CN109516763B - Cellulose fiber/SiO2Composite aerogel material, preparation and application thereof - Google Patents
Cellulose fiber/SiO2Composite aerogel material, preparation and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/76—Use at unusual temperatures, e.g. sub-zero
- C04B2111/763—High temperatures
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention relates to a cellulose fiber/SiO2The composite aerogel material is prepared by taking organic siloxane as a precursor and cellulose fiber as a framework, growing silica gel on the surface of the cellulose fiber in situ by a sol-gel method and a one-step thermal reaction method to prepare composite wet gel fiber, replacing a solvent, and drying at normal temperature and normal pressure. The composite aerogel has good thermal insulation performance and mechanical property, meets the requirement of clothing, has hydrophobic surface, moisture permeability and air permeability, is less affected by moisture compared with the traditional thermal insulation material, and is suitable for various low-temperature cold-proof thermal clothes.
Description
Technical Field
The invention belongs to aerogel materials for cold-proof clothes and the preparation and application fields thereof, and particularly relates to cellulose fiber/SiO2Composite aerogel materials, their preparation and use.
Background
With the gradual improvement of living standard of people, new requirements are put forward on cold-proof warm-keeping clothes, and the cold-proof warm-keeping clothes not only have basic heat preservation performance, but also are pursuing to be light, thin and comfortable. From natural cotton, down, porous synthetic cellucotton, to xinxueli (Thinsulate)TM3M), new heat insulating materials for textiles are continuously emerging. In 2008, aspen corporation, usa, collaborated with golf ball builder 21 element, canada, developed a clothing aerogel named "zero interlayer" with which a windcheat, only 0.3 cm thick, was worn as warm as a4 cm thick down jacket. Although the products complain about poor air permeability, good heat insulation performance and overheating, the appearance of the aerogel opens up a new direction for taking heat insulation materials.
The aerogel is a nano material with a porous three-dimensional network structure, the porosity of the aerogel is up to more than 80%, and the air is filled in the gaps. This structure determines the aerogel with high specific surface area (200-2Per g), low density (0.003-0.35 g/cm)3) Low thermal conductivity (0.012-0.045W/mK), and the like, so that the material is applied to the field of light heat-insulating materialsDomains have natural advantages. However, the conventional aerogel has a large brittleness and a small mechanical strength, and is difficult to use for clothing, and strength and toughness required for clothing can be imparted only by compounding with fibers.
Existing fiber/SiO2Most of the composite aerogel patents use inorganic fibers such as glass fibers and the like as frameworks, and the materials have good high-temperature resistance but are not suitable for low-temperature cold-proof clothes. Although aerogels have been used in Aspen Systems, inc, usa, they have been prepared using a high-cost supercritical drying technique with a polyester fiber skeleton. The fiber used in CN107051339A is one of polyacrylonitrile, aramid fiber or polypropylene fiber, and the dosage of the fiber is only 1.5% of the mass of the aerogel, so that the compressibility of the aerogel is only improved, but the tear resistance requirement of the clothing material is difficult to meet, and the like. CN101948296A mentions cellulose fibers, but it is SiO2The hydrosol is used as a raw material, the surface of the aerogel needs to be subjected to hydrophobic treatment, and meanwhile, a supercritical drying technology is adopted for drying, so that the technical route is relatively long, and the production cost is relatively high.
Disclosure of Invention
The invention aims to provide a cellulose fiber/SiO2The composite aerogel material and the preparation and the application thereof overcome the defects that the prior aerogel can not meet the tear resistance requirement of a clothing material, the surface of the aerogel is required to be subjected to hydrophobic treatment, the technical route is longer, and the production cost is higher.
The invention relates to a cellulose fiber/SiO2Composite aerogel material, which is SiO formed by taking cellulose fiber as a framework and taking organosiloxane as a precursor2The aerogel is loaded on the surface of the cellulose fibers and in the fiber voids.
Preferably, the cellulose fiber is a skeleton, SiO2The aerogel takes organosilane as a precursor and water as a solventFormed in situ on the surface of the cellulose fibres and in the interstices of the fibres by a sol-gel process.
The SiO2The aerogel is hydrophobic SiO2An aerogel.
In the composite aerogel material, SiO2The loading capacity of the aerogel is 30-80%, and the content of the cellulose fiber is 70-20%.
