CN110479218B - Method for preparing super-hydrophobic super-oleophylic aerogel material by taking nano-cellulose and nano-particles as raw materials - Google Patents
Method for preparing super-hydrophobic super-oleophylic aerogel material by taking nano-cellulose and nano-particles as raw materials Download PDFInfo
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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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Abstract
A method for preparing a super-hydrophobic super-oleophylic aerogel material by taking nano-cellulose and nano-particles as raw materials relates to a method for preparing a super-hydrophobic super-oleophylic aerogel material. The invention solves the problems that the prior nano-cellulose aerogel uses fluorine-containing toxic modifier and volatile organic solvent in the preparation process, and needs specific equipment and complex process. The preparation method comprises the following steps: 1. preparing a modified nano-cellulose solution; 2. preparing a modified silicon dioxide solution; 3. mixing; 4. pre-cooling; 5. and (5) freezing. The method is used for preparing the super-hydrophobic super-oleophylic aerogel material by taking the nano-cellulose and the nano-particles as raw materials.
Description
Technical Field
The invention relates to a method for preparing a super-hydrophobic and super-oleophylic aerogel material.
Background
Oil spills have created a significant economic and ecological burden. There are several rescue strategies for catastrophic oil leaks, such as filtration, mechanical extraction, chemical degradation, bioremediation, and adsorption materials. In these processes, the adsorbent materials stand out for their ease of handling, excellent oil capture capability and economic cost effectiveness. The adsorbing material can be used for large-scale petroleum leakage accidents, and has wide application prospect in chemical laboratories, production bases and even families. Nanocellulose-based aerogels have attracted attention for oil-water separation. Compared with other polymer aerogels, nanocellulose aerogels, which are abundant and sustainable to produce, have a greater value due to their environmental protection and biocompatibility. However, the inherent hydrophilicity of cellulose constitutes an obstacle to its use in oil-water separation. At present, various surface modification methods have been developed for preparing cellulose-based aerogels with special wettability, for example, chemical vapor deposition techniques are widely used in hydrophobic modification of cellulose-based aerogels, atomic layer deposition, sol-gel and cold plasma techniques are used for preparing nanocellulose aerogels with special wettability. These methods use fluorine-containing toxic modifiers and volatile organic solvents in the process, and require special equipment and complicated processes, making it difficult to prepare nano aerogel superhydrophobic aerogels on a large scale.
Disclosure of Invention
The invention provides a method for preparing a super-hydrophobic super-oleophylic aerogel material by taking nanocellulose and nanoparticles as raw materials, aiming at solving the problems that a fluorine-containing toxic modifier and a volatile organic solvent are used in the preparation process of the conventional nanocellulose aerogel, and specific equipment and a complex process are required.
A method for preparing a super-hydrophobic super-oleophylic aerogel material by taking nano-cellulose and nano-particles as raw materials comprises the following steps:
1. dispersing nano-cellulose into deionized water through a high-speed homogenizer under the condition that the rotating speed is 1000 r/min-100000 r/min, uniformly dispersing, adding gamma-aminopropyltriethoxysilane under the conditions of magnetic stirring at the rotating speed of 50 r/min-1000 r/min and the adding speed of 10 mL/h-20 mL/h, and then adding a fluorine-free modifier under the magnetic stirring at the rotating speed of 50 r/min-1000 r/min to obtain a modified nano-cellulose solution;
the volume ratio of the mass of the nano-cellulose to the deionized water is 1g (50-600) mL; the mass ratio of the nano-cellulose to the gamma-aminopropyl triethoxysilane is 1 (0.2-8); the mass ratio of the nano-cellulose to the fluorine-free modifier is 1 (0.33-1);
2. adding the nano particles into deionized water, then carrying out ultrasonic dispersion uniformly under the condition that the power is 800-1500W, and sequentially adding hexadecyl trimethoxy silane and 10-88 mass percent formic acid under the magnetic stirring at the rotating speed of 50-1000 r/min to obtain a modified silicon dioxide solution;
the volume ratio of the mass of the nano particles to the deionized water is 1g (15-800) mL; the mass ratio of the nano particles to the hexadecyl trimethoxy silane is 1 (0.22-15.6); the mass ratio of the nano particles to 10 to 88 mass percent of formic acid is 1 (0.5 to 8);
3. mixing the modified nano-cellulose solution and the modified silicon dioxide solution, carrying out ultrasonic treatment for 2-60 min under the condition that the power is 800-1500W, and then uniformly mixing under magnetic stirring at the rotating speed of 50-1000 r/min to obtain a mixed solution;
the volume ratio of the modified nano-cellulose solution to the modified silicon dioxide solution is 1 (0.5-5);
4. freezing the mixed solution for 2-12 h at-12-5 ℃ to obtain a pre-frozen solution;
5. and (3) placing the pre-frozen solution into a vacuum freeze dryer, and freezing for 2-12 h at the temperature of-50 ℃ to-5 ℃ to obtain the super-hydrophobic super-oleophylic aerogel material.
