CN104945004A - Novel regenerated cellulose fiber and aerogel composite material and preparation method thereof - Google Patents
Novel regenerated cellulose fiber and aerogel composite material and preparation method thereof Download PDFInfo
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- CN104945004A CN104945004A CN201510330499.7A CN201510330499A CN104945004A CN 104945004 A CN104945004 A CN 104945004A CN 201510330499 A CN201510330499 A CN 201510330499A CN 104945004 A CN104945004 A CN 104945004A
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Abstract
The invention provides a novel regenerated cellulose fiber and aerogel composite material. The material comprises regenerated cellulose fibers and fiber-based aerogel, wherein the regenerated cellulose fibers are used as a skeleton, and the fiber-based aerogel is adsorbed on the surfaces of the regenerated cellulose fibers. Specifically, a preparation method includes the following operating steps: adding 5-17 parts by weight of cellulose into 80-110 parts by weight of ionic liquid, heating and stirring until cellulose is completely dissolved to obtain a cellulose mixed solution; then, spreading the regenerated cellulose fibers into a regular or irregular shape in a mold, adding the cellulose mixed solution until the solution covers the surfaces of all regenerated cellulose fibers to obtain a primary composite material template; finally, placing the primary composite material template in an environment below zero for freeze-drying, swapping out the ionic liquid, and freeze-drying again to obtain the regenerated cellulose fiber and aerogel composite material.
Description
Technical field:
The invention belongs to textile materials technical field, be specifically related to matrix material of a kind of New Regenerated Cellulosic Fibers-aerogel and preparation method thereof.
Background technology:
Aerogel, be also called solid-state cigarette, frost smoke, it is the lightest known at present solid material, it is by colloidal particle or the high-polymer molecular coalescent solid-state amorphous substance of micro-nano porous network formed mutually, namely replace the liquid in gel with gas and do not change the three-dimensional netted microtexture of gel itself, there is the features such as nanometer porous structure and high hole.
Aerogel is divided three classes according to composition: inorganic aerogels, organic aerogel and composite aerogel three class, these three kinds of aerogels all have bigger serface, low density, lower thermal conductivity, low-refraction, the characteristics such as low-k, heat insulation, sound insulation, Chu Qing, the various fields such as catalysis have huge using value, but the high porosity due to aerogel makes its frame strength low, poor toughness, structural instability, and the higher preparation cost such as its supercritical drying limits the practical application of aerogel, therefore need to improve Mechanical Properties of Aerogels, reduce production cost.
Be at present that to prepare aerogel composite be the effective ways improving Mechanical Properties of Aerogels to reinforcement with fiber, Chinese patent CN 101661839 (publication date 2010.3.3) discloses metal fiber-nanometer carbon fiber dimension-carbon aerogel composite material and Preparation method and use, the binding site of steel fiber is sintered together formation tridimensional network, carbon nano fiber is grown on steel fiber, carbon aerogels coating is with on nanofiber, obtained material can be used as electrode materials, this material adopts carbon material to prepare as raw material substantially, cost is higher, preparation technology is comparatively complicated, use range is comparatively limited.
The present invention adopts regenerated cellulose fibre and cellulose base aerogel to prepare matrix material as main raw material, the aerogel material prepared based on Mierocrystalline cellulose also possesses green reproducible feature, and wide material sources, the feature that biodegradable, biocompatibility is excellent, regenerated cellulose fibre also possesses the advantages such as environmental protection ecology, both can be improved the mechanical property of aerogel in conjunction with the matrix material of preparation, production cost can be reduced again, also environmental protection.
Summary of the invention:
The technical problem to be solved in the present invention is to provide matrix material of a kind of New Regenerated Cellulosic Fibers-aerogel and preparation method thereof, regenerated cellulose and cellulose base aerogel is adopted to prepare matrix material as raw material, the raw material of the matrix material of preparation is homogeneous, it is all Mierocrystalline cellulose, possesses the reproducible feature of environmental protection, and wide material sources, cost is lower.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of matrix material of New Regenerated Cellulosic Fibers-aerogel, it is characterized in that, described matrix material comprises regenerated cellulose fibre and aerogel, described aerogel is fiber base aerogel, described regenerated cellulose fibre is skeleton, and described fiber base aerogel is adsorbed in regenerated cellulose fibre surface.
Preferably, the matrix material of described regenerated cellulose fibre-aerogel may be used for insulation, heat insulation, sound insulation and oil suction field.
