CN111074672A - Preparation process of glass fiber aerogel composite paper for low temperature - Google Patents
Preparation process of glass fiber aerogel composite paper for low temperature Download PDFInfo
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- CN111074672A CN111074672A CN201911376913.2A CN201911376913A CN111074672A CN 111074672 A CN111074672 A CN 111074672A CN 201911376913 A CN201911376913 A CN 201911376913A CN 111074672 A CN111074672 A CN 111074672A
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- glass fiber
- paper
- aerogel composite
- preparation process
- low temperature
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Classifications
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/68—Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/36—Inorganic fibres or flakes
- D21H13/38—Inorganic fibres or flakes siliceous
- D21H13/40—Inorganic fibres or flakes siliceous vitreous, e.g. mineral wool, glass fibres
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H23/00—Processes or apparatus for adding material to the pulp or to the paper
- D21H23/02—Processes or apparatus for adding material to the pulp or to the paper characterised by the manner in which substances are added
- D21H23/22—Addition to the formed paper
- D21H23/50—Spraying or projecting
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
Abstract
The invention discloses a preparation process of glass fiber aerogel composite paper for low temperature, which mainly utilizes glass fiber felt paper to saturate and absorb silica sol, gels, ages and modifies the surface under specific conditions, and supercritical fluid CO is used2And drying to prepare the glass fiber aerogel composite heat insulation paper. The low-temperature glass fiber aerogel composite heat insulation paper prepared by the invention has excellent heat insulation performance, mechanical performance, fireproof performance and waterproof performance, and is convenient to construct. The preparation method avoids the step of solvent replacement, has simple and easy operation and controllable process, and can realize continuous production.
Description
Technical Field
The invention belongs to the technical field of chemical materials, and particularly relates to a preparation process of glass fiber aerogel composite heat insulation paper for low temperature.
Background
SiO2The aerogel is a light nano porous amorphous solid material with a controllable structure, the porosity of the aerogel is 80-99.8%, the pore size is 1-100 nm, and the high specific surface area is 200-2(g), the low density range of variation is 3 to 500kg/m3Thermal conductivity less than 0.01 at normal temperature and normal pressure3W/mK, which is lower than the thermal conductivity of static air (0.026W/mK), is the solid material with the lowest thermal conductivity at present.
Currently, the main problems facing the industrialization of silica aerogels include: the preparation process is complex, the preparation period is long, the solvent consumption is large, the waste liquid is much, the strength of the aerogel is low, the brittleness is large and the like, and the application of the silicon dioxide aerogel is limited. The fiber reinforced aerogel can effectively solve the problem and has great practical significance for realizing industrialization.
Currently, companies and research institutes engaged in the research and commercialization of aerogels abroad are mainly focused on the european and american regions and japan; in China, 4-6 enterprises enter SiO in succession since 20122Aerogel thermal insulation industry. The traditional heat-insulating materials commonly used for the existing industrial pipelines comprise rock wool, common glass wool felt, high-alumina silicate cotton, polyurethane and the like, and the rock wool and the high-alumina silicate cotton have the defects of poor heat-insulating property, easy moisture absorption and large installation thickness; the common glass wool felt is not high temperature resistant; polyurethane is not high temperature resistant and flammable. The material with excellent heat preservation performance and hydrophobic and fireproof performance can be accepted by the market and popularized and applied. Therefore, if SiO can be converted into2The aerogel is applied to the heat preservation felt in the industry and is very significant.
Disclosure of Invention
The invention aims to provide a preparation process of glass fiber aerogel composite heat insulation paper for low temperature, and aims to solve the technical problems of complex preparation process, long preparation period, large solvent consumption, more waste liquid, low aerogel strength, high brittleness and the like in the industrialization of silicon dioxide aerogel heat insulation materials.
The method of the invention is to gel and supercritical fluid CO on the glass fiber paper of the saturated absorption silica aerogel glue solution under specific conditions2Drying to form the enhanced aerogel thermal insulation material with excellent thermal insulation performance, high mechanical strength, fire resistance and water resistance. The preparation method avoids the step of solvent replacement, has simple and easy operation and can realize continuous production.
