CN105586770B - A kind of organic aerogel fibrous composite and preparation method thereof - Google Patents

A kind of organic aerogel fibrous composite and preparation method thereof Download PDF

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CN105586770B
CN105586770B CN201610120440.XA CN201610120440A CN105586770B CN 105586770 B CN105586770 B CN 105586770B CN 201610120440 A CN201610120440 A CN 201610120440A CN 105586770 B CN105586770 B CN 105586770B
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organic
fibrous composite
preparation
aerogel
organic aerogel
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CN105586770A (en
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孙伟
唐皓
朱春蓉
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ZHANGJIAGANG WANZHONGYIXIN BIOTECHNOLOGY Co Ltd
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ZHANGJIAGANG WANZHONGYIXIN BIOTECHNOLOGY Co Ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/35Heterocyclic compounds
    • D06M13/355Heterocyclic compounds having six-membered heterocyclic rings
    • D06M13/358Triazines
    • D06M13/364Cyanuric acid; Isocyanuric acid; Derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224Esters of carboxylic acids; Esters of carbonic acid
    • D06M13/2246Esters of unsaturated carboxylic acids
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/325Amines
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/395Isocyanates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/402Amides imides, sulfamic acids
    • D06M13/41Amides derived from unsaturated carboxylic acids, e.g. acrylamide
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/55Epoxy resins
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    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/18Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/20Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34Polyamides

Abstract

The invention discloses a kind of preparation method of organic aerogel fibrous composite.Organic curing agent, organic solvent, catalyst and water are mixed, stir to obtain mixed solution;Mixed solution is sprayed on fiber base material, obtains organic aerogel fibrous composite.The present invention preparation method is simple, cost is relatively low, base material is used as using fibrous material, using spraying, immersion, brushes etc. that mode is organic aerogel and fiber base material stabilization is combined together, and organic aerogel has certain thickness on fiber base material;The organic aerogel fibrous composite being prepared has good sound-insulating function.

