CN109853292A - A kind of preparation method of the compound aerosil sheathing paper of ceramic fiber paper - Google Patents
A kind of preparation method of the compound aerosil sheathing paper of ceramic fiber paper Download PDFInfo
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- CN109853292A CN109853292A CN201811554745.7A CN201811554745A CN109853292A CN 109853292 A CN109853292 A CN 109853292A CN 201811554745 A CN201811554745 A CN 201811554745A CN 109853292 A CN109853292 A CN 109853292A
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Abstract
The invention discloses a kind of preparation methods of the compound aerosil sheathing paper of ceramic fiber paper, method includes the following steps: the 1) preparation of aerosil glue；The raw material of the aerosil glue includes silicon source presoma, hydrolyst, additive and solvent；2) molding of ceramic fiber paper aeroge；3) aging of molding ceramic fiber paper aeroge and surface are modified；4) drying and detection for the ceramic fiber paper aeroge that aging and surface are modified.The compound aerosil sheathing paper of ceramic fiber paper prepared by the present invention has excellent heat-proof quality, mechanical performance, fire prevention and waterproof performance, easy for construction；The preparation method avoids solvent replacement step, and operation is simple, and process control, production can serialization.
Description
Technical field
The present invention relates to a kind of preparation methods of the compound aerosil sheathing paper of ceramic fiber paper, belong to chemical industry
Field of material technology.
Background technique
Aerosil is a kind of light nanoporous amorphous solid-state material of structure-controllable, and porosity is up to
80%~99.8%, bore hole size is 1~100nm, high-specific surface area 200-1000 m2/ g, 3~500kg/ of low-density variation range
m3, it is current that thermal conductivity is also lower than the thermal conductivity of still air (0.026 W/m K) less than 0.013 W/m K under normal temperature and pressure
The minimum solid material of thermal conductivity.
Preparation process complexity, the long preparation period, solvent that current aerosil heat-barrier material industrialization faces
The technical problems such as consumption is big, waste liquid is more, aeroge intensity is low, brittleness is big.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation sides of the compound aerosil sheathing paper of ceramic fiber paper
Method, by the ceramic fiber paper of saturated absorption aerosil glue in specified conditions gel, supercritical fluid CO2It is dry,
The enhanced aerogel heat-insulating material of excellent, high mechanical strength, fire prevention and waterproof performance is formed with heat-proof quality, and the present invention mentions
The preparation method of confession avoids solvent replacement step, and operation is simple, and production can serialization.
The technical scheme of the present invention is realized as follows:
A kind of preparation method of the compound aerosil sheathing paper of ceramic fiber paper of the invention: the following steps are included:
1) preparation of aerosil glue；The raw material of the aerosil glue includes silicon source presoma, water
Solve catalyst, additive and solvent；
2) molding of ceramic fiber paper aeroge；
3) aging of molding ceramic fiber paper aeroge and surface are modified；
4) drying and detection for the ceramic fiber paper aeroge that aging and surface are modified.
In preceding method, the silicon source presoma includes ethyl orthosilicate, methyl orthosilicate, one in trim,ethylchlorosilane
Kind or two or more mixtures.
In preceding method, the hydrolyst includes pure water, hydrochloric acid, nitric acid, sulfuric acid, oxalic acid, acetic acid, ammonium hydroxide, carbonic acid
The mixture of one or more of ammonium, ammonium hydrogen carbonate.
In preceding method, the ceramic fiber paper paper includes the ceramic fiber paper that ceramic fiber paper etc. is 2-5 μm with diameter
Made of material, homogeneous paper of the thickness in 0.2 ~ 2mm.
In preceding method, the solvent includes methanol, ethyl alcohol, butanol etc., and one in the straight chain alcohol of 95% or more mass fraction
Kind or two or more mixtures.
In preceding method, the preparation of the aerosil glue includes the component of following volume ratio: positive silicic acid second
Ester: 95% dehydrated alcohol: water catalyst=10:(40~100): (1~5).
In preceding method, the ceramic fiber paper airsetting gum forming is by aerosil glue spray ceramic fine
It ties up on paper, makes fine ceramic fiber paper saturation absorption glue of making pottery, ceramic fiber paper paper without being bubbled, being recessed, uniformly put down by upper and lower surface
It is whole, it is re-fed into 15~25min of standing in 55~60 DEG C of environment, forms ceramic fiber paper aeroge alcogel.
