CN104945004B - A kind of composite of New Regenerated Cellulosic Fibers aeroge and preparation method thereof - Google Patents
A kind of composite of New Regenerated Cellulosic Fibers aeroge and preparation method thereof Download PDFInfo
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- CN104945004B CN104945004B CN201510330499.7A CN201510330499A CN104945004B CN 104945004 B CN104945004 B CN 104945004B CN 201510330499 A CN201510330499 A CN 201510330499A CN 104945004 B CN104945004 B CN 104945004B
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Abstract
The present invention provides a kind of composite of New Regenerated Cellulosic Fibers aeroge, including regenerated celulose fibre and fiber base aeroge, and regenerated celulose fibre is skeleton, and fiber base aeroge is adsorbed in regenerated celulose fibre surface, and specific operating procedure is：By weight, in the ionic liquid that 5 17 parts of cellulose is added to 80 100 parts, heating stirring to cellulose is completely dissolved, obtain cellulose mixed solution, then in a mold, regenerated celulose fibre is paved into rule or irregular shape, add cellulose mixed solution, the surface of all regenerated celulose fibres is covered to solution, obtain preliminary composite template, finally preliminary composite template is placed under subzero environment and is freeze-dried, then ionic liquid displacement is come out, it is finally freeze-dried again to handle the composite for obtaining regenerated celulose fibre aeroge.
Description
Technical field：
The invention belongs to textile material technical field, and in particular to a kind of New Regenerated Cellulosic Fibers-aeroge is answered
Condensation material and preparation method thereof.
Background technology：
Aeroge, also known as solid-state cigarette, frost smoke, are the most light solid materials being currently known, it be by colloidal particle or
High-polymer molecular mutually coalesces the micro-nano porous network solid-state amorphous substance of composition, i.e., liquid in gel is replaced with gas and
Gel three-dimensional netted microstructure is not in itself changed, with nanometer porous structure and the features such as high hole.
Aeroge is divided into three classes according to composition：Inorganic aerogels, organic aerogel and the class of composite aerogel three, these three gas
Gel all has the characteristics such as bigger serface, low-density, lower thermal conductivity, low-refraction, low-k, in heat-insulated, sound insulation, storage
The various fields such as hydrogen, catalysis have a huge application value, but are due to that the high porosity of aeroge makes its frame strength low, tough
Property poor, structural instability, and the higher preparation cost such as its supercritical drying limits the practical application of aeroge, therefore needs
Improve Mechanical Properties of Aerogels, reduce production cost.
It is to improve the effective ways of Mechanical Properties of Aerogels to prepare aerogel composite by reinforcement of fiber at present, in
State 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 metallic fiber is sintered together to form tridimensional network, and carbon nano-fiber is grown on
On metallic fiber, in carbon aerogels coating and nanofiber, obtained material may be used as electrode material, and the material is used substantially
Carbon material is prepared as raw material, and cost is higher, and preparation technology is complex, relatively limited using scope.
The present invention prepares composite with cellulose base aeroge using regenerated celulose fibre as primary raw material, with fibre
The aerogel material prepared based on dimension element is also equipped with green reproducible feature, and wide material sources, biodegradable, biology
The characteristics of excellent compatibility, regenerated celulose fibre also possesses the advantages of environmental protection is ecological, and both are combined into the compound of preparation
Material can improve the mechanical property of aeroge, and production cost can be reduced again, also environmental protection.
The content of the invention：
The technical problem to be solved in the present invention is to provide a kind of composite of New Regenerated Cellulosic Fibers-aeroge and
Its preparation method, composite, the composite of preparation are prepared using regenerated cellulose and cellulose base aeroge as raw material
Raw material it is homogeneous, be all cellulose, possess the reproducible feature of environmental protection, and wide material sources, cost is relatively low.
In order to solve the above technical problems, the technical scheme is that：
A kind of composite of New Regenerated Cellulosic Fibers-aeroge, it is characterised in that the composite is included again
Raw cellulose fibre and aeroge, the aeroge are fiber base aeroge, and the regenerated celulose fibre is skeleton, the fibre
Wiki aeroge is adsorbed in regenerated celulose fibre surface.
Preferably, the composite of the regenerated celulose fibre-aeroge can be used for insulation, heat-insulated, sound insulation and suction
Oily field.