The technical scheme of the invention is as follows:
preparation of glass fiber aerogel composite heat insulation paper for low temperatureThe preparation process includes one-step silica sol preparation, soaking glass fiber paper to absorb silica sol in vacuum condition, gelling and ageing in specific condition, surface modification with alkylating reagent, and supercritical fluid CO2And drying to prepare the glass fiber aerogel composite heat insulation paper. The method comprises the following steps:
1) preparing silica sol;
2) homogenizing and compounding the sol and the glass fiber paper to prepare wet gel;
3) aging and hydrophobic modification of wet gel;
4) drying the wet gel to prepare glass fiber aerogel composite heat insulation paper;
5) and (5) post-treating the glass fiber aerogel composite heat insulation paper.
In the foregoing method, the raw materials of the silica sol include a silicon source precursor, purified water, a catalyst, and a solvent.
In the foregoing method, the silicon source precursor includes one or a mixture of two or more of tetraethoxysilane, methyl orthosilicate, and trimethylchlorosilane.
In the method, the purified water is deionized water
The catalyst in the method comprises one or a mixture of more than two of ammonia water, ammonium carbonate, ammonium bicarbonate and ammonium fluoride.
In the method, the glass fiber paper is made of glass fiber materials with the diameter of nanometer, the density is not more than 200kg/m3, and the texture is uniform.
In the method, the solvent comprises methanol, ethanol, butanol and the like, and the mass fraction of the solvent is more than 96% of one or more than two of linear alcohols.
In the method, the silica sol is prepared from the following components in molar ratio: ethyl orthosilicate, 99% industrial alcohol, purified water, catalyst 1, (14.81-98.88), (2.22-5.55) and (0.04-0.24).
In the method, the step of preparing the wet gel by uniformly compounding the sol and the glass fiber paper refers to uniformly spraying the silica sol on the glass fiber paper in a vacuum environment to enable the glass fiber paper to adsorb the glue solution in a saturated manner, and standing for 50-70 min to form the wet gel.
In the method, the aging is to put the wet gel into an ethanol solution to be soaked for 24 hours at the temperature of 40-45 ℃.
In the method, the surface modification is to soak the aged wet gel in an ethanol solution added with an alkylating agent (one or a mixture of more than two of additives, the dosage is 1-1.3% of the volume of the material wet material) at 50-60 ℃ for 12 h.
In the method, the drying is to put the surface modified wet gel into a drying kettle, inject carbon dioxide gas into the drying kettle, keep the temperature and pressure in the drying kettle in the supercritical state of the carbon dioxide gas to contact with the material, dissolve the solvent in the material into the supercritical fluid, and collect the fluid from the extraction outlet of the extraction kettle.
In the method, the supercritical temperature is 45-55 ℃, and the pressure is 10-18 MPa; the flow of the carbon dioxide gas passing through the extraction kettle is 200-250 kg/h, and the extraction time is 8-12 h.
In the method, the post-treatment of the glass fiber aerogel composite heat insulation paper also comprises a detection step, wherein three points of the extracted materials are randomly selected under the optimal process conditions, two pieces of 300 x 300mm materials are taken, and the density, the heat conductivity coefficient, the hydrophobicity and the mechanical strength are measured.
Compared with the prior art, the invention has the following characteristics: the carbon dioxide fluid in a supercritical state is used as a drying medium, the solvent is recycled in the same system, the solvent consumption is low, and the selling price is low, so the extraction cost is low, no environmental pollution is caused, and the like. The preparation period is short, only 3 days, a roll of complete glass fiber composite aerogel thermal insulation material can be prepared, and the prior art needs 6-7 days. The glass fiber mat is used as the aerogel reinforcing base material, the heat conducting performance of glass fibers can be well reduced, the brittleness of the aerogel is improved, and the heat conducting coefficient of the glass fiber composite aerogel heat-insulating material produced by the invention is 0.015-0.018W/mK at normal temperature. The invention has simple process and strong production continuity.
