CN113636824B - Preparation method of enhanced silicon dioxide aerogel composite material - Google Patents
Preparation method of enhanced silicon dioxide aerogel composite material Download PDFInfo
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- CN113636824B CN113636824B CN202110962892.3A CN202110962892A CN113636824B CN 113636824 B CN113636824 B CN 113636824B CN 202110962892 A CN202110962892 A CN 202110962892A CN 113636824 B CN113636824 B CN 113636824B
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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
- 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
- C04B20/10—Coating or impregnating
- C04B20/1051—Organo-metallic compounds; Organo-silicon compounds, e.g. bentone
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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 belongs to the field of heat insulation materials, and discloses a preparation method of a reinforced silica aerogel composite material.
Description
Technical Field
The invention belongs to the field of heat insulation materials, and particularly relates to a preparation method of an anti-powder-dropping aerogel felt.
Background
At present, developing new energy, improving the utilization rate of the existing energy and saving energy have attracted great attention from various countries. Therefore, the reasonable utilization of energy and the energy conservation have important significance on the sustainable development of the society in China. The adoption of new technology and new process to develop environment-friendly heat-insulating material is one of the most effective and economic measures for saving energy.
SiO 2 Aerogel is a new super heat-insulating material, has extremely low heat conductivity coefficient which is far lower than that of static air at normal temperature by 0.25W/m.K, has incomparable heat-insulating and heat-preserving effects compared with other materials, has low density, is waterproof, flame-retardant, green and environment-friendly, is corrosion-resistant, is not easy to age, has long service life, and is called as the super heat-insulating material. At present, the method is mainly used for industrial pipelines, industrial furnace bodies, escape capsules, transportation,Heat preservation and insulation in the fields of household appliances, glass and the like.
The existing preparation method of the silica aerogel generally takes water glass, orthosilicate ester and the like as silicon sources, and the silica aerogel is prepared by adding an acidic organic solvent for reaction, and then the silica aerogel material is obtained through the processes of gelation, aging and drying. The aerogel skeleton is a three-dimensional network formed by crosslinking silica clusters, and the crosslinking degree of the three-dimensional network influences the flexibility of the aerogel.
At the same time, siO is used for reasons of its preparation 2 The aerogel felt generally has the condition that the felt body drops aerogel powder in the transportation, construction and use processes, the powder dropping condition not only brings inconvenience to the construction, but also brings threat to the health of constructors, and simultaneously the performance of the aerogel felt can be reduced. Therefore, on the premise of ensuring good heat insulation performance of the aerogel felt, the development of the aerogel composite material without powder falling is necessary to ensure the health of production and use personnel and meet various requirements of the market. At present, the powder falling prevention scheme is that glass fiber cloth, aluminum foil cloth and the like are pasted on the surface of an aerogel fiber felt, the mode is high in labor cost and not beneficial to large-scale production, the flexibility of the material is reduced after the front side and the back side are pasted, the material is not easy to curl and bend, and storage, transportation, construction and installation are not convenient enough. The coating preparation technology of the surface of the aerogel felt is one of the recently developed methods for avoiding the dusting of the aerogel felt. The surface of the aerogel is coated with solvent-based coating to prevent slag falling, and the solvent-based coating can bring environmental pollution, and can cause the solvent to permeate into the aerogel to damage a pore structure and reduce the heat-insulating property of the aerogel.
At present, the strength and elasticity of the silicon dioxide aerogel composite material are poor, so that the application range of the aerogel is greatly expanded due to the fact that the silicon dioxide aerogel composite material is easy to wear and abrade and has powder falling. Therefore, the preparation of the silicon dioxide aerogel composite material with high elasticity, high reinforcement and no powder falling has very important significance.
Disclosure of Invention
The invention aims to provide a preparation method of a reinforced silica aerogel composite material.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a reinforced silicon dioxide aerogel composite material comprises the following steps:
(1) Pretreatment of the fiber material:
(a) First pretreatment: hydroxylating the fiber material; (b) a second pretreatment: dipping the hydroxylated fiber material in a silicon source solution for 4-24h;
(2) Preparing a silica wet gel material, namely dipping the fiber material obtained in the step (1) in silica sol catalyzed by a gelling catalyst before gelling to prepare the silica wet gel material or dipping the fiber material in the silica sol and then catalyzing and gelling by the gelling catalyst to prepare the silica wet gel material;
(3) And drying treatment: and (3) drying the silica wet gel material obtained in the step (2) to obtain the enhanced silica aerogel composite material.
Preferably, in step (1), the hydroxylation treatment process of the fiber material is as follows: placing the fiber material in a volume ratio of 3:1 from 98% of 2 SO 4 And 30% of H 2 O 2 Treating the mixed solution for 20-40min, cooling, taking out, washing with deionized water, and drying at 80-100 ℃ to obtain the hydroxylated fiber material.