The beneficial effects of the invention are:
1. the nano-cellulose is used as a raw material, is a natural degradable biomass material, has abundant reserves and is environment-friendly.
2. The super-hydrophobic super-oleophylic aerogel material prepared by the invention has higher strength, can withstand the pressure of a 200g weight to keep a stable structure, and water drops can not stay on the surface of the aerogel in the contact angle test process, so that the aerogel has a good hydrophobic effect.
3. The hydrophobic super-oleophylic aerogel material prepared by the invention is used as a novel oil absorption material, has high adsorption speed, can reach adsorption balance in 10s, has large adsorption capacity, can reach 32.95g/g of maximum adsorption capacity of carbon tetrachloride and 13.01g/g of maximum adsorption capacity of n-hexane, is simple and environment-friendly, can be applied to the treatment of oily wastewater, can complete continuous and efficient separation of an oil-water mixture under the assistance of a suction pump, and has the pressure range of-0.01 MPa-0.02 MPa for the suction pump.
4. The super-hydrophobic nano cellulose aerogel prepared by the invention is prepared by taking water as an environment and modifying by adopting a fluorine-free modifier, meets the requirements of environmental protection and no toxicity, has a simple preparation process, and reduces the links of solvent replacement.
5. The experimental scheme of the invention has the advantages of high feasibility, simple operation process, less capital investment, short preparation period, mild reaction conditions, no need of large-scale instruments and equipment, realization of large-scale industrial production and processing and wide application prospect.
The invention provides a method for preparing a super-hydrophobic super-oleophylic aerogel material by taking nano-cellulose and nano-particles as raw materials.
Drawings
FIG. 1 is a scanning electron microscope image of a super-hydrophobic super-oleophilic aerogel material prepared in example one under the condition that the ruler is 2 μm;
FIG. 2 is a scanning electron microscope image of the super-hydrophobic super-oleophilic aerogel material prepared in the first example under the condition that the ruler is 1 μm;
FIG. 3 is a scanning electron microscope image of the superhydrophobic and superoleophilic aerogel material prepared according to example one at a scale of 100 nm;
FIG. 4 is a physical representation of a superhydrophobic and superoleophilic aerogel material prepared according to example one as placed in water;
FIG. 5 is a physical diagram of a superhydrophobic and superoleophilic aerogel material prepared according to example one under a weight pressure of 200 g;
FIG. 6 is a diagram showing a light oil on the surface of water;
FIG. 7 is a diagram illustrating the process of adsorbing light oil on the water surface by the super-hydrophobic super-oleophilic aerogel material prepared in the first example;
FIG. 8 is a diagram of a process in which the super-hydrophobic super-oleophilic aerogel material prepared in the first example is taken out after the adsorption of light oil on the water surface is completed;
FIG. 9 is a diagram of a bottom portion of a water containing heavy oil;
FIG. 10 is a schematic diagram of the adsorption process of the super-hydrophobic super-oleophilic aerogel material prepared in the first example on heavy oil at the bottom of water;
FIG. 11 is a schematic representation of a process of the super-hydrophobic super-oleophilic aerogel material prepared in the first example after adsorption of heavy oil on water bottom is completed;
FIG. 12 is a graph of a downward movement of a water droplet during a contact angle test for a superhydrophobic and superoleophilic aerogel material prepared according to example one;
FIG. 13 is a diagram showing a water drop pressing down on a substance during a contact angle test of a superhydrophobic and superoleophilic aerogel material prepared according to example one;
FIG. 14 is a graph of a water droplet moving upward during a contact angle test of a superhydrophobic and superoleophilic aerogel material prepared according to example one embodiment;
fig. 15 is a real image of the super-hydrophobic super-oleophilic aerogel material prepared in example one, wherein the water drop does not stay on the surface during the contact angle test.
