CN108530016A - A kind of preparation method of compound heat-insulation aerogel material - Google Patents
A kind of preparation method of compound heat-insulation aerogel material Download PDFInfo
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- CN108530016A CN108530016A CN201810273057.7A CN201810273057A CN108530016A CN 108530016 A CN108530016 A CN 108530016A CN 201810273057 A CN201810273057 A CN 201810273057A CN 108530016 A CN108530016 A CN 108530016A
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- 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
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- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- 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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- 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
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Abstract
The present invention provides a kind of preparation methods of compound heat-insulation aerogel material, include the following steps：（1）Dopamine hydrochloric acid solution is configured, pH value is adjusted；（2）Alumina silicate fiber felt, basalt fibre felt and mullite polycrystalline fibre is added, impregnates oscillation；（3）It is cleaned after taking-up, dries to obtain treated composite fibre；（4）Take titanium tetrachloride and deionized water that solution A is mixed to obtain；（5）Take ethyl orthosilicate and ethyl alcohol that solution B is mixed to obtain；（6）Solution A and solution B are mixed；（7）It is put into ice-water bath, propylene oxide stirring is added；（8）Composite fibre is added, stirs evenly, pours into mold, seal aging；（9）It takes out, impregnates in acetone；（10）It takes out and is drying to obtain from acetone.Material prepared by this method has extraordinary heat insulation, has extraordinary mechanical property, and bending strength, flexibility is good, and compressive strength is high, extraordinary to avoid the case where material is broken suddenly.
Description
Technical field
The present invention relates to a kind of preparation methods of compound heat-insulation aerogel material.
Background technology
SiO2Aeroge is the Performances of Novel Nano-Porous metre hole multifunctional solid material that current density is minimum and heat-proof quality is best, in object
The fields such as Physicochemical, calorifics, optics and electricity have extensive development and application prospect.But due to SiO2Aeroge has very big
Porosity（Up to 99%）And infrared transmittivity（3~5 μm）, keep its mechanical property and high temperature heat-proof quality poor, greatly
Limit SiO2Development and energy-saving application of the aeroge in every field.Therefore improve SiO2Aeroge mechanics and high temperature are heat-insulated
Performance becomes research hotspot both domestic and external, and it is to improve SiO to use fiber composite enhancing2Mechanical Properties of Aerogels and heat-proof quality
Maximally efficient approach.
Invention content
Technical problems to be solved：The object of the present invention is to provide a kind of preparation method of compound heat-insulation aerogel material,
Prepared material thermal conductivity is very low, has extraordinary heat insulation, while having extraordinary mechanical property, and bending is strong
Degree, flexibility is good, and compressive strength is high, extraordinary to avoid the case where material is broken suddenly.
Technical solution：A kind of preparation method of compound heat-insulation aerogel material, ingredient by weight, including following step
Suddenly：
（1）50-80 parts of dopamine hydrochloric acid solutions are configured, adjust pH value to 9-10；
（2）5-10 parts of alumina silicate fiber felts, 1-3 parts of basalt fibre felts and 2-5 parts of mullite polycrystalline fibres are added, are protected from light immersion
Vibrate 15-20h；
（3）It is cleaned with deionized water after taking-up, treated composite fibre is dried to obtain at 30-40 DEG C；
（4）Titanium tetrachloride and deionized water is taken to mix, stirring and dissolving obtains solution A, wherein the volume of titanium tetrachloride and deionized water
Than being 1:3；
（5）Ethyl orthosilicate and ethyl alcohol is taken to mix, stirring and dissolving obtains solution B, wherein the volume ratio of ethyl orthosilicate and ethyl alcohol is
3:1；
（6）30-50 parts of solution As and 20-30 parts of solution Bs are mixed, 2-3h is stirred；
（7）It is put into ice-water bath, 3-5 parts of propylene oxide is added, stir 30-40min；
（8）Composite fibre is added, stirs evenly, pours into mold, be sealed in aging 24-27h at 50-55 DEG C；
（9）It takes out, impregnates in acetone for 24 hours, an acetone is replaced per 8h；
（10）It is taken out from acetone, through supercritical CO2It is drying to obtain.
