CN113694844A - Preparation process of aerogel felt - Google Patents
Preparation process of aerogel felt Download PDFInfo
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- CN113694844A CN113694844A CN202111095836.0A CN202111095836A CN113694844A CN 113694844 A CN113694844 A CN 113694844A CN 202111095836 A CN202111095836 A CN 202111095836A CN 113694844 A CN113694844 A CN 113694844A
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
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- B01J19/126—Microwaves
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Abstract
The invention discloses a preparation process of aerogel felt, which comprises the following steps: (1) mixing the sol and the gel catalyst to obtain a mixed solution; (2) compounding the mixed solution with a fiber felt to form a wet gel felt; (3) conveying the wet gel felt into a microwave cavity for microwave heating gel and curing; (4) conveying the wet gel felt to a heat preservation section for normal temperature curing; (5) and (3) drying the wet gel felt solidified at the normal temperature by using supercritical carbon dioxide to obtain the aerogel felt. According to the invention, the inside and the outside of the wet gel felt are simultaneously heated by microwave heating, the wet gel felt is uniformly heated and can be gelled simultaneously, the problem that the gel on the outside of the wet gel felt is fast and the gel on the inside of the wet gel felt is slow due to the traditional water tank heating process is avoided, the problem that the gel inside the wet gel felt is perfect by reducing the running speed of a belt or lengthening the transportation distance is further avoided, the running speed is improved by 2-4 times on the premise that the transportation distance is not changed, and the production efficiency is greatly improved.
Description
Technical Field
The invention belongs to the technical field of chemical materials, and particularly relates to a preparation process of an aerogel felt.
Background
In recent years, the development of microwave chemistry has been related to various fields of chemical reactions, and a large number of experiments have proved that microwaves can greatly improve the reaction rate of some chemical reactions, so that some reactions which are difficult to be carried out under common conditions can be rapidly carried out. Through being applied to aerogel process in the aerogel material preparation process with microwave curing technique, solidify wet gel felt, effectively solve traditional water tank heating and be heated the inequality, the slow scheduling problem of gel speed, improve gel production line operating speed greatly, and then improve production efficiency, reduce manufacturing cost, can improve aerogel material performance index simultaneously. At home and abroad, the microwave curing technology is widely applied and plays a great role in preparing aerogel materials. After 2014, the technology has been intensively studied in universities such as Nanjing industry university, national defense science and technology university, Zhejiang university, Guangzhou university and the like. At present, the aerogel microwave curing technology is mainly used for laboratory research, and the industrial application is not mature.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a preparation process of aerogel felt.
A preparation process of aerogel felt comprises the following steps:
(1) mixing the sol and the gel catalyst to obtain a mixed solution, wherein the mixing comprises the steps of preheating the sol and the gel catalyst to 30-60 ℃, and then mixing the sol and the gel catalyst according to the weight ratio of 10: (0.1-1) are mixed evenly; the sol is prepared by mixing and hydrolyzing a silicon source precursor, a solvent and a hydrolysis catalyst; the silicon source precursor comprises one or a mixture of more than two of tetraethoxysilane, methyl orthosilicate, trimethylchlorosilane, methyltriethoxysilane and methyltrimethoxysilane; the solvent comprises one or the combination of more than two of methanol, ethanol, butanol and linear chain alcohol with the mass fraction of more than 96%; the hydrolysis catalyst comprises one or the combination of more than two of hydrochloric acid, oxalic acid, nitric acid, sulfuric acid, acetic acid, ammonia water, ammonium carbonate and ammonium bicarbonate; the gel catalyst is formed by mixing an alkaline catalyst and an organic solvent, wherein the alkaline catalyst is one or a mixture of more than two of 25-28% concentrated ammonia water, 1-90% ammonium fluoride aqueous solution, a silane coupling agent KH502 and a silane coupling agent KH550, and the organic solvent is one or a mixture of two of refined methanol and 95% ethanol;
(2) compounding the mixed solution with a fiber felt to form a wet gel felt;
(3) conveying the wet gel felt into a microwave cavity for microwave heating gel and curing, and keeping the temperature inside and outside the gel felt at 55-60 ℃; the microwave cavity is a square cylinder structure which is made of 15-25mm polypropylene plates and is provided with openings at two ends, the height of the microwave cavity is 2-10 times of the thickness of the wet gel felt, the length of the microwave cavity is 8-12m, the width of the microwave cavity is larger than the width of a belt so as to ensure the normal conveying of the belt, a plurality of groups of magnetrons are arranged on the outer sides of the upper end and the lower end of the microwave cavity, protective housings are arranged on the outer sides of the magnetrons, the number of the magnetrons is less than 120, and the rated power of each group of magnetrons is 1 kw;
(4) conveying the wet gel felt to a heat preservation section for normal temperature solidification, wherein the heat preservation section is arranged at an outlet of the microwave cavity and consists of a heat preservation cover plate arranged above a belt, and the length of the heat preservation section is 8-16m so as to slow down heat exchange between the wet gel felt after microwave heating and the outside and prevent the wet gel felt from being rapidly cooled;
(5) and (3) drying the wet gel felt solidified at the normal temperature by using supercritical carbon dioxide to obtain the aerogel felt.
