CN109680485A - The compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber - Google Patents
The compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber Download PDFInfo
- Publication number
- CN109680485A CN109680485A CN201811554746.1A CN201811554746A CN109680485A CN 109680485 A CN109680485 A CN 109680485A CN 201811554746 A CN201811554746 A CN 201811554746A CN 109680485 A CN109680485 A CN 109680485A
- Authority
- CN
- China
- Prior art keywords
- oxidization fiber
- fibrofelt
- hydrophobic silica
- silica aerogel
- insulation quilt
- 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.)
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Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/05—Cellulose or derivatives thereof
- D06M15/09—Cellulose ethers
Abstract
The invention discloses a kind of compound preparation methods from hydrophobic silica aerogel insulation quilt of oxidization fiber, method includes the following steps: 1) from the preparation of hydrophobic silica aerogel glue；The raw material from hydrophobic silica aerogel glue has silicon source presoma, hydrolyst, additive and solvent；2) molding of oxidization fiber fibrofelt aeroge；3) ageing of oxidization fiber fibrofelt aeroge after molding；4) drying and detection of the oxidization fiber fibrofelt aeroge after being aged.The compound aerosil insulation quilt of oxidization fiber prepared by the present invention has excellent thermal insulation property, mechanical performance, fire prevention and waterproof performance, easy for construction.Preparation method avoids solvent replacement step, and operation is simple, and process control can be mass.
Description
Technical field
The present invention relates to a kind of compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber, belonging to
Work field of material technology.
Background technique
SiO2Aeroge 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/m of low-density variation range3,
Thermal conductivity 0.016W/mK under normal temperature and pressure, it is also lower than the thermal conductivity of still air (0.026 W/mK), it is that current thermal conductivity is minimum
Solid material.
Currently, the main problem that aerosil industrialization faces include: preparation process complexity, long preparation period,
The disadvantages of solvent-oil ratio is big, waste liquid is more, aeroge intensity is low, brittleness is big, limits the application of aerosil.Fiber
Enhanced aeroge can realize that its industrialization is of great immediate significance with this problem of effective solution.
Currently, the external research for being engaged in aeroge and commercialized company and research institution be concentrated mainly on European and American areas and
Japan；At home, 4~6 enterprises enter SiO in succession since 20122Aerogel heat-insulating keeps the temperature industry.And existing industry pipe
The common Conventional insulation in road has rock wool, common oxidization fiber blanket, high aluminium silicate wool, polyurethane etc..Rock wool, high aluminium silicate wool
The big disadvantage of poor thermal insulation property, the easy moisture absorption, installation thickness；Common oxidization fiber fibrofelt non-refractory；Polyurethane non-refractory, easily
Combustion.And then a kind of excellent thermal insulation performance, hydrophobic fireproof material can obtain the approval in market and be promoted and applied.Therefore, such as
Fruit can be by SiO2Aeroge is applied on the insulation quilt in industry, is very significant.
Summary of the invention
The purpose of the present invention is to provide a kind of compound preparations from hydrophobic silica aerogel insulation quilt of oxidization fiber
Technique, to solve preparation process complexity, the long preparation period, solvent consumption that aerosil thermal insulation material industrialization faces
The technical problems such as amount is big, waste liquid is more, aeroge intensity is low, brittleness is big.
The technical scheme of the present invention is realized as follows:
A kind of compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber of the invention, this method include with
Lower step:
1) from the preparation of hydrophobic silica aerogel glue；The raw material from hydrophobic silica aerogel glue has silicon source
Presoma, hydrolyst, additive and solvent；
2) molding of oxidization fiber fibrofelt aeroge；
3) ageing of oxidization fiber fibrofelt aeroge after molding；
4) drying and detection of the oxidization fiber fibrofelt aeroge after being aged.
In preceding method, the silicon source presoma includes ethyl orthosilicate, methyl orthosilicate, trim,ethylchlorosilane, methyl
The mixture of one or more of trimethoxy silane.
In preceding method, the hydrolyst includes pure water, hydrochloric acid, nitric acid, sulfuric acid, acetic acid, ammonium hydroxide, ammonium carbonate, carbon
The mixture of one or more of sour hydrogen ammonium.
In preceding method, the oxidization fiber fibrofelt includes oxidization fiber Nomex, oxidization fiber centrifugal cotton, oxidization fiber force fit plate
Deng using diameter as made of nanoscale oxidization fiber Fiber Materials, density is not more than 250kg/m3, homogeneous plate or felt.
In preceding method, the additive includes ethyl cellulose, n,N-Dimethylformamide, N, N- dimethylacetamide
The mixture of one or more of amine, formamide, acetamide and alkylating reagent.
