CN111302827A - Preparation method of high-temperature-resistant fiber-reinforced silica aerogel heat-insulation composite material - Google Patents
Preparation method of high-temperature-resistant fiber-reinforced silica aerogel heat-insulation composite material Download PDFInfo
- Publication number
- CN111302827A CN111302827A CN202010276772.3A CN202010276772A CN111302827A CN 111302827 A CN111302827 A CN 111302827A CN 202010276772 A CN202010276772 A CN 202010276772A CN 111302827 A CN111302827 A CN 111302827A
- Authority
- CN
- China
- Prior art keywords
- fiber
- inorganic ceramic
- composite material
- ceramic fiber
- aerogel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/76—Use at unusual temperatures, e.g. sub-zero
- C04B2111/763—High temperatures
-
- 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
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
-
- 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
Abstract
The invention discloses a preparation method of a high-temperature-resistant fiber-reinforced silica aerogel heat-insulation composite material, and aims to enable the preparation method to be simple in process, environment-friendly and low in cost, and the prepared material is high-temperature-resistant and low in heat conductivity. The technical scheme is that an inorganic ceramic fiber prefabricated part is prepared; then preparing silicon dioxide sol; then carrying out vacuum impregnation to obtain a fiber/sol mixture; aging the re-gel, drying at normal pressure to obtain SiO in the prepared material2Aerogel is uniformly filled in pores of inorganic ceramic fiber prefabricated member, the inorganic ceramic fiber prefabricated member and SiO2The mass ratio of the aerogel matrix is 1: 0.4-1.0. The invention has simple preparation process, low cost, no need of supercritical drying equipment, no need of complex surface modification and solvent replacement process, low raw material price, simple equipment and environmental requirementThe method has the advantages of low cost, short time consumption of the whole process flow, suitability for industrial production, high material use temperature which can reach 1000 ℃, good hydrophobicity and low density.
Description
Technical Field
The invention relates to a preparation method of a heat insulation material, in particular to a preparation method of a silica aerogel heat insulation composite material which is light in weight, high temperature resistant and simple in preparation process.
Background
The aerogel is a nano porous material formed by mutually aggregating nano particles, and has low density and high specific surface area (200-1000 m)2(iv)/g), high porosity (95%), and very low thermal conductivity (0.014W/m.k at room temperature thermal conductivity) [ m.a. aegoerter, n.leventis, m.m. koebel, Aerogels Handbook, Springer, New York,2011, i.e. aerogel Handbook ]. Kim and the like use glass fiber as a reinforcing phase and tetraethoxysilane as a silicon source, and prepare the fiber-reinforced aerogel composite material by drying at normal pressure, but the solvent replacement and surface modification require 3 days. [ C.Y.Kim, J.K.Lee, B.I.Kim, Synthesis and pore analysis of aerogel-glass fiber composites by incorporating drying method, Colloids and Surfaces A: Physicochem. Eng.Aspectrs, 2008, 313-. The Tanmha et al adopts a sol-gel method to compound high-purity silica glass fiber into silica aerogel, and carries out surface modification by using normal hexane of trimethylchlorosilane for 1 day before drying at normal pressure; followed by up to 4 days of solvent replacement [ Haemaya, Populus, grand Notopterygium, Koelreuteria, Jinhuo, southeast, Von Yan, Von Dali, preparation of fiber composite silica aerogel material, functional material 2014,16: 16139-. It is found that silica aerogel is sintered at higher temperature, resulting in the destruction of nano-porous structure, so the temperature of using silica aerogel is below 800 ℃ [ T.Y.Wei, T.F.Chang, S.Y.Lu.preparation of monolithic silica aerogel of low thermal conductivity organic compression, Journal of American Ceramic Society,2007,90(7):2003-2007 ], i.e. the preparation of silica aerogel block with low thermal conductivity by atmospheric drying.
Patent document CN101318659A discloses a method for preparing silica aerogel composite material by atmospheric drying, and the methodThe material is prepared by adopting a sol-gel and normal pressure drying process, wherein the process comprises solvent replacement for nearly 180 hours and surface modification for 6 hours, and the thermal conductivity of the material at 25 ℃ is only 0.020W/m.K. Patent document CN101671030B discloses preparation of fiber-toughened SiO by drying under normal pressure2A method for producing a silica aerogel composite material, which comprises subjecting an aerogel composite material to a sol-gel process and a drying process under normal pressure, wherein the solvent substitution and the surface modification are repeated a plurality of times during the drying process, and the thermal conductivity at 25 ℃ of the silica aerogel composite material is less than 0.04W/m.K.
