CN108623325B - Preparation method of aerogel composite material - Google Patents
Preparation method of aerogel composite material Download PDFInfo
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- CN108623325B CN108623325B CN201710162210.4A CN201710162210A CN108623325B CN 108623325 B CN108623325 B CN 108623325B CN 201710162210 A CN201710162210 A CN 201710162210A CN 108623325 B CN108623325 B CN 108623325B
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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
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
- C04B38/085—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances of micro- or nanosize
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C67/00—Shaping techniques not covered by groups B29C39/00 - B29C65/00, B29C70/00 or B29C73/00
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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
- C04B20/0016—Granular materials, e.g. microballoons
- C04B20/002—Hollow or porous granular materials
- C04B20/0036—Microsized or nanosized
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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
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0003—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability making use of electric or wave energy or particle radiation
- C04B40/001—Electromagnetic waves
- C04B40/0017—Irradiation, i.e. gamma -, X -, UV rays
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/02—Selection of the hardening environment
- C04B40/0204—Selection of the hardening environment making use of electric or wave energy or particle radiation
- C04B40/0213—Electromagnetic waves
- C04B40/0222—Irradiation, i.e. gamma -, X -, UV rays
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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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Abstract
The invention provides a preparation method of an aerogel composite material, wherein the aerogel composite material consists of aerogel and a resin phase for bonding the aerogel. The preparation method comprises the following steps: (1) mixing materials, namely uniformly mixing aerogel and resin powder; (2) paving, namely paving a layer of mixture obtained in the step (1) on a mould substrate; (3) melting, namely rapidly heating the resin powder in the mixture obtained in the step (2) to be molten in a step scanning mode by using a laser; (4) alternately spreading and melting, and alternately repeating the step (2) and the step (3) on the previous deposition layer; (5) and (5) curing. The aerogel composite material disclosed by the invention has better heat insulation and heat preservation performance, light transmittance, safety performance and sound insulation and noise reduction performance, and is suitable for the fields of doors and windows, curtain wall glass, lighting roofs and the like of green buildings, ultralow energy consumption buildings and near-zero energy consumption buildings.
Description
Technical Field
The invention relates to the technical field of preparation of composite materials, in particular to a preparation method of an aerogel composite material.
Background
The aerogel is a light nano solid material which is formed by mutually gathering nano-scale ultrafine particles to form a nano porous network structure and is filled with gaseous dispersion media in network pores. The porosity is as high as 99.8%, the typical size of the holes is 1-40 nm, and the specific surface area is 400-1200 m2In terms of/g, and a density as low as 3kg/m3The heat conductivity coefficient at room temperature can be as low as below 0.010W/(m.k), and the light-weight, light-transmitting, heat-insulating, heat-preserving, sound-insulating, fireproof and impact-resistant light-weight material has excellent chemical stability and non-inflammability. Due to the characteristics, the silica aerogel material has wide application potential in the aspects of thermal, acoustic, optical, microelectronic, particle detection and the like.
However, the conventional sol-gel process is complicated, and the comprehensive technical threshold for producing large-size complete transparent aerogel plates is extremely high, which not only relates to the material technology, but also relates to numerous technical fields such as the process technology and the process equipment technology, and therefore, the large-size complete aerogel is difficult to prepare. In addition, because the aerogel is fragile material, breaking strength is relatively poor, can not use alone, can only regard as cavity glass's sandwich layer to use, has restricted the application range of aerogel in the transparent envelope field of building to a certain extent, because glass is from great, has increased the load of building undoubtedly moreover, makes the building have certain potential safety hazard. Therefore, it is highly desirable to develop a transparent, large-sized, high-strength and lightweight building energy-saving material having excellent heat insulation and preservation properties.
Disclosure of Invention
In order to obtain a large-size, high-strength and light-weight building energy-saving material with excellent heat insulation performance, the solution of the invention is as follows: (1) the problem that the aerogel and resin are difficult to mix is solved by adopting a transparent heat-insulating aerogel technology with silicon hydroxyl on the surface and hydrophobic property inside. Because the surface of the aerogel has a large amount of Si-OH energy which has compatibility and bonding effect with the active functional groups on the surface of the resin, the wetting and coating effect of the resin on the surface of the aerogel is further improved, the interface bonding strength of the aerogel and the resin is increased, on one hand, the uniform distribution of the aerogel in the resin is favorably improved, and on the other hand, the heat insulation and preservation performances of the aerogel and the high-strength and high-toughness performance of the resin are fully exerted. (2) And (3) a rapid curing and forming process. Since aerogels are light, they tend to delaminate, making uniform distribution in the resin difficult. According to the invention, the resin powder in the mixture of the aerogel and the resin powder is rapidly heated to be molten by using the laser in a step scanning manner, and then is rapidly cured, so that the layering phenomenon is greatly reduced, namely, the viscosity of the resin binder is adjusted by controlling the laser heating energy and the moving-out speed, the aerogel is effectively prevented from layering, the uniform distribution of the aerogel in a resin matrix is realized, meanwhile, the structural characteristics of the aerogel nano-pores are not damaged, and the excellent characteristics of the aerogel are fully exerted. In addition, the rapid curing molding process can be automatically, directly and rapidly molded into various shapes and structures, equipment and molds of the traditional production line are not needed, leftover materials cannot be produced additionally, the utilization rate of materials is improved, and the manufacturing cost is saved.
