CN114479536A - Diatomite hybrid supermolecule thermal insulation material and preparation method thereof - Google Patents
Diatomite hybrid supermolecule thermal insulation material and preparation method thereof Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
- C09D1/04—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates with organic additives
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
Abstract
The invention belongs to the technical field of green, energy-saving and environment-friendly building materials, and particularly relates to a diatomite hybrid supermolecule thermal insulation material and a preparation method thereof, wherein the diatomite hybrid supermolecule thermal insulation material comprises the following raw material components in parts by weight: 15-35 parts of diatomite; 1-4 parts of a silane coupling agent A; 10-50 parts of ethanol; 1-5 parts of an emulsifier; 10-50 parts of viscous high-molecular monomer; 0.2-0.8 part of initiator; 10-50 parts of organic acid; 5-30 parts of a surfactant; 30-90 parts of sodium silicate; 4-10 parts of aluminum nitrate; 0.5-3 parts of a silane coupling agent B; 10-50 parts of non-viscous high-molecular monomer; 1500 portions of water and 2000 portions. The diatomite hybrid supermolecule thermal insulation material has a supermolecule thermal insulation material with a nano-pore structure, can be widely applied to interior wall thermal insulation coatings, can effectively improve the indoor temperature, has a good thermal insulation effect, and is small in use amount; the method has the advantages of simple process, convenient operation and wide application.
Description
Technical Field
The invention belongs to the technical field of green, energy-saving and environment-friendly building materials, and particularly relates to a diatomite hybrid supermolecule thermal insulation material and a preparation method thereof.
Background
At present, the heating mode generally adopted in China is mainly a radiator convection heating mode, such as floor heating, radiators and the like, and radiation heating systems such as infrared electrothermal films and the like are gradually popularized because the heat distribution is more uniform and the heat action efficiency on human bodies and other objects is higher. The indoor heat conduction mode is mainly radiation and convection, no matter convection heating or radiation heating is adopted, the heat radiation plays an important role in indoor heat, and when the heat radiation reaches the surface of a wall body, the heat radiation can be absorbed by the wall body and then is lost to the outdoors.
The energy consumption of heating in winter is the main energy consumption of Chinese buildings, and the requirement of the government of China on the energy saving of the buildings is continuously improved. In order to embody the fair heat utilization and get rid of the concentrated heating habit with low efficiency, the energy-saving method of household heat metering is implemented for the energy-saving reconstruction projects of new buildings and existing buildings. However, the existing building energy-saving heat-insulating measures only aim at the external protective structure of the building, and heat-insulating measures are generally not adopted among the partition walls of the buildings in the building, so that different temperatures may exist among different buildings, thereby generating hot pressing, and the heat loss phenomenon can occur in a room with high temperature, namely, the heat flows from the room with high temperature to a room with low temperature. The unfair heat consumption phenomenon easily causes various problems and contradictions, for example, the heat loss in households is serious, so that the heat consumption between neighbors is not uniform, the unfair phenomenon is caused, and the high building energy consumption is achieved, so that the popularization of the energy-saving policy of the buildings in China is influenced. Although the existing house can be used for heat preservation of an inner wall, the existing house has large heat loss and poor heat preservation effect and occupies certain house space, so that a plurality of users can remove the heat preservation layer of the inner wall during decoration. Therefore, it is necessary to find an inner wall thermal insulation material with good thermal insulation effect and small usage amount.
Disclosure of Invention
The invention aims to provide a diatomite hybridized supermolecule thermal insulation material and a preparation method thereof, the diatomite hybridized supermolecule thermal insulation material has a supermolecule thermal insulation material with a nano-pore structure, can be widely applied to interior wall thermal insulation coatings, can effectively improve the indoor temperature, has a good thermal insulation effect, and is small in use amount; the method has the advantages of simple process, convenient operation and wide application.
The invention provides a diatomite hybrid supramolecular thermal insulation material which comprises the following raw material components in parts by weight:
according to the technical scheme, the diatomite is natural diatomite with a microporous structure, and is reacted with the coupling agent, the initiator and the high-molecular monomer to obtain the diatomite hybrid supermolecule thermal insulation material which can be widely applied to interior wall thermal insulation coatings, the indoor temperature can be effectively improved, the thermal insulation effect is good, and by adding the viscous and non-viscous high-molecular monomer, a product with a high-porosity structure is formed after polymerization, the thermal conductivity can be effectively reduced, and the thermal insulation effect is improved.
