CN115432726A - Modified nano-alumina and preparation method and application thereof - Google Patents
Modified nano-alumina and preparation method and application thereof Download PDFInfo
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- CN115432726A CN115432726A CN202210891427.XA CN202210891427A CN115432726A CN 115432726 A CN115432726 A CN 115432726A CN 202210891427 A CN202210891427 A CN 202210891427A CN 115432726 A CN115432726 A CN 115432726A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/021—After-treatment of oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/30—Oxides other than silica
- C04B14/303—Alumina
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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
- 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
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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
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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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
- 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
Abstract
The invention relates to the field of C04B35/10, in particular to modified nano alumina and a preparation method and application thereof, wherein 80-120 parts by weight of nano alumina and 1-8 parts by weight of a modifier are adopted, and the nano alumina is modified by adopting a specific modifier and then applied to the preparation of a nano microporous thermal insulation plate, so that the agglomeration of nano particles is effectively inhibited, the bonding force among nano alumina particles is improved, and the obtained modified nano alumina has excellent compatibility and dispersibility in a nano microporous thermal insulation plate system, so that the mechanical property of the nano alumina thermal insulation plate is effectively improved, the cracking phenomenon in use at high temperature is effectively inhibited, and the nano alumina thermal insulation plate has high practical application and popularization values.
Description
Technical Field
The invention relates to the field of C04B35/10, in particular to modified nano-alumina and a preparation method and application thereof.
Background
With the improvement of national requirements on energy conservation and emission reduction, the traditional thermal insulation material cannot adapt to the high-speed development of the industry. The search for novel high-efficiency refractory heat-insulating materials has become a common demand in industries such as petrifaction, metallurgy, ceramic kilns and the like. Super insulation, proposed by Hunt a.j. 1992, is an insulation material that has a thermal conductivity less than that of still air at the temperature of use. At present, the gas phase is used for nano SiO 2 Or gas phase nano Al 2 O 3 The nano microporous heat-insulating plate used as a main material is well popularized and used in industry.
However, the nano microporous thermal insulation plate produced in the market at present is mainly formed by pressing powder, and the powder lacks bonding force, so that the material is low in strength and easy to crack. The product is easy to generate larger linear shrinkage when used at high temperature; chinese patent CN111285662B discloses a method for preparing a high-heat-insulation nano-microporous heat-insulation plate, which specifically adopts fumed silica, fumed aluminum dioxide, an opacifier and fibers as raw materials, so that the provided nano-microporous heat-insulation plate has a high heat-insulation effect, but the fumed silica and the fumed aluminum dioxide nanoparticles adopted have high surface energy and large specific surface area, and are easy to agglomerate in the blending process to form secondary particles, so that the performance of the nano-microporous heat-insulation plate is reduced.
Therefore, aiming at the problems, the invention provides the modified nano-alumina and the preparation method thereof, so that when the provided modified nano-alumina is applied to the subsequent preparation of the nano-microporous thermal insulation plate, the nano-particle agglomeration is effectively inhibited, the mechanical property of the nano-microporous thermal insulation plate is greatly improved, the cracking phenomenon in use at high temperature is effectively inhibited, and the modified nano-alumina has high practical application and popularization values.
Disclosure of Invention
The invention provides modified nano-alumina, which at least comprises the following raw materials in parts by weight: 80-120 parts of nano alumina and 1-8 parts of modifier.
As a preferable technical scheme, the mass ratio of the nano alumina to the modifier is 100: (2-5).
As a preferable technical scheme, the purity of the nano alumina is more than or equal to 99.99 percent, and the particle size of the nano alumina is 10-50nm. Preferably, the particle size of the nano alumina is 10-30nm; the product numbers of the nano-alumina are A810837, A801481 and A800941, which are from Shanghai Michelin Biochemical technology Co., ltd.
The inventor finds that the purity of the raw material nano alumina is controlled to be more than or equal to 99.99 percent in the process of preparing the modified nano alumina, so that the influence of impurities in the nano alumina on the stability of the modification process is avoided, the nano alumina has higher reaction activity, is easy to fully react with a modifier, and the purity of the prepared modified nano alumina is ensured.