Detailed Description
The first embodiment is as follows: the embodiment of the invention relates to a method for preparing a super-hydrophobic super-oleophylic aerogel material by taking nano-cellulose and nano-particles as raw materials, which comprises the following steps:
1. dispersing nano-cellulose into deionized water through a high-speed homogenizer under the condition that the rotating speed is 1000 r/min-100000 r/min, uniformly dispersing, adding gamma-aminopropyltriethoxysilane under the conditions of magnetic stirring at the rotating speed of 50 r/min-1000 r/min and the adding speed of 10 mL/h-20 mL/h, and then adding a fluorine-free modifier under the magnetic stirring at the rotating speed of 50 r/min-1000 r/min to obtain a modified nano-cellulose solution;
the volume ratio of the mass of the nano-cellulose to the deionized water is 1g (50-600) mL; the mass ratio of the nano-cellulose to the gamma-aminopropyltriethoxysilane is 1 (0.2-8); the mass ratio of the nano-cellulose to the fluorine-free modifier is 1 (0.33-1);
2. adding the nano particles into deionized water, then carrying out ultrasonic dispersion uniformly under the condition that the power is 800-1500W, and sequentially adding hexadecyl trimethoxy silane and 10-88 mass percent formic acid under the magnetic stirring at the rotating speed of 50-1000 r/min to obtain a modified silicon dioxide solution;
the volume ratio of the mass of the nano particles to the deionized water is 1g (15-800) mL; the mass ratio of the nano particles to the hexadecyl trimethoxy silane is 1 (0.22-15.6); the mass ratio of the nano particles to 10 to 88 mass percent of formic acid is 1 (0.5 to 8);
3. mixing the modified nano-cellulose solution and the modified silicon dioxide solution, carrying out ultrasonic treatment for 2-60 min under the condition that the power is 800-1500W, and then uniformly mixing under magnetic stirring at the rotating speed of 50-1000 r/min to obtain a mixed solution;
the volume ratio of the modified nano-cellulose solution to the modified silicon dioxide solution is 1 (0.5-5);
4. freezing the mixed solution for 2-12 h at the temperature of-12-5 ℃ to obtain a pre-frozen solution;
5. and (3) putting the pre-frozen solution into a vacuum freeze dryer, and freezing for 2-12 h at the temperature of-50 ℃ to-5 ℃ to obtain the super-hydrophobic super-oleophylic aerogel material.
The beneficial effects of this embodiment are: 1. the nano-cellulose is used as a raw material, is a natural degradable biomass material, has abundant reserves and is environment-friendly.
2. The super-hydrophobic super-oleophylic aerogel material prepared by the embodiment has higher strength, can stand the pressure of a 200g weight and keep stable in structure, and in the contact angle test process, water drops can not stay on the surface of the aerogel, so that the aerogel has a good hydrophobic effect.
3. The hydrophobic super-oleophylic aerogel material prepared by the embodiment is used as a novel oil absorption material, has high adsorption speed, can reach adsorption balance in 10s, has large adsorption capacity, can reach 32.95g/g of the maximum adsorption capacity of carbon tetrachloride, can reach 13.01g/g of the maximum adsorption capacity of n-hexane, is simple in method, green and environment-friendly, can be applied to treatment of oily wastewater, can complete continuous and efficient separation of an oil-water mixture under the assistance of a suction pump, and has the pressure range of-0.01 MPa-0.02 MPa for the suction pump.
4. The super-hydrophobic nano-cellulose aerogel prepared by the embodiment is prepared by taking water as the environment and modified by the fluorine-free modifier, so that the environment-friendly and non-toxic requirements are met, the preparation process is simple, and the link of solvent replacement is reduced.