Preferably, in the above technical solution, the silane coupling agent a is KH-570, and the silane coupling agent B is a 151. In the technical scheme, KH-570 is used as a coupling agent, so that the mechanical strength, weather resistance and corrosion resistance of the composite material can be improved; a151 is vinyl triethoxysilane, is soluble in water, and has the functions of both a coupling agent and a crosslinking agent.
Preferably, in the above technical solution, the ethanol is 95% ethanol or absolute ethanol; the emulsifier is any one of sodium dodecyl sulfate and sodium dodecyl sulfate.
Preferably, in the above technical solution, the viscous polymer monomer is any one of butyl acrylate and butyl methacrylate; the non-viscous high molecular monomer is any one of methyl acrylate, methyl methacrylate, acrylonitrile and styrene.
Preferably, in the above technical scheme, the organic acid is one or more of citric acid, oxalic acid and glacial acetic acid; the surfactant is a cationic surfactant and is any one of cetyl trimethyl ammonium bromide and cetyl trimethyl ammonium chloride; the initiator is a peroxide initiator and is any one of ammonium persulfate and potassium persulfate.
Preferably, in the above technical scheme, the modulus of the sodium silicate is 2.8-3.4; the aluminum nitrate is analytically pure aluminum nitrate nonahydrate; the water is distilled water or deionized water.
The invention also comprises a preparation method of the diatomite hybrid supramolecular thermal insulation material, which comprises the following specific steps:
s1, dispersing diatomite in water with total water amount of 2/3-3/4 according to a ratio, and then stirring for 30-60min at room temperature at the stirring speed of 300-;
s2, dissolving the silane coupling agent A in ethanol, slowly dripping the silane coupling agent A into the dispersion liquid prepared in the step S1 under the stirring condition, and continuously stirring for 20-30min after the silane coupling agent A is added;
s3, adding an emulsifier into the dispersion prepared in S2, dropwise adding a viscous high-molecular monomer after the emulsifier is completely dissolved, adding half of an initiator after the monomer is dropwise added, and heating to 70-80 ℃ under the stirring condition for polymerization for 3-5 h;
s4, adding sodium silicate dissolved in a small amount of water in advance into the mixed solution after polymerization of S3, and stirring for 30-60min at 70-80 ℃;
s5, dissolving a surfactant and an organic acid in a small amount of water, slowly dripping the water into the reaction system of S4, stirring the mixture for 30 to 60 minutes at the temperature of between 70 and 80 ℃, then adding aluminum nitrate, and continuously stirring the mixture for 30 to 60 minutes at the temperature of between 70 and 80 ℃;
s6, dissolving the silane coupling agent B in a non-viscous high molecular monomer, adding the silane coupling agent B into the reaction system of S5, adding the rest initiator, and stirring for 60-120min at 70-90 ℃;
s7, after the mixed solution of the S6 is completely reacted, naturally cooling to room temperature, then carrying out operations such as filtering, washing and the like, and drying at the temperature of 80-100 ℃;
s8, calcining the dried powder in an inert atmosphere at the temperature of 600-800 ℃ for 1-5h, and fully cooling to obtain the diatomite hybrid supramolecular thermal insulation material.
Preferably, in the above technical scheme, each step is performed in a temperature-controlled closed stainless steel container.
Preferably, in the above technical solutions S2, S3, and S5, the dropping of the silane coupling agent, the viscous polymer monomer, and the surfactant is performed using a dropping funnel provided in a stainless steel container.
Preferably, in the above technical solution S7, the drying device is an electric heating drying box; in S8, the high-temperature calcination apparatus is a high-temperature tube furnace.
Compared with the prior art, the method has the beneficial effects that:
the diatomite hybrid supermolecule thermal insulation material is a supermolecule thermal insulation material with a nano-pore structure, can be widely applied to interior wall thermal insulation coatings, can effectively improve the indoor temperature, has a good thermal insulation effect, is small in using amount, can save the cost, can effectively improve the mechanical strength and weather resistance of a product by adding two different coupling agents, and is good in construction performance; the method has the advantages of simple process, convenient operation and wide application.
Drawings
FIG. 1 is a physical diagram of the testing method of the present invention, wherein a is a test chart of a control 3cm foamed cement board, and b is a test chart of a 6mm sample prepared from the diatomite hybrid supramolecular insulation material prepared in example 3.
Detailed Description
The technical features of the present invention described above and those described in detail below (as an embodiment) can be combined with each other to form a new or preferred technical solution, but the present invention is not limited to these embodiments, and the embodiments also do not limit the present invention in any way.
The experimental procedures in the following examples are conventional unless otherwise specified. The formulations according to the following examples are all commercially available products and are commercially available, unless otherwise specified.