In preceding method, the aging is that ceramic fiber paper aeroge alcogel is put into 35~45 DEG C of leachings in ethanol solution
Bubble is for 24 hours.
In preceding method, the surface modification is that the ceramic fiber paper aeroge alcogel of aging is put into added with alkylation
The ethyl alcohol of reagent (for the mixture of one or more of additive, dosage is 1~2% times of material alcogel volume) is molten
50~60 DEG C of immersion 12h in liquid.
In preceding method, the drying is that the modified ceramic fiber paper aerogel material of aging or surface is put into extraction kettle
In, by CO2Fluid injects extraction kettle, and temperature and pressure is in CO in adjusting extraction kettle2The supercriticality and material of fluid,
It is dissolved in the solvent in material among supercritical fluid, is exported from the extraction of extraction kettle and collect fluid.
In preceding method, the supercritical temperature is 45~55 DEG C, and pressure is 10~18MPa；CO2 fluid passes through extraction kettle
Flow be 300~500kg/h, extraction time be 5~8h.
In preceding method, the detecting step is will to extract material out under optimum process condition to randomly select at 3 points (3 points are answered
Can reflect the performance of bulk roll of material as far as possible), it takes 300 × 300mm material to be superimposed total 10mm, measures density, thermal coefficient, hydrophobic
Property, mechanical strength.
By adopting the above-described technical solution, compared with prior art, the present invention the invention has the characteristics that: faced with super
CO under boundary's state2Fluid is recycled in the same system as dried medium, the solvent, and solvent consumption is few, and price is cheap,
Therefore extract it is at low cost, the features such as non-environmental-pollution.Short preparation period, only 3d, so that it may it is fine to prepare a roll of complete ceramics
Tie up the compound aerogel heat-insulating material of paper.Ceramic fiber paper paper is used as aeroge enhancing base materials, can reduce ceramic fibre well
The heating conduction of paper paper improves aeroge crispness, the compound aerogel heat-proof material of the ceramic fiber paper that the present invention produces
The thermal coefficient of material at normal temperature is 0.015~0.022W/mK.Present invention process is simple, and continuous production is strong.
Specific embodiment
Technical solution of the present invention is described in further detail below with reference to embodiment.
The preparation method of the compound aerosil sheathing paper of a kind of ceramic fiber paper of the invention: including following step
It is rapid:
1) preparation of aerosil glue, the raw material of the aerosil glue include silicon source presoma, water
Solve catalyst, additive and solvent；The silicon source presoma includes ethyl orthosilicate, methyl orthosilicate, in trim,ethylchlorosilane
One or more kinds of mixtures；The hydrolyst includes pure water, hydrochloric acid, nitric acid, sulfuric acid, oxalic acid, acetic acid, ammonia
The mixture of one or more of water, ammonium carbonate, ammonium hydrogen carbonate；The solvent includes methanol, ethyl alcohol, butanol etc., matter
Measure the mixture of one or more of straight chain alcohol of 95% or more score；The preparation of the aerosil glue
Component including following volume ratio: ethyl orthosilicate: 95% dehydrated alcohol: water catalyst=10:(40~100): (1~5)；
2) molding of ceramic fiber paper aeroge, the ceramic fiber paper paper include ceramic fiber paper etc. with diameter for 2-5 μm
Made of ceramic fiber paper material, homogeneous paper of the thickness in 0.2 ~ 2mm；The ceramic fiber paper airsetting gum forming be by
Aerosil glue sprays on ceramic fiber paper, makes fine ceramic fiber paper saturation absorption glue of making pottery, ceramic fiber paper
Without being bubbled, being recessed, the equal uniform ground of upper and lower surface is re-fed into 15~25min of standing in 55~60 DEG C of environment, it is fine to form ceramics paper
Tie up paper aeroge alcogel；
3) aging of molding ceramic fiber paper aeroge and surface are modified, and the aging is to coagulate ceramic fiber paper aeroge alcohol
Glue, which is put into ethanol solution, to be impregnated for 24 hours for 35~45 DEG C；The surface modification is by the ceramic fiber paper aeroge alcogel of aging
It is put into that (for the mixture of one or more of additive, dosage is 1~2% times of material alcogel added with alkylating reagent
Volume) ethanol solution in 50~60 DEG C of immersion 12h；
4) drying and detection for the ceramic fiber paper aeroge that aging and surface are modified, the drying are that aging or surface is modified
Ceramic fiber paper aerogel material be put into extraction kettle, by CO2Fluid injects extraction kettle, adjusts temperature and pressure in extraction kettle
In CO2The supercriticality and material of fluid, are dissolved in the solvent in material among supercritical fluid, from extraction kettle
Collect fluid in extraction outlet；The supercritical temperature is 45~55 DEG C, and pressure is 10~18MPa；CO2 fluid passes through extraction kettle
Flow is 300~500kg/h, and extraction time is 5~8h；The detecting step is that will to extract material out under optimum process condition random
Choose the performance of bulk roll of material (can should reflect as far as possible) at 3 points at 3 points, 300 × 300mm material taken to be superimposed total 10mm, measure density,
Thermal coefficient, hydrophobicity, mechanical strength.