The cellulose fiber/SiO of the invention2A method of preparing a composite aerogel material, comprising:
soaking cellulose fiber into organic siloxane hydrosol, reacting under closed condition to obtain fiber composite wet gel, and performing solvent replacement and drying to obtain cellulose fiber/SiO2Compounding aerogel materials.
The preferred mode of the above preparation method is as follows:
the cellulose fiber is one of plant cellulose fiber and bacterial cellulose fiber; according to the fiber thickness, the cellulose fiber is preferably superfine fiber and nanofiber. According to the fiber form, the cellulose fiber non-woven fabrics are made by various processes and technologies.
The organic siloxane is organic siloxane containing hydrophobic groups.
Further preferably, the organosiloxane is one or more of methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane and dimethyldiethoxysilane.
The organic siloxane hydrosol is specifically as follows: the organosiloxane is added into a dilute acid aqueous solution containing a surfactant and an alkali precursor.
The surfactant is cetyl trimethyl ammonium chloride or cetyl trimethyl ammonium bromide; the alkali precursor is urea or thiourea; the diluted acid aqueous solution is 0.6-3 mmol/L sulfuric acid aqueous solution, 1.2-6 mmol/L hydrochloric acid aqueous solution or 5-10 mmol/L acetic acid aqueous solution.
The reaction is condensation polymerization reaction of silica sol and cellulose at 40-100 ℃ for 1-3 days.
One such method of the inventionPrepared cellulose fiber/SiO2Compounding aerogel materials.
The invention also provides a cold-proof warm-keeping textile which adopts a laminating method to laminate the cellulose fiber/SiO2The upper surface and the lower surface of the composite aerogel are compounded with dustproof breathable fabrics.
The cellulose fiber/SiO of the invention2The composite aerogel material is applied to cold-proof and warm-keeping textiles.
Advantageous effects
(1) According to the invention, the organic siloxane containing hydrophobic groups is used as a precursor, so that the final composite aerogel has hydrophobic performance, the structural damage and the performance reduction caused by the collapse of holes due to the water absorption effect of hydrophilic aerogel are avoided, and compared with the traditional heat-insulating material, the hydrophobic composite aerogel fabric is less affected by moisture.
(2) The invention adopts a one-step thermal polymerization method, and hydrolyzes an alkali precursor into alkali at a proper temperature to promote condensation reactions between silica sol and between silica sol and cellulose fibers, so that the silica aerogel grows in situ on the cellulose fibers. Preparation of SiO by sol-gelation due to abundant hydroxyl groups on the surface of cellulose fiber2The aerogel can participate in the polycondensation reaction in the process, so that the fiber and SiO can be ensured without modifying the surface of the fiber2The aerogel has good interface combination, and is beneficial to prolonging the service life of the composite aerogel.
(3) The composite aerogel material obtained by the invention has good thermal insulation performance, mechanical properties meeting the requirements of clothes, moisture permeability, air permeability and hydrophobic surface. The traditional heat-insulating material is easy to absorb water, the heat conductivity coefficient of water is almost 21 times larger than that of air, and the heat-insulating property is obviously reduced as long as the moisture regain is 15%. Therefore, compared with the traditional heat-insulating material, the hydrophobic composite aerogel material has less influence on heat insulation and heat preservation performance by moisture, is more suitable for various cold-proof and warm-keeping clothes in humid and low-temperature environments, and has the advantages of simple and safe preparation process, lower cost and easy large-scale production.
(4) The fiber obtained by the inventionCellulose fiber/SiO2The mechanical property of the composite aerogel meets the basic requirements of cold protective clothing, the air permeability is more than 100mm/s, and the moisture permeability is more than 6000g/m2The surface contact angle is more than 90 degrees and the specific surface area is more than 150g/mm2Density less than 0.25g/cm3The thermal conductivity coefficient is 0.01-0.03W/m.K, the maximum service temperature is 300 ℃, and the tear strength is more than 6.5N.
