CN111849019A - Preparation method of cellulose composite aerogel - Google Patents
Preparation method of cellulose composite aerogel Download PDFInfo
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- CN111849019A CN111849019A CN202010756753.0A CN202010756753A CN111849019A CN 111849019 A CN111849019 A CN 111849019A CN 202010756753 A CN202010756753 A CN 202010756753A CN 111849019 A CN111849019 A CN 111849019A
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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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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- 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
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
- C08J2201/0502—Elimination by evaporation or heat degradation of a liquid phase the liquid phase being organic
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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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- C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2351/02—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to polysaccharides
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Abstract
The invention discloses a preparation method of cellulose composite aerogel, which comprises the following steps: (1) preparing a cellulose solution; (2) sequentially adding N, N-methylene bisacrylamide and dopamine hydrochloride into a cellulose solution, and putting the mixture into an oven for reaction to prepare cellulose composite hydrogel; (3) and carrying out primary freeze drying, solvent replacement and secondary freeze drying on the cellulose composite hydrogel to obtain the cellulose composite aerogel. The cellulose composite aerogel prepared by the preparation method has the advantages of good structural stability, impact resistance, simple and controllable preparation method, small pollution and low cost.
Description
Technical Field
The invention relates to a preparation method of an aerogel, and more particularly relates to a preparation method of a cellulose composite aerogel.
Background
The aerogel material has wide application prospect in a plurality of fields such as building energy conservation, new energy, chemical engineering, aerospace and the like, the traditional aerogel is inorganic aerogel represented by silicon dioxide, and the application of the traditional aerogel is limited due to the defects of low strength, poor toughness, easiness in crushing and the like; the organic aerogel represented by resorcinol/formaldehyde and melamine/formaldehyde polycondensate which is developed later has the defect of poor thermal stability, and the cellulose aerogel derived from the development of natural material cellulose has the characteristics of a traditional aerogel nano porous structure, has the advantages of greenness, reproducibility, good biocompatibility, good toughness, easiness in processing and the like, and has wide application prospects in the fields of adsorption, medical pharmacy, electromagnetic shielding and the like. The cellulose aerogel has the properties of light weight, low density, large specific surface area and the like, and lays the application foundation of the cellulose aerogel in flexible devices or soft materials. In order to exert the mechanical properties and characteristics of the cellulose aerogel, the properties of the cellulose aerogel are often improved by modification, for example, the compression resilience of the cellulose aerogel is improved by high-temperature carbonization, the mechanical properties of the cellulose aerogel are improved by compounding rice materials, or the structural stability and the mechanical properties of the cellulose aerogel are improved by chemical modification or grafting, but the compression resistance of the cellulose aerogel can be improved only to a certain extent by the above method, the texture of the cellulose aerogel still presents a soft state, and the cellulose aerogel still can be damaged or deformed when the cellulose aerogel is impacted by external force, so that the properties or the attractiveness of the cellulose aerogel are influenced.
From the above, it is concluded that the excellent properties of the cellulose aerogel come from low density, large porosity and high specific surface area, but this also results in soft quality, low mechanical strength, weak impact resistance, and easy collapse under load, so that the practical application is greatly limited by the environment or the field. In order to improve the impact resistance and the structural stability of the cellulose aerogel, the invention provides the characteristic that the N, N-methylene bisacrylamide polymer is crosslinked and combined with dopamine hydrochloride oxidative autopolymerization, and simultaneously, the internal microstructure of the aerogel is adjusted by two times of freeze drying, so that the cellulose composite aerogel has good structural stability and larger impact resistance.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method of cellulose composite aerogel with good structural stability and good impact resistance.
The technical scheme is as follows: the preparation method of the cellulose composite aerogel comprises the following steps:
(1) preparing a cellulose solution;
(2) sequentially adding N, N-methylene bisacrylamide and dopamine hydrochloride into a cellulose solution, and putting the mixture into an oven for reaction to prepare cellulose composite hydrogel;
(3) and carrying out primary freeze drying, solvent replacement and secondary freeze drying on the cellulose composite hydrogel to obtain the cellulose composite aerogel.
Wherein the step 1 of preparing the cellulose solution comprises the following steps:
(11) mixing sodium hydroxide, urea and water uniformly;
(12) cooling the mixed solution to-10 to-15 ℃;
(13) and adding microcrystalline cellulose into the mixed solution, and stirring until the microcrystalline cellulose is completely dissolved to obtain a cellulose solution.