Embodiment 1:
Ethyl orthosilicate, 99% industrial methanol, hydrolyst, additive are uniformly mixed according to the volume ratio of 16 ︰, 128 ︰, 5 ︰ 1
5h is reacted, colloidal sol is obtained；Be 21300mm by length, width 1500mm, with a thickness of 10mm, bulk density is 120 ~ 135kg/m
3 fiberglass needled mat and colloidal sol is mixed with dipping, and obtains colloidal sol glass mat precursor.By colloidal sol glass mat precursor in
40h is impregnated in 50 ~ 55 DEG C of ethanol solutions and makees ripening, is added alkylating reagent and is surface-treated, obtains colloidal sol fiber
Felt.Colloidal sol glass mat is subjected to supercritical CO2It is dried, drying temperature is 53 DEG C, drying pressure 14.5MPa, CO2
Gas flow is 2600kg/h, and drying time 5.5h obtains hydrophobic nano aerogel insulating material.By hydrophobic nano gas
Gel heat-insulating material carries out shape extrusion according to length × width x thickness=1500mm × 600mm × 10mm specification, obtains scale cun and dredges
Water type nanoporous aerogel heat-insulating material.Flameproof fabric and hot melt adhesive are all wrapped into scale cun hydrophobic nano aerogel heat-insulating material
The two sides of material obtains the anti-picking hydrophobic nano aerogel heat-proof piece of surfacing after laminator is suppressed.
Embodiment 2:
Ethyl orthosilicate, 99% industrial methanol, hydrolyst, additive are uniformly mixed according to the volume ratio of 16 ︰, 112 ︰, 5 ︰ 1
5h is reacted, colloidal sol is obtained；Be 61300mm by length, width 1500mm, with a thickness of 3mm, bulk density is 90 ~ 115kg/m3
Fiberglass needled mat and colloidal sol be mixed with dipping, obtain colloidal sol glass mat precursor.By colloidal sol glass mat precursor in
40h is impregnated in 50 ~ 55 DEG C of ethanol solutions and makees ripening, is added alkylating reagent progress surface and is modified, obtains colloidal sol fiber
Felt.Colloidal sol glass mat is subjected to supercritical CO2It is dried, drying temperature is 55 DEG C, drying pressure 14MPa, CO2Gas
Body flow is 2500kg/h, and drying time 3h obtains hydrophobic nano aerogel insulating material.By hydrophobic nano aeroge
Heat-insulating material carries out shape extrusion according to length × width x thickness=1500mm × 1200mm × 3mm specification, obtains scale cun hydrophobic type
Nanoporous aerogel heat-insulating material.Flameproof fabric and hot melt adhesive are all wrapped into scale cun hydrophobic nano aerogel insulating material
Two sides obtains the anti-picking hydrophobic nano aerogel heat-proof piece of surfacing after laminator is suppressed.
Certainly, above is specific application example of the invention, and there are other embodiments of the invention, all using equivalent
The technical solution that replacement or equivalent transformation are formed, all falls within protection scope of the presently claimed invention.
Claims (9)
1. a kind of preparation method of the compound aerosil sheathing paper of ceramic fiber paper, it is characterised in that: this method packet
Include following steps:
1) preparation of aerosil glue；The raw material of the aerosil glue includes silicon source presoma, water
Solve catalyst, additive and solvent；
2) molding of ceramic fiber paper aeroge；
3) aging of molding ceramic fiber paper aeroge and surface are modified；
4) drying and detection for the ceramic fiber paper aeroge that aging and surface are modified.