Drawings
FIG. 1 shows the flexible cellulose fiber/SiO in example 12A composite aerogel photo;
FIG. 2 shows the cellulose fiber/SiO in example 12A topography of the composite aerogel; wherein a is a cross-sectional view; b is an outer surface diagram;
FIG. 3 shows the cellulose fiber/SiO in example 12TG profile of composite aerogel;
FIG. 4 shows the cellulose fiber/SiO in example 12Surface contact angle plot of composite aerogel.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The test methods or criteria for performance data in the examples are as follows: the specific surface area test adopts a nitrogen adsorption specific surface area tester (NT1LX-1, Quantacathoneggsi company, USA), the surface contact angle test adopts a full-automatic video microcosmic contact angle measuring instrument (OCA40Micro, Germany dataphysics company), the heat-resisting temperature test adopts a thermal weight loss analyzer to test in air atmosphere (the temperature rise speed is 10 ℃/min, TG209F1, Germany speed-resistant company), the heat conductivity test standard GB/T11048-
Example 1
Cellulose fiber/SiO for cold-proof clothes2Preparation of the composite aerogel material:
(1) 15ml of an aqueous acetic acid solution (concentration: 5mmol), 0.8g of cetyltrimethoxysilane ammonium chloride (CTAC) and 5.0g of urea were uniformly mixed in a beaker at room temperature, 7ml of methyltrimethoxysilane was added to the mixed solution, and the mixture was stirred with a magnetic stirrer for 0.5 hour. Selecting cotton cellulose fiber non-woven fabric with proper size, putting the cotton cellulose fiber non-woven fabric into a mould, and adding silica sol to ensure that the cellulose fiber is completely impregnated by the sol. After the mold was sealed, gelation was carried out at 80 ℃ and aging was carried out for two days.
(2) And (3) carrying out solvent replacement on the wet gel, firstly placing the wet gel in a deionized water-isopropanol (1: 1) solution for 1 day, taking out the wet gel, placing the wet gel in an isopropanol solvent for 1 day, finally replacing the wet gel in a normal hexane solvent for 1 day, and drying the wet gel at normal temperature and normal pressure. Further laminating the fibers on the cellulose/SiO2Dustproof breathable fabrics on the upper surface and the lower surface of the composite aerogel.
Cellulose fiber/SiO for cold-proof clothes prepared in the example2In composite aerogel materials, SiO2The loading capacity of the aerogel is 46.4 percent, the cellulose fiber content is 53.6 percent, and the moisture permeability is more than 8880g/m2The surface contact angle is more than 105 degrees, the heat resistance temperature is 300 ℃, and the specific surface area is more than 354.9g/m2Density 0.25g/cm3The thermal conductivity coefficient is 0.018W/m.K, and the tear strength is 7.1N.
Example 2
Cellulose fiber/SiO for cold-proof clothes2Preparation of the composite aerogel material:
(1) 15ml of hydrochloric acid (concentration: 3mmol), 0.8g of cetyltrimethylammonium bromide and 5.0g of thiourea were uniformly mixed in a beaker at room temperature, 3ml of methyltriethoxysilane and 2ml of dimethyldimethoxysilane were added to the mixed solution, and the mixture was stirred with a magnetic stirrer for 0.5 hour. Selecting a nano bacterial cellulose membrane with a proper size, putting the nano bacterial cellulose membrane into a mould, and adding silica sol to ensure that the cellulose fiber is completely impregnated by the sol. After the mold was sealed, gelation was carried out at 80 ℃ and aging was carried out for two days.
(2) And (3) carrying out solvent replacement on the wet gel, firstly placing the wet gel in a deionized water-isopropanol (1: 1) solution for 1 day, taking out the wet gel, placing the wet gel in an isopropanol solvent for 1 day, finally replacing the wet gel in a normal hexane solvent for 1 day, and drying the wet gel at normal temperature and normal pressure. Further laminating the fibers on the cellulose/SiO2The upper surface and the lower surface of the composite aerogel are compounded with dustproof breathable fabrics.
Cellulose fiber/SiO for cold-proof clothes prepared in the example2In composite aerogel materials, SiO2The aerogel has a loading capacity of 50%, an air permeability of more than 100mm/s and a moisture permeability of more than 6000g/m2The surface contact angle is more than 110 degrees, the heat resistance temperature is 300 ℃, and the specific surface area is more than 395.4g/m2Density of 0.24g/cm3The thermal conductivity was 0.014W/mK, and the tear strength was 6.5N.