It is further preferred that the supercritical CO2Dry operating process is：
The first step：Gel is placed in autoclave, kettle is sealed, uses CO2Purging displaces the air in kettle；
Second step：It is filled with CO2, in 30-35 DEG C of temperature, pressure is dry 40-60min under 7-8MPa；
Third walks：Slow release CO2To normal pressure, then with CO2Autoclave is purged, room temperature is down to and completes.
It is further preferred that the size of the alumina silicate fiber felt and basalt fibre felt is long 50mm, wide 30mm, thickness 50
μm。
It is further preferred that the length of the mullite polycrystalline fibre is 30-50mm.
It is further preferred that a concentration of 5-10mg/mL of the dopamine hydrochloric acid solution.
Advantageous effect：
1. the present invention is handled fibrofelt and fiber with dopamine, the functional group in dopamine can by fiber and
It is effectively combined between gel, improves the switching performance of composite material interface.
2. the present invention is with supercritical CO2Gel is dried in method, can effectively prevent the reunion of composite fibre, make
Fiber dispersion is more uniform, obtains stable aeroge skeleton.
3. material thermal conductivity of the present invention is very low, there is extraordinary heat insulation, while there is extraordinary mechanical property
Can, bending strength reaches as high as 1.32MPa, and flexibility is good, and compressive strength reaches as high as 0.20MPa, extraordinary to avoid
The case where material is broken suddenly.
Specific implementation mode
Embodiment 1
A kind of preparation method of compound heat-insulation aerogel material, ingredient by weight, include the following steps：
（1）50 parts of dopamine hydrochloric acid solutions are configured, adjust pH value to 9；
（2）5 parts of alumina silicate fiber felts, 1 part of basalt fibre felt and 2 parts of mullite polycrystalline fibres are added, are protected from light immersion oscillation
15h；
（3）It is cleaned with deionized water after taking-up, treated composite fibre is dried to obtain at 30 DEG C；
（4）Titanium tetrachloride and deionized water is taken to mix, stirring and dissolving obtains solution A, wherein the volume of titanium tetrachloride and deionized water
Than being 1:3；
（5）Ethyl orthosilicate and ethyl alcohol is taken to mix, stirring and dissolving obtains solution B, wherein the volume ratio of ethyl orthosilicate and ethyl alcohol is
3:1；
（6）30 parts of solution As and 20 parts of solution Bs are mixed, 2h is stirred；
（7）It is put into ice-water bath, 3 parts of propylene oxide is added, stir 30min；
（8）Composite fibre is added, stirs evenly, pours into mold, is sealed at 50 DEG C aging for 24 hours；
（9）It takes out, impregnates in acetone for 24 hours, an acetone is replaced per 8h；
（10）It takes out, is placed in autoclave from acetone, seal kettle, use CO2Purging displaces the air in kettle；
（11）It is filled with CO2, in 30 DEG C of temperature, pressure is dry 40min under 7MPa；
（12）Slow release CO2To normal pressure, then with CO2It purges autoclave, is down to room temperature to obtain the final product.
Embodiment 2
A kind of preparation method of compound heat-insulation aerogel material, ingredient by weight, include the following steps：
（1）60 parts of dopamine hydrochloric acid solutions are configured, adjust pH value to 9；
（2）7 parts of alumina silicate fiber felts, 2 parts of basalt fibre felts and 3 parts of mullite polycrystalline fibres are added, are protected from light immersion oscillation
17h；
（3）It is cleaned with deionized water after taking-up, treated composite fibre is dried to obtain at 35 DEG C；
（4）Titanium tetrachloride and deionized water is taken to mix, stirring and dissolving obtains solution A, wherein the volume of titanium tetrachloride and deionized water
Than being 1:3；
（5）Ethyl orthosilicate and ethyl alcohol is taken to mix, stirring and dissolving obtains solution B, wherein the volume ratio of ethyl orthosilicate and ethyl alcohol is
3:1；
（6）35 parts of solution As and 25 parts of solution Bs are mixed, 2.5h is stirred；
（7）It is put into ice-water bath, 4 parts of propylene oxide is added, stir 35min；
（8）Composite fibre is added, stirs evenly, pours into mold, be sealed in aging 25h at 52 DEG C；
（9）It takes out, impregnates in acetone for 24 hours, an acetone is replaced per 8h；
（10）It takes out, is placed in autoclave from acetone, seal kettle, use CO2Purging displaces the air in kettle；
（11）It is filled with CO2, in 31 DEG C of temperature, pressure is dry 45min under 7.2MPa；
（12）Slow release CO2To normal pressure, then with CO2It purges autoclave, is down to room temperature to obtain the final product.