5. The experimental scheme of the embodiment has the advantages of high feasibility, simple operation process, low capital investment, short preparation period, mild reaction conditions, no need of large-scale instruments and equipment, realization of large-scale industrial production and processing, and wide application prospect.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the particle size of the nano particles in the second step is 7 nm-40 nm. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and the nano particles in the step two are nano silicon dioxide, nano titanium dioxide, nano ferroferric oxide, nano calcium carbonate, nano kaolin or nano alumina. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: in the first step, the fluorine-free modifier is hexadecyl trimethoxy silane. The others are the same as in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the volume ratio of the mass of the nano-cellulose to the deionized water in the step one is 1g (100-600) mL; the mass ratio of the nano-cellulose to the gamma-aminopropyltriethoxysilane in the first step is 1 (0.5-8); the mass ratio of the nano-cellulose to the fluorine-free modifier in the step one is 1 (1.3-1). The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: dispersing the nano-cellulose into deionized water through a high-speed homogenizer under the condition that the rotating speed is 5000 r/min-100000 r/min, uniformly dispersing, adding gamma-aminopropyltriethoxysilane under the conditions of magnetic stirring at the rotating speed of 100 r/min-1000 r/min and the adding speed of 15 mL/h-20 mL/h, and then adding a fluorine-free modifier under the magnetic stirring at the rotating speed of 100 r/min-1000 r/min to obtain a modified nano-cellulose solution. The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the volume ratio of the mass of the nano particles to the deionized water in the step two is 1g (15-500) mL; the mass ratio of the nano particles to the hexadecyl trimethoxy silane in the second step is 1 (1.2-15.6); the mass ratio of the nano particles to 10 to 88 mass percent of formic acid in the second step is 1 (1.1 to 8). The others are the same as in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: and secondly, adding the nano particles into deionized water, then ultrasonically dispersing the nano particles uniformly under the condition that the power is 1000-1500W, and sequentially adding hexadecyl trimethoxy silane and 50-88 mass percent formic acid under the magnetic stirring at the rotating speed of 100-1000 r/min to obtain the modified silicon dioxide solution. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: the volume ratio of the modified nano-cellulose solution to the modified silicon dioxide solution in the third step is 1 (2-5). The others are the same as in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: in the fifth step, the solution which is frozen in advance is placed in a vacuum freeze dryer and is frozen for 8 to 12 hours at the temperature of between 50 ℃ below zero and 10 ℃ below zero. The others are the same as in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a method for preparing a super-hydrophobic super-oleophylic aerogel material by taking nano-cellulose and nano-particles as raw materials is characterized by comprising the following steps:
1. dispersing nano-cellulose into deionized water through a high-speed homogenizer under the condition that the rotating speed is 100000r/min, uniformly dispersing, adding gamma-aminopropyltriethoxysilane under the conditions that the magnetic stirring is carried out at the rotating speed of 1000r/min and the adding speed is 20mL/h, and then adding hexadecyl trimethoxysilane under the magnetic stirring is carried out at the rotating speed of 1000r/min to obtain a modified nano-cellulose solution;
the volume ratio of the mass of the nano-cellulose to the deionized water is 1g; the mass ratio of the nano-cellulose to the gamma-aminopropyltriethoxysilane is 1; the mass ratio of the nano-cellulose to the hexadecyl trimethoxy silane is 1.3;
2. adding the nano particles into deionized water, then ultrasonically dispersing the nano particles uniformly under the condition that the power is 900W, and sequentially adding hexadecyl trimethoxy silane and 88 mass percent formic acid under the magnetic stirring at the rotating speed of 600r/min to obtain a modified silicon dioxide solution;
the volume ratio of the mass of the nanoparticles to the deionized water is 1g; the mass ratio of the nano particles to the hexadecyl trimethoxy silane is 1.2; the mass ratio of the nano particles to 88% of formic acid is 1.1;
3. mixing the modified nano-cellulose solution and the modified silicon dioxide solution, carrying out ultrasonic treatment for 45min under the condition that the power is 900W, and then uniformly mixing under the magnetic stirring at the rotating speed of 1000r/min to obtain a mixed solution;
the volume ratio of the modified nano-cellulose solution to the modified silicon dioxide solution is 1;
4. freezing the mixed solution at-12 deg.C for 6h to obtain pre-frozen solution;
5. and (3) placing the pre-frozen solution into a vacuum freeze dryer, and freezing for 12h at the temperature of-50 ℃ to obtain the super-hydrophobic super-oleophylic aerogel material.
The grain size of the nano-particles in the second step is 7 nm-40 nm;
the nano particles in the second step are nano silicon dioxide;
the total volume of the modified nano-cellulose solution and the modified silicon dioxide solution mixed in the step three is 10mL.
FIG. 1 is a scanning electron microscope picture of the super-hydrophobic super-oleophilic aerogel material prepared in the first example under the condition that the ruler is 2 μm, and FIG. 2 is a scanning electron microscope picture of the super-hydrophobic super-oleophilic aerogel material prepared in the first example under the condition that the ruler is 1 μm.
FIG. 3 is a scanning electron microscope image of the super-hydrophobic super-oleophilic aerogel material prepared in example one under the condition that the ruler is 100nm, and it can be seen that the average particle size of the modified nano-silica particles is about 50nm and the modified nano-silica particles are uniformly distributed.
