CN110724301A - Method for preparing cellulose-based aerogel in bidirectional gradient manner - Google Patents
Method for preparing cellulose-based aerogel in bidirectional gradient manner Download PDFInfo
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- 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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- 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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- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
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- C08J2301/04—Oxycellulose; Hydrocellulose
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
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Abstract
The invention discloses a method for preparing cellulose-based aerogel in a bidirectional gradient manner, and aims to prepare the cellulose-based aerogel with a honeycomb structure and realize high-added-value application of the cellulose-based aerogel. The method is characterized by comprising the following steps: 1) manufacturing a heat insulation wedge-shaped body, placing the heat insulation wedge-shaped body at the bottom of a plastic mold, placing the mold on a metal heat conducting rod, and placing the metal heat conducting rod in a liquid nitrogen container; 2) adding cellulose or cellulose-based aqueous solution into a mold; 3) adding liquid nitrogen into the container to freeze and mold the solution; 4) drying and demoulding. The cellulose aerogel prepared by the invention has wide application prospects in the aspects of material adsorption, heat insulation protection, drug carriers and the like.
Description
Technical Field
The invention relates to a method for preparing cellulose-based aerogel in a bidirectional gradient manner, which is simple to operate, and the obtained cellulose-based aerogel belongs to the field of natural polymers, forestry engineering, packaging engineering and new materials.
Background
Compared with the traditional inorganic aerogel (such as silicon aerogel), the aerogel not only has a unique three-dimensional network structure, but also has low density, high porosity, high specific surface area, excellent heat resistance, high conductivity and mechanical stability. Currently, aerogels are widely used in various fields, for example, as gas adsorbents, catalyst carriers, oil-water separation materials, and the like. Therefore, exploring a preparation process which is economical, environment-friendly, simple in process and rich in raw materials becomes the research focus of the aerogel material.
Cellulose is the most common raw material for preparing aerogels, and is widely found in plants and their processed products, marine organisms, bacteria, and the like. The plants and processed products thereof are most abundant in sources, and comprise bamboo, wood, cotton, straws, straw pulp, fruits and vegetables, waste newspapers and the like. The mechanical property of the lignocellulose is excellent; the purity of cotton cellulose is highest; the fruit and vegetable cellulose has wide source, and the fiber form is slightly inferior to wood and bamboo, but slightly stronger than wheat straw and other fibers. Other biomass cellulose also includes animal cellulose (such as knapsack animal), bacterial cellulose (such as Acetobacter xylinum), and marine biological cellulose (such as sea squirt cellulose and seaweed). The bacterial cellulose has the most uniform structure and has the characteristics of good biocompatibility, shape memory capability, high crystallinity, good air permeability, tensile strength and the like; the marine biological cellulose has larger length-diameter ratio, good toughness, excellent mechanical property, thermal stability, corrosion resistance and high crystallinity. Based on the extensive resource reserve and excellent properties of cellulose, it becomes an ideal raw material for preparing aerogels.
The research on the structure-activity relationship between the structure and the performance of the material becomes a popular research field, and the structure of the cellulose-based aerogel has an important influence on the application of the cellulose-based aerogel. At present, the existing methods for preparing aerogels are mainly freeze-drying methods, wherein the freezing mode comprises uniform refrigerator freezing or liquid nitrogen freezing, and the drying process mainly comprises vacuum drying, critical point drying, atmospheric pressure drying and the like. However, most of the current preparation methods make the aerogel present an isotropic morphological structure, and even if a unidirectional gradient freezing preparation method is adopted, the obtained aerogel presents an anisotropic structural feature, but the cross section still maintains an isotropic structure, which is not favorable for elastic recovery of the aerogel after compression. At present, no report is available for preparing the cellular cellulose-based aerogel by adopting a bidirectional gradient freezing mode. The method is simple to operate and environment-friendly, and the prepared honeycomb cellulose-based aerogel can be applied to industries with high added values, such as energy storage, sound insulation, adsorption and the like.
Disclosure of Invention
The invention aims to provide a method for preparing cellulose-based aerogel in a bidirectional gradient manner, and aims to prepare the cellulose-based aerogel with a honeycomb structure and realize high value-added application of the cellulose-based aerogel. The invention takes cellulose as a raw material and adopts a bidirectional gradient freezing mode to prepare the cellulose-based aerogel with a three-dimensional anisotropic structure.