As a preferable technical scheme, the modifier structure contains one of vinyl, aminopropyl, epoxy group and glycidyl ether oxygen functional group; preferably, the modifier is selected from one or a combination of more of vinyltriethoxysilane, aminopropyltrimethoxysilane, aminopropyltriethoxysilane and 3-glycidoxypropyltrimethoxysilane.
Based on the system, a modifier with a specific functional group is introduced into the system by control, the modifier is firstly subjected to hydrolysis reaction to form silicon hydroxyl, then subjected to condensation reaction, subjected to hydrogen bond combination with hydroxyl adsorbed on the surface of nano alumina, and finally dehydrated to obtain modified nano alumina; the introduction of the modifier can react with a large amount of hydroxyl groups on the surface of the nano alumina, effectively reduce the surface energy of the nano alumina, increase the steric hindrance of the surface of the modified nano alumina, effectively inhibit the particle agglomeration, and further improve the stability of the modified nano alumina applied to the subsequent preparation process of the nano microporous insulation board.
On the other hand, when the modified nano-alumina prepared by adopting the modifier with the specific functional group is applied to the process of preparing the nano-microporous thermal insulation plate, the bonding force among nano-alumina particles is effectively improved, and meanwhile, the obtained modified nano-alumina has excellent compatibility and dispersibility in a nano-microporous thermal insulation plate system, so that the mechanical property of the nano-alumina thermal insulation plate is effectively improved, and the cracking phenomenon of the nano-alumina thermal insulation plate used at high temperature is effectively inhibited.
The invention also provides a preparation method of the modified nano-alumina, which at least comprises the following steps:
(1) Adding the nano alumina and the modifier into a high-speed blender for blending according to the parts by weight;
(2) And then heating to 200-220 ℃ for modification reaction to obtain the modified starch.
Preferably, the rotating speed of the high-speed blender in the step (1) is 300-400rpm.
Preferably, the blending time in the step (1) is 40-60min.
Preferably, the modification reaction time in the step (2) is 45-60min.
The third aspect of the invention provides an application of modified nano-alumina, which is applied to preparing a nano-microporous heat insulation plate;
as a preferred technical scheme, the raw materials for preparing the nano-microporous thermal insulation plate at least comprise the following components in parts by weight: 50-70 parts of modified nano aluminum oxide, 15-40 parts of infrared shielding agent and 10-15 parts of inorganic chopped fiber;
as a preferred technical scheme, the infrared shielding agent is silicon carbide and/or nano titanium oxide;
in a preferred embodiment, the inorganic chopped fibers are ceramic fibers and/or glass fibers.
The preparation method of the nano microporous thermal insulation plate comprises the steps of adding the modified nano alumina, the infrared shielding agent and the inorganic short-cut fibers into a high-speed blender according to parts by weight, mixing and stirring for 20-30min to obtain a mixed material, and then carrying out dry pressing on the mixed material to obtain the nano microporous thermal insulation plate.
Preferably, the pressure of the dry pressing molding is 5-12MPa, and the time is 5-10min.
Advantageous effects
1. The invention provides modified nano-alumina and a preparation method thereof, so that when the modified nano-alumina is applied to the subsequent preparation of a nano-microporous thermal insulation plate, the agglomeration of nano-particles is effectively inhibited, the mechanical property of the nano-microporous thermal insulation plate is greatly improved, the cracking phenomenon in use at high temperature is effectively inhibited, and the modified nano-alumina has high practical application and popularization values.
2. Based on the system, the purity of the raw material nano alumina is controlled to be more than or equal to 99.99%, impurities in the nano alumina are prevented from influencing the stability of the modification process, the nano alumina has higher reaction activity and is easy to fully react with a modifier, and the purity of the prepared modified nano alumina is ensured.
3. Based on the system, the introduction of the modifier can react with a large amount of hydroxyl groups on the surface of the nano-alumina, so that the surface energy of the nano-alumina is effectively reduced, the steric hindrance of the surface of the prepared modified nano-alumina is increased, the particle agglomeration is effectively inhibited, and the stability of the modified nano-alumina applied to the subsequent preparation process of the nano-microporous thermal insulation plate is further improved.
