CN110396214A - A kind of preparation method of anisotropic fiber element base aeroge - Google Patents
A kind of preparation method of anisotropic fiber element base aeroge Download PDFInfo
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- CN110396214A CN110396214A CN201810371493.8A CN201810371493A CN110396214A CN 110396214 A CN110396214 A CN 110396214A CN 201810371493 A CN201810371493 A CN 201810371493A CN 110396214 A CN110396214 A CN 110396214A
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- cellulose
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- aqueous solution
- grinding tool
- fiber element
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- Health & Medical Sciences (AREA)
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Abstract
The invention discloses a kind of preparation methods of anisotropic fiber element base aeroge, and this method uses cellulose or cellulose base aqueous solution for raw material, easy to operate, high-efficient.It is characterized by comprising the following steps: 1) raw material is placed in plastics grinding tool；2) plastics grinding tool is placed on metal heat-conduction bar；3) metal heat-conduction bar provides freezing gradient during liquid nitrogen frozen；4) sample freezed is placed in drying in drying equipment, demoulds after dry and obtains the cellulose aerogels of anisotropic structure.Cellulose aerogels prepared by the present invention have large-sized anisotropic structure, substance absorption, it is heat-insulated protection, in terms of have broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation method of anisotropic fiber element base aeroge, this method operation is simple, acquisition
Cellulose base aeroge belongs to natural polymer subdomains, also belongs to Forestry Engineering, Packaging Engineering, field of new materials.
Background technique
Cellulose is renewable organic resource abundant in nature, is widely present in plant material, in cellulose
In type, the occupation rate of lignocellulosic is higher, and lignocellulosic is that natural reproducible timber is obtained by a series of processing
Fibrous matter, main source are timber, and therefore, a large amount of lignocellulosic is that cellulose quantitatively provides development and utilization
Basis.Cellulose has many advantages, such as that specific gravity is small, dispersed strong, soft paving property is good, large specific surface area, in heat preservation, insulation and anti-corruption
There is application value in the fields such as erosion.Therefore, can overcome existing for aeroge itself by the obtained aeroge of matrix of cellulose
The disadvantages of frangible.
The structure of cellulose base aeroge develops its follow up functional and application has highly important influence.Currently,
The preparation of aeroge mainly includes two processes of drying of the freezing preparation and gel of hydrogel.Currently, the freezing preparation of gel
It mostly uses that refrigerator freezing or liquid nitrogen frozen technology, and the drying means that gel is used is relatively broad, it is secondary such as supercritical drying
Critical drying, critical point drying, vacuum drying, freeze-drying and atmosphere pressure desiccation etc..However, currently, traditional fibre element water
The aeroge of the freezing mode preparation of solution is presented isotropic morphosis, and pore opening is uniformly and pore size phase
Deng, this aeroge not only has strong structure both shrinks feature, and isotropic mechanical property keeps its brittleness big, rigidity
Difference.Currently, the report of anisotropic fiber element base aeroge is prepared using gradient freezing mode not yet.This method operation letter
Single, high-efficient, there are no pollution to the environment, prepared anisotropic fiber element base aeroge, can be applied to acoustic material, prevents
UV materials, solar battery etc. have high value added product or industry.
Summary of the invention
It is an object of the invention to propose a kind of preparation method of anisotropic fiber element base aeroge, its object is to make
The standby cellulose base aeroge with anisotropic structure, realizes its value added applications.The present invention using cellulose as raw material,
Using gradient freezing mode, the cellulose base aeroge with anisotropic structure is prepared.
The purpose of the present invention is what is be achieved through the following technical solutions:
(1) it takes a certain amount of cellulose stirred evenly or cellulose base aqueous solution is raw material.
(2) cellulose or cellulose base aqueous solution are added in plastics grinding tool.
(3) the plastics grinding tool equipped with cellulose or cellulose base aqueous solution is placed on metal heat-conduction bar, metal heat-conducting
Stick is placed in liquid nitrogen container.
(4) a certain amount of liquid nitrogen is added in liquid nitrogen container, until making the cellulose freeze forming in grinding tool.
(5) the cellulose grinding tool freezed is put into drying equipment, dry a period of time.
(6) demoulding obtains anisotropic fiber element base aeroge after drying.