The solution of the invention is realized by the following steps: a method of preparing an aerogel composite, comprising the steps of:
(1) mixing materials, namely uniformly mixing resin powder and aerogel;
(2) paving, namely paving a layer of mixture obtained in the step (1) on a mould substrate;
(3) melting, namely rapidly heating the resin in the mixture obtained in the step (2) to be molten in a step scanning manner by using a laser;
(4) and (3) alternately spreading and melting, and alternately repeating the step (2) and the step (3) on the previous deposition layer for solidification.
Therefore, through the steps of mixing, paving, laser rapid heating, rapid curing and the like, the aerogel composite material which is composed of aerogel and resin phase bonded with the aerogel and has heat insulation and preservation performance can be obtained. According to the invention, the resin in the mixture of the aerogel and the resin powder is rapidly heated to be molten by using a laser in a step scanning manner, and then is rapidly cured, however, the aerogel is light and easy to delaminate, and uniform distribution is difficult to realize. In addition, the rapid curing forming process can automatically, directly and rapidly form the heat insulation boards with various shapes and structures, the problems that the heat insulation boards with special and complex shapes are difficult to prepare in online production and the like are solved, equipment, dies and the like of a traditional production line are not needed, the manufacturing cost is saved, and meanwhile, the utilization rate of materials is also improved. The obtained aerogel composite material uses transparent aerogel which is light in weight, has excellent heat insulation performance, sound insulation and noise reduction performance and energy absorption performance as functional components, resin is added as a reinforcing binder, and the composite material consisting of the aerogel and the resin is prepared due to the fact that the resin is light in weight, high in compressive strength and hardness and easy to obtain large size.
Another technical solution of the present invention is that, on the basis of the above, the spreading in the step of repeating the spreading and melting is performed before the mixture is heated by a laser until the resin powder is melted and solidified. Therefore, the aerogel and the resin phase have better interface bonding performance.
Another technical solution of the present invention is that, on the basis of the above, the spreading in the step of repeating the spreading and melting is performed after the mixed material is heated by a laser until the resin powder is melted and solidified. Therefore, the aerogel and the resin phase have better interface bonding performance.
On the basis, the curing process is ultraviolet radiation curing or natural cooling curing or cooling curing. Therefore, the aerogel/resin composite material is quickly cured, and the phenomenon of layering of the aerogel in the resin is avoided.
The other technical scheme of the invention is that on the basis, the volume ratio of the aerogel to the resin phase in the aerogel composite material is 0.1-9: 1. So, the aerogel accounts for than can be very little, is equivalent to ordinary resin board this moment, and the aerogel accounts for than can be very big, is equivalent to the aerogel material this moment, consequently according to performance needs, the volume ratio scope of aerogel and resin powder can be 0.1:1 to 9: 1.
the other technical scheme of the invention is that on the basis of the above, the aerogel has the characteristics of internal hydrophobicity and surface hydrophilicity. So, adopt the surface to have the hydroxyl of silicon, inside is the transparent adiabatic aerogel technique of hydrophobic characteristic, solve the problem that aerogel and resin are difficult to mix, because the aerogel surface has a large amount of Si-OH can have compatible and bonding effect with the active functional group on resin surface, further improve the wetting cladding effect of resin on the aerogel surface, increase the interface bonding strength of aerogel and resin, be favorable to improving the evenly distributed of aerogel in the resin is inside on the one hand, on the other hand the high tenacity performance of high strength of performance such as thermal-insulated heat preservation and the resin of full play aerogel.
The other technical scheme of the invention is that on the basis, the shape of the aerogel can be massive, granular or powder, and is determined according to performance requirements.
Another technical solution of the present invention is to provide the resin with thermosetting resin or thermoplastic resin.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is a cross-sectional view of the aerogel composite of the present invention;
wherein:
1-a resin phase; 2-aerogel.
Detailed Description
The present invention will now be described in detail with reference to the drawings, which are given by way of illustration and explanation only and should not be construed to limit the scope of the present invention in any way. Furthermore, features from embodiments in this document and from different embodiments may be combined accordingly by a person skilled in the art from the description in this document.