The present invention also provides a kind of preparation method of matrix material of New Regenerated Cellulosic Fibers-aerogel, it is characterized in that: comprise the following steps:
(1) by weight, added by the Mierocrystalline cellulose of 5-17 part in the ionic liquid of 80-100 part, heated and stirred is dissolved completely to Mierocrystalline cellulose, obtains cellulose mixed solution;
(2) in a mold, regenerated cellulose fibre is paved into regular or irregularly shaped, adds cellulose mixed solution prepared by step (1), cover the surface of all regenerated cellulose fibres to solution, obtain preliminary composite template;
(3) preliminary composite template prepared by step (2) is placed in lyophilize under subzero environment, then by ionic liquid displacement out, finally obtains the matrix material of regenerated cellulose fibre-aerogel again through lyophilize process.
Preferred as technique scheme, in described step (1), Mierocrystalline cellulose is regrowth or the residuum of process for processing.
Preferred as technique scheme, in described step (1), Heating temperature is 70-75 DEG C, and churning time is 2-6h.
Preferred as technique scheme, in described step (2), regular shape is the layer of fibers of the orthogonal or oblique of some layers, and irregularly shaped is the non-woven fabrics form that 1-10cm is thick.
Preferred as technique scheme, in described step (2), in preliminary composite template, the diameter of regenerated cellulose fibre is 5-7 μm, and the massfraction shared by regenerated cellulose fibre is 50-75%.
Preferred as technique scheme, in described step (3), the temperature of subzero environment is-4 DEG C--20 DEG C.
Preferred as technique scheme, in described step (3), the cryodesiccated time is 2-4h.
Preferred as technique scheme, in described step (3), the pore size of the matrix material of regenerated cellulose fibre-aerogel is micro/nano level, and porosity is 12-23%.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention adopts regenerated cellulose fibre as the skeleton of matrix material, physical strength is better, there is excellent biological activity, biological degradability and biocompatibility, moisture absorption and performance of keeping humidity good, environmental protection, cellulose base aerogel adopts Mierocrystalline cellulose to prepare as raw material, except possess traditional aerogel a little except, also there is environmental protection, biodegradable effect, therefore combine both materials the matrix material prepared, the mechanical property of matrix material can not only be improved, biological activity and consistency good, can green degrade, to environment without pressure, and cellulosic abundance, cost is lower, the production cost of matrix material can be reduced, improve its economic worth, expand its use range.
(2) present method adopts solion solution Mierocrystalline cellulose, and solion liquid is a kind of green solvent, recyclable recycling, the method environment-friendly high-efficiency more of relatively traditional dissolving cellulos.
(3) present method adopt raw material and reagent be all green product, in the process of preparation, liquid can not produce environmentally harmful material, and therefore present method belongs to green technology, is suitable for extensively promoting the use of.
Embodiment:
Describe the present invention in detail below in conjunction with specific embodiment, be used for explaining the present invention in this illustrative examples of the present invention and explanation, but not as a limitation of the invention.
Embodiment 1:
(1) by weight, add in the ionic liquid of 80 parts by the regrowth of the process for processing of 5 parts or residuum Mierocrystalline cellulose, 70 DEG C of heated and stirred 6h, dissolve completely to Mierocrystalline cellulose, obtain cellulose mixed solution.
(2) in a mold, the regenerated cellulose fibre of 5 μm is paved into 50 layers of orthogonal layer of fibers of rule, add cellulose mixed solution prepared by step (1), the surface of all regenerated cellulose fibres is covered to solution, obtain preliminary composite template, the massfraction wherein shared by regenerated cellulose fibre is 50%.
(3) preliminary composite template prepared by step (2) is placed in lyophilize 4h under the subzero environment of-4 DEG C, then by ionic liquid displacement out, the matrix material of regenerated cellulose fibre-aerogel is finally obtained again through lyophilize 2h process.
Embodiment 2:
(1) by weight, add in the ionic liquid of 100 parts by the regrowth of the process for processing of 17 parts or residuum Mierocrystalline cellulose, 75 DEG C of heated and stirred 2h, dissolve completely to Mierocrystalline cellulose, obtain cellulose mixed solution.
(2) in a mold, the regenerated cellulose fibre of 7 μm is paved into the layer of fibers of 35 layers of oblique of rule, add cellulose mixed solution prepared by step (1), the surface of all regenerated cellulose fibres is covered to solution, obtain preliminary composite template, the massfraction wherein shared by regenerated cellulose fibre is 75%.
(3) preliminary composite template prepared by step (2) is placed in lyophilize 2h under the subzero environment of-20 DEG C, then by ionic liquid displacement out, the matrix material of regenerated cellulose fibre-aerogel is finally obtained again through lyophilize 2h process.
Embodiment 3:
(1) by weight, add in the ionic liquid of 95 parts by the regrowth of the process for processing of 15 parts or residuum Mierocrystalline cellulose, 70 DEG C of heated and stirred 4h, dissolve completely to Mierocrystalline cellulose, obtain cellulose mixed solution.