Embodiment 3
A kind of preparation method of compound heat-insulation aerogel material, ingredient by weight, include the following steps：
（1）70 parts of dopamine hydrochloric acid solutions are configured, adjust pH value to 10；
（2）9 parts of alumina silicate fiber felts, 2 parts of basalt fibre felts and 4 parts of mullite polycrystalline fibres are added, are protected from light immersion oscillation
18h；
（3）It is cleaned with deionized water after taking-up, treated composite fibre is dried to obtain at 35 DEG C；
（4）Titanium tetrachloride and deionized water is taken to mix, stirring and dissolving obtains solution A, wherein the volume of titanium tetrachloride and deionized water
Than being 1:3；
（5）Ethyl orthosilicate and ethyl alcohol is taken to mix, stirring and dissolving obtains solution B, wherein the volume ratio of ethyl orthosilicate and ethyl alcohol is
3:1；
（6）40 parts of solution As and 25 parts of solution Bs are mixed, 2-3h is stirred；
（7）It is put into ice-water bath, 4 parts of propylene oxide is added, stir 35min；
（8）Composite fibre is added, stirs evenly, pours into mold, be sealed in aging 25h at 53 DEG C；
（9）It takes out, impregnates in acetone for 24 hours, an acetone is replaced per 8h；
（10）It takes out, is placed in autoclave from acetone, seal kettle, use CO2Purging displaces the air in kettle；
（11）It is filled with CO2, in 33 DEG C of temperature, pressure is dry 50min under 7.5MPa；
（12）Slow release CO2To normal pressure, then with CO2It purges autoclave, is down to room temperature to obtain the final product.
Embodiment 4
A kind of preparation method of compound heat-insulation aerogel material, ingredient by weight, include the following steps：
（1）80 parts of dopamine hydrochloric acid solutions are configured, adjust pH value to 10；
（2）10 parts of alumina silicate fiber felts, 3 parts of basalt fibre felts and 5 parts of mullite polycrystalline fibres are added, are protected from light immersion oscillation
20h；
（3）It is cleaned with deionized water after taking-up, treated composite fibre is dried to obtain at 40 DEG C；
（4）Titanium tetrachloride and deionized water is taken to mix, stirring and dissolving obtains solution A, wherein the volume of titanium tetrachloride and deionized water
Than being 1:3；
（5）Ethyl orthosilicate and ethyl alcohol is taken to mix, stirring and dissolving obtains solution B, wherein the volume ratio of ethyl orthosilicate and ethyl alcohol is
3:1；
（6）50 parts of solution As and 30 parts of solution Bs are mixed, 3h is stirred；
（7）It is put into ice-water bath, 5 parts of propylene oxide is added, stir 40min；
（8）Composite fibre is added, stirs evenly, pours into mold, be sealed in aging 27h at 55 DEG C；
（9）It takes out, impregnates in acetone for 24 hours, an acetone is replaced per 8h；
（10）It takes out, is placed in autoclave from acetone, seal kettle, use CO2Purging displaces the air in kettle；
（11）It is filled with CO2, in 35 DEG C of temperature, pressure is dry 60min under 8MPa；
（12）Slow release CO2To normal pressure, then with CO2It purges autoclave, is down to room temperature to obtain the final product.