Wherein the mass ratio of the sodium hydroxide to the urea to the water in the step 11 is 7-8: 11-12: 81, in the step 13, the particle size of the microcrystalline cellulose is 50 +/-10 mu m, and the concentration of the obtained cellulose solution is 2-4 wt%.
In the step 2, after N, N-methylene bisacrylamide is completely dissolved in the cellulose solution, dopamine hydrochloride is added, and the mass ratio of the N, N-methylene bisacrylamide to the cellulose is 2: 0.1-0.8, wherein the mass ratio of dopamine hydrochloride to cellulose is 2: 0.1-0.5, and the temperature of the oven is 60-100 ℃; and 3, firstly freezing for 5-8 h during primary freeze drying, then drying for 12-16 h in a freeze dryer, carrying out solvent replacement by using a tert-butyl alcohol aqueous solution during solvent replacement, firstly washing and removing impurities by using water and an ethanol solution during solvent replacement, firstly freezing for 5-8 h during secondary freeze, and then drying for 12-16 h in the freeze dryer.
The synthesis principle is as follows: the method utilizes the mutual crosslinking of cellulose and N, N-methylene bisacrylamide and the characteristic of oxidative self-polymerization of dopamine hydrochloride, and simultaneously adjusts the internal microstructure of the aerogel by two times of freeze drying, so that the cellulose composite aerogel has good structural stability and larger shock resistance, a relatively stable three-dimensional structure is formed by the primary freeze drying, the internal three-dimensional microstructure of the aerogel is further adjusted under the action of ice crystal growth during the secondary freeze drying, and in addition, the tertiary butanol is used as a replacement solvent, so that the pore characteristics of the aerogel can be kept as far as possible. And finally, freeze drying to obtain the final cellulose composite aerogel.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: 1. the prepared cellulose composite aerogel has good structural stability and impact resistance; 2. the preparation method is simple and controllable, and has little pollution and low cost.
Drawings
FIG. 1 is a graph of an impact test of the present invention;
FIG. 2 is a stress-strain graph of example 1;
fig. 3 is a stress-strain graph of example 2.
Detailed Description
Example 1
(1) Uniformly mixing 7g of sodium hydroxide, 12g of urea and 81g of water, cooling to-12 ℃, and completely dissolving 4g of microcrystalline cellulose in a sodium hydroxide-urea-water solution on a magnetic stirrer to obtain a 4 wt% cellulose solution, wherein the particle size of the microcrystalline cellulose is 50 microns;
(2) taking 50g of cellulose solution, adding 0.6g of N, N-Methylene Bisacrylamide (MBA) into a beaker, stirring for 3 hours until the N, N-Methylene Bisacrylamide (MBA) is completely dissolved, and then adding a solvent according to a mass ratio of 2: 0.2, adding 0.2g of dopamine DA hydrochloride, continuously stirring for 12h, subpackaging 5ml of each mixed solution into 10ml of beakers, sealing, and placing in a 90 ℃ oven for reaction for 12h to obtain the cellulose composite hydrogel;
(3) freezing the cellulose composite hydrogel at-15 ℃ for 5h, then drying in a dryer for 12h to obtain primary cellulose composite aerogel, washing the primary cellulose aerogel by using an ethanol solution and deionized water in sequence to remove impurities, then performing solvent replacement by using a tert-butyl alcohol aqueous solution, freezing at-15 ℃ for 5h, and drying in the dryer for 12h to obtain the cellulose composite aerogel.
Example 2
The difference between this example and example 1 is: in the preparation of the cellulose composite hydrogel, 40g of a cellulose solution, 0.4g of N, N-methylenebisacrylamide MBA and 0.1g of dopamine DA hydrochloride were used, and the oven temperature was 60 ℃.