(2) in a mold, the regenerated cellulose fibre of 5 μm is paved into the non-woven fabrics form that irregular 1cm is thick, add cellulose mixed solution prepared by step (1), the surface of all regenerated cellulose fibres is covered to solution, obtain preliminary composite template, the massfraction wherein shared by regenerated cellulose fibre is 75%.
(3) preliminary composite template prepared by step (2) is placed in lyophilize 3h under the subzero environment of-20 DEG C, then by ionic liquid displacement out, the matrix material of regenerated cellulose fibre-aerogel is finally obtained again through lyophilize 4h process.
Embodiment 4:
(1) by weight, add in the ionic liquid of 95 parts by the regrowth of the process for processing of 12 parts or residuum Mierocrystalline cellulose, 75 DEG C of heated and stirred 5h, dissolve completely to Mierocrystalline cellulose, obtain cellulose mixed solution.
(2) in a mold, the regenerated cellulose fibre of 7 μm is paved into the non-woven fabrics form that irregular 10cm is thick, add cellulose mixed solution prepared by step (1), the surface of all regenerated cellulose fibres is covered to solution, obtain preliminary composite template, the massfraction wherein shared by regenerated cellulose fibre is 50%.
(3) preliminary composite template prepared by step (2) is placed in lyophilize 4h under the subzero environment of-4 DEG C, then by ionic liquid displacement out, the matrix material of regenerated cellulose fibre-aerogel is finally obtained again through lyophilize 4h process.
Embodiment 5:
(1) by weight, add in the ionic liquid of 90 parts by the regrowth of the process for processing of 8 parts or residuum Mierocrystalline cellulose, 70 DEG C of heated and stirred 4.5h, dissolve completely to Mierocrystalline cellulose, obtain cellulose mixed solution.
(2) in a mold, the regenerated cellulose fibre of 6 μm is paved into the layer of fibers of 60 layers of oblique of rule, add cellulose mixed solution prepared by step (1), the surface of all regenerated cellulose fibres is covered to solution, obtain preliminary composite template, the massfraction wherein shared by regenerated cellulose fibre is 65%.
(3) preliminary composite template prepared by step (2) is placed in lyophilize 2h under the subzero environment of-20 DEG C, then by ionic liquid displacement out, the matrix material of regenerated cellulose fibre-aerogel is finally obtained again through lyophilize 2.5h process.
Embodiment 6:
(1) by weight, add in the ionic liquid of 80 parts by the regrowth of the process for processing of 15 parts or residuum Mierocrystalline cellulose, 75 DEG C of heated and stirred 6h, dissolve completely to Mierocrystalline cellulose, obtain cellulose mixed solution.
(2) in a mold, the regenerated cellulose fibre of 7 μm is paved into the non-woven fabrics form that irregular 5cm is thick, add cellulose mixed solution prepared by step (1), the surface of all regenerated cellulose fibres is covered to solution, obtain preliminary composite template, the massfraction wherein shared by regenerated cellulose fibre is 55%.
(3) preliminary composite template prepared by step (2) is placed in lyophilize 3.5h under the subzero environment of-10 DEG C, then by ionic liquid displacement out, the matrix material of regenerated cellulose fibre-aerogel is finally obtained again through lyophilize 2h process.
Embodiment 7:
(1) by weight, add in the ionic liquid of 85 parts by the regrowth of the process for processing of 7 parts or residuum Mierocrystalline cellulose, 72 DEG C of heated and stirred 3h, dissolve completely to Mierocrystalline cellulose, obtain cellulose mixed solution.
(2) in a mold, the regenerated cellulose fibre of 7 μm is paved into the layer of fibers of 50 layers of oblique of rule, add cellulose mixed solution prepared by step (1), the surface of all regenerated cellulose fibres is covered to solution, obtain preliminary composite template, the massfraction wherein shared by regenerated cellulose fibre is 62%.
(3) preliminary composite template prepared by step (2) is placed in lyophilize 2h under the subzero environment of-15 DEG C, then by ionic liquid displacement out, the matrix material of regenerated cellulose fibre-aerogel is finally obtained again through lyophilize 2h process.
After testing, the result of the porosity of the matrix material of regenerated cellulose fibre-aerogel prepared of embodiment 1-6, thermal conductivity and physical strength is as follows:
As seen from the above table, the porosity of the matrix material of regenerated cellulose fibre-aerogel prepared by the present invention is moderate, thermal conductivity and physical strength good.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (10)
1. the matrix material of New Regenerated Cellulosic Fibers-aerogel, it is characterized in that, described matrix material comprises regenerated cellulose fibre and aerogel, described aerogel is fiber base aerogel, described regenerated cellulose fibre is skeleton, and described fiber base aerogel is adsorbed in regenerated cellulose fibre surface.