Description

A kind of organic aerogel-fibrous composite and preparation method thereof
Technical field
The present invention relates to a kind of organic aerogel-fibrous composite and preparation method thereof, belong to organic aerogel technology Field.
Background technology
Aeroge is the most light solid material being currently known, and has continuous three-dimensional net structure, can according to its composition To be divided into:Inorganic aerogels, organic aerogel and carbon aerogels.Aeroge is that a kind of generally acknowledged new lightweight nanometer is more simultaneously Hole amorphous solid-state material.It is bright that the unique nanostructured of aeroge makes it have in the application of mechanics, optics, acoustics, calorifics etc. Aobvious advantage, such as it has high porosity, high-specific surface area, low-density, low-refraction, lower thermal conductivity, low acoustic impedance, low bullet The characteristics such as property modulus, strong absorption property.Research to aeroge at present is concentrated mainly on the fields such as calorifics, electronics, absorption, research Most is the aerosil in inorganic aerogels, and the organic aerogel of most study is resorcinol-formaldehyde airsetting Glue.Just the research direction of aeroge is concentrated mainly in the preparation technology of aeroge at present, and to aerogel composite Study less, and preparation technology is complicated, and cost is higher.
Application number 96196880.X provides a kind of preparation method of the aerogel composite containing fiber, preparation technology In need to use a kind of binding agent(Polyvinyl butyral resin or polyvinyl alcohol), pressurized, heated, and raw material in technique are needed during bonding Mixing need to suppress mixing at high temperature under high pressure, preparation technology is complicated, and condition requires harsh, and cost is higher;Application number 201510330499.7 after ionic liquid heating stirring, the method for freeze-drying, which is successfully prepared, can be applied to sound-insulating and heat-insulating Regenerated cellulose-the aerogel composite in field, the porosity of obtained aerogel composite is 12 ~ 23%, but it is made Heating stirring stage mixing time in standby technique is long(2-4h), freeze-drying need to be repeated, and preparation technology is complicated, cost It is high;Application number 201510458672.1 has been successfully made acoustic insulating ear plug of different shapes with polyureas aeroge, achieves preferably Soundproof effect, but be simply made of simple polyureas aeroge;Application number 201510710928.3 by polyureas aeroge with Other construction materials have been combined a kind of sound-insulating construction material, but simply by the sound-insulating characteristic of polyureas aeroge It has been applied on construction material.
The content of the invention
In view of the deficienciess of the prior art, the invention provides a kind of organic aerogel-fibrous composite and its system Preparation Method.
To achieve these goals, the present invention is to realize by the following technical solutions:
A kind of preparation method of organic aerogel-fibrous composite, by organic curing agent, organic solvent, catalyst and Water mixes, and stirs to obtain mixed solution;Mixed solution is sprayed on fiber base material, obtains organic aerogel-fiber Composite.
A kind of preparation method of described organic aerogel-fibrous composite, the organic curing agent(g), You Jirong Agent(mL), catalyst(μ L) and water(μ L) unit deal ratio be 1:2:40:20~1:10:15:60.
A kind of preparation method of described organic aerogel-fibrous composite, the organic curing agent are hexa-methylene One or more in diisocyanate trimer, epoxy resin, vinylamide, cyanate, tertiary amine or acrylate.
Organic solvent described in a kind of preparation method of described organic aerogel-fibrous composite is ethanol, acetone, second One or more in nitrile, isopropanol or DMF.
A kind of preparation method of described organic aerogel-fibrous composite, the catalyst are polyurethane, triethylamine Or the one or more in DMSO.
A kind of preparation method of described organic aerogel-fibrous composite, the fiber base material are glass fibre, wood Matter fiber, nylon or PP fibers.
A kind of preparation method of described organic aerogel-fibrous composite, spraying use hairbrush or plastics watering can, or Using the method directly soaked.
A kind of organic aerogel-fibrous composite that described preparation method is prepared.
Beneficial effects of the present invention:
Preparation method of the invention is simple, cost is relatively low, using fibrous material as base material, using spraying, immersion, brushes Organic aerogel and fiber base material is stable is combined together etc. mode, and organic aerogel have on fiber base material it is certain Thickness;Organic aerogel-the fibrous composite being prepared has good sound-insulating function.
The organic aerogel being prepared-fibrous composite relevant parameter is as follows:
Nanofiber average diameter:20nm to 200 nm;
Specific surface area is big, 1m2/g-200 m2/g;
Density is low, light weight, 5 kg/m3- 400 kg/m3
Porosity:60-99.9%.
Brief description of the drawings
Fig. 1 is the electron microscope SEM figures of organic aerogel-fibrous composite.
Fig. 2 is the optical microscope of organic aerogel-fibrous composite.
Embodiment
To be easy to understand the technical means, the inventive features, the objects and the advantages of the present invention, with reference to Embodiment, the present invention is expanded on further.
Embodiment 1
A kind of preparation method of organic aerogel-fibrous composite, by organic curing agent hexamethylene diisocyanate Tripolymer 12g, the mL of organic solvent-acetone 96, the mL of water 0.4 and the mL of catalyst polyurethane 0.03 are thoroughly mixed uniformly, are obtained It is 1 kg/m to obtain density range3- 40 kg/m3Organic nano airsetting sol solution, directly with atomizing watering can spray to PP fibre In dimension.After the completion of spraying, after room temperature reaction 3 hours, natural air drying.The average pore size of the porous nanometer material of acquisition is 50 nm, nanofiber average diameter are 100nm, specific surface area 100m2/ g, density 8kg/m3, porosity 90%.
Fig. 1 is the electron microscope SEM figures of organic aerogel-fibrous composite.As illustrated, organic aerogel-fibre Dimension composite is nanometer fibrous porous nanometer material.
Fig. 2 is the optical microscope of organic aerogel-fibrous composite.As shown in the figure, it can be seen that organic airsetting Glue is combined together well with fiber base material, and aeroge is presented with fibre structure mostly, and is distributed along substrate fiber.
Embodiment 2
By organic curing agent epoxy resin 8g, organic solvent acetonitrile 16mL, the mL of water 0.16, catalyst of triethylamine 0.32mL is thoroughly mixed uniformly, and acquisition density range is 1 kg/m3- 40 kg/m3Organic nano airsetting sol solution, use Hairbrush is brushed on nylon fiber.After having brushed, after room temperature reaction 5 hours, natural air drying.The porous nanometer material of acquisition Average pore size is 70 nm, and nanofiber average diameter is 140nm, specific surface area 120m2/ g, density 6kg/m3, porosity For 95%.
Embodiment 3
By organic curing agent cyanate 16g, organic solvent absolute ethyl alcohol 120mL, the mL of water 0.72, catalyst DMSO 0.18mL is thoroughly mixed uniformly, and acquisition density range is 1 kg/m3- 40 kg/m3Organic nano airsetting sol solution, directly Connect and wood fibre is immersed in resulting solution, after immersion is reacted 1 day, natural air drying.The porous nanometer material of acquisition Average pore size is 45 nm, and nanofiber average diameter is 70nm, specific surface area 80m2/ g, density 10kg/m3, porosity is 80%。
Embodiment 4
By organic curing agent tertiary amine 16g, organic solvent isopropanol 96mL, the mL of water 0.32, the mL of catalyst of triethylamine 0.24 It is thoroughly mixed uniformly, acquisition density range is 1 kg/m3- 40 kg/m3Organic nano airsetting sol solution, directly by wood Matter fiber is immersed in resulting solution, after immersion is reacted 1 day, natural air drying.The average hole of the porous nanometer material of acquisition Footpath is 45 nm, and nanofiber average diameter is 70nm, specific surface area 80m2/ g, density 10kg/m3, porosity 85%.
Embodiment 5
By organic curing agent acrylate 12g, organic solvent DMF 70mL, water 0.24mL, catalyst of triethylamine 0.18mL It is thoroughly mixed uniformly, acquisition density range is 1 kg/m3- 40 kg/m3Organic nano airsetting sol solution, directly by wood Matter fiber is immersed in resulting solution, after immersion is reacted 1 day, natural air drying.The average hole of the porous nanometer material of acquisition Footpath is 45 nm, and nanofiber average diameter is 70nm, specific surface area 100m2/ g, density 10kg/m3, porosity 85%.
Embodiment 6
By organic curing agent vinylamide 12g, organic solvent isopropanol 120mL, the mL of water 0.72, catalyst of triethylamine 0.18mL is thoroughly mixed uniformly, and acquisition density range is 1 kg/m3- 40 kg/m3Organic nano airsetting sol solution, directly Connect and wood fibre is immersed in resulting solution, after immersion is reacted 1 day, natural air drying.The porous nanometer material of acquisition Average pore size is 45 nm, and nanofiber average diameter is 50nm, specific surface area 100m2/ g, density 10kg/m3, porosity For 95%.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (5)