Example 3
(1) Uniformly mixing 7g of sodium hydroxide, 12g of urea and 81g of water, cooling to-12 ℃, and completely dissolving 2g of microcrystalline cellulose in a sodium hydroxide-urea-water solution on a magnetic stirrer to obtain a 2 wt% cellulose solution, wherein the grain diameter of the microcrystalline cellulose is 40 mu m;
(2) taking 50g of cellulose solution, adding 0.3g of N, N-Methylene Bisacrylamide (MBA), stirring for 2 hours until the N, N-Methylene Bisacrylamide (MBA) is completely dissolved, then adding 0.15g of dopamine hydrochloride (DA), continuously stirring for 12 hours, subpackaging 5ml of mixed solution into 10ml of beakers, sealing, and placing in a 100 ℃ oven for reaction for 12 hours to obtain cellulose composite hydrogel;
(3) freezing the cellulose composite hydrogel at-15 ℃ for 5h, then drying in a dryer for 12h to obtain primary cellulose composite aerogel, washing the primary cellulose aerogel by using an ethanol solution and deionized water in sequence to remove impurities, then performing solvent replacement by using a tert-butyl alcohol aqueous solution, freezing at-15 ℃ for 5h, and drying in the dryer for 12h to obtain the cellulose composite aerogel.
Example 4
(1) Uniformly mixing 7g of sodium hydroxide, 12g of urea and 81g of water, cooling to-12 ℃, and completely dissolving 3g of microcrystalline cellulose in a sodium hydroxide-urea-water solution on a magnetic stirrer to obtain a 3 wt% cellulose solution, wherein the grain diameter of the microcrystalline cellulose is 60 mu m;
(2) putting 40g of cellulose solution into a beaker, adding 0.24g of N, N-Methylene Bisacrylamide (MBA), stirring for 2 hours until the N, N-Methylene Bisacrylamide (MBA) is completely dissolved, then adding 0.1g of dopamine hydrochloride (DA), continuously stirring for 10 hours, subpackaging 5ml of mixed solution into 10ml of beakers, sealing, and placing in an oven at 80 ℃ for reaction for 12 hours to obtain cellulose composite hydrogel;
(3) freezing the cellulose composite hydrogel at-15 ℃ for 5h, then drying in a dryer for 12h to obtain primary cellulose composite aerogel, washing the primary cellulose aerogel by using an ethanol solution and deionized water in sequence to remove impurities, then performing solvent replacement by using a tert-butyl alcohol aqueous solution, freezing at-15 ℃ for 5h, and drying in the dryer for 12h to obtain the cellulose composite aerogel.
Comparative example 1
(1) Uniformly mixing 7g of sodium hydroxide, 12g of urea and 81g of water, cooling to-12 ℃, and completely dissolving 4g of microcrystalline cellulose in a sodium hydroxide-urea-water solution on a magnetic stirrer to obtain a 4 wt% cellulose solution;
(2) taking 50g of cellulose solution, subpackaging 5ml of the cellulose solution into 10ml of beakers, sealing, and placing the beakers in a 90 ℃ oven for reaction for 12 hours to obtain cellulose hydrogel;
(3) freezing cellulose hydrogel at-15 ℃ for 5h, then drying in a dryer for 12h to obtain primary cellulose composite aerogel, washing the primary cellulose aerogel by using ethanol solution and deionized water in sequence to remove impurities, performing solvent replacement by using tert-butyl alcohol aqueous solution, freezing at-15 ℃ for 5h, and drying in the dryer for 12h to obtain the cellulose aerogel.
And (3) test results: the cellulose aerogel without MBA and DA has soft texture, can change the shape of the aerogel by being squeezed by hands, and has poor structural stability and impact resistance
Comparative example 2
The differences between this comparative example and example 1 are: when the cellulose composite aerogel is prepared, the cellulose composite aerogel is frozen at the temperature of-15 ℃ for 5 hours and then dried in a drier for 12 hours, so that the cellulose composite aerogel is obtained. And (3) test results: the cellulose composite aerogel prepared without washing with a water/ethanol solution and replacement with a water/tert-butyl alcohol solvent has impurities on the surface falling off during transfer and compression, and has adverse effects on subsequent use.
As can be seen from fig. 1(a) and 1(b), the cellulose composite aerogel obtained in example 1 can maintain good structural stability under the pressure of 500g weight, and the cellulose composite aerogel is not deformed or damaged by the 20cm height free falling hit with 500g weight. From fig. 2 and fig. 3, it can be seen that the cellulose composite aerogel has a section of approximately linear stress curve in the strain range of 0-10%, which is an embodiment of the basic skeleton supporting force of the aerogel itself when the aerogel is just stressed, and then the gradual stress increase in the strain range of 10-60% is considered as the sliding friction force between fibers or sheets, the extrusion deformation of internal pores, and the like, which also results in slow stress increase; as the strain increases, the pores are substantially compacted and the pressure will act on the aerogel matrix, with a rapid rise in stress.