In conclusion, the prepared Silica (SiO) was dried under atmospheric pressure2) The aerogel heat-insulation composite material needs repeated complex operations for many times due to the solvent replacement and surface modification processes in the preparation process, and the replaced solvent is wasted greatly, so that the manufacturing cost of the material is high, and the preparation period is long; therefore, the problem of preparing the silica aerogel thermal insulation composite material with high efficiency and low cost is urgently needed to be solved by adopting a simple preparation process under the condition of not reducing the good performance of the silica aerogel thermal insulation composite material and omitting the tedious solvent replacement and surface modification processes.
Disclosure of Invention
The invention aims to solve the technical problem of providing high-temperature-resistant fiber-reinforced SiO2A preparation method of an aerogel heat insulation composite material. The material has the advantages of high temperature resistance, low thermal conductivity, low density, good hydrophobicity and the like. The preparation method has the advantages of simple process, normal-pressure drying, no need of complicated processes such as surface modification and solvent replacement, environmental protection, low cost and easy batch production.
The high-temperature resistant fiber reinforced SiO of the invention2The aerogel heat-insulating composite material is prepared from an inorganic ceramic fiber prefabricated part and SiO2Aerogel matrix, inorganic ceramic fiber preform and SiO2The mass ratio of the aerogel matrix is 1: 0.4-1.0, and SiO is subjected to vacuum impregnation, gel aging and normal pressure drying by using a silica sol precursor2The aerogel is uniformly filled into the pores of the inorganic ceramic fiber prefabricated member. The apparent density of the inorganic ceramic fiber prefabricated part is 0.16-0.28 g/cm3。
The preparation method comprises the following steps:
the first step, preparing an inorganic ceramic fiber preform, the method comprises:
according to the apparent density (range of 0.16-0.28 g/cm) of the inorganic ceramic fiber prefabricated part3) Calculating the mass of the required inorganic ceramic fiber by adopting the mass (density) multiplied by the volume, clamping and fixing the weighed inorganic ceramic fiber by using a mold, and enabling the fiber arrangement direction to be vertical to the heat flow direction in heat insulation use to obtain an inorganic ceramic fiber prefabricated member;
the inorganic ceramic fiber is any one of quartz fiber, alumina silicate fiber, alumina fiber or mullite fiber.
Secondly, preparing the silica sol by the following steps:
using silicon salt as precursor, adding hexadecyl trimethyl ammonium bromide (CH)3(CH2)15N(Br)(CH3)3) Adding absolute ethyl alcohol (CH)3CH2OH, concentration>99%) and deionized water (H)2O), nitric acid (HNO) is added3) And ammonia (NH)3·H2O), preparing the silica sol by adopting an acid-base two-step method, wherein the specific process comprises the following steps: firstly, mixing and stirring silicon salt, hexadecyl trimethyl ammonium bromide, absolute ethyl alcohol and deionized water for 10 minutes to obtain a mixed solution, then dripping nitric acid into the mixed solution, continuously stirring for 10 minutes, standing for 1-2 hours to fully hydrolyze the silicon salt to obtain a hydrolyzed mixed solution. And dropwise adding ammonia water into the hydrolyzed mixed solution, and stirring for 10 minutes to obtain the silica sol. Wherein the molar ratio of each component is silicon salt: cetyl trimethylammonium bromide: anhydrous ethanol: deionized water: nitric acid: ammonia water 1: 7.9X 10-3:5.09～7.63:15.93～23.89:2.87×10-3：2.87×10-3～9.85×10-3。
The above-mentioned silicon salt is methyl trimethoxy silane (CH)3Si(OCH3)3) Methyltriethoxysilane (CH)3Si(OC2H5)3) Dimethyldimethoxysilane (Si (OCH)3)2(CH3)2) Dimethyl diethoxySilane ((CH)3)2Si(OC2H5)2) Trimethylmethoxysilane (CH)3OSi(CH3)3) Trimethylethoxysilane (C)2H5OSi(CH3)3) At least one of (1).