FIG. 4 is a physical representation of a superhydrophobic and superoleophilic aerogel material prepared according to example one as placed in water; as can be seen from the figure, a bright passage is formed on the surface of the super-hydrophobic super-oleophylic aerogel material, which indicates that the prepared aerogel has good super-hydrophobicity.
FIG. 5 is a physical diagram of the super-hydrophobic super-oleophilic aerogel material prepared in the first example under a weight of 200g, and it can be seen that the super-hydrophobic super-oleophilic aerogel material can keep stable structure under the pressure of 200 g.
The super-hydrophobic and super-oleophilic aerogel material prepared in the first embodiment is used for adsorbing light oil n-hexane in water, and FIG. 6 is a physical diagram of the water surface containing light oil; FIG. 7 is a schematic diagram illustrating the adsorption process of light oil on water surface by the superhydrophobic and superoleophilic aerogel material prepared in the first embodiment; FIG. 8 is a schematic diagram illustrating a process of the super-hydrophobic super-oleophilic aerogel material prepared in the first embodiment after adsorption of light oil on the water surface is completed; the test shows that 0.3681g of the super-hydrophobic super-oleophilic aerogel material can adsorb 4.79g of n-hexane (13.01 g/g).
Adsorbing carbon tetrachloride with heavy oil in water by using the super-hydrophobic super-oleophilic aerogel material prepared in the first embodiment, and fig. 9 is a diagram of a real object containing heavy oil at the bottom of a water; FIG. 10 is a schematic diagram of the adsorption process of the super-hydrophobic super-oleophilic aerogel material prepared in the first example on heavy oil at the bottom of water; FIG. 11 is a schematic diagram of the process of the super-hydrophobic super-oleophilic aerogel material prepared in the first example after the adsorption of heavy oil on the water bottom is completed and the material is taken out; 0.366g of aerogel was tested to be able to adsorb 12.06g of carbon tetrachloride (32.95 g/g).
A contact angle test is performed on the super-hydrophobic super-oleophylic aerogel material prepared in the first embodiment, because the super-hydrophobic super-oleophylic aerogel material prepared in the first embodiment has good hydrophobicity, water drops cannot stay on the surface of the aerogel, and fig. 12 is a real image of downward movement of the water drops in the contact angle test process of the super-hydrophobic super-oleophylic aerogel material prepared in the first embodiment; FIG. 13 is a diagram of a water drop pressing down on a super-hydrophobic super-oleophilic aerogel material prepared according to example one during a contact angle test; FIG. 14 is a graph of a water droplet moving upward during a contact angle test of a superhydrophobic and superoleophilic aerogel material prepared according to example one embodiment; FIG. 15 is a physical representation of a superhydrophobic and superoleophilic aerogel material prepared according to example one in which a water droplet did not settle on the surface during a contact angle test; through the drop of water droplet on this aerogel press the test, can observe when the water droplet uses certain power to press after contacting this aerogel surface, the in-process liquid droplet that pulls back can not stay at the aerogel surface, therefore this aerogel has good hydrophobic effect.
The super-hydrophobic super-oleophylic aerogel material prepared in the first embodiment is clamped by tweezers and placed into various organic solvents (normal hexane, acetone, toluene, xylene, carbon tetrachloride, ethyl acetate, cyclohexane, dichloromethane, gasoline and vegetable oil), then the mass of the super-hydrophobic super-oleophylic aerogel material after adsorption is recorded every 2s, and it can be found that the mass of the super-hydrophobic super-oleophylic aerogel material does not change after adsorption for 10s any more, so that the super-hydrophobic super-oleophylic aerogel material prepared in the first embodiment has high adsorption speed, can reach adsorption balance within 10s, and can reach 32.95g/g of maximum adsorption capacity for carbon tetrachloride.
The super-hydrophobic and super-oleophylic aerogel material prepared in the first embodiment can be used for continuously and efficiently separating an oil-water mixture with the assistance of a suction pump, and the pressure range of the suction pump is-0.01 MPa-0.02 MPa.