Preferably, the composite mode of the mixed liquor and the fiber felt is a spraying method, namely the mixed liquor is uniformly sprayed to the surface of the fiber felt through a spraying device, and the mixed liquor is settled and permeated to enter and fill the pores in the fiber felt by utilizing the self gravity of the mixed liquor to form the wet gel felt.
Preferably, the composite mode of the mixed solution and the fiber felt is an impregnation method, namely the mixed solution is injected into a tray, the fiber felt is immersed into the mixed solution, and the mixed solution is settled and permeated by utilizing the self gravity of the mixed solution to enter and fill the pores in the fiber felt to form the wet gel felt.
Compared with the prior art, the preparation process of the aerogel felt has the beneficial effects that: 1. according to the invention, the inside and the outside of the wet gel felt are simultaneously heated by microwave heating, the wet gel felt is uniformly heated and can be gelled simultaneously, the problem that the gel on the outside of the wet gel felt is fast and the gel on the inside of the wet gel felt is slow due to the traditional water tank heating process is avoided, the problem that the gel inside the wet gel felt is perfect by reducing the running speed of a belt or lengthening the transportation distance is further avoided, the running speed is improved by 2-4 times on the premise that the transportation distance is not changed, and the production efficiency is greatly improved; 2. according to the invention, the sol in the wet gel felt is rapidly heated to 55-60 ℃ by microwave heating, which is several times to ten times of that of the traditional water tank, and the high temperature can accelerate the gelling rate, so that the consumption of the gel catalyst can be reduced, the raw material cost can be reduced, the content of the gel catalyst in the wet gel felt can be reduced, and the product quality can be effectively improved; 3. the production method has the advantages that the production continuity is high, the safety is high, the heat conductivity coefficient of the produced aerogel felt at normal temperature is 0.016-0.021W/m.K, and all performance indexes meet the relevant national standards.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of the structure of a microwave cavity used in the aerogel blanket manufacturing process of the present invention.
Shown in the figure are 1-protective shell, 2-microwave cavity, 3-magnetron.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
It should be understood that the structures, proportions, and dimensions shown in the drawings and described herein are for illustrative purposes only and are not intended to limit the scope of the present invention, which is defined by the claims, but rather by the claims. In addition, the terms such as "upper" and "lower" used in the present specification are for convenience of description only and are not intended to limit the scope of the present invention, and changes or modifications of the relative relationship thereof may be made without substantial technical changes and may be considered as the scope of the present invention.