Thirdly, vacuum impregnation is carried out, and the method comprises the following steps:
3.1 placing the inorganic ceramic fiber prefabricated part into an open iron box, placing the iron box into a vacuum impregnation tank, and vacuumizing to-0.1 MPa to-0.05 MPa;
3.2 injecting the silica sol into an iron box through a pipeline, fully permeating the silica sol into pores of the inorganic ceramic fiber prefabricated part by adopting a vacuumizing mode, ensuring that the liquid level of the silica sol is 5 cm higher than the highest point of the fiber prefabricated part, completely covering the prefabricated part with the silica sol, and maintaining the pressure for 1-2 hours;
3.3 introducing air into the vacuum impregnation tank to restore the pressure in the vacuum impregnation tank to normal pressure, and taking out the fiber/sol mixture (together with the iron box).
Fourthly, aging the gel by the following method:
and (3) putting the iron box filled with the fiber/sol mixture into a water bath kettle at 40-55 ℃ for standing and aging, heating to 60-70 ℃ after the silica sol in the pores of the inorganic ceramic prefabricated part is gelled, continuing to stand and age for 1-2 days, and taking out a sample from the iron box to obtain a fiber/gel composite.
Step five, drying under normal pressure, which comprises the following steps:
and (3) placing the fiber/gel composite after the gel aging into a drying oven, firstly drying for 24-48 hours at 60-70 ℃, then drying for 12-24 hours at 75-80 ℃, and finally drying for 12-24 hours at 100-120 ℃ to obtain the high-temperature-resistant fiber reinforced silica aerogel heat-insulation composite material. The high-temperature-resistant fiber-reinforced silica aerogel heat-insulation composite material has the characteristic of intrinsic hydrophobicity, the particle size of the particles is within the range of 400nm to 3 mu m, and the high temperature of 1000 ℃ can be resisted.
The invention can achieve the following beneficial effects:
the invention is based on a sol-gel technology, uses silicon salt as a precursor and uses nitric acid and ammonia water as catalysts to prepare silicon dioxide sol by an acid-base two-step method, then mixes the silicon dioxide sol with a fiber prefabricated part, and obtains the silicon dioxide aerogel heat insulation composite material by normal pressure drying treatment.
Therefore, the invention has the following advantages compared with the prior art:
(1) the silica aerogel heat-insulation composite material prepared by the method has high use temperature which can reach 1000 ℃. The matrix is silicon dioxide aerogel with large grain diameter, and the aerogel is not easy to sinter when used at high temperature due to large grain diameter, and the inorganic ceramic fiber has high temperature resistance. Therefore, the prepared fiber reinforced silica aerogel heat insulation composite material has higher temperature resistance, is subjected to heat treatment for 1200 seconds at 1000 ℃ in a muffle furnace, and has thickness shrinkage<1.6 percent. Meanwhile, the aerogel has a porous structure, so that the density and gaseous heat conduction of the composite material are reduced, the inorganic ceramic fiber can effectively block heat radiation at high temperature, and the density of the silicon dioxide aerogel composite material prepared by the method is ensured<0.4g/cm3Thermal conductivity at 1000 deg.C<1.018W/m·K。
(2) The silica aerogel heat-insulating composite material prepared by the method has good hydrophobicity (the contact angle is larger than 140 degrees, and the contact angle is larger than 100 degrees, the hydrophobicity is generally considered to be good), and hydrophobic treatment is not needed. The alkyl contained on the precursor (methyltrimethoxysilane, dimethyldimethoxysilane and the like) does not participate in the reaction and is directly attached to the surface and the inside of the pores of the aerogel composite material, so that the aerogel composite material has better in-situ hydrophobicity.
(3) The invention has simple preparation process and low cost. The invention takes methyltrimethoxysilane, methyltriethoxysilane or dimethyldiethoxysilane and other silicon salts as precursors to prepare silica sol, and vacuum impregnation is carried out on a fiber prefabricated member made of quartz fiber, aluminum silicate fiber, alumina fiber, mullite fiber or zirconia fiber, wherein the apparent density range of cellucotton is 0.16-0.30 g/cm3Clamping and fixing the cellucotton by using a mold, and enabling the fiber arrangement direction to be vertical to the heat flow direction in heat insulation use to obtain a cellucotton prefabricated part; then proceed withDrying under normal pressure to obtain the silicon dioxide aerogel composite material. The preparation process does not need supercritical drying equipment and omits complicated surface modification and solvent replacement processes.