The embodiment of the invention provides a preparation method of an aerogel composite material, which comprises the following steps:
(1) uniformly mixing resin powder and aerogel;
(2) laying a layer of mixture on the mould substrate;
(3) rapidly heating the obtained mixture by a laser in a step scanning mode until the resin powder is molten and the aerogel is not molten;
(4) alternately repeating step (2) and step (3) on the previous deposition layer;
(5) and curing to obtain the aerogel composite material.
Thus, through the steps of mixing, paving, laser rapid heating, rapid curing and the like, an aerogel composite material with heat insulation and preservation performance, which is composed of aerogel and a resin phase bonding the aerogel, can be obtained, as shown in fig. 1. According to the invention, the resin in the mixture of the aerogel and the resin powder is rapidly heated to be molten by using a laser in a step scanning manner, and then is rapidly cured, however, the aerogel is light and easy to delaminate, and uniform distribution is difficult to realize. In addition, the rapid curing forming process can automatically, directly and rapidly form the heat insulation boards with various shapes and structures, the problems that the heat insulation boards with special and complex shapes are difficult to prepare in online production and the like are solved, equipment, dies and the like of a traditional production line are not needed, the manufacturing cost is saved, and meanwhile, the utilization rate of materials is also improved. The obtained aerogel composite material uses transparent aerogel which is light in weight, has excellent heat insulation performance, sound insulation and noise reduction performance and energy absorption performance as functional components, resin is added as a reinforcing binder, and the composite material consisting of the aerogel and the resin is prepared due to the fact that the resin is light in weight, high in compressive strength and hardness and easy to obtain large size.
In another embodiment of the present invention, based on the above embodiment, the spreading in the step of repeating the spreading and melting is performed before the mixture is heated by the laser until the resin powder is melted and solidified. Therefore, the aerogel and the resin phase have better interface bonding performance.
In another embodiment of the present invention, based on the above embodiment, the spreading in the step of repeating the spreading and melting is performed after the mixture is heated by a laser until the resin powder is melted and solidified. Therefore, the aerogel and the resin phase have better interface bonding performance.
On the basis of the above embodiment, in another embodiment of the present invention, the curing process is ultraviolet radiation curing, natural cooling curing, or cooling curing. Therefore, the aerogel/resin composite material is quickly cured, and the phenomenon of layering of the aerogel in the resin is avoided.
Based on the above embodiment, in another embodiment of the present invention, the volume ratio of the aerogel to the resin phase in the aerogel composite is 0.1-9: 1. So, the aerogel accounts for than can be very little, is equivalent to ordinary resin board this moment, and the aerogel accounts for than can be very big, is equivalent to the aerogel material this moment, consequently according to performance needs, the volume ratio scope of aerogel and resin powder can be 0.1:1 to 9: 1.
in another embodiment of the present invention, based on the above embodiments, the aerogel has internal hydrophobic and surface hydrophilic characteristics. So, adopt the surface to have the hydroxyl of silicon, inside is the transparent adiabatic aerogel technique of hydrophobic characteristic, solve the problem that aerogel and resin are difficult to mix, because the aerogel surface has a large amount of Si-OH can have compatible and bonding effect with the active functional group on resin surface, further improve the wetting cladding effect of resin on the aerogel surface, increase the interface bonding strength of aerogel and resin, be favorable to improving the evenly distributed of aerogel in the resin is inside on the one hand, on the other hand the high tenacity performance of high strength of performance such as thermal-insulated heat preservation and the resin of full play aerogel.
On the basis of the above embodiment, in another embodiment of the present invention, the shape of the aerogel can be block, granular, or powder, and is determined according to performance requirements.
In another embodiment of the present invention, on the basis of the above embodiment, the resin is a thermosetting resin or a thermoplastic resin.
On the basis of the above embodiment, in another embodiment of the present invention, a thermal insulation composite material is prepared by the following steps:
(1) uniformly mixing the resin powder and the transparent blocky aerogel in a certain ratio according to the volume ratio of 0.1:1 of the aerogel to the resin powder, wherein the resin is thermosetting resin;
(2) firstly, laying a layer of mixture on a mould substrate;
(3) rapidly heating the obtained mixture by a laser in a step scanning mode until the resin powder is molten and the aerogel is not molten;
(4) alternately repeating steps (2) and (3) on the surface of the previously deposited layer before the resin is cured;
(5) and curing to obtain the aerogel composite material.
The aerogel composite material obtained through the steps is 10mm in thickness, and the test result shows that the visible light transmittance is 90% and the thermal conductivity coefficient is 0.101W/m.k.