Preferably, the fibrous material is one or a combination of two or more of the following group of fibrous materials: quartz fibers, glass fibers, high silica fibers, carbon fibers, mullite fibers, basalt fibers, silicon carbide fibers, silicon nitride fibers, alumina fibers, and boron nitride fibers.
Preferably, in step (1), the silicon source is alkylalkoxysilane; the alkyl alkoxy silane comprises one or more than two of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, vinyl triethoxy silane, propyl trimethoxy silane or propyl triethoxy silane.
Preferably, in the step (2), the silica sol is obtained by mixing a silicon source, ethanol, water = 1: 2 to 60: 1 to 30 in a molar ratio; the silicon source is one or more than two of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate or alkyl alkoxy silane; the alkyl alkoxy silane comprises one or more than two of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, vinyl triethoxy silane, propyl trimethoxy silane or propyl triethoxy silane; the gelling catalyst is one or a combination of two of alkaline catalysts such as sodium hydroxide, potassium hydroxide, ammonia water and ammonium fluoride aqueous solution; the gelling catalyst adjusts the pH of the silica sol to 6-8.
Preferably, step (2) further comprises adding an acidic catalyst to the silica sol prior to adding the gel catalyst. The pH of the solution is adjusted to 2-6.
Preferably, the acidic catalyst is one or a combination of more than two of sulfuric acid, hydrochloric acid, hydrofluoric acid, oxalic acid, acetic acid or benzenesulfonic acid.
Preferably, the step (2) further comprises a gel aging process of the silica wet gel material, specifically, the silica wet gel material is aged for 8-24 hours at room temperature or at 30-60 ℃ by heating.
Preferably, the silica wet gel material further comprises a solvent replacement process before drying, specifically, the silica wet gel material is placed in absolute ethyl alcohol for solvent replacement.
Preferably, the drying treatment is one of supercritical drying, freeze drying and atmospheric drying.
The reinforced silica aerogel composite material prepared by the preparation method.
Has the beneficial effects that:
according to the invention, the fiber material is subjected to hydroxylation treatment, so that a large number of hydroxyl groups are attached to the fiber material, and further alkyl alkoxy silane is adopted for pretreatment, so that hydroxyl groups on the surface of the fiber material react with partial Si-OR groups on a silicon source to form strong chemical bond combination, in the sol-gel process, si-OR groups inside fiber pores react with Si-OR groups and partial hydroxyl groups on the surface of the fiber material after the silicon source treatment reaction to form strong Si-O-Si chemical bond, a complex space network framework is formed between fibers and silica aerogel, the strong bonding force between the fibers and the aerogel is ensured, the framework strength of the silica aerogel composite material can be greatly improved, and the silica aerogel composite material has excellent compression performance compared with the existing silica aerogel composite material.
In general, the phenomenon of powder falling of the silicon dioxide aerogel composite material is mainly caused by weak binding force between aerogel particles and fibers, and the aerogel particles are easy to separate from a fiber matrix under the vibration condition.
According to the invention, the fibers are pretreated by adopting the alkylalkoxysilane, so that the surfaces of the fibers are provided with Si-R groups, and the silica sol can be well combined in a reaction manner, namely, hydrophobic groups are introduced during the preparation of the silica sol, so that the traditional hydrophobic modification step can be avoided, the preparation period is shortened, and potential safety hazards caused by the use of a large amount of modified solution in the surface modification process can be avoided to a certain extent. In addition, si-R groups exist on the network framework of the fiber material, so that the uniformity of surface hydrophobic groups in the silica sol and gel in the system can be ensured, and the problem of unstable network framework caused by internal hydrophobic property loss and particle aggregation in the sol particle nucleation and condensation process is avoided, so that the aerogel composite material obtained by the method has high-strength, more complete and uniform aerogel network framework.
Detailed Description
The present invention will be further described with reference to the following specific examples. It is to be understood that the following examples are illustrative of the present invention only and are not intended to limit the scope of the present invention.
Example 1
(1) Pretreatment of the fiber material:
(a) First pretreatment: hydroxylating the fiber material; (b) second pretreatment: the hydroxylated fibre material is treated by immersion in a methyltrimethoxysilane solution for 12h.
(2) Uniformly mixing a silicon source, ethanol and water, sequentially adding a gelling catalyst to ensure that the pH of the solution is 7, uniformly stirring to obtain catalyzed silica sol, and soaking a fiber material into the catalyzed silica sol to gel to obtain fiber-reinforced silica wet gel;
(3) And aging the gel: carrying out aging treatment on the fiber reinforced silica wet gel for 16h at room temperature;
(4) And solvent replacement: placing the fiber-reinforced silica wet gel subjected to gel aging treatment in absolute ethyl alcohol for solvent replacement;
(5) And drying treatment: and carrying out supercritical drying treatment on the fiber-reinforced silica wet gel subjected to solvent replacement to obtain the reinforced silica aerogel composite material.