In preceding method, the solvent includes methanol, ethyl alcohol, butanol etc., and one in the straight chain alcohol of 96% 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: methyltrimethoxysilane: 99% industrial alcohol: water catalyst: additive=10:3:(50~150): (3~6): (0.3~
1.1)。
In preceding method, the oxidization fiber fibrofelt is from hydrophobic aerogel molding will be from hydrophobic silica aerogel glue
Liquid spray on oxidization fiber fibrofelt, make oxidization fiber fibrofelt saturation absorption glue, oxidization fiber fibrofelt without be bubbled, recess, on
Lower surface uniform ground is re-fed into 30~35 DEG C, while pH value is formed pre- to stand 20~25min in 8~9 alkaline environment
Oxygen silk fiber felt wet gel material.
In preceding method, the ageing is that oxidization fiber fibrofelt wet gel material is put into 35~45 DEG C of leachings in ethanol solution
Steep 30h.
In preceding method, the drying is the material barrel that the oxidization fiber fibrofelt wet gel material of ageing is put into extraction kettle
In, carbon dioxide gas is injected into extraction kettle, keeps temperature and pressure in extraction kettle in the supercriticality of carbon dioxide gas,
And and material, 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 40~50 DEG C, and pressure is 10~18MPa；Carbon dioxide gas passes through
The flow of extraction kettle is 200~250kg/h, extraction time 10h.
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), every takes two pieces of 300 × 300mm material, measurement density, thermal coefficient, hydrophobicity,
Mechanical strength.
By adopting the above-described technical solution, compared with prior art, the present invention using after supercritical extraction technique, greatly
Amplitude improves production efficiency, and simultaneously for recycling for extractant, the application of situ aggregation method all be further reduced
Cost；Simple process, continuous production are strong.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
A kind of compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber of the invention, this method packet
Include following steps:
1) from the preparation of hydrophobic silica aerogel glue；The raw material from hydrophobic silica aerogel glue has silicon source
Presoma, hydrolyst, additive and solvent；The silicon source presoma includes ethyl orthosilicate, methyl orthosilicate, trimethyl
The mixture of one or more of chlorosilane, methyltrimethoxysilane；The hydrolyst includes pure water, salt
Acid, nitric acid, sulfuric acid, acetic acid, the mixture of one or more of ammonium hydroxide, ammonium carbonate, ammonium hydrogen carbonate；The additive packet
It includes in ethyl cellulose, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, formamide, acetamide and alkylating reagent
One or more kinds of mixtures；The solvent includes methanol, ethyl alcohol, butanol etc., in the straight chain alcohol of 96% or more mass fraction
One or more kinds of mixtures；The preparation of the aerosil glue includes the component of following volume ratio: just
Silester: methyltrimethoxysilane: 99% industrial alcohol: water catalyst: additive=10:3:(50~150): (3~6):
(0.3~1.1)；
2) molding of oxidization fiber fibrofelt aeroge；The oxidization fiber fibrofelt include oxidization fiber Nomex, oxidization fiber centrifugal cotton,
For oxidization fiber force fit plate etc. using diameter as made of nanoscale oxidization fiber Fiber Materials, density is not more than 250kg/m3, and quality is equal
Even plate or felt；The oxidization fiber fibrofelt is that will exist from hydrophobic silica aerogel glue spray from hydrophobic aerogel molding
On oxidization fiber fibrofelt, make oxidization fiber fibrofelt saturation absorption glue, for oxidization fiber fibrofelt without being bubbled, being recessed, upper and lower surface is equal
It is even smooth, 30~35 DEG C are re-fed into, while pH value forms oxidization fiber fiber to stand 20~25min in 8~9 alkaline environment
Felt wet gel material；
3) ageing of oxidization fiber fibrofelt aeroge after molding；The ageing is to be put into oxidization fiber fibrofelt wet gel material
35~45 DEG C of immersion 30h in ethanol solution；
4) drying and detection of the oxidization fiber fibrofelt aeroge after being aged；The drying is that the oxidization fiber fibrofelt that will be aged is wet
Gel rubber material is put into the material barrel of extraction kettle, and carbon dioxide gas is injected extraction kettle, keeps temperature and pressure in extraction kettle
In the supercriticality of carbon dioxide gas, and and material, it is dissolved in the solvent in material among supercritical fluid, from
Collect fluid in the extraction outlet of extraction kettle；The supercritical temperature is 40~50 DEG C, and pressure is 10~18MPa；Carbon dioxide gas
The flow that body passes through extraction kettle is 200~250kg/h, extraction time 10h；The detecting step is will be under optimum process condition
Extract material out and randomly select the performance of bulk roll of material (can should reflect as far as possible) at 3 points at 3 points, every takes 300 × 300mm material two
Block measures density, thermal coefficient, hydrophobicity, mechanical strength.
