyl ammonium bromide as an emulsifier and 15g of octyl phenol polyoxyethylene ether in a container, adding 2L of 1mol/L hydrochloric acid, stirring, adding 136.4g of phase-change paraffin melt with the phase-change temperature of 40 ℃ and the phase-change temperature of 30 ℃ after the emulsifier is dissolved, and homogenizing and emulsifying in a constant-temperature water bath kettle with the temperature of 45 ℃ for 60min to obtain the oil-in-water emulsion. And transferring the emulsion into a reaction bottle, dropwise adding 2L of 0.4mol/L sodium silicate solution, stirring for reaction for 4 hours, and cooling to room temperature after the reaction is finished. And filtering, washing and drying the solid-liquid mixture to obtain the white powdery phase change microcapsule.
Preparation of composite phase-change insulation board
According to the weight percentage, 85 percent of commercial vitrified microsphere inorganic thermal mortar powder and 15 percent of the phase change microcapsule material are weighed and mixed to obtain a dry material.
The phase change microcapsule material and the composite phase change insulation board prepared by the embodiment are respectively tested, and the test method comprises the following steps:
and (3) carrying out the performance test of the microcapsule by using a Differential Scanning Calorimeter (DSC), wherein the test temperature range is from-10 ℃ to 20 ℃ above the phase change temperature of the phase change material, and the temperature rise and fall rate is 5 ℃/min. The results are shown in Table 1.
And performing performance test on the composite insulation board by referring to the general technical requirements of the JG/T435-2014 inorganic lightweight aggregate fireproof insulation board. The results are shown in Table 2.
TABLE 1
Figure BDA0003033930410000121
TABLE 2
Item Compressive strength (MPa) Tensile strength (MPa) Combustion performance
Example 1 5.6 0.62 Class A
Example 2 6 0.64 Class A
Example 3 6.3 0.66 Class A
Example 4 6.6 0.67 Class A
Comparative example 1 7.2 0.71 Class A
Comparative example 2 2.8 0.32 Class A
It can be seen that the phase change microcapsule materials prepared in examples 1 to 4 can use cement-based or other inorganic gel materials as wall materials, and have good latent heat of phase change. The prepared composite phase change insulation board does not greatly influence the mechanical property of the insulation board.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (12)

1. The preparation method of the phase change microcapsule material is characterized by comprising the following steps:
1) taking a phase-change material, granulating and preparing phase-change material particles;
2) utilizing gas to enable the phase change material particles to be in a solid fluidized state, enabling the temperature to reach the phase change temperature of the phase change material, and introducing an inorganic gel material to enable the inorganic gel material to coat the phase change material particles to prepare a phase change microcapsule intermediate;
3) hydrating the phase change microcapsule intermediate;
the introducing time of the inorganic gel material is 15min-120 min;
the method for hydrating the phase change microcapsule intermediate comprises the following steps: and (3) utilizing water vapor to enable the phase change microcapsule intermediate to be in a solid fluidization state, enabling the temperature to be 1-5 ℃ lower than the phase change temperature of the phase change material, continuously introducing the water vapor, and hydrating for 10-70 min.
2. The method for preparing the phase-change microcapsule material according to claim 1, wherein the volume ratio of the phase-change material particles to the inorganic gel material is 1 (0.3-0.9).
3. The method for preparing phase change microcapsule material according to claim 2, wherein the phase change material is selected from one or more of n-dodecane, n-pentadecane, n-hexadecane, n-octadecane, n-nonadecane, n-eicosane, n-docosane, paraffin and natural cocoa fatty acid mixture.
4. The method for preparing the phase-change microcapsule material according to claim 2, wherein the inorganic gel material comprises one or more of a cement-based gel material and an alkali-activated gel material.
5. The method for preparing the phase change microcapsule material according to claim 4, wherein the cement-based gel material is selected from one or more of portland cement, aluminate cement, sulphoaluminate cement and pozzolanic cement.
6. The method for preparing a phase-change microcapsule material according to claim 4, wherein the inorganic gel material further comprises an additive.
7. The method for preparing a phase-change microcapsule material according to claim 6, wherein the additive is a redispersible latex powder.
8. The method of claim 1, wherein the gas is hot air.
9. The method for preparing a phase-change microcapsule material according to claim 1, further comprising the steps of wetting the phase-change microcapsule intermediate after hydration, and then repeating the steps 2) and 3)1 to 3 times.
10. The method for preparing a phase-change microcapsule material according to claim 9, further comprising a step of drying the product of step 3) to prepare a phase-change microcapsule.
11. A phase change microcapsule material prepared by the method for preparing a phase change microcapsule material according to any one of claims 1 to 10.
12. A composite phase change insulation board, characterized by comprising the phase change microcapsule material of claim 11.
CN202110438327.7A 2021-04-22 2021-04-22 Phase-change microcapsule material, preparation method thereof and composite phase-change insulation board Active CN113185218B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110438327.7A CN113185218B (en) 2021-04-22 2021-04-22 Phase-change microcapsule material, preparation method thereof and composite phase-change insulation board