Example 1
A preparation process of aerogel felt comprises the following steps:
(1) ethyl orthosilicate, methanol, purified water and concentrated hydrochloric acid are mixed according to the proportion of 10: 80: 1.2: 0.025, preheating the sol and a gel catalyst to 30-60 ℃, and then uniformly mixing the sol and the gel catalyst according to a ratio of 20:1 to obtain a mixed solution, wherein the gel catalyst is formed by mixing an alkaline catalyst and an organic solvent, the alkaline catalyst is one or a mixture of more than two of 25-28% concentrated ammonia water, 1-90% ammonium fluoride aqueous solution, a silane coupling agent KH502 and a silane coupling agent KH550, and the organic solvent is one or a mixture of two of refined methanol and 95% ethanol;
(2) uniformly spraying the mixed solution onto the surface of the fibrofelt through a spraying device, and settling and permeating the mixed solution into and filling the pores in the fibrofelt by utilizing the self gravity of the mixed solution to form a wet gel felt, wherein the fibrofelt is 28m long, 1.5m wide and 10mm thick;
(3) conveying the wet gel felt into a microwave cavity 2 at a speed of 2m/min for microwave heating gel and curing, and keeping the temperature inside and outside the gel felt at 55-60 ℃; the microwave cavity is a square cylinder structure which is made of 15mm polypropylene plates and is provided with openings at two ends, the height of the microwave cavity 2 is 100mm, the length of the microwave cavity 2 is 10m, the width of the microwave cavity 2 is 1.52m so as to ensure that a belt can be normally conveyed, a plurality of groups of magnetrons 3 are arranged on the outer sides of the upper end and the lower end of the microwave cavity 2, a protective shell 1 is arranged on the outer side of each magnetron 3, the number of the magnetrons 3 is 84 groups, the rated power of each group of the magnetrons 3 is 1kw, the opening degree of each group is 50%, the output power of the microwave cavity 2 can be adjusted between 0 kw and 1kw according to the actual heating effect, and the uniform speed, the ascending and descending speed operation or the section time pause are determined according to the gel effect of the wet gel felt;
(4) conveying the wet gel felt to a heat preservation section for normal temperature curing, wherein the heat preservation section is arranged at an outlet of the microwave cavity and consists of a heat preservation cover plate arranged above a belt, the heat preservation plate is made of stainless steel plates and clamps rock wool, the thickness of the heat preservation plate is 100mm, the length of the heat preservation section is 10m, the width of the heat preservation section is 1.52m, and the height of the heat preservation section is 200 mm;
(5) and (3) drying the wet gel felt solidified at the normal temperature by using supercritical carbon dioxide to obtain the aerogel felt.
Example 2
A preparation process of aerogel felt comprises the following steps:
(1) ethyl orthosilicate, methanol, purified water and concentrated hydrochloric acid are mixed according to the proportion of 10: 80: 1.2: 0.025, preheating the sol and a gel catalyst to 30-60 ℃, and then uniformly mixing the sol and the gel catalyst according to a ratio of 20:1 to obtain a mixed solution, wherein the gel catalyst is formed by mixing an alkaline catalyst and an organic solvent, the alkaline catalyst is one or a mixture of more than two of 25-28% concentrated ammonia water, 1-90% ammonium fluoride aqueous solution, a silane coupling agent KH502 and a silane coupling agent KH550, and the organic solvent is one or a mixture of two of refined methanol and 95% ethanol;
(2) continuously injecting the mixed solution into a tray, allowing the fibrofelt to pass through the tray along the length direction, and settling and permeating the mixed solution by utilizing the self gravity of the mixed solution to enter and fill the pores in the fibrofelt to form a wet gel felt, wherein the fibrofelt is 28m long, 1.5m wide and 10mm thick;
(3) conveying the wet gel felt into a microwave cavity 2 at a speed of 2m/min for microwave heating gel and curing, and keeping the temperature inside and outside the gel felt at 55-60 ℃; the microwave cavity 2 is a square cylinder structure which is made of 15mm polypropylene plates and is provided with openings at two ends, the height of the microwave cavity 2 is 100mm, the length of the microwave cavity 2 is 10m, the width of the microwave cavity 2 is 1.52m so as to ensure that a belt can be normally conveyed, a plurality of groups of magnetrons 3 are arranged on the outer sides of the upper end and the lower end of the microwave cavity 2, a protective shell 1 is arranged on the outer side of each magnetron 3, the number of the magnetrons 3 is 84 groups, the rated power of each group of the magnetrons 3 is 1kw, the opening degree of each group is 50%, the output power of the microwave cavity can be adjusted between 0 kw and 1kw according to the actual heating effect, and the uniform speed, the ascending and descending speed operation or the section time pause are determined according to the gel effect of the wet gel felt;
(4) conveying the wet gel felt to a heat preservation section for normal temperature curing, wherein the heat preservation section is arranged at an outlet of the microwave cavity and consists of a heat preservation cover plate arranged above a belt, the heat preservation plate is made of stainless steel plates and clamps rock wool, the thickness of the heat preservation plate is 100mm, the length of the heat preservation section is 10m, the width of the heat preservation section is 1.52m, and the height of the heat preservation section is 200 mm;
(5) and (3) drying the wet gel felt solidified at the normal temperature by using supercritical carbon dioxide to obtain the aerogel felt.