Embodiment 1:
A kind of compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber is the following steps are included: from hydrophobic two
The preparation of silica aerogel glue → oxidization fiber fibrofelt aeroge molding → oxidization fiber after molding fibrofelt aeroge
Ageing → ageing after oxidization fiber fibrofelt aeroge drying and detection.According to the group assignment system colloidal sol of such as volume ratio: just
Silester: methyltrimethoxysilane: 99% industrial alcohol: water catalyst: then additive=10:3:50:3:1.1 will
It is being 250kg/m3's with density made of nanoscale oxidization fiber Fiber Materials from hydrophobic silica aerogel glue spray
On homogeneous oxidization fiber fibrofelt, make oxidization fiber fibrofelt saturation absorption glue, oxidization fiber fibrofelt without be bubbled, recess,
Upper and lower surface uniform ground is re-fed into 35 DEG C, while it is fine to form oxidization fiber to stand 25min in 8~9 alkaline environment for pH value
Tie up felt wet gel material；Then oxidization fiber fibrofelt wet gel material is put into 45 DEG C of immersion 30h in ethanol solution；Again will later
The oxidization fiber fibrofelt wet gel material of ageing is put into the material barrel of extraction kettle, and carbon dioxide gas is injected extraction kettle, is protected
Temperature and pressure in extraction kettle is held in the supercriticality of carbon dioxide gas, and and material, keep the solvent in material molten
Solution is among supercritical fluid；Supercritical temperature is 50 DEG C, pressure 16MPa；The flow that carbon dioxide gas passes through extraction kettle
For 250kg/h, extraction time 10h；Collection fluid to no solution is exported from the extraction of extraction kettle to be discharged, and is shut down and is taken out material.
Material out will be extracted to randomly select 3 points the performance of bulk roll of material (3 points can should reflect as far as possible), every take 300 ×
Two pieces of 300mm material, measure density, thermal coefficient, hydrophobicity, mechanical strength.Obtain test result: hot coefficient be 0.016~
0.019W/mK, hydrophobic angle are 126 °, and compressive strength is 89.6(25% deformation).
Claims (9)
1. a kind of compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber, it is characterised in that: this method
The following steps are included:
1) from the preparation of hydrophobic silica aerogel glue；The raw material from hydrophobic silica aerogel glue has silicon source
Presoma, hydrolyst, additive and solvent；
2) molding of oxidization fiber fibrofelt aeroge；
3) ageing of oxidization fiber fibrofelt aeroge after molding；
4) drying and detection of the oxidization fiber fibrofelt aeroge after being aged.
2. the compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber according to claim 1,
Be characterized in that: the silicon source presoma include ethyl orthosilicate, methyl orthosilicate, in trim,ethylchlorosilane, methyl trimethoxy oxygroup
One or more mixtures of silane；The hydrolyst includes pure water, hydrochloric acid, nitric acid, sulfuric acid, acetic acid, ammonium hydroxide,
The combination of one or more of ammonium carbonate, ammonium hydrogen carbonate；The additive includes ethyl cellulose, N, N- dimethyl methyl
The combination of one or more of amide, DMAC N,N' dimethyl acetamide, formamide, acetamide and alkylating reagent；It is described
Solvent includes the combination of one or more of straight chain alcohol of methanol, ethyl alcohol, butanol, 96% or more mass fraction.
3. the compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber according to claim 2,
Be characterized in that: the aerosil glue is formulated by the component of following volume ratio: ethyl orthosilicate: methyl trimethoxy
Oxysilane: 99% industrial alcohol: hydrolyst: additive=10:3:50~150:3~6:0.3~1.1, by situ poly-
It is legal, so that the aeroge prepared is carried hydrophobicity.
4. the compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber according to claim 1,
It is characterized in that: by sol solutions spray on oxidization fiber fibrofelt, making oxidization fiber fibrofelt saturation absorption glue, be re-fed into 30~35
20~25min is stood in DEG C alkaline environment, forms oxidization fiber fibrofelt wet gel material.
5. the compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber according to claim 4,
Be characterized in that: the oxidization fiber fibrofelt is using diameter as made of nanoscale oxidization fiber Fiber Materials, and density is not more than
250kg/m3, homogeneous plate or felt.
6. the compound preparation process from hydrophobic silica aerogel insulation quilt of oxidization fiber according to claim 1,
Be characterized in that: the ageing is that oxidization fiber fibrofelt wet gel material is put into 35~45 DEG C of immersion 30h in ethanol solution.