The present invention also provides a kind of preparation method of the composite of New Regenerated Cellulosic Fibers-aeroge, its feature
It is：Comprise the following steps：
(1) by weight, in the ionic liquid that 5-17 parts of cellulose is added to 80-100 parts, heating stirring to fiber
Element is completely dissolved, and obtains cellulose mixed solution；
(2) in a mold, regenerated celulose fibre is paved into rule or irregular shape, adds prepared by step (1)
Cellulose mixed solution, the surface of all regenerated celulose fibres is covered to solution, preliminary composite template is obtained；
(3) the preliminary composite template for preparing step (2) is placed under subzero environment and is freeze-dried, then by ionic liquid
Body is cemented out, finally freeze-dried again to handle the composite for obtaining regenerated celulose fibre-aeroge.
As the preferred of above-mentioned technical proposal, in the step (1), cellulose is the regrowth or residue of production and processing
Thing.
As the preferred of above-mentioned technical proposal, in the step (1), heating-up temperature is 70-75 DEG C, and mixing time is 2-
6h。
As the preferred of above-mentioned technical proposal, in the step (2), if regular shape is that dried layer is orthogonal or fibre of oblique
Layer is tieed up, irregular shape is the thick non-woven fabrics forms of 1-10cm.
As the preferred of above-mentioned technical proposal, in the step (2), regenerated celulose fibre in preliminary composite template
A diameter of 5-7 μm, mass fraction shared by regenerated celulose fibre is 50-75%.
As the preferred of above-mentioned technical proposal, in the step (3), the temperature of subzero environment is -4 DEG C -- 20 DEG C.
As the preferred of above-mentioned technical proposal, in the step (3), the time of freeze-drying is 2-4h.
As the preferred of above-mentioned technical proposal, in the step (3), the composite of regenerated celulose fibre-aeroge
Pore size be micro/nano level, porosity is 12-23%.
Compared with prior art, the invention has the advantages that：
(1) present invention is using skeleton of the regenerated celulose fibre as composite, and mechanical strength is preferable, with excellent
Bioactivity, biological degradability and biocompatibility, moisture absorption and performance of keeping humidity are good, environmental protection, and cellulose base aeroge is to adopt
Prepared with cellulose as raw material, except possess traditional aeroge a little in addition to, also with environmental protection, biodegradable work(
Effect, therefore both materials are combined to the composite of preparation, can not only improve the mechanical property of composite, bioactivity and
Compatibility is good, can green degrade, to environment no pressure, and the abundance of cellulose, cost is relatively low, can reduce composite wood
The production cost of material, improves its economic value, expands it and uses scope.
(2) this method uses solion solution cellulose, and solion liquid is a kind of green solvent, recyclable to repeat profit
With the method for relatively conventional dissolving cellulose is more environmentally-friendly efficiently.
(3) liquid will not be produced and had to environment during the raw material and reagent of this method use are all green product, preparation
Harmful material, therefore this method belongs to green technology, is suitable for being widely popularized and uses.
Embodiment：
Describe the present invention in detail below in conjunction with specific embodiment, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1：
(1) by weight, by the regrowth of 5 parts of production and processing or the ionic liquid of 80 parts of residue cellulose addition
In body, 70 DEG C of heating stirring 6h are completely dissolved to cellulose, obtain cellulose mixed solution.
(2) in a mold, 5 μm of regenerated celulose fibre is paved into 50 layers of orthogonal fibrous layer of rule, step is added
(1) cellulose mixed solution prepared, the surface of all regenerated celulose fibres is covered to solution, preliminary composite mould is obtained
Mass fraction shared by plate, wherein regenerated celulose fibre is 50%.
(3) the preliminary composite template for preparing step (2), which is placed under -4 DEG C of subzero environment, is freeze-dried 4h, then
Ionic liquid displacement is come out, finally freeze-dried 2h processing obtains the composite of regenerated celulose fibre-aeroge again.
Embodiment 2：
(1) by weight, by the regrowth of 17 parts of production and processing or the ion of 100 parts of residue cellulose addition
In liquid, 75 DEG C of heating stirring 2h are completely dissolved to cellulose, obtain cellulose mixed solution.
(2) in a mold, 7 μm of regenerated celulose fibre is paved into the fibrous layer of 35 layers of oblique of rule, step is added
(1) cellulose mixed solution prepared, the surface of all regenerated celulose fibres is covered to solution, preliminary composite mould is obtained
Mass fraction shared by plate, wherein regenerated celulose fibre is 75%.
(3) the preliminary composite template for preparing step (2), which is placed under -20 DEG C of subzero environment, is freeze-dried 2h, so
Ionic liquid displacement is come out afterwards, finally freeze-dried 2h processing obtains the composite wood of regenerated celulose fibre-aeroge again
Material.