4. The modified nano-alumina prepared by adopting the modifier with specific functional groups is applied to the process of preparing the nano-microporous thermal insulation plate, so that the bonding force among nano-alumina particles is effectively improved, and the obtained modified nano-alumina has excellent compatibility and dispersibility in a nano-microporous thermal insulation plate system, thereby effectively improving the mechanical property of the nano-alumina thermal insulation plate and effectively inhibiting the cracking phenomenon used at high temperature.
Detailed Description
Example 1
The embodiment 1 of the invention provides modified nano alumina, which comprises the following raw materials in parts by weight: 100 parts of nano alumina and 2 parts of modifier.
The purity of the nano alumina is more than 99.99 percent, and the particle size of the nano alumina is 10nm. The product number of the nano alumina is A800941, which is sourced from Shanghai Michelin Biochemical technology, inc.
The modifier is vinyl triethoxysilane.
In another aspect, embodiment 1 of the present invention provides a method for preparing modified nano aluminum oxide, including the following steps:
(1) Adding the nano alumina and the modifier into a high-speed blender for blending according to the parts by weight;
(2) And then heating to 200 ℃ for modification reaction to obtain the modified starch.
The rotating speed of the high-speed blender in the step (1) is 300rpm.
The blending time in the step (1) is 45min.
The modification reaction time in the step (2) is 45min.
The third aspect of embodiment 1 of the invention provides an application of modified nano alumina, which is applied to preparing a nano microporous insulation board;
the nano microporous insulation board comprises the following raw materials in parts by weight: 50 parts of modified nano aluminum oxide, 15 parts of infrared shielding agent and 10 parts of inorganic chopped fiber;
the infrared shielding agent is nano titanium oxide; the nano titanium oxide is R012669, and is from Shanghai Yi En chemical technology Co.
The inorganic chopped fibers are glass fibers.
The preparation method of the nano microporous thermal insulation plate comprises the steps of adding the modified nano alumina, the infrared shielding agent and the inorganic short-cut fibers into a high-speed blender according to parts by weight, controlling the stirring speed to be 300rpm, mixing and stirring for 20min to obtain a mixed material, and then carrying out dry pressing on the mixed material to obtain the nano microporous thermal insulation plate.
The pressure of the dry pressing molding is 5MPa, and the time is 5min.
Example 2
Embodiment 2 of the present invention provides, on the one hand, a modified nano alumina, which is prepared from the following raw materials in parts by weight: 100 parts of nano aluminum oxide and 3 parts of modifier.
The purity of the nano alumina is 99.99%, and the particle size of the nano alumina is 20nm. The product number of the nano alumina is A810837, which is from Shanghai Michelin Biochemical technology Co., ltd.
The modifier is a combination of aminopropyl trimethoxy silane and 3-glycidyl ether oxygen propyl trimethoxy silane; the mass ratio of the aminopropyltrimethoxysilane to the 3-glycidoxypropyltrimethoxysilane is 2.
The embodiment 2 of the invention provides a preparation method of modified nano-alumina, which comprises the following steps:
(1) Adding the nano alumina and the modifier into a high-speed blender for blending according to the parts by weight;
(2) And then heating to 210 ℃ for modification reaction to obtain the modified polycarbonate.
The rotating speed of the high-speed blender in the step (1) is 350rpm.
The blending time in the step (1) is 50min.
The modification reaction time in the step (2) is 50min.
The third aspect of the embodiment 2 of the invention provides an application of modified nano alumina, which is applied to preparing a nano microporous insulation board;
the nano microporous insulation board comprises the following raw materials in parts by weight: 60 parts of modified nano-alumina, 25 parts of infrared shielding agent and 12 parts of inorganic chopped fiber;
the infrared shielding agent is silicon carbide, has the grain diameter of 100nm and is sourced from Shanghai Po micro application materials technology Limited company;
the inorganic chopped fibers are glass fibers.
The preparation method of the nano microporous thermal insulation plate comprises the steps of adding the modified nano alumina, the infrared shielding agent and the inorganic short fibers into a high-speed blender in parts by weight, controlling the stirring speed to be 350rpm, mixing and stirring for 25min to obtain a mixed material, and then carrying out dry pressing and forming on the mixed material to obtain the nano microporous thermal insulation plate.
The pressure of the dry pressing molding is 7MPa, and the time is 8min.
Example 3
Embodiment 3 of the present invention provides a modified nano alumina, which comprises the following raw materials, by weight: 100 parts of nano alumina and 5 parts of modifier.
The purity of the nano alumina is 99.99%, and the particle size of the nano alumina is 30nm. The product number of the nano alumina is A801481, and the nano alumina is from Shanghai Michelin Biochemical technology Co.
The modifier is 3-glycidoxypropyltrimethoxysilane.
In another aspect, embodiment 3 of the present invention provides a method for preparing a modified nano aluminum oxide, including the following steps:
(1) Adding the nano alumina and the modifier into a high-speed blender for blending according to the parts by weight;
(2) And then heating to 215 ℃ for modification reaction to obtain the modified polycarbonate.
The rotating speed of the high-speed blender in the step (1) is 350rpm.
The blending time in the step (1) is 55min.
The modification reaction time in the step (2) is 55min.
The third aspect of the embodiment 3 of the invention provides an application of modified nano alumina, which is applied to preparing a nano microporous thermal insulation board;
the preparation raw materials of the nano microporous insulation board comprise the following components in parts by weight: 70 parts of modified nano-alumina, 40 parts of infrared shielding agent and 15 parts of inorganic chopped fiber;
the infrared shielding agent is nano titanium oxide; the nano titanium oxide is R012669, and is from Shanghai Yi En chemical technology Co.
The inorganic chopped fibers are glass fibers.
The preparation method of the nano microporous thermal insulation plate comprises the steps of adding the modified nano alumina, the infrared shielding agent and the inorganic short fibers into a high-speed blender in parts by weight, controlling the stirring speed to be 350rpm, mixing and stirring for 28min to obtain a mixed material, and then carrying out dry pressing and forming on the mixed material to obtain the nano microporous thermal insulation plate.
The pressure of the dry pressing molding is 10MPa, and the time is 10min.
Comparative example 1
Comparative example 1 of the present invention provides a modified nano alumina, which is the same as example 1 in the specific embodiment, except that the modifier is a titanate coupling agent 101.
Comparative example 2
Comparative example 2 of the present invention provides a modified nano alumina, which is similar to example 1, except that the modifier is (3-glycidoxypropyl) triethoxysilane.
Performance test method
The thermal conductivity, linear shrinkage and compression resistance of the nano microporous thermal insulation boards prepared in the examples and the comparative examples are tested, and the performance test results are shown in table 1.
TABLE 1,
Claims (10)
1. The modified nano-alumina is characterized by comprising the following preparation raw materials in parts by weight: 80-120 parts of nano alumina and 1-8 parts of modifier.
2. The modified nano alumina of claim 1, wherein the mass ratio of the nano alumina to the modifier is 100: (2-5).
3. The modified nano alumina according to claim 1 or 2, wherein the purity of the nano alumina is not less than 99%, and the particle size of the nano alumina is 10-50nm.
4. The modified nano-alumina of claim 3, wherein the modifier structure comprises one of vinyl, aminopropyl, epoxy and glycidyl ether oxygen functional groups.
5. The modified nano-alumina of claim 4, wherein the modifier is selected from one or a combination of vinyl triethoxysilane, aminopropyl trimethoxysilane, aminopropyl triethoxysilane, and 3-glycidoxypropyl trimethoxysilane.
6. A method for preparing modified nano alumina according to any one of claims 1 to 5, characterized by comprising at least the following steps:
(1) Adding the nano aluminum oxide and the modifier into a high-speed blender for blending according to the parts by weight;
(2) And then heating to 200-220 ℃ for modification reaction to obtain the modified starch.
7. The method for preparing modified nano alumina according to claim 6, wherein the blending time in the step (1) is 40-60min; the modification reaction time in the step (2) is 45-60min.
8. Use of a modified nano alumina according to any one of claims 1 to 5 for the preparation of nano microporous thermal insulation panels.
9. The application of the modified nano alumina as claimed in claim 8, wherein the raw materials for preparing the nano microporous thermal insulation board at least comprise the following components in parts by weight: 50-70 parts of modified nano-alumina, 15-40 parts of infrared shielding agent and 10-15 parts of inorganic chopped fiber.
10. The use of the modified nano alumina of claim 9, wherein the inorganic chopped fibers are ceramic fibers and/or glass fibers.
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