Claims (1)
1. A method for preparing a super-hydrophobic and super-oleophylic aerogel material by taking nano-cellulose and nano-particles as raw materials is characterized by comprising the following steps:
1. dispersing nano-cellulose into deionized water through a high-speed homogenizer under the condition that the rotating speed is 100000r/min, uniformly dispersing, adding gamma-aminopropyltriethoxysilane under the conditions that the magnetic stirring is carried out at the rotating speed of 1000r/min and the adding speed is 20mL/h, and then adding hexadecyl trimethoxysilane under the magnetic stirring is carried out at the rotating speed of 1000r/min to obtain a modified nano-cellulose solution;
the volume ratio of the mass of the nano-cellulose to the deionized water is 1g; the mass ratio of the nano-cellulose to the gamma-aminopropyltriethoxysilane is 1; the mass ratio of the nano-cellulose to the hexadecyl trimethoxy silane is 1.3;
2. adding nano silicon dioxide into deionized water, then, ultrasonically dispersing the nano silicon dioxide uniformly under the condition that the power is 900W, and sequentially adding hexadecyl trimethoxy silane and 88 mass percent formic acid under the magnetic stirring at the rotating speed of 600r/min to obtain a modified silicon dioxide solution;
the volume ratio of the mass of the nano silicon dioxide to the deionized water is 1g; the mass ratio of the nano silicon dioxide to the hexadecyl trimethoxy silane is 1.2; the mass ratio of the nano silicon dioxide to 88% of formic acid is 1.1;
3. mixing the modified nano-cellulose solution and the modified silicon dioxide solution, carrying out ultrasonic treatment for 45min under the condition that the power is 900W, and then uniformly mixing under the magnetic stirring at the rotating speed of 1000r/min to obtain a mixed solution;
the volume ratio of the modified nano-cellulose solution to the modified silicon dioxide solution is 1;
4. freezing the mixed solution at-12 deg.C for 6 hr to obtain pre-frozen solution;
5. placing the pre-frozen solution in a vacuum freeze dryer, and freezing for 12 hours at the temperature of-50 ℃ to obtain the super-hydrophobic super-oleophylic aerogel material;
the particle size of the nano silicon dioxide in the step two is 7nm to 40nm;
the total volume of the modified nano-cellulose solution and the modified silicon dioxide solution mixed in the third step is 10mL.
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| CN115028882B (en) * | 2022-06-27 | 2023-06-23 | 南京林业大学 | Preparation method and application of self-cleaning cellulose nano crystal aerogel |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3346507A (en) * | 1962-06-04 | 1967-10-10 | Monsanto Co | Process of preparing an organo-silica aerogel |
| CN103756006A (en) * | 2014-01-20 | 2014-04-30 | 东北林业大学 | Preparation method of ultralight and hydrophobic nano fibrillated cellulose aerogel with high oil absorption |
| CN105056901A (en) * | 2015-07-31 | 2015-11-18 | 东北林业大学 | Superhydrophobic and super-oleophilic adsorbent with straw as raw material and preparation method thereof |
| CN105566673A (en) * | 2015-12-17 | 2016-05-11 | 中国科学院兰州化学物理研究所 | Preparation method of multifunctional cellulose elastic aerogel |
| CN105670393A (en) * | 2016-04-22 | 2016-06-15 | 南京林业大学 | Preparation of super-hydrophobic coating with nanocrystalline cellulose/silicon dioxide composite template process |
-
2019
- 2019-09-03 CN CN201910828551.XA patent/CN110479218B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3346507A (en) * | 1962-06-04 | 1967-10-10 | Monsanto Co | Process of preparing an organo-silica aerogel |
| CN103756006A (en) * | 2014-01-20 | 2014-04-30 | 东北林业大学 | Preparation method of ultralight and hydrophobic nano fibrillated cellulose aerogel with high oil absorption |
| CN105056901A (en) * | 2015-07-31 | 2015-11-18 | 东北林业大学 | Superhydrophobic and super-oleophilic adsorbent with straw as raw material and preparation method thereof |
| CN105566673A (en) * | 2015-12-17 | 2016-05-11 | 中国科学院兰州化学物理研究所 | Preparation method of multifunctional cellulose elastic aerogel |
| CN105670393A (en) * | 2016-04-22 | 2016-06-15 | 南京林业大学 | Preparation of super-hydrophobic coating with nanocrystalline cellulose/silicon dioxide composite template process |
Non-Patent Citations (1)
| Title |
|---|
| Delignified wood with unprecedented anti-oil properties for the highly efficient separation of crude oil/water mixtures;Wu, MB，et al.;《JOURNAL OF MATERIALS CHEMISTRY A》;20190728;第7卷(第28期);第16735-16741页 * |
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