Comparative example 1
The present embodiment is with embodiment 1 the difference is that replacing basalt fibre felt with alumina silicate fiber felt, specially：
A kind of preparation method of compound heat-insulation aerogel material, ingredient by weight, include the following steps：
（1）50 parts of dopamine hydrochloric acid solutions are configured, adjust pH value to 9；
（2）6 parts of alumina silicate fiber felts and 2 parts of mullite polycrystalline fibres are added, are protected from light immersion oscillation 15h；
（3）It is cleaned with deionized water after taking-up, treated composite fibre is dried to obtain at 30 DEG C；
（4）Titanium tetrachloride and deionized water is taken to mix, stirring and dissolving obtains solution A, wherein the volume of titanium tetrachloride and deionized water
Than being 1:3；
（5）Ethyl orthosilicate and ethyl alcohol is taken to mix, stirring and dissolving obtains solution B, wherein the volume ratio of ethyl orthosilicate and ethyl alcohol is
3:1；
（6）30 parts of solution As and 20 parts of solution Bs are mixed, 2h is stirred；
（7）It is put into ice-water bath, 3 parts of propylene oxide is added, stir 30min；
（8）Composite fibre is added, stirs evenly, pours into mold, is sealed at 50 DEG C aging for 24 hours；
（9）It takes out, impregnates in acetone for 24 hours, an acetone is replaced per 8h；
（10）It takes out, is placed in autoclave from acetone, seal kettle, use CO2Purging displaces the air in kettle；
（11）It is filled with CO2, in 30 DEG C of temperature, pressure is dry 40min under 7MPa；
（12）Slow release CO2To normal pressure, then with CO2It purges autoclave, is down to room temperature to obtain the final product.
Comparative example 2
The present embodiment is with embodiment 1 the difference is that not containing titanium tetrachloride, specially：
A kind of preparation method of compound heat-insulation aerogel material, ingredient by weight, include the following steps：
（1）50 parts of dopamine hydrochloric acid solutions are configured, adjust pH value to 9；
（2）5 parts of alumina silicate fiber felts, 1 part of basalt fibre felt and 2 parts of mullite polycrystalline fibres are added, are protected from light immersion oscillation
15h；
（3）It is cleaned with deionized water after taking-up, treated composite fibre is dried to obtain at 30 DEG C；
（4）Ethyl orthosilicate and ethyl alcohol is taken to mix, stirring and dissolving obtains solution B, wherein the volume ratio of ethyl orthosilicate and ethyl alcohol is
3:1；
（5）It is put into ice-water bath, 3 parts of propylene oxide is added, stir 30min；
（6）Composite fibre is added, stirs evenly, pours into mold, is sealed at 50 DEG C aging for 24 hours；
（7）It takes out, impregnates in acetone for 24 hours, an acetone is replaced per 8h；
（8）It takes out, is placed in autoclave from acetone, seal kettle, use CO2Purging displaces the air in kettle；
（9）It is filled with CO2, in 30 DEG C of temperature, pressure is dry 40min under 7MPa；
（10）Slow release CO2To normal pressure, then with CO2It purges autoclave, is down to room temperature to obtain the final product.
Comparative example 3
The present embodiment is with embodiment 1 the difference is that not handled with bar amine hydrochloric acid solution, specially：
A kind of preparation method of compound heat-insulation aerogel material, ingredient by weight, include the following steps：
（1）5 parts of alumina silicate fiber felts, 1 part of basalt fibre felt and 2 parts of mullite polycrystalline fibres are dried into obtain processing at 30 DEG C
Composite fibre afterwards；
（2）Titanium tetrachloride and deionized water is taken to mix, stirring and dissolving obtains solution A, wherein the volume of titanium tetrachloride and deionized water
Than being 1:3；
（3）Ethyl orthosilicate and ethyl alcohol is taken to mix, stirring and dissolving obtains solution B, wherein the volume ratio of ethyl orthosilicate and ethyl alcohol is
3:1；
（4）30 parts of solution As and 20 parts of solution Bs are mixed, 2h is stirred；
（5）It is put into ice-water bath, 3 parts of propylene oxide is added, stir 30min；
（6）Composite fibre is added, stirs evenly, pours into mold, is sealed at 50 DEG C aging for 24 hours；
（7）It takes out, impregnates in acetone for 24 hours, an acetone is replaced per 8h；
（8）It takes out, is placed in autoclave from acetone, seal kettle, use CO2Purging displaces the air in kettle；
（9）It is filled with CO2, in 30 DEG C of temperature, pressure is dry 40min under 7MPa；
（10）Slow release CO2To normal pressure, then with CO2It purges autoclave, is down to room temperature to obtain the final product.