(4) The method has the advantages of low price of raw materials, simple equipment, lower requirement on environment, short time consumption of the whole process flow and suitability for industrial production.
Drawings
FIG. 1 is a general flow diagram of the present invention.
Figure 2 is a photomicrograph of a composite prepared in accordance with the present invention.
FIG. 3(a) is a scanning electron micrograph (500 times magnification) of the inventive material; FIG. 3(b) is a scanning electron micrograph (50000 times magnification) of the aerogel in the area of the dashed box in FIG. 3(a) after further magnification.
Fig. 4 is a graph of the high temperature thermal conductivity of the material of the present invention.
Detailed Description
The invention is further illustrated by the following examples, in which the high temperature thermal conductivity of the material is measured by using a PDB-12-4Y/P flat thermal conductivity meter, and the contact angle of the material is measured by using a Kruss DSA100 contact angle measuring instrument. The temperature resistance of the material is tested by adopting a muffle furnace, the testing temperature is 1000 ℃, and the time is 1200 s. These examples should not be construed as limiting the scope of the invention.
Example 1:
(1) molding the fiber prefabricated part: weighing a certain mass of mullite fibrofelt to ensure that the density of the clamped fiber prefabricated member is 0.16g/cm3Clamping and fixing the weighed mullite fiber by using a mold, and enabling the fiber arrangement direction to be vertical to the heat flow direction in heat insulation use to obtain a mullite fiber prefabricated part;
(2) preparing a silica sol: adding cetyl trimethyl ammonium bromide, absolute ethyl alcohol and deionized water into methyltrimethoxysilane, and mixing and stirring for 10 minutes; adding 160ml of 0.1mol/L nitric acid, continuously stirring for 10 minutes, and standing for 2 hours; then adding 160mL of 0.1mol/L ammonia water, and continuously stirring for 10 minutes to obtain silica sol, wherein the mass ratio of methyltrimethoxysilane: cetyl trimethyl ammonium Bromide: anhydrous ethanol: deionized water: nitric acid: the molar ratio of ammonia water is 1: 7.9X 10-3:5.09:15.93:2.87×10-3:2.87×10-3；
(3) Vacuum impregnation:
3.1 placing the mullite fiber prefabricated part into an open iron box, placing the iron box into a vacuum impregnation tank, and vacuumizing to-0.1 MPa;
3.2 injecting the silica sol into an iron box through a pipeline, fully permeating the silica sol into pores of the mullite fiber prefabricated part in a vacuumizing mode, ensuring that the silica sol completely covers the prefabricated part, and keeping the pressure for 1 hour, wherein the liquid level of the silica sol exceeds 2 cm of the highest point of the mullite fiber prefabricated part;
3.3 introducing air into the vacuum impregnation tank to restore the pressure in the vacuum impregnation tank to normal pressure, and taking out the fiber/sol mixture (together with the iron box);
(4) aging the gel: putting the iron box filled with the fiber/sol mixture into a water bath kettle at 45 ℃ for standing, heating to 60 ℃ after gelling, continuing standing and aging for 1 day, and taking out a sample from the iron box to obtain a fiber/gel composite;
(5) drying under normal pressure: and (3) putting the fiber/gel composite after the gel aging into a drying box, firstly drying at 60 ℃ for 48 hours, then drying at 80 ℃ for 20 hours, and finally drying at 100 ℃ for 20 hours to obtain the silica aerogel thermal insulation composite.
The density of the silica aerogel thermal insulation composite material prepared by the embodiment is 0.19g/cm3And the thermal conductivity coefficient at 1000 ℃ is 0.085W/m.K.
FIG. 2 is a photomicrograph of example 1. As can be seen from fig. 2, the sample surface was flat and free of cracks.
FIG. 3 is a scanning electron micrograph of the microstructure of example 1. As can be seen from fig. 3(a), the composite material is composed of ceramic fibers and an aerogel matrix, which is filled in the gaps between the fibers and tightly wrapped around the fibers; from FIG. 3(b) (scale bar 200nm), it can be seen that the typical pearl chain type nanoporous aerogel network structure is presented after the aerogel in the dotted line box of FIG. 3(a) (scale bar 20 μm) is enlarged.