The present invention has the advantage that cellulosic material source used by 1) this method is wide compared with prior art
It is general, it include lignocellulosic, the preparation method of herbaceous plant cellulose, bamboo cellulose, bacteria cellulose etc., cellulose is more
Sample, including Mechanical Method, chemical method, bioanalysis.2) cellulose base aqueous solution range is wide, including cellulose/inorganic nano-particle is multiple
Heshui solution, cellulose/graphene compound aqueous solution, cellulose/carbon nano compound aqueous solution, grafting modification cellulose
Aqueous solution.3) anisotropic structure is presented in the cellulose base aeroge prepared, and temperature gradient guides equipment simple, without freezing
Rate monitoring, cellulose is at anisotropic regular lamellar structure.4) anisotropic fiber element base aeroge prepared by the present invention
Size can be controlled by the size of plastics grinding tool and metal heat-conduction bar.5) this method is easy to operate, quickly, high-efficient, right
Environmental nonpollution is a kind of environmentally protective preparation method.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) photograph on cellulose base aeroge vertical direction.
Fig. 2 is the Micro-CT scanning figure of cellulose base aeroge.
Specific embodiment
Advantages of the present invention and other details, but the specific material quoted in embodiment are further illustrated in the examples below
Material and dosage and other conditions should not be regarded as having carried out inappropriate limitation to the present invention.
Embodiment 1
(1) taking the TEMPO oxycellulose aqueous solution that 20mL concentration is 0.3% is raw material.
(2) cellulose aqueous solution is added in the cylinder-shaped vinyon grinding tool that diameter is 2cm.
(3) the plastics grinding tool equipped with cellulose aqueous solution is placed on copper heat conductive rod, copper heat conductive rod is placed on liquid nitrogen appearance
In device.
(4) enough liquid nitrogen are added in liquid nitrogen container, until making the cellulose freeze forming in grinding tool.
(5) the cellulose grinding tool freezed is put into freeze drier, it is 2 days dry.
(6) demoulding obtains the cellulose base aeroge of anisotropic structure after drying.
Embodiment 2
(1) taking the mechanical lapping cellulose aqueous solution that 50mL concentration is 0.5% is raw material.
(2) cellulose aqueous solution is added in the cuboid acrylic plastics grinding tool that bottom surface is 5 × 5cm.
(3) the plastics grinding tool equipped with cellulose aqueous solution is placed on iron heat conductive rod, iron heat conductive rod is placed on liquid nitrogen appearance
In device.
(4) enough liquid nitrogen are added in liquid nitrogen container, until making the cellulose freeze forming in grinding tool.
(5) the cellulose grinding tool freezed is put into supercritical dryer, it is 3 days dry.
(6) demoulding obtains the cellulose base aeroge of anisotropic structure after drying.
Embodiment 3
(1) taking cellulose/hydroxyethyl meth acrylate aqueous solution that 50mL concentration is 1% is raw material, cellulose and ethoxy first
The mass ratio of base acrylate is 8:1.
(2) cellulose aqueous solution is added in the cuboid polycarbonate plastic grinding tool that bottom surface is 3 × 5cm.
(3) the plastics grinding tool equipped with cellulose aqueous solution is placed on alloy heat conductive rod, alloy heat conductive rod is placed on liquid
In nitrogen cascade.
(4) enough liquid nitrogen are added in liquid nitrogen container, until making the cellulose freeze forming in grinding tool.
(5) the cellulose grinding tool freezed is put into freeze drier, it is 3 days dry.
(6) demoulding obtains the cellulose base aeroge of anisotropic structure after drying.
Embodiment 4
(1) taking the enzymatic treatment cellulose aqueous solution that 50mL concentration is 0.8% is raw material.
(2) cellulose aqueous solution is added in the cylinder-shaped polytetrafluoroethylplastic plastic grinding tool that diameter is 8cm.
(3) the plastics grinding tool equipped with cellulose aqueous solution is placed on alloy heat conductive rod, alloy heat conductive rod is placed on liquid
In nitrogen cascade.
(4) enough liquid nitrogen are added in liquid nitrogen container, until making the cellulose freeze forming in grinding tool.
(5) the cellulose grinding tool freezed is put into freeze drier, it is 3 days dry.
(6) demoulding obtains the cellulose base aeroge of anisotropic structure after drying.
Embodiment 5
(1) taking cellulose/graphene mixed aqueous solution that 25mL concentration is 0.1% is raw material, cellulose/graphene mixing mixing
Mass ratio is 10:1.
(2) cellulose aqueous solution is added in the cylinder-shaped polypropylene grinding tool that diameter is 8cm.
(3) the plastics grinding tool equipped with cellulose aqueous solution is placed on copper heat conductive rod, alloy heat conductive rod is placed on liquid nitrogen
In container.
(4) enough liquid nitrogen are added in liquid nitrogen container, until making the cellulose freeze forming in grinding tool.