2. the preparation method of the compound aerosil sheathing paper of ceramic fiber paper according to claim 1, special
Sign is: the silicon source presoma includes one or more of ethyl orthosilicate, methyl orthosilicate, trim,ethylchlorosilane
Mixture；The hydrolyst includes pure water, hydrochloric acid, nitric acid, sulfuric acid, oxalic acid, acetic acid, ammonium hydroxide, ammonium carbonate, in ammonium hydrogen carbonate
A combination of one or more；The solvent includes in the straight chain alcohol of methanol, ethyl alcohol, butanol, 95% or more mass fraction
A combination of one or more.
3. the preparation method of the compound aerosil sheathing paper of ceramic fiber paper according to claim 2, special
Sign is: the aerosil glue is formulated by the component of following volume ratio: ethyl orthosilicate: 95% anhydrous second
Alcohol: water catalyst=10:40~200:1~5.
4. the preparation method of the compound aerosil sheathing paper of ceramic fiber paper according to claim 1, special
Sign is: the molding of the ceramic fiber paper aeroge is to spray aerosil glue on ceramic fiber paper paper,
Make ceramic fiber paper paper saturation absorption glue, stands 15~25min, form the alcogel of ceramic fiber paper aeroge.
5. the preparation method of the compound aerosil sheathing paper of ceramic fiber paper according to claim 4, special
Sign is: it is made of 2-5 μm of ceramic fiber paper material that the ceramic fiber paper, which is with diameter, and thickness is between 0.2-2mm
Paper, homogeneous paper.
6. the preparation method of the compound aerosil sheathing paper of ceramic fiber paper according to claim 1, special
Sign is: the aging is to be put into the alcogel of ceramic fiber paper in ethanol solution to impregnate for 24 hours for 35~45 DEG C；The table
Face modification is that the alcogel of the ceramic fiber paper aeroge of aging is put into the ethanol solution added with alkylating reagent 50
~60 DEG C of immersion 12h.
7. the preparation method of the compound aerosil sheathing paper of ceramic fiber paper according to claim 1, special
Sign is: the drying is that the modified ceramic fiber paper aerogel material of aging and surface is put into extraction kettle, by CO2Stream
Body injects extraction kettle, and temperature and pressure is in CO in adjusting extraction kettle2With material under the supercriticality of fluid, make in material
Solvent be dissolved among supercritical fluid, from separating still discharge gate collect solvent, it is compound to prepare hydrophilic ceramic fiber paper
Type aerosil sheathing paper.
8. the preparation method of the compound aerosil sheathing paper of ceramic fiber paper according to claim 7, special
Sign is: the CO2Fluid controlled at 45~55 DEG C, pressure is 10~18MPa；CO2The flow that fluid passes through extraction kettle
For 300~500kg/h, extraction time is 5~8h.
9. the preparation method of the compound aerosil sheathing paper of ceramic fiber paper according to claim 1, special
Sign is: the detecting step is will to extract material out to randomly select at 3 points, and 300 × 300mm material is taken to be superimposed total 10mm, is measured close
Degree, thermal coefficient, hydrophobicity and/or mechanical strength.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111074672A (en) * | 2019-12-27 | 2020-04-28 | 贵州航天乌江机电设备有限责任公司 | Preparation process of glass fiber aerogel composite paper for low temperature |
| CN113443890A (en) * | 2021-07-29 | 2021-09-28 | 贵州航天乌江机电设备有限责任公司 | Aerogel heat insulation sleeve for battery and preparation method thereof |
| CN114075799A (en) * | 2021-07-16 | 2022-02-22 | 摩根热陶瓷上海有限公司 | Heat-resistant compressed paper, preparation method thereof and battery module |
| CN116393052A (en) * | 2023-03-31 | 2023-07-07 | 广东埃力生科技股份有限公司 | Aerogel product, and preparation method and preparation system thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111074672A (en) * | 2019-12-27 | 2020-04-28 | 贵州航天乌江机电设备有限责任公司 | Preparation process of glass fiber aerogel composite paper for low temperature |
| CN114075799A (en) * | 2021-07-16 | 2022-02-22 | 摩根热陶瓷上海有限公司 | Heat-resistant compressed paper, preparation method thereof and battery module |
| CN113443890A (en) * | 2021-07-29 | 2021-09-28 | 贵州航天乌江机电设备有限责任公司 | Aerogel heat insulation sleeve for battery and preparation method thereof |
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| CN116393052B (en) * | 2023-03-31 | 2023-12-26 | 广东埃力生科技股份有限公司 | Aerogel product, and preparation method and preparation system thereof |
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Application publication date: 20190607 |