Fig. 4 is a high temperature thermal conductivity curve for example 1. As can be seen from the figure, the high temperature thermal conductivity of example 1 increases with the increase of temperature, the high temperature thermal conductivity is low, and the thermal conductivity at 1000 ℃ is only 0.085W/m.K.
Examples 2 to 324
In the first step of the fiber preform forming process, the type and the apparent density of the fiber have important influences on the temperature resistance, the high-temperature thermal conductivity and the like of the composite material. In the second step of the preparation process of the silica sol, the proportion of the raw materials has important influence on the performance of the material. The process parameters from the third step to the fifth step, such as vacuum degree, dwell time, gelling temperature and time, aging temperature and time, drying temperature and time, have no substantial influence on the properties of the material.
Therefore, the technological parameters influencing the performance of the composite material mainly comprise 3 parameters of fiber types, fiber apparent density and raw material proportion in silica sol (the content of methyltrimethoxysilane, hexadecyl trimethyl ammonium bromide and nitric acid is a fixed value, and the content of absolute ethyl alcohol, the content of deionized water and the content of ammonia water can be changed). Examples 2-324 were therefore primarily varied in these 3 process parameters to further explain the invention. The process parameters used in examples 2 to 423 are shown in Table 1, and the process parameters are the same as in example 1 except for the process parameters written in the Table.
TABLE 1 preparation Process parameters and Material Properties of fiber-reinforced silica aerogel thermal insulation composite
Claims (7)
1. A preparation method of a high-temperature-resistant fiber-reinforced silica aerogel heat-insulation composite material is characterized by comprising the following steps:
the first step, preparing an inorganic ceramic fiber preform, the method comprises:
calculating the mass of the required inorganic ceramic fiber by adopting the mass which is density multiplied by volume according to the apparent density of the inorganic ceramic fiber prefabricated member, clamping and fixing the weighed inorganic ceramic fiber by using a mould, and enabling the fiber arrangement direction to be vertical to the heat flow direction in heat insulation use to obtain the inorganic ceramic fiber prefabricated member;
secondly, preparing the silica sol by the following steps:
taking silicate as precursor, adding cetyl trimethyl ammonium bromide (CH)3(CH2)15N(Br)(CH3)3Adding absolute ethyl alcohol and deionized water, adding nitric acid and ammonia water, and preparing the silica sol by adopting an acid-base two-step method, wherein the specific process comprises the following steps: firstly, mixing and stirring silicon salt, hexadecyl trimethyl ammonium bromide, absolute ethyl alcohol and deionized water for 10 minutes to obtain a mixed solution, then dripping nitric acid into the mixed solution, continuously stirring for 10 minutes, standing for 1-2 hours to fully hydrolyze the silicon salt to obtain a hydrolyzed mixed solution; then dropwise adding ammonia water into the hydrolyzed mixed solution, and stirring for 10 minutes to obtain the dioxygenDissolving silica sol; wherein the molar ratio of each component is silicon salt: cetyl trimethylammonium bromide: anhydrous ethanol: deionized water: nitric acid: ammonia water 1: 7.9X 10-3:5.09～7.63:15.93～23.89:2.87×10-3：2.87×10-3～9.85×10-3；
Thirdly, vacuum impregnation is carried out, and the method comprises the following steps:
3.1 placing the inorganic ceramic fiber prefabricated part into an open iron box, placing the iron box into a vacuum impregnation tank, and vacuumizing to-0.1 MPa to-0.05 MPa;
3.2 injecting the silica sol into an iron box through a pipeline, fully permeating the silica sol into the pores of the inorganic ceramic fiber prefabricated part by adopting a vacuumizing mode, ensuring that the prefabricated part is completely covered by the silica sol, and maintaining the pressure for 1-2 hours;
3.3, introducing air into the vacuum impregnation tank to restore the pressure in the vacuum impregnation tank to normal pressure, and taking out the fiber/sol mixture together with the iron box;
fourthly, aging the gel by the following method:
placing the iron box filled with the fiber/sol mixture into a water bath kettle at 40-55 ℃ for standing and aging, heating to 60-70 ℃ after silica sol in pores of the inorganic ceramic prefabricated part is gelled, continuing to stand and age for 1-2 days, and taking out a sample from the iron box to obtain a fiber/gel composite;
step five, drying under normal pressure, which comprises the following steps:
and (3) placing the fiber/gel composite after the gel aging into a drying oven, firstly drying for 24-48 hours at 60-70 ℃, then drying for 12-24 hours at 75-80 ℃, and finally drying for 12-24 hours at 100-120 ℃ to obtain the high-temperature-resistant fiber reinforced silica aerogel heat-insulation composite material.