Embodiment 3：
(1) by weight, by the regrowth of 15 parts of production and processing or the ion of 95 parts of residue cellulose addition
In liquid, 70 DEG C of heating stirring 4h are completely dissolved to cellulose, obtain cellulose mixed solution.
(2) in a mold, 5 μm of regenerated celulose fibre is paved into the thick non-woven fabrics forms of irregular 1cm, adds step
(1) cellulose mixed solution prepared, the surface of all regenerated celulose fibres is covered to solution, preliminary composite mould is obtained
Mass fraction shared by plate, wherein regenerated celulose fibre is 75%.
(3) the preliminary composite template for preparing step (2), which is placed under -20 DEG C of subzero environment, is freeze-dried 3h, so
Ionic liquid displacement is come out afterwards, finally freeze-dried 4h processing obtains the composite wood of regenerated celulose fibre-aeroge again
Material.
Embodiment 4：
(1) by weight, by the regrowth of 12 parts of production and processing or the ion of 95 parts of residue cellulose addition
In liquid, 75 DEG C of heating stirring 5h are completely dissolved to cellulose, obtain cellulose mixed solution.
(2) in a mold, 7 μm of regenerated celulose fibre is paved into the thick non-woven fabrics forms of irregular 10cm, adds step
Suddenly the cellulose mixed solution that prepared by (1), the surface of all regenerated celulose fibres is covered to solution, preliminary composite is obtained
Mass fraction shared by template, wherein regenerated celulose fibre is 50%.
(3) the preliminary composite template for preparing step (2), which is placed under -4 DEG C of subzero environment, is freeze-dried 4h, then
Ionic liquid displacement is come out, finally freeze-dried 4h processing obtains the composite of regenerated celulose fibre-aeroge again.
Embodiment 5：
(1) by weight, by the regrowth of 8 parts of production and processing or the ionic liquid of 90 parts of residue cellulose addition
In body, 70 DEG C of heating stirring 4.5h are completely dissolved to cellulose, obtain cellulose mixed solution.
(2) in a mold, 6 μm of regenerated celulose fibre is paved into the fibrous layer of 60 layers of oblique of rule, step is added
(1) cellulose mixed solution prepared, the surface of all regenerated celulose fibres is covered to solution, preliminary composite mould is obtained
Mass fraction shared by plate, wherein regenerated celulose fibre is 65%.
(3) the preliminary composite template for preparing step (2), which is placed under -20 DEG C of subzero environment, is freeze-dried 2h, so
Ionic liquid displacement is come out afterwards, finally freeze-dried 2.5h processing obtains the compound of regenerated celulose fibre-aeroge again
Material.
Embodiment 6：
(1) by weight, by the regrowth of 15 parts of production and processing or the ion of 80 parts of residue cellulose addition
In liquid, 75 DEG C of heating stirring 6h are completely dissolved to cellulose, obtain cellulose mixed solution.
(2) in a mold, 7 μm of regenerated celulose fibre is paved into the thick non-woven fabrics forms of irregular 5cm, adds step
(1) cellulose mixed solution prepared, the surface of all regenerated celulose fibres is covered to solution, preliminary composite mould is obtained
Mass fraction shared by plate, wherein regenerated celulose fibre is 55%.
(3) the preliminary composite template for preparing step (2), which is placed under -10 DEG C of subzero environment, is freeze-dried 3.5h,
Then ionic liquid displacement is come out, finally freeze-dried 2h processing obtains the compound of regenerated celulose fibre-aeroge again
Material.
Embodiment 7：
(1) by weight, by the regrowth of 7 parts of production and processing or the ionic liquid of 85 parts of residue cellulose addition
In body, 72 DEG C of heating stirring 3h are completely dissolved to cellulose, obtain cellulose mixed solution.
(2) in a mold, 7 μm of regenerated celulose fibre is paved into the fibrous layer of 50 layers of oblique of rule, step is added
(1) cellulose mixed solution prepared, the surface of all regenerated celulose fibres is covered to solution, preliminary composite mould is obtained
Mass fraction shared by plate, wherein regenerated celulose fibre is 62%.
(3) the preliminary composite template for preparing step (2), which is placed under -15 DEG C of subzero environment, is freeze-dried 2h, so
Ionic liquid displacement is come out afterwards, finally freeze-dried 2h processing obtains the composite wood of regenerated celulose fibre-aeroge again
Material.