Wherein in the step (1), the fiber material is glass fiber. The hydroxylation treatment process of the fiber material comprises the following steps: placing the fiber material in a volume ratio of 3:1 from 98% of 2 SO 4 And 30% of H 2 O 2 Treating the mixed solution for 30min, cooling, taking out, washing with deionized water, and drying at 100 ℃ to obtain the hydroxylated fiber material.
In the step (2), a silicon source, ethanol and water are = 1: 6: 2 in molar ratio, and the silicon source is tetraethoxysilane. The gelling catalyst is ammonia water.
The reinforced silicon dioxide aerogel composite material is prepared by the method.
The enhanced silica aerogel composite material obtained by the embodiment has the thermal conductivity coefficient of 0.02 w/(m DEG C), and the compressive strength of 1.28Mpa.
Example 2
(1) Pretreatment of the fiber material:
(a) First pretreatment: hydroxylating the fiber material; (b) second pretreatment: the hydroxylated fibrous material was dip treated in a solution of dimethyldimethoxysilane for 10h.
(2) Uniformly mixing a silicon source, ethanol and water to obtain silica sol, uniformly stirring to obtain silica sol, soaking a fiber material into the silica sol, and then adding a gelling catalyst to obtain fiber-reinforced silica wet gel;
(3) And aging the gel: aging the fiber-reinforced silica wet gel for 12 hours at the temperature of 50 ℃;
(4) And solvent replacement: placing the fiber reinforced silica wet gel subjected to gel aging treatment in absolute ethyl alcohol for solvent replacement;
(5) And (3) drying treatment: and carrying out supercritical drying treatment on the fiber-reinforced silica wet gel subjected to solvent replacement to obtain the reinforced silica aerogel composite material.
Wherein in the step (1), the fiber material is high silica fiber. The hydroxylation treatment process of the fiber material comprises the following steps: placing the fiber material in a volume ratio of 3:1 by 98% of 2 SO 4 And 30% of H 2 O 2 Treating the mixed solution for 20min, cooling, taking out, washing with deionized water, and drying at 90 ℃ to obtain the hydroxylated fiber material.
In the step (2), according to a molar ratio, the silicon source, the ethanol and the water are = 1: 10: 4, and the silicon source is methyl orthosilicate. The gelling catalyst is ammonium fluoride, and the pH of the sol is adjusted to 6.
The reinforced silicon dioxide aerogel composite material is prepared by the method.
The enhanced silica aerogel composite material obtained by the embodiment has the thermal conductivity coefficient of 0.021 w/(m DEG C), and the compressive strength of 1.32Mpa.
Example 3
(1) Pretreatment of the fiber material:
(a) First pretreatment: hydroxylating the fiber material; (b) a second pretreatment: the hydroxylated fibre material was dip treated in a solution of dimethyldiethoxysilane for 16h.
(2) Uniformly mixing a silicon source, ethanol and water, sequentially adding a gelling catalyst to ensure that the pH of the solution is 6.5, uniformly stirring to obtain catalyzed silica sol, and soaking a fiber material into the catalyzed silica sol to gel to obtain fiber-reinforced silica wet gel;
(3) And aging the gel: aging the fiber-reinforced silica wet gel for 10 hours at the temperature of 60 ℃;
(4) And solvent replacement: placing the fiber reinforced silica wet gel subjected to gel aging treatment in absolute ethyl alcohol for solvent replacement;
(5) And drying treatment: and carrying out supercritical drying treatment on the fiber-reinforced silica wet gel subjected to solvent replacement to obtain the reinforced silica aerogel composite material.
Wherein in the step (1), the fiber material is pre-oxidized fiber. The hydroxylation treatment process of the fiber material comprises the following steps: placing the fiber material in a volume ratio of 3:1 by 98% of 2 SO 4 And 30% of H 2 O 2 Treating the mixed solution for 35min, cooling, taking out, washing with deionized water, and drying at 80 ℃ to obtain the hydroxylated fiber material.
In the step (2), according to a molar ratio, silicon source, ethanol and water are = 1: 35: 10, and the silicon source is methyltriethoxysilane.
The gelling catalyst is a mixed solution of ammonium fluoride and ammonia water.
The reinforced silicon dioxide aerogel composite material is prepared by the method.
The enhanced silica aerogel composite material obtained by the embodiment has the thermal conductivity coefficient of 0.02 w/(m DEG C), and the compressive strength of 1.24Mpa.
Example 4
The preparation process includes adding acid catalyst sulfuric acid to regulate pH to 5 before adding gel catalyst in step 2 and the other steps are the same as in example 1.
The reinforced silica aerogel composite material is prepared by the method.