(5) the cellulose grinding tool freezed is put into freeze drier, it is 3 days dry.
(6) demoulding obtains the cellulose base aeroge of anisotropic structure after drying.
Claims (8)
1. a kind of preparation method of anisotropic fiber element base aeroge, it is characterised in that: the following steps are included:
Raw material: using the cellulose or cellulose base aqueous solution stirred evenly as raw material；
Modes of emplacement: cellulose or cellulose base aqueous solution are added in plastics grinding tool；
Freezing mode: the plastics grinding tool equipped with cellulose or cellulose base aqueous solution is placed on metal heat-conduction bar, metal is led
Hot pin is placed in liquid nitrogen container, and a certain amount of liquid nitrogen is added in liquid nitrogen container, until making the cellulose base solution in grinding tool
Freeze forming；
Be dried: the cellulose grinding tool freezed be put into drying equipment, after dry a period of time demoulding obtain it is each to
The cellulose aerogels of anisotropic approach.
2. a kind of preparation method of anisotropic fiber element base aeroge as described in claim 1, it is characterised in that: step
(1) cellulosic material is lignocellulosic, plant cellulose, bacteria cellulose.
3. a kind of preparation method of anisotropic fiber element base aeroge as described in claim 1, it is characterised in that: step
(1) cellulosic material is the cellulose of TEMPO oxidation preparation, Mechanical Method preparation, enzymatic isolation method preparation, supercritical ultrasonics technology preparation.
4. a kind of preparation method of anisotropic fiber element base aeroge as described in claim 1, it is characterised in that: step
(1) the cellulose base aqueous solution be cellulose/inorganic nano-particle compound aqueous solution, cellulose/graphene compound aqueous solution,
Cellulose/carbon nano compound aqueous solution, grafting modification cellulose aqueous solution, wherein solid content shared by cellulose be more than
50%。
5. a kind of preparation method of anisotropic fiber element base aeroge as described in claim 1, it is characterised in that: step
(1) total solid content is 0.05% ~ 1.5% in the cellulose or cellulose base aqueous solution.
6. a kind of preparation method of anisotropic fiber element base aeroge as described in claim 1, it is characterised in that: step
(1) the plastics grinding tool is low temperature resistant resin abrasive tools, preferably polytetrafluoroethylene, acrylic, polyethylene, polycarbonate, polypropylene.
7. a kind of preparation method of anisotropic fiber element base aeroge as described in claim 1, it is characterised in that: step
(1) metal heat-conduction bar is preferably copper rod, iron staff, aluminium bar, silver-colored stick, golden stick, zinc bar, alloy bar, cross-sectional width or diameter
Greater than grinding tool cross-sectional width or diameter.
8. a kind of preparation method of anisotropic fiber element base aeroge as described in claim 1, it is characterised in that: step
(1) drying equipment is preferably freeze drier, supercritical dryer, sub-critical drying machine, vacuum drier.
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| CN201810371493.8A CN110396214A (en) | 2018-04-24 | 2018-04-24 | A kind of preparation method of anisotropic fiber element base aeroge |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140079931A1 (en) * | 2011-03-25 | 2014-03-20 | Cellutech Ab | Cellulose-based materials comprising nanofibrillated cellulose from native cellulose |
| CN105315482A (en) * | 2015-12-02 | 2016-02-10 | 南京林业大学 | Anisotropic nano-cellulose/montmorillonite composite aerogel and preparation method thereof |
| CN107057107A (en) * | 2017-04-13 | 2017-08-18 | 昆明理工大学 | It is a kind of to be freeze-dried the method for preparing cellulose aerogels |
| CN107556495A (en) * | 2017-07-10 | 2018-01-09 | 南京林业大学 | A kind of preparation method of functional nano cellulose composite aerogel |
-
2018
- 2018-04-24 CN CN201810371493.8A patent/CN110396214A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140079931A1 (en) * | 2011-03-25 | 2014-03-20 | Cellutech Ab | Cellulose-based materials comprising nanofibrillated cellulose from native cellulose |
| CN105315482A (en) * | 2015-12-02 | 2016-02-10 | 南京林业大学 | Anisotropic nano-cellulose/montmorillonite composite aerogel and preparation method thereof |
| CN107057107A (en) * | 2017-04-13 | 2017-08-18 | 昆明理工大学 | It is a kind of to be freeze-dried the method for preparing cellulose aerogels |
| CN107556495A (en) * | 2017-07-10 | 2018-01-09 | 南京林业大学 | A kind of preparation method of functional nano cellulose composite aerogel |
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Application publication date: 20191101 |