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110438327.7A CN113185218B (en) 2021-04-22 2021-04-22 Phase-change microcapsule material, preparation method thereof and composite phase-change insulation board

Publications (2)

Publication Number Publication Date
CN113185218A CN113185218A (en) 2021-07-30
CN113185218B true CN113185218B (en) 2022-06-03

Family

ID=76978610

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110438327.7A Active CN113185218B (en) 2021-04-22 2021-04-22 Phase-change microcapsule material, preparation method thereof and composite phase-change insulation board

Country Status (1)

Country Link
CN (1) CN113185218B (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109321210A (en) * 2018-10-15 2019-02-12 中国科学院上海应用物理研究所 A kind of method preparing metal casing high-temperature phase-change heat storage microcapsules and thus obtained heat accumulation microcapsules
CN111171793A (en) * 2020-01-06 2020-05-19 西安建筑科技大学 Inorganic heat-storage unfired ceramsite and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109321210A (en) * 2018-10-15 2019-02-12 中国科学院上海应用物理研究所 A kind of method preparing metal casing high-temperature phase-change heat storage microcapsules and thus obtained heat accumulation microcapsules
CN111171793A (en) * 2020-01-06 2020-05-19 西安建筑科技大学 Inorganic heat-storage unfired ceramsite and preparation method thereof

Also Published As

Publication number Publication date
CN113185218A (en) 2021-07-30

Similar Documents

Publication Publication Date Title
CN102417340B (en) Gypsum-based phase change energy storage polymer thermal insulation mortar and preparation method thereof
Hekimoğlu et al. Thermal management performance and mechanical properties of a novel cementitious composite containing fly ash/lauric acid-myristic acid as form-stable phase change material
CN100522867C (en) Polystyrene foam particle heat-insulating mortar
CN101391872B (en) Novel thermal insulation composite material composition and method of making the same
CN100387544C (en) Phase change anticracking grout and preparation method of used phase change material particulate
CN102167529B (en) Thermal insulation fire-proof aggregate with polystyrene particle-coated expanded and vitrified bead mortar and preparation method thereof
CN109721312A (en) A kind of A grades of non-ignitable aeroge polyphenylene heat insulation slab and preparation method thereof
CN107265962A (en) A kind of superthermal insulation aerogel foam concrete and preparation method thereof
CN107056210A (en) A kind of enhanced Thistle board of energy storage, its preparation method and application
Gencel et al. Development, characterization and thermo-regulative performance of microencapsulated phase change material included-glass fiber reinforced foam concrete as novel thermal energy effective-building material
CN106882947B (en) A kind of environmentally protective phase-transition heat-preserving cracking resistance coagulates the preparation method of spraying mortar fastly
CN104311108A (en) Hydrophobic inorganic nano insulation board and preparation method thereof
CN102795780A (en) Low-temperature microcrystalline foam glass and preparation method thereof
CN107265963A (en) A kind of superthermal insulation aerogel foam concrete and preparation method thereof
CN107266114A (en) A kind of aerogel heat-insulating masonry mortar and preparation method thereof
CN105819814A (en) Desulfurized gypsum base machine-sprayed thermal insulation mortar and preparation method thereof
CN113185218B (en) Phase-change microcapsule material, preparation method thereof and composite phase-change insulation board
CN109133981A (en) A kind of gypsum base plastering mortar
CN108484212A (en) A kind of hollow tiny pearl thermal insulation mortar and preparation method thereof
CN106116439B (en) Thermal insulation mortar
CN110272261B (en) Fireproof heat-insulating material and preparation method thereof
CN100596292C (en) Multifunctional heat insulating plaster
Durmuş et al. Thermal Characterization of Foam Concrete Panels Containing Expanded Perlite-Polystyrene, Foam and Aerogel Layer
CN111620607A (en) Foamed concrete and preparation method thereof
CN109796170A (en) A kind of phase transformation temp auto-controlled cement foaming insulation board and its production method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant