CN107266774B - Aerogel composite material and preparation method thereof - Google Patents
Aerogel composite material and preparation method thereof Download PDFInfo
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- CN107266774B CN107266774B CN201610214830.3A CN201610214830A CN107266774B CN 107266774 B CN107266774 B CN 107266774B CN 201610214830 A CN201610214830 A CN 201610214830A CN 107266774 B CN107266774 B CN 107266774B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
Abstract
The invention discloses an aerogel composite material and a preparation method thereof. The preparation method of the aerogel composite material comprises the following steps: (1) mixing the aerogel powder and the hot melt adhesive powder, and mechanically stirring; (2) and (3) carrying out hot-press molding on the dry mixture obtained in the step (1). The aerogel powder in the aerogel composite material is of a nano porous structure, has excellent heat insulation performance and mechanical property, and has a huge market application prospect.
Description
Technical Field
The invention relates to a heat-insulating material, in particular to an aerogel composite material and a preparation method thereof, belonging to the fields of light weight, heat insulation, sound insulation materials and the like.
Background
The aerogel is a light solid material which is formed by accumulating nano-scale particles and has nano-scale holes, has extremely high porosity and specific surface area, extremely low density and solid content, chemical inertness and incombustibility, shows excellent characteristics of light weight, heat preservation, heat insulation, fire prevention, sound insulation, shock absorption and energy absorption, and can be widely applied to military fields of national defense and military industry, security and antiterrorism and the like and civil fields of green buildings, heat transmission, public transportation, financial equipment protection and the like.
However, because of the inherent defects of aerogel, such as low strength and high brittleness, the mechanical properties of aerogel and composite materials can be expected to be improved by compounding aerogel with other materials on the premise of not damaging the nano porous structure of aerogel.
Disclosure of Invention
In order to solve the technical problems, the invention provides an aerogel composite material and a preparation method thereof.
The aerogel composite material mainly comprises aerogel powder and a hot melt adhesive, wherein the aerogel powder is in a nano porous structure in the hot melt adhesive.
In one embodiment, the hot melt adhesive is one or more of ethylene-vinyl acetate copolymer powder, ethylene ethyl acrylate copolymer powder, polyvinyl alcohol powder, polyethylene powder, polyvinyl chloride powder and polyurethane powder.
A method of preparing an aerogel composite, comprising the steps of:
(1) mixing the aerogel powder and the hot melt adhesive powder, and mechanically stirring;
(2) and (3) carrying out hot-press molding on the dry mixture obtained in the step (1).
In one embodiment, the phase change energy storage material, the flame retardant and other heat insulation materials can be added in the step (1).
In one embodiment, the phase change energy storage material is one or more of inorganic water and salt, higher aliphatic hydrocarbon, polyalcohol and polyhydroxy carboxylic acid which are coated by microcapsules; the flame retardant is a char forming agent, a foaming agent and a catalyst; the charring agent is one or more of pentaerythritol, starch, dipentaerythritol, erythritol, sorbitol and inositol; the foaming agent is one or more of melamine, urea, polyamide, dicyandiamide, chlorinated paraffin, polyurea, melamine and glycine; the catalyst is one or more of ammonium polyphosphate, ammonium bicarbonate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium sulfate and formic acid; the flame retardant also comprises one or more of magnesium hydroxide, modified magnesium hydroxide, aluminum hydroxide, modified aluminum hydroxide and borax.
In one embodiment, step (1) is preceded by a step of hydrophobically modifying the aerogel powder.
In one embodiment, the hydrophobic modification is to perform hydrophobic modification on the aerogel powder in a closed hydrophobic modifier gas phase environment.
In one embodiment, the hydrophobic modifier is one or more mixtures of trimethylchlorosilane, hexamethyldisilazane, hexamethyldisiloxane, methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane.
In one embodiment, the hot press molding in the step (2) is performed at 50-300 ℃, under 0.01-100 MPa, and for 10-300 min.
The aerogel composite material has the heat conductivity coefficient of 0.015-0.035W/m.K, excellent mechanical properties, no powder falling on the surface and wide application prospect.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The embodiment of the aerogel composite material mainly comprises aerogel powder and hot melt adhesive, wherein the aerogel powder is in a nano porous structure in the hot melt adhesive.
Therefore, the aerogel composite material provided by the invention takes the aerogel powder as the filler to provide the properties of heat preservation, heat insulation, sound insulation and the like, and takes the hot melt adhesive as the matrix to provide the mechanical properties.
In this embodiment, the hot melt adhesive is one or more of ethylene-vinyl acetate copolymer powder, ethylene ethyl acrylate copolymer powder, polyvinyl alcohol powder, polyethylene powder, polyvinyl chloride powder, and polyurethane powder.
So, different hot melt adhesives have different physical and chemical properties and mechanical properties, select a hot melt adhesive or multiple hot melt adhesive is compound according to the application demand for aerogel combined material performance and application are diversified.
A method of preparing an aerogel composite, comprising the steps of:
(1) mixing the aerogel powder and the hot melt adhesive powder, and mechanically stirring;
(2) and (3) carrying out hot-press molding on the dry mixture obtained in the step (1).
In addition, the mass ratio of the aerogel powder to the hot melt adhesive powder in the step (1) can be 1 (0.1-10), heat insulation materials such as vitrified micro-beads, expanded perlite, ceramic micro-beads, expanded polystyrene particles and expanded polyurethane particles can be added in the step (1), the particle size of the aerogel powder can be 0.01-20 mm, and the particle size of the hot melt adhesive powder can be 10-200 mu m; in the step (2), the hot melt adhesive has certain viscosity and fluidity by utilizing the process, the viscosity of the hot melt adhesive is adjusted by regulating and controlling the parameters of the hot pressing process, the rate of the hot melt adhesive entering the surface nano-pores of the aerogel powder is controlled, the aerogel powder and the hot melt adhesive have good interface combination, and most nano-porous structures of the aerogel are guaranteed to be reserved.
Therefore, the preparation method of the aerogel composite material is simple in process, practical, low in price and suitable for industrial production.
In one embodiment, the phase change energy storage material and the flame retardant can be added in the step (1).
In one embodiment, the phase change energy storage material is one or more of inorganic water and salt, higher aliphatic hydrocarbon, polyalcohol and polyhydroxy carboxylic acid which are coated by microcapsules; the flame retardant is a char forming agent, a foaming agent and a catalyst; the charring agent is one or more of pentaerythritol, starch, dipentaerythritol, erythritol, sorbitol and inositol; the foaming agent is one or more of melamine, urea, polyamide, dicyandiamide, chlorinated paraffin, polyurea, melamine and glycine; the catalyst is one or more of ammonium polyphosphate, ammonium bicarbonate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium sulfate and formic acid; the flame retardant also comprises one or more of magnesium hydroxide, modified magnesium hydroxide, aluminum hydroxide, modified aluminum hydroxide and borax.
Therefore, the phase-change energy storage material can absorb or release a large amount of heat energy through phase change and has an energy storage effect, when the aerogel composite material is used for a building wall, the indoor temperature of the building can be adjusted, the building comfort level is improved, energy is saved, and the linear shrinkage value of the aerogel composite material can be reduced by adding the phase-change energy storage material; adding a carbon forming agent, a foaming agent and a catalyst into the aerogel composite material, so that the aerogel composite material expands when encountering fire, a foam carbon layer is generated on the surface, and heat is prevented from being transferred to the base material; because magnesium hydroxide, aluminum hydroxide, borax and the like can generate dehydration endothermic reaction when being heated, the addition of magnesium hydroxide, aluminum hydroxide, borax and the like into the aerogel composite material can prolong the time of transferring heat to the base material and improve the fire resistance limit.
In this embodiment, step (1) includes a step of hydrophobic modification of the aerogel powder.
Therefore, in the existing aerogel preparation method, the precursor, the replacement solvent and the drying process have great influence on the hydrophobicity of the aerogel, and if the contact angle of the surface of the aerogel and water is more than 90 degrees, the surface hydrophilic modification can be directly carried out without carrying out hydrophobic modification in advance; if the contact angle of the surface of the aerogel with water is less than 90 °, hydrophobic modification is required in advance.
In this embodiment, the hydrophobic modification is to perform hydrophobic modification on the aerogel powder in a closed hydrophobic modifier gas-phase environment.
So, carry out hydrophobic modification to aerogel powder in inclosed hydrophobic modifier gaseous phase environment, except showing the modification effect who improves aerogel powder, inside nanometer porous structure is not destroyed when guaranteeing follow-up hydrophilic modification, still shows improvement modification efficiency and production efficiency, reduction in production cost.
In this embodiment, the hydrophobic modifier is one or more of trimethylchlorosilane, hexamethyldisilazane, hexamethyldisiloxane, methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, and N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane.
Therefore, different hydrophobic modifiers and the aerogel have different reactivity, and the aerogel powder is modified by selecting one or more hydrophobic modifiers, so that the modification efficiency and the modification effect are improved.
In this embodiment, the temperature of the hot press molding in the step (2) is 50 to 300 ℃, the pressure is 0.01 to 100MPa, and the processing time is 10 to 300 min.
So, carry out hot briquetting through the dry blend of constituteing aerogel powder and hot melt adhesive powder and handle for the hot melt adhesive bonds aerogel powder together, remains the nanometer porous structure of aerogel, improves aerogel combined material's mechanical properties.
The thermal conductivity coefficient of the aerogel composite material is 0.015-0.035W/m.K, the aerogel composite material has excellent mechanical property, powder does not fall off, and the aerogel composite material has a wide application prospect.
The following is a detailed description of the embodiments.
Example 1
SiO is prepared by the following steps2Aerogel composite material:
(1) detection of SiO to be treated by contact Angle measuring apparatus2The contact angle of the surface of the aerogel powder and water is 55 degrees, and then the SiO with the particle size of 56 mu m is used2Placing the aerogel powder in a vacuum heating furnace, placing the weighed hexamethyldisilazane in the vacuum heating furnace by using a container, heating and gasifying, and carrying out hydrophobic modification for 1.5h to obtain hydrophobic SiO2Aerogel powder, detecting hydrophobic SiO with contact angle measuring instrument2The contact angle between the surface of the aerogel powder and water is 147 degrees;
(2) mixing the aerogel powder, the aluminum hydroxide powder and the EVA hot melt adhesive powder in the step (1) according to the mass ratio of 1:1, and mechanically stirring for 30min at the stirring speed of 1500 revolutions per minute;
(3) carrying out hot pressing treatment on the dry mixture obtained in the step (2) at 105 ℃, 1MPa for 20min to obtain SiO2An aerogel composite. Table 1 shows SiO obtained in this example2Performance index of aerogel composite.
TABLE 1 SiO2Performance index of aerogel composites
Example 2
SiO is prepared by the following steps2Aerogel composite material:
(1) detection of SiO to be treated by contact Angle measuring apparatus2The contact angle of the surface of the aerogel powder and water is 45 degrees, and then SiO with the particle size of 12mm is added2Placing the aerogel powder in a vacuum heating furnace, placing the weighed trimethylchlorosilane in the vacuum heating furnace by using a container, heating and gasifying, and performing hydrophobic modification for 1.5h to obtain hydrophobic SiO2Aerogel powder, detecting hydrophobic SiO with contact angle measuring instrument2The contact angle between the surface of the aerogel powder and water is 146 degrees;
(2) weighing the SiO prepared in the step (1) according to the mass ratio of 1:0.52Mechanically stirring the aerogel powder, the microcapsule-coated octadecane and the EAA hot melt adhesive for 10min at the stirring speed of 1500 revolutions per minute;
(3) carrying out hot pressing treatment on the dry mixture obtained in the step (2) at the temperature of 110 ℃, the pressure of 0.1MPa and the time of 20min to obtain SiO2An aerogel composite. Table 2 shows SiO produced in this example2Performance index of aerogel composite.
TABLE 2 SiO2Performance index of aerogel composites
Example 3
SiO is prepared by the following steps2Aerogel composite material:
(1) detection of SiO to be treated by contact Angle measuring apparatus2The contact angle between the surface of the aerogel powder and water is 45 degrees, and then SiO with the grain diameter of 0.1mm is added2Placing the aerogel powder in a vacuum heating furnace, placing the weighed hexamethyldisilazane in the vacuum heating furnace by using a container, heating and gasifying, and carrying out hydrophobic modification for 1.5h to obtain hydrophobic SiO2Aerogel powder, detecting hydrophobic SiO with contact angle measuring instrument2The contact angle between the surface of the aerogel powder and water is 141 degrees;
(2) weighing SiO in the step (1) according to the mass ratio of 1:12Mixing the aerogel powder and the PU hot melt adhesive, and mechanically stirring for 30min at the stirring speed of 1000 revolutions per minute;
(3) carrying out hot pressing treatment on the dry mixed material obtained in the step (2) at the temperature of 190 ℃, the pressure of 20MPa and the time of 15min to obtain SiO2An aerogel composite. Table 3 shows SiO obtained in this example2Performance index of aerogel composite.
TABLE 3 SiO2Performance index of aerogel composites
Example 4
SiO is prepared by the following steps2Aerogel composite material:
(1) SiO with particle size of 77 μm to be treated was detected by using a contact angle measuring instrument2The contact angle between the surface of the aerogel powder and water is 140 degrees according to the detection result, and then the SiO is obtained2The aerogel powder has hydrophobicity;
(2) weighing SiO in the step (1) according to the mass ratio of 1:0.82Mixing the aerogel powder and the PVA hot melt adhesive, and mechanically stirring for 30min at the stirring speed of 1500 revolutions per minute;
(3) carrying out hot pressing treatment on the dry mixed material obtained in the step (2) at the temperature of 100 ℃, the pressure of 10MPa and the time of 15min to obtain SiO2An aerogel composite. Table 4 shows SiO obtained in this example2Performance index of aerogel composite.
TABLE 4 SiO2Performance index of aerogel composites
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (1)
1. The preparation method of the aerogel composite material comprises the following steps of preparing SiO2Aerogel composite material:
(1) detection of SiO to be treated by contact Angle measuring apparatus2The contact angle between the surface of the aerogel powder and water is 45 degrees, and then SiO with the grain diameter of 0.1mm is added2Placing the aerogel powder in a vacuum heating furnace, placing the weighed hexamethyldisilazane in the vacuum heating furnace by using a container, heating and gasifying, and carrying out hydrophobic modification for 1.5h to obtain hydrophobic SiO2Aerogel powder, detecting hydrophobic SiO with contact angle measuring instrument2The contact angle between the surface of the aerogel powder and water is 141 degrees;
(2) weighing the SiO prepared in the step (1) according to the mass ratio of 1:12Mixing the aerogel powder and the PU hot melt adhesive, and mechanically stirring for 30min at the stirring speed of 1000 revolutions per minute;
(3) carrying out hot pressing treatment on the dry mixed material obtained in the step (2) at the temperature of 190 ℃, the pressure of 20MPa and the time of 15min to obtain SiO2An aerogel composite having a thermal conductivity of 0.025W/mK and a bulk weight of 261 kg/m3The compressive strength is 3.8MPa, and the flexural strength is 2.7 MPa.
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| CN109385254B (en) * | 2018-11-26 | 2021-03-26 | 同济大学 | Graphene elastic polymer phase-change composite material and preparation method thereof |
| CN111619192A (en) * | 2019-02-27 | 2020-09-04 | 南通市通州区先锋誉佳衬布厂 | Composite material containing aerogel, composite fabric and preparation method of composite material |
| CN109912874A (en) * | 2019-03-18 | 2019-06-21 | 罗瑞尔纳米合成材料(江苏)有限公司 | A kind of preparation method of nano porous high-efficiency heat insulation polyethylene film |
| CN111825901A (en) * | 2019-04-15 | 2020-10-27 | 江苏泛亚微透科技股份有限公司 | Silicon dioxide aerogel flexible elastic heat insulation composite material and preparation method thereof |
| CN110540696A (en) * | 2019-09-26 | 2019-12-06 | 广州恩沣新材料科技有限公司 | Aerogel EVA light breathable heat-insulation composite material and preparation method thereof |
| CN111269557A (en) * | 2020-04-14 | 2020-06-12 | 烟台恒诺新材料有限公司 | Preparation method of hollow nano microsphere modified high-molecular heat-insulation material |
| CN112796114B (en) * | 2020-12-04 | 2022-10-11 | 卿星 | Method for modifying textile through low-temperature melting and bonding of composite powder |
| CN114804818B (en) * | 2022-05-24 | 2023-04-11 | 巩义市泛锐熠辉复合材料有限公司 | Low-cost aerogel composite material and preparation method thereof |
| CN116120620A (en) * | 2023-03-07 | 2023-05-16 | 北京清冠科技有限公司 | Preparation method of low-density aerogel/polyvinyl chloride foam composite material |
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| WO1997010187A1 (en) * | 1995-09-11 | 1997-03-20 | Hoechst Research & Technology | Aerogel and adhesive-containing composite, process for its production and its use |
| DE19533564A1 (en) * | 1995-09-11 | 1997-03-13 | Hoechst Ag | Fibrous airgel composite material |
| WO2007047970A2 (en) * | 2005-10-21 | 2007-04-26 | Cabot Corporation | Aerogel based composites |
| CN101143981A (en) * | 2007-09-14 | 2008-03-19 | 哈尔滨工业大学 | Powder coating containing aerogel particles and preparing method thereof |
| CN101880418B (en) * | 2010-06-30 | 2012-08-22 | 华南理工大学 | Transparent EVA heat insulating material and preparation method thereof |
| CN102881909B (en) * | 2011-07-13 | 2015-02-04 | 北京林业大学 | Defluorination carbon electrode and its preparation method |
| CN104558745A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Thermal insulation raw material, thermal insulation material and multilayered composite material |
| CN103641201A (en) * | 2013-12-03 | 2014-03-19 | 北京林业大学 | Preparation method of fluoride removal electric adsorption lanthanum-loaded electrode for drinking water and fluoride removal electrode |
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| DE4342548A1 (en) * | 1993-12-14 | 1995-06-22 | Hoechst Ag | Xerogels, processes for their manufacture and their use |
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