The present invention is described in further detail below with reference to examples:
example 1
The diatomite hybrid supramolecular thermal insulation material comprises the following raw material components in parts by weight:
the preparation method comprises the following specific steps:
s1, adding diatomite into a temperature-controlled closed stainless steel container which is filled with 1000mL of water and is provided with a dropping funnel according to a ratio for dispersion, and then stirring for 30min at room temperature, wherein the stirring speed is 500 r/min;
s2, dissolving the silane coupling agent A in ethanol, slowly dripping the silane coupling agent A into the dispersion liquid prepared in the step S1 under the stirring condition, and continuously stirring for 20min after the silane coupling agent A is added;
s3, adding an emulsifier into the dispersion prepared in S2, dropwise adding a viscous high-molecular monomer after the emulsifier is completely dissolved, adding half of an initiator after the monomer is dropwise added, and heating to 70 ℃ under the stirring condition for polymerization for 5 hours;
s4, adding sodium silicate dissolved in 300mL of water in advance into the mixed solution after polymerization of S3, and stirring for 60min at 70 ℃;
s5, dissolving a surfactant and an organic acid in 200mL of water, slowly dropwise adding the water into the reaction system of S4, stirring for 60min at 70 ℃, then adding aluminum nitrate, and continuously stirring for 60min at 70 ℃;
s6, dissolving the silane coupling agent B in a non-viscous high molecular monomer, adding the silane coupling agent B into the reaction system of S5, adding the rest initiator, and stirring for 120min at 70 ℃;
s7, after the mixed liquor of the S6 is completely reacted, naturally cooling to room temperature, then carrying out operations such as filtering, washing and the like, and drying in an electric heating drying box at 80 ℃;
s8, calcining the dried powder in an inert atmosphere in a 600 ℃ high-temperature tubular furnace for 5 hours, and fully cooling to obtain the diatomite hybrid supramolecular thermal insulation material.
Example 2
The diatomite hybrid supramolecular thermal insulation material comprises the following raw material components in parts by weight:
the preparation method comprises the following specific steps:
s1, adding diatomite into a temperature-controlled closed stainless steel container which is filled with 1200mL of water and is provided with a dropping funnel according to a ratio for dispersion, and then stirring for 40min at room temperature, wherein the stirring speed is 400 r/min;
s2, dissolving the silane coupling agent A in ethanol, slowly dripping the silane coupling agent A into the dispersion liquid prepared in the step S1 under the stirring condition, and continuously stirring for 25min after the silane coupling agent A is added;
s3, adding an emulsifier into the dispersion prepared in S2, dropwise adding a viscous high-molecular monomer after the emulsifier is completely dissolved, adding half of an initiator after the monomer is dropwise added, and heating to 75 ℃ under the stirring condition for polymerization for 4 hours;
s4, adding sodium silicate dissolved in 250mL of water in advance into the mixed solution after polymerization of S3, and stirring for 50min at 75 ℃;
s5, dissolving a surfactant and an organic acid in 150mL of water, slowly dropwise adding the water into the reaction system of S4, stirring for 50min at 75 ℃, then adding aluminum nitrate, and continuously stirring for 50min at 75 ℃;
s6, dissolving the silane coupling agent B in a non-viscous high molecular monomer, adding the silane coupling agent B into the reaction system of S5, adding the rest initiator, and stirring for 100min at the temperature of 75 ℃;
s7, after the mixed liquor of the S6 is completely reacted, naturally cooling to room temperature, then carrying out operations such as filtering, washing and the like, and drying in an electric heating drying oven at 85 ℃;
s8, calcining the dried powder in an inert atmosphere in a high-temperature tube furnace at 650 ℃ for 4 hours, and fully cooling to obtain the diatomite hybrid supramolecular thermal insulation material.