Based on the above embodiment, in another embodiment of the present invention, an aerogel composite is prepared by the following steps:
(1) uniformly mixing the resin powder and the transparent granular aerogel in a certain ratio according to the volume ratio of 5:1 of the aerogel to the resin powder, wherein the resin is thermoplastic resin;
(2) firstly, laying a layer of mixture on a mould substrate;
(3) rapidly heating the obtained mixture by a laser in a step scanning mode until the resin powder is molten and the aerogel is not molten;
(4) after the resin of the former deposition layer is cured, alternately repeating the step (2) and the step (3) on the surface of the resin;
(5) and curing to obtain the aerogel composite material.
The aerogel composite material obtained through the steps is 10mm in thickness, and the test result shows that the visible light transmittance is 85% and the thermal conductivity is 0.032W/m.k.
Based on the above embodiment, in another embodiment of the present invention, an aerogel composite is prepared by the following steps:
(1) uniformly mixing the resin powder and the transparent powdery aerogel in a fixed ratio according to the volume ratio of the aerogel to the resin powder of 2:1, wherein the resin is thermosetting resin;
(2) firstly, laying a layer of mixture on a mould substrate;
(3) rapidly heating the obtained mixture by a laser in a step scanning mode until the resin powder is molten and the aerogel is not molten;
(4) after the resin of the former deposition layer is cured, alternately repeating the step (2) and the step (3) on the surface of the resin;
(5) obtaining the aerogel composite material.
The aerogel composite material obtained through the steps is 10mm in thickness, and the test result shows that the visible light transmittance is 80% and the thermal conductivity coefficient is 0.040W/m.k.
Based on the above embodiment, in another embodiment of the present invention, an aerogel composite is prepared by the following steps:
(1) uniformly mixing the resin powder and the transparent granular aerogel in a certain ratio according to the volume ratio of the aerogel to the resin powder of 9:1, wherein the resin is thermoplastic resin;
(2) firstly, laying a layer of mixture on a mould substrate;
(3) rapidly heating the obtained mixture by a laser in a step scanning mode until the resin powder is molten and the aerogel is not molten;
(4) after the resin of the former deposition layer is cured, alternately repeating the step (2) and the step (3) on the surface of the resin;
(5) obtaining the aerogel composite material.
The aerogel composite material obtained through the steps is 10mm in thickness, and the test result shows that the visible light transmittance is 77% and the thermal conductivity coefficient is 0.020W/m.k.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A method for preparing an aerogel composite, comprising the steps of: (1) mixing materials, namely uniformly mixing resin powder and aerogel;
(2) paving, namely paving a layer of mixture obtained in the step (1) on a mould substrate;
(3) melting, namely rapidly heating the resin powder in the mixture obtained in the step (2) to be molten in a step scanning mode by using a laser;
(4) alternately spreading and melting, and alternately repeating the step (2) and the step (3) on the previous deposition layer;
(5) curing;
the aerogel surface has a large amount of Si-OH which can be compatible and bonded with the active functional groups on the surface of the resin.
2. A method of preparing an aerogel composite as claimed in claim 1, wherein the paving in step (4) is performed before the resin in step (3) is cured.
3. The method of claim 1, wherein the paving in step (4) is performed after the resin in step (3) is cured.
4. The method for preparing an aerogel composite according to claim 1, 2 or 3, wherein the curing process is ultraviolet radiation curing or natural cooling curing or cooling curing.
5. The method of claim 1, wherein the volume ratio of aerogel to resin is 0.1-9: 1.
6. the method of claim 1, wherein the aerogel has an internal hydrophobic, surface hydrophilic character.
7. The method of claim 1, wherein the aerogel is in the form of one of a block, a granule, and a powder.
8. The method of claim 1, wherein the resin is a thermosetting resin or a thermoplastic resin.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0340707B1 (en) * | 1988-05-03 | 1992-08-19 | BASF Aktiengesellschaft | Insulating material with a density of 0,1 to 0,4 g/cm3 |
| CN1196035A (en) * | 1995-09-11 | 1998-10-14 | 德国赫彻斯特研究技术两合公司 | Aerogel and adhesive-containing composite, process for its production and its use |
| CN1196036A (en) * | 1995-09-11 | 1998-10-14 | 德国赫彻斯特研究技术两合公司 | Fibre-containing aerogel composite material |
-
2017
- 2017-03-17 CN CN201710162210.4A patent/CN108623325B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0340707B1 (en) * | 1988-05-03 | 1992-08-19 | BASF Aktiengesellschaft | Insulating material with a density of 0,1 to 0,4 g/cm3 |
| CN1196035A (en) * | 1995-09-11 | 1998-10-14 | 德国赫彻斯特研究技术两合公司 | Aerogel and adhesive-containing composite, process for its production and its use |
| CN1196036A (en) * | 1995-09-11 | 1998-10-14 | 德国赫彻斯特研究技术两合公司 | Fibre-containing aerogel composite material |
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