2. The method for preparing a high temperature resistant fiber reinforced silica aerogel thermal insulation composite as claimed in claim 1, wherein the inorganic ceramic fiber in the first step is any one of quartz fiber, alumina silicate fiber, alumina fiber or mullite fiber.
3. The method for preparing a refractory fiber reinforced silica aerogel thermal insulation composite as claimed in claim 1, wherein the concentration of the absolute ethanol in the second step is more than 99%.
4. The method of claim 1, wherein the silicon salt is methyltrimethoxysilane (CH) in the second step3Si(OCH3)3Methyl triethoxysilane or CH3Si(OC2H5)3Dimethyldimethoxysilane, i.e. Si (OCH)3)2(CH3)2Dimethyldiethoxysilane (CH)3)2Si(OC2H5)2Trimethylmethoxysilane or CH3OSi(CH3)3Trimethylethoxysilane, i.e. C2H5OSi(CH3)3At least one of (1).
5. The method for preparing a high temperature resistant fiber reinforced silica aerogel thermal insulation composite material as claimed in claim 1, wherein in step 3.2, the liquid level of the silica sol is required to exceed the highest point of the fiber preform by 5 cm when the silica sol is fully infiltrated into the pores of the inorganic ceramic fiber preform by means of vacuum pumping.
6. The method for preparing the high temperature resistant fiber reinforced silica aerogel thermal insulation composite material as claimed in claim 1, wherein in the prepared high temperature resistant fiber reinforced silica aerogel thermal insulation composite material, SiO2Aerogel is uniformly filled in pores of inorganic ceramic fiber prefabricated member, the inorganic ceramic fiber prefabricated member and SiO2The mass ratio of the aerogel matrix is 1: 0.4-1.0.
7. The method for preparing a high-temperature-resistant fiber-reinforced silica aerogel heat-insulation composite material as claimed in claim 1, wherein the apparent density of the inorganic ceramic fiber preform is 0.16-0.28 g/cm3。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010276772.3A CN111302827A (en) | 2020-04-10 | 2020-04-10 | Preparation method of high-temperature-resistant fiber-reinforced silica aerogel heat-insulation composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010276772.3A CN111302827A (en) | 2020-04-10 | 2020-04-10 | Preparation method of high-temperature-resistant fiber-reinforced silica aerogel heat-insulation composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111302827A true CN111302827A (en) | 2020-06-19 |
Family
ID=71150361
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010276772.3A Pending CN111302827A (en) | 2020-04-10 | 2020-04-10 | Preparation method of high-temperature-resistant fiber-reinforced silica aerogel heat-insulation composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111302827A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250418A (en) * | 2020-10-22 | 2021-01-22 | 航天特种材料及工艺技术研究所 | Lightweight toughened heat-insulation composite material member and preparation method and application thereof |
| CN112321313A (en) * | 2020-11-30 | 2021-02-05 | 宁德时代新能源科技股份有限公司 | Ceramic fiber aerogel composite material and preparation method thereof |
| CN112609453A (en) * | 2020-11-25 | 2021-04-06 | 南京工业大学 | High-strength high-elasticity low-thermal-conductivity silica aerogel heat insulation sheet and preparation method thereof |
| CN113277822A (en) * | 2021-05-27 | 2021-08-20 | 中广核研究院有限公司 | Aerogel composite material and preparation method and application thereof |
| CN113833938A (en) * | 2021-09-17 | 2021-12-24 | 新华盛节能科技股份有限公司 | Mesoporous silica heat-insulating material and preparation method thereof |
| CN114249575A (en) * | 2021-11-22 | 2022-03-29 | 航天特种材料及工艺技术研究所 | Surface densification method for aerogel heat-proof material |
| CN114592356A (en) * | 2022-03-18 | 2022-06-07 | 陈栋 | Heat insulation material for firefighting clothes and preparation method thereof |