Detailed Description
The present invention will be described in further detail with reference to examples.
The preparation process of the glass fiber aerogel composite heat insulation paper for low temperature comprises the following steps: silica sol preparation → homogeneous compounding of the sol and the glass fiber paper to prepare wet gel → wet gel aging and modification → drying → detection. Preparing the following silica sol in molar ratio: ethyl orthosilicate, 99% industrial alcohol, water: catalyst 1:15:2.8: 0.1. The water is deionized water, the catalyst is ammonium fluoride solution with the mass fraction of 4%, and the gel reaction time is 2 h. Spraying the sol on a substrate with a thickness of 0.5mm and a density of 160kg/m3The glass fiber paper is coated with the gel solution, so that the glass fiber paper can adsorb the gel solution in a saturated way, no bubbling or sinking exists, the upper surface and the lower surface are uniform and smooth, and the gel is prepared into wet gel. And (3) soaking the glass fiber aerogel wet material in an ethanol solution at the temperature of 40 ℃ for 24h for aging. Putting the aged wet gel into a drying kettle, injecting carbon dioxide gas into the drying kettle, and keeping the temperature and pressure in the drying kettle to be in contact with the material in a supercritical state of the carbon dioxide gas, so that the solvent in the material is dissolved in the supercritical fluid, wherein the supercritical temperature is 45 ℃ and the pressure is 14 MPa; the flow rate of the carbon dioxide gas passing through the extraction kettle is 2000kg/h, fluid is collected from an extraction outlet of the extraction kettle until no solution is discharged, and the machine is stopped to take out materials.
Three points (three points should reflect the performance of the whole roll of material as much as possible) are randomly selected for the extracted material, two pieces of material with the size of 300mm by 300mm are taken, and the density, the thermal conductivity coefficient, the hydrophobicity and the mechanical strength are measured. And (3) measuring related data: the material has the thickness of 0.52mm, the density of 220kg/m3, the normal-temperature heat conductivity coefficient of 0.017W/mK, the hydrophobicity of 99.4 percent and the combustion grade of S4.
Of course, the above is only a specific application example of the present invention, and other embodiments of the present invention are also within the scope of the present invention.
Claims (9)
1. A preparation process of glass fiber aerogel composite paper for low temperature is characterized by comprising the following steps: the method comprises the steps of preparing silica sol by adopting a one-step method, enabling glass fiber paper to absorb the silica sol in a saturated way by adopting an impregnation method under the vacuum condition, gelling and aging under the specific condition, modifying the surface by an alkylating agent, and using supercritical fluid CO2And drying to prepare the glass fiber aerogel composite heat insulation paper.
2. The preparation process of the glass fiber aerogel composite paper for low temperature according to claim 1, which is characterized in that: the process comprises the following steps of,
1) preparing silica sol;
2) homogenizing and compounding the sol and the glass fiber paper to prepare wet gel;
3) aging and hydrophobic modification of wet gel;
4) drying the wet gel to prepare glass fiber aerogel composite heat insulation paper;
5) and (5) post-treating the glass fiber aerogel composite heat insulation paper.
3. The preparation process of the glass fiber aerogel composite paper for low temperature according to claim 2, characterized in that: the raw materials of the silica sol comprise a silicon source precursor, purified water, a catalyst and a solvent; the silicon source precursor comprises one or a mixture of more than two of tetraethoxysilane, methyl orthosilicate and trimethylchlorosilane; the purified water is deionized water; the catalyst comprises one or the combination of more than two of ammonia water, ammonium carbonate, ammonium bicarbonate and ammonium fluoride; 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%.
4. The preparation process of the glass fiber aerogel composite paper for low temperature according to claim 2 or 3, characterized in that: the silica sol is prepared from the following components in molar ratio: ethyl orthosilicate, 99% industrial alcohol, purified water, catalyst 1, (14.81-98.88), (2.22-5.55) and (0.04-0.24).