Claims (10)
1. Cellulose fiber/SiO2The composite aerogel material is characterized in that the material is SiO formed by taking cellulose fiber as a framework and taking organosiloxane as a precursor2The aerogel is loaded on the surface of the cellulose fiber and in the fiber gaps; wherein the composite aerogel is prepared by the following method: soaking cellulose fiber into organic siloxane hydrosol, reacting under closed condition to obtain fiber composite wet gel, and performing solvent replacement and drying to obtain cellulose fiber/SiO2A composite aerogel material; wherein the drying is normal temperature and normal pressure drying.
2. The composite aerogel material of claim 1, wherein the composite aerogel material comprises SiO2The loading capacity of the aerogel is 30-80%, and the content of the cellulose fiber is 70-20%.
3. Cellulose fiber/SiO according to claim 12A method of preparing a composite aerogel material, comprising:
soaking cellulose fiber into organic siloxane hydrosol, reacting under closed condition to obtain fiber composite wet gel, replacing solvent, and drying at normal temperature and normal pressure to obtain cellulose fiber/SiO2Composite aerogel materials。
4. The preparation method according to claim 3, characterized in that the cellulose fiber is one or more of plant cellulose fiber and bacterial cellulose fiber; the organic siloxane is one or more of methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane and dimethyldiethoxysilane.
5. The method according to claim 3, characterized in that the organosiloxane hydrosol is in particular: the organosiloxane is added into a dilute acid aqueous solution containing a surfactant and an alkali precursor.
6. The method according to claim 5, wherein the surfactant is cetyltrimethylammonium chloride or cetyltrimethylammonium bromide; the alkali precursor is urea or thiourea; the diluted acid aqueous solution is 0.6-3 mmol/L sulfuric acid aqueous solution, 1.2-6 mmol/L hydrochloric acid aqueous solution or 5-10 mmol/L acetic acid aqueous solution.
7. The method according to claim 3, wherein the reaction is a polycondensation reaction at 40 to 100 ℃ for 1 to 3 days.
8. The method according to claim 3, wherein the solvent displacement is specifically: first, the mixture is displaced in deionized water/isopropanol solution for 1 to 3 days, then displaced in isopropanol solvent for 1 to 3 days, and then displaced in n-hexane solvent for 1 to 3 days.
9. A cold-proof and warm-keeping textile characterized in that the cellulose fiber/SiO of claim 1 is laminated2The upper surface and the lower surface of the composite aerogel are compounded with dustproof breathable fabrics.
10. Cellulose fiber/SiO according to claim 12The application of the composite aerogel material in cold-proof and warm-keeping textiles.
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| CN110180472A (en) * | 2019-05-31 | 2019-08-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Anti-bacterial fibre/titanium dioxide aerogel composite and its preparation and application |
| CN110127706A (en) * | 2019-06-06 | 2019-08-16 | 广东工业大学 | A kind of preparation method of compound aerosil |
| CN110539536B (en) * | 2019-08-23 | 2021-08-03 | 江苏大毛牛新材料有限公司 | Lightweight silica aerogel composite thermal insulation fabric and preparation method thereof |
| CN111268917B (en) * | 2019-11-19 | 2023-06-20 | 重庆文理学院 | Two-step primary nano Kong Ganfa composite vacuum heat-insulating core material and preparation method thereof |
| CN111393851B (en) * | 2020-03-20 | 2022-06-24 | 上海大音希声新型材料有限公司 | Aerogel heat-insulation composite material and preparation method thereof |
| CN111302827A (en) * | 2020-04-10 | 2020-06-19 | 中国人民解放军国防科技大学 | Preparation method of high-temperature-resistant fiber-reinforced silica aerogel heat-insulation composite material |
| CN111560172B (en) * | 2020-06-01 | 2023-05-12 | 山东省科学院新材料研究所 | Biomass fiber reinforced organic silicon aerogel composite material and preparation method and application thereof |
| CN111893649B (en) * | 2020-07-17 | 2022-07-26 | 3M创新有限公司 | Thermal insulation material, method for preparing thermal insulation material and product prepared from thermal insulation material |
| CN112662015B (en) * | 2020-12-24 | 2022-09-02 | 中国科学技术大学 | Flame-retardant nano-cellulose composite aerogel with oriented structure and preparation method thereof |
| CN115627633A (en) * | 2022-09-21 | 2023-01-20 | 王欣然 | Cold-proof breathable fabric and preparation method thereof |
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