| CN115108809A (en) * | 2022-07-11 | 2022-09-27 | 中国人民解放军国防科技大学 | Preparation method of high-temperature-resistant modified silica aerogel heat-insulation composite material |
| CN115490476A (en) * | 2022-09-20 | 2022-12-20 | 天元建设集团有限公司 | Fireproof flame-retardant cement mortar and preparation method thereof |
| CN116425554A (en) * | 2023-04-27 | 2023-07-14 | 郑州大学 | Boron nitride@silicon dioxide composite ceramic aerogel and preparation method thereof |
| CN116876111A (en) * | 2023-07-20 | 2023-10-13 | 中国人民解放军海军工程大学 | High-temperature-resistant ceramic aerogel fiber and preparation method thereof |
| CN116876111B (en) * | 2023-07-20 | 2024-05-03 | 中国人民解放军海军工程大学 | High-temperature-resistant ceramic aerogel fiber and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0834678A (en) * | 1994-07-27 | 1996-02-06 | Matsushita Electric Works Ltd | Aerogel panel |
| CN1803602A (en) * | 2005-12-20 | 2006-07-19 | 长安大学 | Method for preparing brucite fiber reinforced SiO2 aerogel heat-insulating material |
| CN104261798A (en) * | 2014-09-18 | 2015-01-07 | 中国人民解放军国防科学技术大学 | High-temperature-resistant SiCOB aerogel heat-insulation composite material and preparation method thereof |
| CN108329046A (en) * | 2018-02-26 | 2018-07-27 | 中国人民解放军国防科技大学 | Preparation method of carbon aerogel heat insulation composite material |
| CN109516763A (en) * | 2019-01-07 | 2019-03-26 | 东华大学 | A kind of cellulose fibre/SiO2Aerogel composite and its preparation and application |
-
2020
- 2020-04-10 CN CN202010276772.3A patent/CN111302827A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0834678A (en) * | 1994-07-27 | 1996-02-06 | Matsushita Electric Works Ltd | Aerogel panel |
| CN1803602A (en) * | 2005-12-20 | 2006-07-19 | 长安大学 | Method for preparing brucite fiber reinforced SiO2 aerogel heat-insulating material |
| CN104261798A (en) * | 2014-09-18 | 2015-01-07 | 中国人民解放军国防科学技术大学 | High-temperature-resistant SiCOB aerogel heat-insulation composite material and preparation method thereof |
| CN108329046A (en) * | 2018-02-26 | 2018-07-27 | 中国人民解放军国防科技大学 | Preparation method of carbon aerogel heat insulation composite material |
| CN109516763A (en) * | 2019-01-07 | 2019-03-26 | 东华大学 | A kind of cellulose fibre/SiO2Aerogel composite and its preparation and application |
Non-Patent Citations (2)
| Title |
|---|
| DONGXUAN DU等: "Facile synthesis of silica aerogel composites via ambient-pressure drying without surface modification or solvent exchange", 《VACUUM》 * |
| 罗燚等: "常压干燥制备SiO2气凝胶复合材料研究进展", 《材料导报》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250418A (en) * | 2020-10-22 | 2021-01-22 | 航天特种材料及工艺技术研究所 | Lightweight toughened heat-insulation composite material member and preparation method and application thereof |
| CN112609453A (en) * | 2020-11-25 | 2021-04-06 | 南京工业大学 | High-strength high-elasticity low-thermal-conductivity silica aerogel heat insulation sheet and preparation method thereof |
| CN112321313A (en) * | 2020-11-30 | 2021-02-05 | 宁德时代新能源科技股份有限公司 | Ceramic fiber aerogel composite material and preparation method thereof |
| CN113277822A (en) * | 2021-05-27 | 2021-08-20 | 中广核研究院有限公司 | Aerogel composite material and preparation method and application thereof |
| CN113833938A (en) * | 2021-09-17 | 2021-12-24 | 新华盛节能科技股份有限公司 | Mesoporous silica heat-insulating material and preparation method thereof |
| CN114249575B (en) * | 2021-11-22 | 2023-03-10 | 航天特种材料及工艺技术研究所 | Surface densification method for aerogel heat-proof material |
| CN114249575A (en) * | 2021-11-22 | 2022-03-29 | 航天特种材料及工艺技术研究所 | Surface densification method for aerogel heat-proof material |
| CN114592356A (en) * | 2022-03-18 | 2022-06-07 | 陈栋 | Heat insulation material for firefighting clothes and preparation method thereof |
| CN115108809A (en) * | 2022-07-11 | 2022-09-27 | 中国人民解放军国防科技大学 | Preparation method of high-temperature-resistant modified silica aerogel heat-insulation composite material |