2. the matrix material of a kind of New Regenerated Cellulosic Fibers-aerogel according to claim 1, is characterized in that, the matrix material of described regenerated cellulose fibre-aerogel may be used for insulation, heat insulation, sound insulation and oil suction field.
3. a preparation method for the matrix material of New Regenerated Cellulosic Fibers-aerogel, is characterized in that: comprise the following steps:
(1) by weight, added by the Mierocrystalline cellulose of 5-17 part in the ionic liquid of 80-100 part, heated and stirred is dissolved completely to Mierocrystalline cellulose, obtains cellulose mixed solution;
(2) in a mold, regenerated cellulose fibre is paved into regular or irregularly shaped, adds cellulose mixed solution prepared by step (1), cover the surface of all regenerated cellulose fibres to solution, obtain preliminary composite template;
(3) preliminary composite template prepared by step (2) is placed in lyophilize under subzero environment, then by ionic liquid displacement out, finally obtains the matrix material of regenerated cellulose fibre-aerogel again through lyophilize process.
4. the preparation method of the matrix material of a kind of New Regenerated Cellulosic Fibers-aerogel according to claim 3, is characterized in that: in described step (1), Mierocrystalline cellulose is regrowth or the residuum of process for processing.
5. the preparation method of the matrix material of a kind of New Regenerated Cellulosic Fibers-aerogel according to claim 3, it is characterized in that: in described step (1), Heating temperature is 70-75 DEG C, and churning time is 2-6h.
6. the preparation method of the matrix material of a kind of New Regenerated Cellulosic Fibers-aerogel according to claim 3, it is characterized in that: in described step (2), regular shape is the layer of fibers of the orthogonal or oblique of some layers, and irregularly shaped is the non-woven fabrics form that 1-10cm is thick.
7. the preparation method of the matrix material of a kind of New Regenerated Cellulosic Fibers-aerogel according to claim 3, it is characterized in that: in described step (2), in preliminary composite template, the diameter of regenerated cellulose fibre is 5-7 μm, and the massfraction shared by regenerated cellulose fibre is 50-75%.
8. the preparation method of the matrix material of a kind of New Regenerated Cellulosic Fibers-aerogel according to claim 3, it is characterized in that: in described step (3), the temperature of subzero environment is-4 DEG C--20 DEG C.
9. the preparation method of the matrix material of a kind of New Regenerated Cellulosic Fibers-aerogel according to claim 3, it is characterized in that: in described step (3), the cryodesiccated time is 2-4h.
10. the preparation method of the matrix material of a kind of New Regenerated Cellulosic Fibers-aerogel according to claim 3, it is characterized in that: in described step (3), the pore size of the matrix material of regenerated cellulose fibre-aerogel is micro/nano level, and porosity is 12-23%.
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| CN105884356A (en) * | 2016-04-15 | 2016-08-24 | 华东师范大学 | Preparation method of carbon nanorod aerogel based on nanocellulose |
| CN106007654A (en) * | 2016-05-24 | 2016-10-12 | 加新科技(深圳)有限公司 | Basalt fiber composite cellulose multifunctional aerogel material and preparation method thereof |
| CN106435820A (en) * | 2016-09-21 | 2017-02-22 | 东莞市联洲知识产权运营管理有限公司 | Aerogel fibers based on silicon dioxide and cellulose and preparation method of aerogel fibers |
| CN107137979A (en) * | 2017-05-11 | 2017-09-08 | 武汉纺织大学 | A kind of micrometer fibers three-dimensional framework/polymer nanofiber composite filter material and preparation method thereof |
| CN107287698A (en) * | 2017-06-20 | 2017-10-24 | 中国科学技术大学 | A kind of preparation method of carbon nano-fiber aeroge |
| CN111269455A (en) * | 2020-04-15 | 2020-06-12 | 新乡化纤股份有限公司 | Preparation method of novel cellulose aerogel |
| CN111662037A (en) * | 2020-06-12 | 2020-09-15 | 贵州凯襄新材料有限公司 | Concrete retarder and preparation method thereof |
| CN114031808A (en) * | 2021-12-13 | 2022-02-11 | 罗莱生活科技股份有限公司 | Regenerated cellulose fiber/aerogel composite material and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105884356A (en) * | 2016-04-15 | 2016-08-24 | 华东师范大学 | Preparation method of carbon nanorod aerogel based on nanocellulose |
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| CN114031808A (en) * | 2021-12-13 | 2022-02-11 | 罗莱生活科技股份有限公司 | Regenerated cellulose fiber/aerogel composite material and preparation method thereof |
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