5. The preparation process of the glass fiber aerogel composite paper for low temperature according to claim 2, characterized in that: the wet gel is prepared by uniformly compounding the sol and the glass fiber paper, namely, the silica sol is uniformly sprayed on the glass fiber paper in a vacuum environment, so that the glass fiber paper is saturated and adsorbs glue solution, and the wet gel is formed after standing for 50-70 min.
6. The preparation process of the glass fiber aerogel composite paper for low temperature according to claim 5, characterized in that: the glass fiber paper is made of glass fiber materials with the diameter of nanometer, the density is not more than 200kg/m3, and the paper is uniform in texture.
7. The preparation process of the glass fiber aerogel composite paper for low temperature according to claim 2, characterized in that: the aging is to put the wet gel into an ethanol solution to be soaked for 24 hours at the temperature of 35-45 ℃; the surface modification is to put the aged wet gel into an ethanol solution added with an alkylating reagent to be soaked for 12 hours at 50-60 ℃.
8. The preparation process of the glass fiber aerogel composite paper for low temperature according to claim 2, characterized in that: and the drying is to place the wet gel with the modified surface into a supercritical carbon dioxide drying system for drying, inject carbon dioxide gas into an extraction kettle, keep the temperature and pressure in the extraction kettle in a supercritical state of the carbon dioxide gas to be contacted with the material, dissolve the solvent in the material into the supercritical fluid, and collect the fluid from an extraction outlet of the extraction kettle.
9. The preparation process of the glass fiber aerogel composite paper for low temperature according to claim 8, which is characterized in that: the supercritical temperature of the carbon dioxide gas is 45-55 ℃, and the pressure is 10-18 MPa; the flow of the carbon dioxide gas passing through the drying kettle is 2000-2500 kg/h, and the extraction time is 8-12 h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911376913.2A CN111074672A (en) | 2019-12-27 | 2019-12-27 | Preparation process of glass fiber aerogel composite paper for low temperature |
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| CN201911376913.2A CN111074672A (en) | 2019-12-27 | 2019-12-27 | Preparation process of glass fiber aerogel composite paper for low temperature |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115852739A (en) * | 2022-11-29 | 2023-03-28 | 南京聚力纤维材料有限公司 | Ultrathin glass fiber paper composite aerogel and preparation method thereof |
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| CN104496402A (en) * | 2014-12-18 | 2015-04-08 | 贵州航天乌江机电设备有限责任公司 | Process for preparing glass fiber composite type silicon dioxide aerogel insulation quilt |
| CN106587908A (en) * | 2016-12-26 | 2017-04-26 | 贵州航天乌江机电设备有限责任公司 | Preparation process of high-temperature-resistant hydrophobic silicon dioxide aerogel heat-isolating blanket |
| CN109853292A (en) * | 2018-12-18 | 2019-06-07 | 贵州航天乌江机电设备有限责任公司 | A kind of preparation method of the compound aerosil sheathing paper of ceramic fiber paper |
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2019
- 2019-12-27 CN CN201911376913.2A patent/CN111074672A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104496402A (en) * | 2014-12-18 | 2015-04-08 | 贵州航天乌江机电设备有限责任公司 | Process for preparing glass fiber composite type silicon dioxide aerogel insulation quilt |
| CN106587908A (en) * | 2016-12-26 | 2017-04-26 | 贵州航天乌江机电设备有限责任公司 | Preparation process of high-temperature-resistant hydrophobic silicon dioxide aerogel heat-isolating blanket |
| CN109853292A (en) * | 2018-12-18 | 2019-06-07 | 贵州航天乌江机电设备有限责任公司 | A kind of preparation method of the compound aerosil sheathing paper of ceramic fiber paper |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115852739A (en) * | 2022-11-29 | 2023-03-28 | 南京聚力纤维材料有限公司 | Ultrathin glass fiber paper composite aerogel and preparation method thereof |
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Application publication date: 20200428 |
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