Claims (9)
1. The preparation method of the cellulose composite aerogel is characterized by comprising the following steps:
(1) preparing a cellulose solution;
(2) sequentially adding N, N-methylene bisacrylamide and dopamine hydrochloride into a cellulose solution, and putting the mixture into an oven for reaction to prepare cellulose composite hydrogel;
(3) and carrying out primary freeze drying, solvent replacement and secondary freeze drying on the cellulose composite hydrogel to obtain the cellulose composite aerogel.
2. The method for preparing cellulose composite aerogel according to claim 1, wherein the step 1 of preparing cellulose solution comprises the following steps:
(11) mixing sodium hydroxide, urea and water uniformly;
(12) cooling the mixed solution to-10 to-15 ℃;
(13) and adding microcrystalline cellulose into the mixed solution, and stirring until the microcrystalline cellulose is completely dissolved to obtain a cellulose solution.
3. The preparation method of the cellulose composite aerogel according to claim 2, wherein the mass ratio of sodium hydroxide, urea and water in the step 11 is 7-8: 11-12: 81, in the step 13, the particle size of the microcrystalline cellulose is 50 +/-10 mu m, and the concentration of the obtained cellulose solution is 2-4 wt%.
4. The preparation method of the cellulose composite aerogel according to claim 1, wherein in the step 2, dopamine hydrochloride is added after N, N-methylene-bis-acrylamide is completely dissolved in the cellulose solution, and the mass ratio of N, N-methylene-bis-acrylamide to cellulose is 2: 0.1-0.8, wherein the mass ratio of dopamine hydrochloride to cellulose is 2: 0.1 to 0.5.
5. The preparation method of the cellulose composite aerogel according to claim 1, wherein the temperature of the oven in the step 2 is 60-100 ℃.
6. The preparation method of the cellulose composite aerogel according to claim 1, wherein the primary freeze drying in the step 3 is performed for 5-8 hours, and then the primary freeze drying is performed for 12-16 hours in a freeze dryer.
7. The method for preparing cellulose composite aerogel according to claim 1, wherein the solvent substitution in step 3 is performed using an aqueous solution of t-butanol.
8. The method for preparing the cellulose composite aerogel according to claim 1 or 7, wherein the solvent replacement in the step 3 is performed by washing with water and ethanol solution to remove impurities.
9. The preparation method of the cellulose composite aerogel according to claim 1 or 7, wherein the secondary freezing in the step 3 is performed for 5-8 hours, and then the secondary freezing is performed for 12-16 hours in a freeze dryer.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113637234A (en) * | 2021-07-28 | 2021-11-12 | 江苏理工学院 | Elastic cellulose aerogel and preparation method and application thereof |
| CN114805909A (en) * | 2022-06-10 | 2022-07-29 | 中山大学 | Application of acrylamide in preparation of aerogel |
| CN115403823A (en) * | 2022-10-09 | 2022-11-29 | 西北大学 | Preparation method of plant cellulose aerogel with bionic structure, high compression resistance and high heat insulation performance |
| CN115466436A (en) * | 2022-09-05 | 2022-12-13 | 西南大学 | Intermediate layer heat insulation material for fresh fruit and vegetable express insulation box and insulation box |
| CN115558152A (en) * | 2022-10-14 | 2023-01-03 | 南京农业大学 | Dual-drying degradable nano-cellulose composite antibacterial aerogel and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113637234A (en) * | 2021-07-28 | 2021-11-12 | 江苏理工学院 | Elastic cellulose aerogel and preparation method and application thereof |
| CN114805909A (en) * | 2022-06-10 | 2022-07-29 | 中山大学 | Application of acrylamide in preparation of aerogel |
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| CN115466436A (en) * | 2022-09-05 | 2022-12-13 | 西南大学 | Intermediate layer heat insulation material for fresh fruit and vegetable express insulation box and insulation box |
| CN115466436B (en) * | 2022-09-05 | 2023-10-31 | 西南大学 | Intermediate layer heat preservation material for fresh fruit and vegetable express delivery heat preservation box and heat preservation box |
| CN115403823A (en) * | 2022-10-09 | 2022-11-29 | 西北大学 | Preparation method of plant cellulose aerogel with bionic structure, high compression resistance and high heat insulation performance |
| CN115558152A (en) * | 2022-10-14 | 2023-01-03 | 南京农业大学 | Dual-drying degradable nano-cellulose composite antibacterial aerogel and preparation method and application thereof |
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