The purpose of the invention is realized by the following technical scheme:
(1) the heat insulation wedge is manufactured and placed at the bottom of the plastic mold, the plastic mold is placed on the metal heat conduction rod, and the metal heat conduction rod is placed in the liquid nitrogen container.
(2) Taking a certain amount of uniformly stirred cellulose or cellulose base aqueous solution as a raw material, and adding the raw material into a plastic mould.
(3) And adding a certain amount of liquid nitrogen into the liquid nitrogen container until the cellulose or cellulose-based aqueous solution in the mold is frozen and molded.
(4) And putting the frozen cellulose solid block and the mould into drying equipment, and drying for a period of time.
(5) And (4) demolding after drying to obtain the regular honeycomb structure cellulose-based aerogel.
Compared with the prior art, the invention has the following advantages: 1) the cellulose raw material adopted by the method has wide sources, and comprises plants and processed products thereof, marine organisms, bacteria and the like. The cellulose can be prepared by various methods including chemical method, mechanical method and biological method. 2) The cellulose/cellulose-based aqueous solution has a wide range and comprises a pure cellulose aqueous solution, a chemical grafting modified cellulose aqueous solution, a cellulose/graphene composite aqueous solution, a cellulose/carbon nano tube composite aqueous solution, a cellulose/inorganic nano particle composite aqueous solution and the like. 3) The prepared cellulose-based aerogel has anisotropy on a three-dimensional structure, the temperature gradient guiding equipment is simple, the freezing rate is not required to be monitored, and the aerogel is in a regular honeycomb structure. 4) The cellulose-based aerogel prepared by the method is controllable in size, and the size of the aerogel can be adjusted by controlling the sizes of the plastic mold, the wedge-shaped body and the metal heat conducting rod.
Drawings
FIG. 1 is a schematic diagram of bi-directional gradient freezing.
FIG. 2 is a scanning electron microscope image of cellulose-based aerogel prepared by different freezing methods.
Detailed Description
Advantages and other details of this invention are further illustrated in the following examples, but the particular materials and amounts thereof recited in the examples, as well as other conditions, should not be construed to unduly limit this invention.
Example 1:
(1) manufacturing a cylindrical polydimethylsiloxane wedge-shaped body with the diameter of 2cm and the inclination angle of 15 degrees, placing the cylindrical polydimethylsiloxane wedge-shaped body at the bottom of a polyethylene plastic mold, placing the plastic mold on a copper heat conducting rod, and placing the copper heat conducting rod in a liquid nitrogen container.
(2) 20mL of a 0.3% strength, stirred aqueous TEMPO-oxidized cellulose solution are taken and introduced into a plastic mould.
(3) Sufficient liquid nitrogen is added to the liquid nitrogen container until the cellulose in the mold is freeze-formed.
(4) And putting the frozen cellulose solid block and the mould into a freeze dryer, and drying for 2 days.
(5) And (4) demoulding after drying to obtain the regular cellular structure cellulose aerogel.
Example 2:
(1) the method comprises the steps of manufacturing a rectangular polyethylene wedge-shaped body with the length and the width of 5 multiplied by 5 cm and the inclination angle of 30 degrees, placing the rectangular polyethylene wedge-shaped body at the bottom of an acrylic plastic mold, placing the plastic mold on an iron heat conducting rod, and placing the iron heat conducting rod in a liquid nitrogen container.
(2) 50mL of a 0.5% mechanically ground aqueous solution of cellulose stirred uniformly was added to a plastic mold.
(3) Sufficient liquid nitrogen is added to the liquid nitrogen container until the cellulose in the mold is freeze-formed.
(4) And putting the frozen cellulose solid block and the mould into a supercritical dryer, and drying for 3 days.
(5) And (4) demoulding after drying to obtain the regular cellular structure cellulose aerogel.
Example 3:
(1) the method comprises the steps of manufacturing a rectangular foam wedge-shaped body with the length and the width of 3 multiplied by 5 cm and the inclination angle of 20 degrees, placing the rectangular foam wedge-shaped body at the bottom of a polycarbonate plastic mold, placing the plastic mold on an alloy heat conducting rod, and placing the alloy heat conducting rod in a liquid nitrogen container.
(2) 50mL of cellulose/hydroxyethyl methacrylate aqueous solution with the concentration of 1% and the mass ratio of the cellulose to the hydroxyethyl methacrylate of 8:1 are taken and added into a plastic mold.
(3) Sufficient liquid nitrogen is added to the liquid nitrogen container until the cellulose in the mold is freeze-formed.