7. oxidization fiber fibrofelt according to claim 1 is from the preparation method of hydrophobic silica aerogel insulation quilt,
Be characterized in that: the drying is that the oxidization fiber fibrofelt wet gel material of ageing is put into the material barrel of extraction kettle, by dioxy
Change carbon gas and inject extraction kettle, maintains temperature and pressure in extraction kettle, to guarantee the supercriticality of carbon dioxide gas,
It when carbon dioxide is in a supercritical state, be dissolved in the solvent in material can among supercritical fluid, from extraction kettle
Extraction outlet collect fluid, it is compound from hydrophobic silica aerogel insulation quilt to prepare oxidization fiber.
8. the compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber according to claim 7,
Be characterized in that: the supercriticality temperature of the carbon dioxide gas is 40~50 DEG C, and pressure is 10~18MPa；Carbon dioxide
The flow that gas passes through extraction kettle is 200~250kg/h, extraction time 10h.
9. the compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber according to claim 1,
Be characterized in that: the detecting step is will to extract material out to randomly select at 3 points, and every takes two pieces of 300 × 300mm material, measures close
Degree, thermal coefficient, hydrophobicity and/or mechanical strength.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811554746.1A CN109680485A (en) | 2018-12-18 | 2018-12-18 | The compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber |
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| CN201811554746.1A CN109680485A (en) | 2018-12-18 | 2018-12-18 | The compound preparation method from hydrophobic silica aerogel insulation quilt of oxidization fiber |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111039295A (en) * | 2019-12-20 | 2020-04-21 | 爱彼爱和新材料有限公司 | Method for preparing silicon dioxide aerogel and self-hydrophobic silicon dioxide aerogel heat-insulating felt pad by one-step method |
| CN111517747A (en) * | 2020-04-21 | 2020-08-11 | 浙江岩谷科技有限公司 | Preparation method of pre-oxidized fiber felt-silica aerogel heat-insulation composite material |
| CN113694844A (en) * | 2021-09-18 | 2021-11-26 | 贵州航天乌江机电设备有限责任公司 | Preparation process of aerogel felt |
| CN113735556A (en) * | 2021-08-13 | 2021-12-03 | 红塔烟草(集团)有限责任公司 | Silicon-containing aerogel composite material and preparation method and application thereof |
| CN117510181A (en) * | 2023-11-07 | 2024-02-06 | 武汉中科先进材料科技有限公司 | Super-hydrophobic and enhanced silicon dioxide aerogel felt and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106495169A (en) * | 2016-10-28 | 2017-03-15 | 浙江省普瑞科技有限公司 | A kind of hydrophobic type aerosil and preparation method thereof |
| CN107935540A (en) * | 2017-12-19 | 2018-04-20 | 贵州航天乌江机电设备有限责任公司 | A kind of preparation process of oxidization fiber fiber composite type aerosil insulation blanket |
-
2018
- 2018-12-18 CN CN201811554746.1A patent/CN109680485A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106495169A (en) * | 2016-10-28 | 2017-03-15 | 浙江省普瑞科技有限公司 | A kind of hydrophobic type aerosil and preparation method thereof |
| CN107935540A (en) * | 2017-12-19 | 2018-04-20 | 贵州航天乌江机电设备有限责任公司 | A kind of preparation process of oxidization fiber fiber composite type aerosil insulation blanket |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111039295A (en) * | 2019-12-20 | 2020-04-21 | 爱彼爱和新材料有限公司 | Method for preparing silicon dioxide aerogel and self-hydrophobic silicon dioxide aerogel heat-insulating felt pad by one-step method |
| CN111039295B (en) * | 2019-12-20 | 2022-04-12 | 爱彼爱和新材料有限公司 | Method for preparing silicon dioxide aerogel and self-hydrophobic silicon dioxide aerogel heat-insulating felt pad by one-step method |
| CN111517747A (en) * | 2020-04-21 | 2020-08-11 | 浙江岩谷科技有限公司 | Preparation method of pre-oxidized fiber felt-silica aerogel heat-insulation composite material |
| CN113735556A (en) * | 2021-08-13 | 2021-12-03 | 红塔烟草(集团)有限责任公司 | Silicon-containing aerogel composite material and preparation method and application thereof |
| CN113694844A (en) * | 2021-09-18 | 2021-11-26 | 贵州航天乌江机电设备有限责任公司 | Preparation process of aerogel felt |
| CN117510181A (en) * | 2023-11-07 | 2024-02-06 | 武汉中科先进材料科技有限公司 | Super-hydrophobic and enhanced silicon dioxide aerogel felt and preparation method thereof |
| CN117510181B (en) * | 2023-11-07 | 2024-04-16 | 武汉中科先进材料科技有限公司 | Super-hydrophobic and enhanced silicon dioxide aerogel felt and preparation method thereof |
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Application publication date: 20190426 |