Example 3
The diatomite hybrid supramolecular thermal insulation material comprises the following raw material components in parts by weight:
the preparation method comprises the following specific steps:
s1, adding diatomite into a temperature-controlled closed stainless steel container which is filled with 1500mL of water and is provided with a dropping funnel according to a ratio for dispersion, and then stirring for 50min at room temperature, wherein the stirring speed is 350 r/min;
s2, dissolving the silane coupling agent A in ethanol, slowly dripping the silane coupling agent A into the dispersion liquid prepared in the step S1 under the stirring condition, and continuously stirring for 28min after the silane coupling agent A is added;
s3, adding an emulsifier into the dispersion prepared in S2, dropwise adding a viscous high-molecular monomer after the emulsifier is completely dissolved, adding half of an initiator after the monomer is dropwise added, and heating to 78 ℃ under the stirring condition for polymerization for 3.5 hours;
s4, adding sodium silicate dissolved in 300mL of water in advance into the mixed solution obtained after polymerization of S3, and stirring for 40min at 78 ℃;
s5, dissolving a surfactant and an organic acid in 200mL of water, slowly dropwise adding the water into the reaction system of S4, stirring for 40min at 78 ℃, then adding aluminum nitrate, and continuously stirring for 40min at 78 ℃;
s6, dissolving the silane coupling agent B in a non-viscous high molecular monomer, adding the silane coupling agent B into the reaction system of S5, adding the rest initiator, and stirring for 80min at the temperature of 80 ℃;
s7, after the mixed liquor of the S6 is completely reacted, naturally cooling to room temperature, then carrying out operations such as filtering, washing and the like, and drying in an electric heating drying oven at 90 ℃;
s8, calcining the dried powder in an inert atmosphere in a high-temperature tubular furnace at 700 ℃ for 3h, and fully cooling to obtain the diatomite hybrid supramolecular thermal insulation material.
Example 4
The diatomite hybrid supramolecular thermal insulation material comprises the following raw material components in parts by weight:
the preparation method comprises the following specific steps:
s1, adding diatomite into a temperature-controlled closed stainless steel container which is filled with 1500mL of water and is provided with a dropping funnel according to a ratio for dispersion, and then stirring for 60min at room temperature, wherein the stirring speed is 300 r/min;
s2, dissolving the silane coupling agent A in ethanol, slowly dripping the silane coupling agent A into the dispersion liquid prepared in the step S1 under the stirring condition, and continuously stirring for 30min after the silane coupling agent A is added;
s3, adding an emulsifier into the dispersion prepared in S2, dropwise adding a viscous high-molecular monomer after the emulsifier is completely dissolved, adding half of an initiator after the monomer is dropwise added, and heating to 80 ℃ under the stirring condition for polymerization for 3 hours;
s4, adding sodium silicate dissolved in 300mL of water in advance into the mixed solution after polymerization of S3, and stirring for 30min at 80 ℃;
s5, dissolving a surfactant and an organic acid in 200mL of water, slowly dropwise adding the water into the reaction system of S4, stirring for 30min at 80 ℃, then adding aluminum nitrate, and continuously stirring for 30min at 80 ℃;
s6, dissolving the silane coupling agent B in a non-viscous high molecular monomer, adding the silane coupling agent B into the reaction system of S5, adding the rest initiator, and stirring for 60min at 90 ℃;
s7, after the mixed liquor of the S6 is completely reacted, naturally cooling to room temperature, then carrying out operations such as filtering, washing and the like, and drying in an electric heating drying oven at 100 ℃;
s8, calcining the dried powder in an inert atmosphere in a high-temperature tube furnace at 800 ℃ for 1h, and fully cooling to obtain the diatomite hybrid supramolecular thermal insulation material.
The diatomite hybrid supramolecular thermal insulation material prepared in the embodiment 3 of the invention is prepared into a sample plate with the thickness of 6mm and a commercially available foamed cement plate with the thickness of 3cm to be used as a control group, and the thermal insulation performance test is carried out.
The test method comprises the following steps: the lowest layer is a heating plate, the middle layer is a test sample, the upper layer is a heat conducting plate, and two temperature sensors are attached to the heat conducting plate. The temperature of the upper layer of the test sample was measured by heating the bottom to about 80 deg.C, wherein the physical diagram of the test method is shown in FIG. 1, and the test results are shown in Table 1.
TABLE 1 Heat insulation Performance test results
Group of | Temperature of heating plate | Left side sensor temperature | Temperature of right side sensor | Average temperature on both sides |
Example 3 sample plate | 80℃ | 23.5℃ | 24.3℃ | 23.9℃ |
Control group sample plate | 79.8℃ | 25.2℃ | 26.1℃ | 25.65℃ |
As can be seen from the test results in Table 1, the temperature difference between the upper and lower sides of the 6mm thick sample plate prepared by using the diatomaceous earth hybrid supramolecular thermal insulation material prepared by the present invention is 56.1 ℃ and the temperature difference between the upper and lower sides of the commercially available 3cm foamed cement plate is 54.15 ℃. Therefore, the temperature difference between the upper and lower parts of the sample with the thickness of 6mm prepared by the method is higher than that of the commercially available foamed cement board with the thickness of 3cm, which shows that the heat conductivity coefficient of the sample prepared by the formula and the method is obviously lower than that of the foamed cement board, and the sample prepared by the method only has the thickness of 6mm and is lower than that of the foamed cement board with the thickness of 3cm, so that the use amount is small, and the heat insulation performance is good.