After testing, the porosity of the composite of regenerated celulose fibre-aeroge prepared by embodiment 1-6, heat conduction system
The result of number and mechanical strength is as follows：
As seen from the above table, the porosity of the composite of regenerated celulose fibre-aeroge prepared by the present invention is moderate, leads
Hot and mechanical strength is good.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (8)
1. a kind of composite of regenerated celulose fibre-aeroge, it is characterised in that the composite includes regenerated fiber
Cellulose fiber and aeroge, the aeroge are fiber base aeroge, and the regenerated celulose fibre is skeleton, the fiber base gas
Gel adsorption in regenerated celulose fibre surface, the composite of the regenerated celulose fibre-aeroge can be used in insulation,
Heat-insulated, sound insulation and oil suction field；
A kind of preparation method of the composite of regenerated celulose fibre-aeroge, comprises the following steps：
(1) by weight, in the ionic liquid that 5-17 parts of cellulose is added to 80-100 parts, heating stirring is complete to cellulose
Fully dissolved, obtains cellulose mixed solution；
(2) in a mold, regenerated celulose fibre is paved into rule or irregular shape, adds fiber prepared by step (1)
Plain mixed solution, the surface of all regenerated celulose fibres is covered to solution, preliminary composite template is obtained；
(3) the preliminary composite template for preparing step (2) is placed under subzero environment and is freeze-dried, and then puts ionic liquid
Swap out and, it is finally freeze-dried again to handle the composite for obtaining regenerated celulose fibre-aeroge.
2. a kind of composite of regenerated celulose fibre-aeroge according to claim 1, it is characterised in that：It is described
In step (1), cellulose is the regrowth or residue of production and processing.
3. a kind of composite of regenerated celulose fibre-aeroge according to claim 1, it is characterised in that：It is described
In step (1), heating-up temperature is 70-75 DEG C, and mixing time is 2-6h.
4. a kind of composite of regenerated celulose fibre-aeroge according to claim 1, it is characterised in that：It is described
In step (2), if regular shape is that dried layer is orthogonal or fibrous layer of oblique, irregular shape is the thick non-woven fabrics shapes of 1-10cm
State.
5. a kind of composite of regenerated celulose fibre-aeroge according to claim 1, it is characterised in that：It is described
In step (2), a diameter of 5-7 μm of regenerated celulose fibre in preliminary composite template, shared by regenerated celulose fibre
Mass fraction is 50-75%.
6. a kind of composite of regenerated celulose fibre-aeroge according to claim 1, it is characterised in that：It is described
In step (3), the temperature of subzero environment is -4 DEG C -- 20 DEG C.
7. a kind of composite of regenerated celulose fibre-aeroge according to claim 1, it is characterised in that：It is described
In step (3), the time of freeze-drying is 2-4h.
8. a kind of composite of regenerated celulose fibre-aeroge according to claim 1, it is characterised in that：It is described
In step (3), the pore size of the composite of regenerated celulose fibre-aeroge 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 |
| CN106007654B (en) * | 2016-05-24 | 2018-02-16 | 加新科技(深圳)有限公司 | A kind of basalt fibre compound cellulose Multifunctional, air gel rubber 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 |
| CN107137979B (en) * | 2017-05-11 | 2020-09-01 | 武汉纺织大学 | Micron fiber three-dimensional framework/polymer nanofiber composite filter material and preparation method thereof |
| CN107287698B (en) * | 2017-06-20 | 2019-10-25 | 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 |
| CN111662037B (en) * | 2020-06-12 | 2022-01-21 | 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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| CN103146017A (en) * | 2013-03-06 | 2013-06-12 | 东北林业大学 | Method for preparing aerogel by quickly dissolving lignocellulose |
| CN103980547A (en) * | 2014-05-27 | 2014-08-13 | 哈尔滨工业大学 | Method for preparing magnetic cellulose aerogel from wastepaper |
| CN104402395A (en) * | 2014-11-18 | 2015-03-11 | 四川睿光科技有限责任公司 | Fiber-reinforced flexible SiO2 aerogel heat-insulation material and preparation method thereof |
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Patent Citations (4)
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|---|---|---|---|---|
| CN102443188A (en) * | 2011-10-26 | 2012-05-09 | 东北林业大学 | Method for preparing amorphous cellulose aerogel with ionic liquid |
| CN103146017A (en) * | 2013-03-06 | 2013-06-12 | 东北林业大学 | Method for preparing aerogel by quickly dissolving lignocellulose |
| CN103980547A (en) * | 2014-05-27 | 2014-08-13 | 哈尔滨工业大学 | Method for preparing magnetic cellulose aerogel from wastepaper |
| CN104402395A (en) * | 2014-11-18 | 2015-03-11 | 四川睿光科技有限责任公司 | Fiber-reinforced flexible SiO2 aerogel heat-insulation material and preparation method thereof |
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