(4) And putting the frozen cellulose solid block and the mould into a freeze dryer, and drying for 3 days.
(5) And (4) demoulding after drying to obtain the cellulose-based aerogel with a regular honeycomb structure.
Example 4:
(1) manufacturing a square vacuum plate wedge-shaped body with the length and width of 8 multiplied by 8cm and the inclination angle of 40 degrees, placing the square vacuum plate wedge-shaped body at the bottom of a polytetrafluoroethylene plastic mold, placing the plastic mold on an alloy heat conducting rod, and placing the alloy heat conducting rod in a liquid nitrogen container.
(2) 50mL of enzyme-treated cellulose/titanium dioxide nanoparticle composite aqueous solution which is uniformly stirred and has the concentration of 0.8 percent is taken as a raw material, the mixing mass ratio of the cellulose/titanium dioxide nanoparticles is 10:1, and the raw material is added into a plastic mould.
(3) Sufficient liquid nitrogen is added to the liquid nitrogen container until the cellulose in the mold is freeze-formed.
(4) And putting the frozen cellulose solid block and the mould into a freeze dryer, and drying for 3 days.
(5) And (4) demoulding after drying to obtain the cellulose-based aerogel with a regular honeycomb structure.
Example 5:
(1) the cylindrical plastic wedge-shaped body with the diameter of 8cm and the inclination angle of 10 degrees is manufactured and placed at the bottom of the polypropylene plastic mold, the plastic mold is placed on the copper heat conducting rod, and the copper heat conducting rod is placed in the liquid nitrogen container.
(2) Taking 25mL of silane modified cellulose aqueous solution which is uniformly stirred and has the concentration of 0.1 percent as a raw material, adding the cellulose/silane mixed solution into a plastic mould, wherein the mass ratio of the cellulose/silane mixed solution is 9: 1.
(3) Sufficient liquid nitrogen is added to the liquid nitrogen container until the cellulose in the mold is freeze-formed.
(4) And putting the frozen cellulose solid block and the mould into a freeze dryer, and drying for 3 days.
(5) And (4) demoulding after drying to obtain the cellulose-based aerogel with a regular honeycomb structure.
Claims (8)
1. A method for preparing cellulose-based aerogel in a bidirectional gradient is characterized by comprising the following steps: the method comprises the following steps: manufacturing a heat insulation wedge-shaped body and placing the heat insulation wedge-shaped body at the bottom of a plastic mould, placing the plastic mould on a metal heat conducting rod, and placing the metal heat conducting rod in a liquid nitrogen container; taking a certain amount of uniformly stirred cellulose or cellulose-based aqueous solution as a raw material, and adding the raw material into a plastic mould; adding a certain amount of liquid nitrogen into a liquid nitrogen container until the cellulose or cellulose-based aqueous solution in the mold is frozen and molded; putting the frozen cellulose solid block and the mould into drying equipment, and drying for a period of time; and (4) demolding after drying to obtain the regular honeycomb structure cellulose-based aerogel.
2. The method of preparing cellulose-based aerogel according to claim 1, wherein: the wedge body in the step (1) is made of a thermal insulation material or a low thermal conductivity material, and is preferably made of a high polymer material, a plastic, a porous material, a vacuum material and a traditional thermal insulation material, such as glass fiber, asbestos, rock wool, silicate and the like.
3. The method for preparing cellulose-based aerogel according to claim 1, wherein the wedge angle in step (1) is 1 ° ~ 80 °.
4. The method of preparing cellulose-based aerogel according to claim 1, wherein: the metal heat conducting rod in the step (1) is preferably a copper rod, an iron rod, an aluminum rod, a silver rod, a gold rod, a zinc rod or an alloy rod, and the width or the diameter of the section of the metal heat conducting rod is larger than that of the section of the mould.
5. The method of preparing cellulose-based aerogel according to claim 1, wherein: the plastic mould in the step (1) is a low temperature resistant resin mould, preferably polytetrafluoroethylene, acrylic, polyethylene, polycarbonate and polypropylene.
6. The method of preparing cellulose-based aerogel according to claim 1, wherein: the cellulose raw material in the step (2) is plant and processed product thereof, marine organism and bacteria, preferably bamboo, wood, cotton, straw pulp, fruits and vegetables, waste newspaper, animal cellulose, bacterial cellulose and marine organism cellulose.