Finally, it should be emphasized that the above-described preferred embodiments of the present invention are merely examples of implementations, and it should be understood that various changes and modifications may be made by those skilled in the art, and any changes, equivalents, improvements and the like, which fall within the spirit and principle of the present invention, should be included in the scope of the present invention.
Claims (10)
2. the diatomite hybrid supramolecular thermal insulation material as claimed in claim 1, wherein silane coupling agent A is KH-570, and silane coupling agent B is A151.
3. The diatomaceous earth hybrid supramolecular thermal insulation material of claim 1, wherein the ethanol is 95% ethanol or absolute ethanol; the emulsifier is any one of sodium dodecyl sulfate and sodium dodecyl sulfate.
4. The diatomite hybrid supramolecular thermal insulation material as claimed in claim 1, wherein the viscous polymer monomer is any one of butyl acrylate and butyl methacrylate; the non-viscous high molecular monomer is any one of methyl acrylate, methyl methacrylate, acrylonitrile and styrene.
5. The diatomite hybrid supramolecular thermal insulation material as claimed in claim 1, wherein the organic acid is one or more of citric acid, oxalic acid and glacial acetic acid; the surfactant is a cationic surfactant and is any one of cetyl trimethyl ammonium bromide and cetyl trimethyl ammonium chloride; the initiator is a peroxide initiator and is any one of ammonium persulfate and potassium persulfate.
6. The diatomite hybrid supramolecular thermal insulation material as claimed in claim 1, wherein the sodium silicate has a modulus of 2.8-3.4; the aluminum nitrate is analytically pure aluminum nitrate nonahydrate; the water is distilled water or deionized water.
7. The preparation method of the diatomite hybrid supramolecular thermal insulation material according to any one of claims 1 to 6, which is characterized by comprising the following specific steps:
s1, dispersing diatomite in water with total water amount of 2/3-3/4 according to a ratio, and then stirring for 30-60min at room temperature at the stirring speed of 300-;
s2, dissolving the silane coupling agent A in ethanol, slowly dripping the silane coupling agent A into the dispersion liquid prepared in the step S1 under the stirring condition, and continuously stirring for 20-30min after the silane coupling agent A is added;
s3, adding an emulsifier into the dispersion prepared in S2, dropwise adding a viscous high-molecular monomer after the emulsifier is completely dissolved, adding half of an initiator after the monomer is dropwise added, and heating to 70-80 ℃ under the stirring condition for polymerization for 3-5 h;
s4, adding sodium silicate dissolved in a small amount of water in advance into the mixed solution after polymerization of S3, and stirring for 30-60min at 70-80 ℃;
s5, dissolving a surfactant and an organic acid in a small amount of water, slowly dripping the water into the reaction system of S4, stirring the mixture for 30 to 60 minutes at the temperature of between 70 and 80 ℃, then adding aluminum nitrate, and continuously stirring the mixture for 30 to 60 minutes at the temperature of between 70 and 80 ℃;
s6, dissolving the silane coupling agent B in a non-viscous high molecular monomer, adding the silane coupling agent B into the reaction system of S5, adding the rest initiator, and stirring for 60-120min at 70-90 ℃;
s7, after the mixed solution of the S6 is completely reacted, naturally cooling to room temperature, then carrying out operations such as filtering, washing and the like, and drying at the temperature of 80-100 ℃;
s8, calcining the dried powder in an inert atmosphere at the temperature of 600-800 ℃ for 1-5h, and fully cooling to obtain the diatomite hybrid supramolecular thermal insulation material.
8. The method for preparing the diatomite hybrid supramolecular thermal insulation material as claimed in claim 7, wherein each step is performed in a temperature-controlled closed stainless steel container.
9. The method for preparing the diatomite hybrid supramolecular thermal insulation material as claimed in claim 7, wherein the silane coupling agent, the viscous polymer monomer and the surfactant are added dropwise in S2, S3 and S5 by using a dropping funnel matched with a stainless steel container.
10. The method for preparing the diatomite hybrid supramolecular thermal insulation material as claimed in claim 7, wherein in S7, the drying equipment is an electric heating drying box; in S8, the high-temperature calcination apparatus is a high-temperature tube furnace.
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CN111849341A (en) * | 2020-07-22 | 2020-10-30 | 绵阳麦思威尔科技有限公司 | Organic-inorganic nano hybrid water-based high-temperature-resistant anticorrosive paint and preparation method thereof |
CN112375488A (en) * | 2020-11-12 | 2021-02-19 | 深圳市瑞晟新材料有限公司 | Aqueous inorganic nano ceramic paint, preparation method and application thereof |
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