The partial properties index of 1 compound heat-insulation aerogel material of table
The partial properties index of compound heat-insulation aerogel material prepared by the method for the present invention is seen the above table, it may be seen that thermal conductivity
Rate is very low, and the thermal conductivity at 300 DEG C, 600 DEG C and 1000 DEG C distinguishes minimum 0.021Wm-1·K-1、0.034W·m-1·
K-1And 0.063Wm-1·K-1, there is extraordinary heat insulation, while there is extraordinary mechanical property, bending strength
1.32MPa is reached as high as, flexibility is good, and compressive strength reaches as high as 0.20MPa, extraordinary to avoid what material was broken suddenly
Situation.
Claims (5)
1. a kind of preparation method of compound heat-insulation aerogel material, it is characterised in that：Ingredient by weight, including following step
Suddenly：
（1）50-80 parts of dopamine hydrochloric acid solutions are configured, adjust pH value to 9-10；
（2）5-10 parts of alumina silicate fiber felts, 1-3 parts of basalt fibre felts and 2-5 parts of mullite polycrystalline fibres are added, are protected from light immersion
Vibrate 15-20h；
（3）It is cleaned with deionized water after taking-up, treated composite fibre is dried to obtain at 30-40 DEG C；
（4）Titanium tetrachloride and deionized water is taken to mix, stirring and dissolving obtains solution A, wherein the volume of titanium tetrachloride and deionized water
Than being 1:3；
（5）Ethyl orthosilicate and ethyl alcohol is taken to mix, stirring and dissolving obtains solution B, wherein the volume ratio of ethyl orthosilicate and ethyl alcohol is
3:1；
（6）30-50 parts of solution As and 20-30 parts of solution Bs are mixed, 2-3h is stirred；
（7）It is put into ice-water bath, 3-5 parts of propylene oxide is added, stir 30-40min；
（8）Composite fibre is added, stirs evenly, pours into mold, be sealed in aging 24-27h at 50-55 DEG C；
（9）It takes out, impregnates in acetone for 24 hours, an acetone is replaced per 8h；
（10）It is taken out from acetone, through supercritical CO2It is drying to obtain.
2. a kind of preparation method of compound heat-insulation aerogel material according to claim 1, it is characterised in that：It is described super
Critical CO2Dry operating process is：
The first step：Gel is placed in autoclave, kettle is sealed, uses CO2Purging displaces the air in kettle；
Second step：It is filled with CO2, in 30-35 DEG C of temperature, pressure is dry 40-60min under 7-8MPa；
Third walks：Slow release CO2To normal pressure, then with CO2Autoclave is purged, room temperature is down to and completes.
3. a kind of preparation method of compound heat-insulation aerogel material according to claim 1, it is characterised in that：The silicon
The size of sour aluminum fiber mat and basalt fibre felt is long 50mm, wide 30mm, 50 μm of thickness.
4. a kind of preparation method of compound heat-insulation aerogel material according to claim 1, it is characterised in that：It is described not
The length for carrying out stone polycrystalline fibre is 30-50mm.
5. a kind of preparation method of compound heat-insulation aerogel material according to claim 1, it is characterised in that：It is described more
A concentration of 5-10mg/mL of bar amine hydrochloric acid solution.
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| CN201810273057.7A CN108530016A (en) | 2018-03-29 | 2018-03-29 | A kind of preparation method of compound heat-insulation aerogel material |
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|---|---|---|---|
| CN201810273057.7A CN108530016A (en) | 2018-03-29 | 2018-03-29 | A kind of preparation method of compound heat-insulation aerogel material |
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ID=63482547
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110540662A (en) * | 2019-10-14 | 2019-12-06 | 陕西科技大学 | Preparation method of polydopamine modified carbon fiber/mullite whisker reinforced resin-based friction material |
| CN113788660A (en) * | 2021-10-27 | 2021-12-14 | 天元建设集团有限公司 | High-strength anti-crack concrete |
-
2018
- 2018-03-29 CN CN201810273057.7A patent/CN108530016A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110540662A (en) * | 2019-10-14 | 2019-12-06 | 陕西科技大学 | Preparation method of polydopamine modified carbon fiber/mullite whisker reinforced resin-based friction material |
| CN113788660A (en) * | 2021-10-27 | 2021-12-14 | 天元建设集团有限公司 | High-strength anti-crack concrete |
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Application publication date: 20180914 |