7. The method of preparing cellulose-based aerogel according to claim 1, wherein: the cellulose-based aqueous solution in the step (2) is a chemical modified cellulose aqueous solution and a cellulose/other substance composite aqueous solution, and comprises a silane modified cellulose aqueous solution, a cross-linked modified cellulose aqueous solution, a graft modified cellulose aqueous solution, a cellulose/inorganic nanoparticle composite aqueous solution, a cellulose/graphene composite aqueous solution and a cellulose/carbon nanotube composite aqueous solution, wherein the cellulose in the composite solution accounts for more than 50% of solid content, and the cellulose comprises micron cellulose and nano cellulose.
8. The method for preparing cellulose-based aerogel according to claim 1, wherein the total solid content of the cellulose or cellulose-based aqueous solution in step (2) is 0.01% ~ 3.0.0%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325506A (en) * | 2018-01-17 | 2018-07-27 | 昆明理工大学 | A kind of preparation method of the modified cellulose aeroge of absorption heavy metal |
| CN111533944A (en) * | 2020-05-08 | 2020-08-14 | 中国科学院空间应用工程与技术中心 | Preparation method of polyimide nanofiber aerogel with controllable microstructure |
| CN112827435A (en) * | 2021-01-22 | 2021-05-25 | 南京信息工程大学 | Device for preparing ordered porous aerogel based on orientation freezing technology |
| CN113637234A (en) * | 2021-07-28 | 2021-11-12 | 江苏理工学院 | Elastic cellulose aerogel and preparation method and application thereof |
| CN114956036A (en) * | 2022-04-29 | 2022-08-30 | 天津科技大学 | Preparation method of super-elastic, super-light and high-compressibility nano-cellulose/aramid nano-fiber carbon aerogel, carbon aerogel and application |
| WO2024164088A1 (en) * | 2023-02-09 | 2024-08-15 | The University Of British Columbia | Aerogels assembled from microfibers, methods for their preparation and uses thereof |
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| CN105017555A (en) * | 2014-04-29 | 2015-11-04 | 中国科学院化学研究所 | Cellulose aerogel and preparation method for hybrid aerogel thereof |
| CN105315482A (en) * | 2015-12-02 | 2016-02-10 | 南京林业大学 | Anisotropic nano-cellulose/montmorillonite composite aerogel and preparation method thereof |
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2018
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20140079931A1 (en) * | 2011-03-25 | 2014-03-20 | Cellutech Ab | Cellulose-based materials comprising nanofibrillated cellulose from native cellulose |
| CN103790248A (en) * | 2014-01-27 | 2014-05-14 | 钟春燕 | Method for preparing building thermal insulation heat-resisting board |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325506A (en) * | 2018-01-17 | 2018-07-27 | 昆明理工大学 | A kind of preparation method of the modified cellulose aeroge of absorption heavy metal |
| CN108325506B (en) * | 2018-01-17 | 2020-08-25 | 昆明理工大学 | Preparation method of modified cellulose aerogel for adsorbing heavy metals |
| CN111533944A (en) * | 2020-05-08 | 2020-08-14 | 中国科学院空间应用工程与技术中心 | Preparation method of polyimide nanofiber aerogel with controllable microstructure |
| CN111533944B (en) * | 2020-05-08 | 2021-10-22 | 中国科学院空间应用工程与技术中心 | Preparation method of polyimide nanofiber aerogel with controllable microstructure |
| CN112827435A (en) * | 2021-01-22 | 2021-05-25 | 南京信息工程大学 | Device for preparing ordered porous aerogel based on orientation freezing technology |
| CN113637234A (en) * | 2021-07-28 | 2021-11-12 | 江苏理工学院 | Elastic cellulose aerogel and preparation method and application thereof |
| CN113637234B (en) * | 2021-07-28 | 2023-03-17 | 江苏理工学院 | Elastic cellulose aerogel and preparation method and application thereof |
| CN114956036A (en) * | 2022-04-29 | 2022-08-30 | 天津科技大学 | Preparation method of super-elastic, super-light and high-compressibility nano-cellulose/aramid nano-fiber carbon aerogel, carbon aerogel and application |
| CN114956036B (en) * | 2022-04-29 | 2023-12-22 | 天津科技大学 | Preparation method of nano cellulose/aramid nanofiber carbon aerogel with super elasticity, super light weight and high compressibility, carbon aerogel and application |
| WO2024164088A1 (en) * | 2023-02-09 | 2024-08-15 | The University Of British Columbia | Aerogels assembled from microfibers, methods for their preparation and uses thereof |
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