| CN115490476A (en) * | 2022-09-20 | 2022-12-20 | 天元建设集团有限公司 | Fireproof flame-retardant cement mortar and preparation method thereof |
| CN115490476B (en) * | 2022-09-20 | 2023-04-18 | 天元建设集团有限公司 | Fireproof flame-retardant cement mortar and preparation method thereof |
| CN116425554A (en) * | 2023-04-27 | 2023-07-14 | 郑州大学 | Boron nitride@silicon dioxide composite ceramic aerogel and preparation method thereof |
| CN116876111A (en) * | 2023-07-20 | 2023-10-13 | 中国人民解放军海军工程大学 | High-temperature-resistant ceramic aerogel fiber and preparation method thereof |
| CN116876111B (en) * | 2023-07-20 | 2024-05-03 | 中国人民解放军海军工程大学 | High-temperature-resistant ceramic aerogel fiber and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111302827A (en) | Preparation method of high-temperature-resistant fiber-reinforced silica aerogel heat-insulation composite material | |
| CN112174144B (en) | Ultrahigh-transparency large-size block silica aerogel and preparation method and application thereof | |
| CN105967728B (en) | A kind of fiber reinforcement Al2O3-SiO2Aeroge effectively insulating composite material and preparation method | |
| CN106747541B (en) | Method for in-situ synthesis of mullite whisker self-toughened mullite ceramic | |
| CN102910926B (en) | Preparation method of high-temperature resistant silicon carbide aerogel heat-insulation composite material | |
| CN103288468A (en) | Preparation method for fiber reinforced carbon-silicon carbide-zirconium carbide-based composite material | |
| CN102745998B (en) | Preparation method for anti-oxidant silica-based ceramic coating with wide temperature range for carbon/carbon composite | |
| CN106809842B (en) | A kind of preparation method of high temperature oxidation resisting Silica Aerogels | |
| CN111099912A (en) | High-temperature-resistant heat-insulation wave-transparent integrated aerogel composite material and preparation process thereof | |
| KR20130123942A (en) | Preparation method of hydrophobic monolith type silica aerogel | |
| CN109251005B (en) | Preparation method of reinforced silica aerogel material | |
| CN104261798A (en) | High-temperature-resistant SiCOB aerogel heat-insulation composite material and preparation method thereof | |
| CN109336545A (en) | A kind of silicon dioxide silica aerogel composite material, preparation method and application | |
| CN106589821A (en) | Preparation method of mullite fiber/epoxy resin composite material | |
| CN105036143B (en) | Preparation method of nano silicon dioxide aerogel | |
| CN106608730A (en) | Carbon-based Si-C-O aerogel thermal insulation composite material and preparation method thereof | |
| Wang et al. | Synthesis of composite insulation materials—expanded perlite filled with silica aerogel | |
| CN112811933A (en) | Preparation method of nanowire-reinforced silicon nitride foamed ceramic composite silicon dioxide aerogel and product thereof | |
| CN108774072B (en) | Rigid heat insulation tile and preparation method thereof | |
| CN110468453B (en) | Preparation method for in-situ growth of high-length-diameter-ratio mullite whiskers | |
| CN110330021B (en) | Ultralow-density aerogel material and preparation method and application thereof | |
| CN102603344A (en) | Preparing process of silicon carbide whisker toughened zirconium diboride ceramic | |
| CN109626954A (en) | A kind of heatproof damp-proof silicon dioxide silica aerogel composite material and its preparation method and application | |
| Wu et al. | SiO2 aerogel multiscale reinforced by glass fibers and SiC nanowhiskers for thermal insulation | |
| CN112030544B (en) | Method for in-situ growth of silicon carbide nanowires on surface of silicon carbide fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20200619 |
|
| WD01 | Invention patent application deemed withdrawn after publication |