The enhanced silica aerogel composite material obtained by the embodiment has the heat conductivity coefficient of 0.022 w/(m DEG C), and the compressive strength of 1.36MPa.
Example 5
The preparation process does not include the gel aging process in step (3), and the other steps are the same as in example 1.
The reinforced silica aerogel composite material is prepared by the method.
The enhanced silica aerogel composite material obtained by the embodiment has the thermal conductivity coefficient of 0.023 w/(m DEG C.), and the compressive strength of 1.32Mpa.
Claims (6)
1. The preparation method of the reinforced silica aerogel composite material is characterized by comprising the following steps:
(1) Pretreatment of the fiber material:
(a) First pretreatment: hydroxylating the fiber material; (b) second pretreatment: dipping the hydroxylated fiber material in a silicon source solution for 4-24h;
(2) Preparing a silica wet gel material, namely dipping the silica sol catalyzed by a gelling catalyst into the fiber material obtained in the step (1) before gelation to prepare the silica wet gel material or dipping the fiber material into the silica sol and then catalyzing and gelling by the gelling catalyst to prepare the silica wet gel material;
(3) And (3) drying treatment: drying the silica wet gel material obtained in the step (2) to obtain the enhanced silica aerogel composite material;
the fiber material is one or the combination of more than two of the following fiber materials: quartz fibers, glass fibers, high silica fibers, carbon fibers, mullite fibers, basalt fibers, silicon carbide fibers, silicon nitride fibers, alumina fibers, and boron nitride fibers;
in the step (1), the silicon source is alkyl alkoxy silane; the alkyl alkoxy silane comprises one or more than two of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, vinyl triethoxy silane, propyl trimethoxy silane or propyl triethoxy silane;
in the step (2), the silica sol is obtained by mixing a silicon source, ethanol, water and water according to the molar ratio of 1 to (2 to 60) to (1 to 30); the silicon source is one or more than two of ethyl orthosilicate, methyl orthosilicate, butyl orthosilicate, isopropyl orthosilicate or alkyl alkoxy silane; the alkyl alkoxy silane comprises one or more than two of methyl trimethoxy silane, dimethyl dimethoxy silane, methyl triethoxy silane, dimethyl diethoxy silane, vinyl triethoxy silane, propyl trimethoxy silane or propyl triethoxy silane; the gelling catalyst is an alkaline catalyst, and the alkaline catalyst is one or a combination of two of sodium hydroxide, potassium hydroxide, ammonia water and ammonium fluoride aqueous solution; the gelling catalyst adjusts the pH of the silica sol to 6-8;
the silica wet gel material also comprises a solvent replacement process before drying, specifically, the silica wet gel material is placed in absolute ethyl alcohol for solvent replacement.
2. The method of preparing a reinforced silica aerogel composite as claimed in claim 1, wherein: in the step (1), the hydroxylation treatment process of the fiber material comprises the following steps: placing the fiber material in a volume ratio of 3:1 by 98% of 2 SO 4 And 30% of H 2 O 2 Treating the mixed solution for 20-40min, cooling, taking out, washing with deionized water, and drying at 80-100 ℃ to obtain the hydroxylated fiber material.
3. The method of preparing a reinforced silica aerogel composite as claimed in claim 1, wherein: and (3) before adding the gelling catalyst in the step (2), adding an acid catalyst into the silica sol, and adjusting the pH of the solution to 2-6.
4. The method of preparing a reinforced silica aerogel composite of claim 3, wherein: the acidic catalyst is one or the combination of more than two of sulfuric acid, hydrochloric acid, hydrofluoric acid, oxalic acid, acetic acid or benzenesulfonic acid.
5. The method of preparing a reinforced silica aerogel composite of claim 1, wherein: the step (2) also comprises a gel aging process of the silica wet gel material, in particular to aging treatment of the silica wet gel material for 8-24h at room temperature or under the condition of heating to 30-60 ℃.
6. A reinforced silica aerogel composite prepared by the method of any of claims 1 to 5.
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| CN114230285B (en) * | 2021-12-29 | 2023-07-04 | 山东汇富建设集团有限公司 | Assembled green building heat-insulation wall structure and assembling method thereof |
| CN114908947B (en) * | 2022-04-26 | 2023-10-20 | 中科润资(重庆)节能科技有限公司 | High-temperature-resistant smoke-proof air duct and manufacturing method thereof |
| CN114988904A (en) * | 2022-05-19 | 2022-09-02 | 中国科学院金属研究所 | Preparation method for realizing ultralow-density and ultralow-heat-conductivity carbon aerogel composite material through surface functionalization of cotton fibers |
| CN117510181B (en) * | 2023-11-07 | 2024-04-16 | 武汉中科先进材料科技有限公司 | Super-hydrophobic and enhanced silicon dioxide aerogel felt and preparation method thereof |
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