  1. A kind of 1. preparation method of organic aerogel-fibrous composite, it is characterised in that by organic curing agent, organic solvent, Catalyst and water mixing, stir to obtain mixed solution;Mixed solution is sprayed on fiber base material, obtains organic airsetting Organic curing agent described in glue-fibrous composite(g), organic solvent(mL), catalyst(μ L) and water(μ L) unit deal ratio For 1:2:40:20 or 1:10:15:60;
    The organic curing agent is hexamethylene diisocyanate trimer, epoxy resin, vinylamide, cyanate, tertiary amine Or the one or more in acrylate;
    The catalyst is the one or more in polyurethane, triethylamine or DMSO.
  2. A kind of 2. preparation method of organic aerogel-fibrous composite according to claim 1, it is characterised in that institute Organic solvent is stated as the one or more in ethanol, acetone, acetonitrile, isopropanol or DMF.
  3. A kind of 3. preparation method of organic aerogel-fibrous composite according to claim 1, it is characterised in that institute It is glass fibre, wood fibre, nylon or PP fibers to state fiber base material.
  4. A kind of 4. preparation method of organic aerogel-fibrous composite according to claim 1, it is characterised in that spray Painting uses hairbrush or plastics watering can, or using the method directly soaked.
  5. 5. a kind of organic aerogel-fibrous composite, it is prepared into as the preparation method described in above 1-4 any claims Arrive.
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Publication number Priority date Publication date Assignee Title
CN106824628A (en) * 2017-04-05 2017-06-13 天津天盈新型建材有限公司 A kind of spraying equipment for preparing aeroge fibrofelt
CN111116974B (en) * 2019-12-30 2021-11-09 东华大学 Nylon nanofiber aerogel material for air filtration and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102285775A (en) * 2011-04-29 2011-12-21 中国人民解放军国防科学技术大学 Organic-fiber reinforced organic-aerogel heat-insulating material and preparation method thereof
JP2013515874A (en) * 2009-12-28 2013-05-09 レンツィング アクチェンゲゼルシャフト Functionalized cellulose molded body and method for its production
CN103334298A (en) * 2013-06-08 2013-10-02 蓝星环境工程有限公司 Active carbon fiber composite material and preparation method thereof
CN104525132A (en) * 2015-01-06 2015-04-22 张家港万众一芯生物科技有限公司 Aerogel material and preparation method and application thereof
CN105536349A (en) * 2015-12-08 2016-05-04 张家港万众一芯生物科技有限公司 Novel nanometer aerogel material for air filtration and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013515874A (en) * 2009-12-28 2013-05-09 レンツィング アクチェンゲゼルシャフト Functionalized cellulose molded body and method for its production
CN102285775A (en) * 2011-04-29 2011-12-21 中国人民解放军国防科学技术大学 Organic-fiber reinforced organic-aerogel heat-insulating material and preparation method thereof
CN103334298A (en) * 2013-06-08 2013-10-02 蓝星环境工程有限公司 Active carbon fiber composite material and preparation method thereof
CN104525132A (en) * 2015-01-06 2015-04-22 张家港万众一芯生物科技有限公司 Aerogel material and preparation method and application thereof
CN105536349A (en) * 2015-12-08 2016-05-04 张家港万众一芯生物科技有限公司 Novel nanometer aerogel material for air filtration and preparation method thereof

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