Three points are randomly selected from the prepared aerogel felt, the selected three points can reflect the performance of the whole roll of material as much as possible, two materials with the size of 300mm multiplied by 300mm are taken, the measured thermal conductivity coefficient is 0.020W/m.K, and the hydrophobic rate is 99.8%.
The scope of the present invention is not limited to the technical solutions disclosed in the embodiments, and any modifications, equivalent substitutions, improvements, etc. made to the above embodiments according to the technical spirit of the present invention fall within the scope of the present invention.
Claims (9)
1. The preparation process of the aerogel felt is characterized by comprising the following steps of:
(1) mixing the sol and the gel catalyst to obtain a mixed solution;
(2) compounding the mixed solution with a fiber felt to form a wet gel felt;
(3) conveying the wet gel felt into a microwave cavity for microwave heating gel and curing, and keeping the temperature inside and outside the gel felt at 55-60 ℃;
(4) conveying the wet gel felt to a heat preservation section for normal temperature curing;
(5) and (3) drying the wet gel felt solidified at the normal temperature by using supercritical carbon dioxide to obtain the aerogel felt.
2. The process for preparing aerogel felt according to claim 1, wherein the step (1) comprises preheating the sol and the gel catalyst to 30-60 ℃, and then mixing the sol and the gel catalyst in a ratio of 10: (0.1-1) are mixed evenly.
3. The preparation process of aerogel felt according to claim 2, wherein the gel catalyst is prepared by mixing an alkaline catalyst and an organic solvent, the alkaline catalyst is one or a mixture of more than two of 25-28% concentrated ammonia water, 1-90% ammonium fluoride aqueous solution, a silane coupling agent KH502 and a silane coupling agent KH550, and the organic solvent is one or a mixture of two of refined methanol and 95% ethanol.
4. The process for preparing aerogel felt according to claim 1 or 2, wherein the sol is prepared by mixing and hydrolyzing a silicon source precursor, a solvent and a hydrolysis catalyst.
5. The preparation process of aerogel felt according to claim 4, wherein the microwave cavity is a square cylinder structure with two open ends made of 15-25mm polypropylene plates, a plurality of groups of magnetrons are arranged on the outer sides of the upper end and the lower end of the microwave cavity, and a protective shell is arranged on the outer side of each magnetron.
6. The process of claim 5, wherein the number of magnetrons is less than 120 groups, and each group of magnetrons has a nominal power of 1 kw.
7. The process of claim 6, wherein the insulation section is disposed at the outlet of the microwave cavity and is a cover plate.
8. The preparation process of aerogel felt according to claim 7, wherein the mixed solution and the fiber felt are mixed by spraying, i.e., the mixed solution is uniformly sprayed onto the surface of the fiber felt by a spraying device, and the mixed solution is settled and permeated by the self gravity of the mixed solution to fill the pores in the fiber felt, thereby forming the wet gel felt.
9. The preparation process of aerogel felt according to claim 7, wherein the mixed solution and the fiber felt are compounded by dipping, i.e., the mixed solution is poured into a tray, the fiber felt is immersed in the mixed solution, and the mixed solution is settled and permeated by the gravity of the mixed solution to fill the pores in the fiber felt, thereby forming the wet aerogel felt.
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| CN202111095836.0A CN113694844A (en) | 2021-09-18 | 2021-09-18 | Preparation process of aerogel felt |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115230205A (en) * | 2022-07-22 | 2022-10-25 | 广东埃力生高新科技有限公司 | Aerogel panel preparation equipment |
| CN115849771A (en) * | 2023-03-01 | 2023-03-28 | 百能(天津)能源科技有限公司 | Aerogel felt and preparation method and application thereof |
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