CN114479197A - Preparation method of oriented structure nano cellulose montmorillonite aerogel - Google Patents
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Abstract
The invention relates to a preparation method of orientated structure nano-cellulose montmorillonite aerogel, which comprises the steps of adding oxidized nano-cellulose into water, and performing ultrasonic treatment to obtain cellulose nano-fiber dispersion liquid; adding a cross-linking agent and montmorillonite into cellulose nano-fiber dispersion liquid, placing the cellulose nano-fiber dispersion liquid into a refrigerator for precooling after ultrasonic dispersion, then carrying out liquid nitrogen directional freezing treatment, and finally carrying out freeze drying to obtain cellulose montmorillonite aerogel; and then the hydrophobic modification is carried out on the montmorillonite nano-fiber through a chemical vapor deposition modification technology to prepare the hydrophobic modified cellulose nano-fiber montmorillonite aerogel. The aerogel has excellent oil absorption capacity and can be used as an oil absorbent. The simple preparation method of the cellulose nano-fiber montmorillonite aerogel is beneficial to promoting the development of aerogel industrialization and solves the problems of high aerogel preparation cost and the like.
Description
Technical Field
The invention belongs to the field of preparation processes of nano-porous materials, and particularly relates to a simple preparation method of oriented structure cellulose nano-fiber montmorillonite aerogel.
Background
In recent years, with the rapid development of world industry, offshore oil resources are developed, the problem of crude oil leakage caused by oil exploitation and transportation is more serious, and oil spillage accidents are increased. The existing oil spill accident treatment method mainly comprises a physical adsorption method, a biological method and a chemical method, wherein the biological method is long in period and low in efficiency; the chemical method is easy to produce secondary pollution, and the physical adsorption method is a better method for treating the ocean oil spill. However, most of the oil absorption materials in the society at present have the defects of low oil absorption efficiency, pollution source, inconvenient secondary treatment, high cost and the like.
Although the traditional chemical synthetic adsorbent such as polypropylene fiber, polyurethane foam and other materials have a certain adsorption effect, the traditional chemical synthetic adsorbent is a petroleum-based material and has the defect of non-biodegradability, and another environmental problem can be caused if the traditional chemical synthetic adsorbent is not properly treated after being used. Therefore, the use of bio-based adsorbents is of great significance. The cellulose is used as a rich biomass resource and has the advantages of no pollution, degradability and the like. Aerogels prepared from Cellulose Nanofibers (CNF) still suffer from some drawbacks such as low strength, poor reusability and low adsorption efficiency, which seriously affect their applications. Montmorillonite (MMT), also known as microcrystalline kaolinite, is a natural silicate mineral. The molecular structural formula is (Al, Mg)2[SiO10](OH)2·n H2O, mainly composed of two SiO2With an Al layer between the tetrahedrons2O3Octahedral. Because montmorillonite has a unique layered nanostructure, interlayer reactivity with a large specific surface area and a large thickness-to-diameter ratio can be designed. When the montmorillonite is compounded with the cellulose, the mechanical property of the cellulose aerogel is greatly improved by the special structure of the montmorillonite.
The preparation and structure and performance of the dangdan Yang (Wangliang, Liuyong. cellulose nanofiber/nano montmorillonite composite aerogel, 2020,41(2):6.) utilize nano montmorillonite to blend and modify nano cellulose, and the flame-retardant and heat-insulating nano cellulose/montmorillonite composite aerogel is prepared based on a freeze-drying method. Zhou et al (Zhou Li Jie, Zhou Huan, Li Jia, etc.. preparation and Properties of nanocellulose-based oil-absorbing aerogel [ J ] forestry engineering report, 2019,4(1):7.) prepared a nanocellulose-based material from bamboo powder, polyvinyl alcohol as a reinforcing phase, a freeze-drying method was used in an acidic environment to prepare a polyvinyl alcohol/nanocellulose composite aerogel, which was subjected to hydrophobic modification treatment with trimethylchlorosilane, and then dipped into a reduced graphene oxide suspension to finally prepare a hydrophobic graphene oxide/polyvinyl alcohol/nanocellulose composite aerogel. The preparation technology research [ J ] of the super-strong adsorption nano-cellulose/polyvinyl alcohol composite aerogel by the rest et al (wild goose, king hankun, Zhang Xuelia. super-strong adsorption nano-cellulose/polyvinyl alcohol composite aerogel, 2020(2):2.) after mixing the carboxyl functionalized nano-cellulose suspension with the polyvinyl alcohol aqueous solution, the polyvinyl alcohol/carboxyl nano-cellulose crosslinked composite aerogel is prepared sequentially through a glutaraldehyde crosslinking freeze-drying process, and the methyl trichlorosilane is used as a silane modifier, so that the water contact angle of the modified composite aerogel with good compression resilience reaches (150.3+1.2) ° and the adsorption capacity to oils and non-polar organic solvents is between 44 and 96g/g, but the freeze-drying process is too complex, the price of the carboxyl functionalized nano-cellulose is too high, and the mass production cannot be realized.
Disclosure of Invention
The invention aims to solve a series of problems of weak oil absorption capacity, low strength, complex production process and high preparation cost in the prior art, and provides a simple preparation method of nano cellulose montmorillonite aerogel with an oriented structure.
The technical scheme of the invention is as follows: a preparation method of nano-cellulose montmorillonite aerogel with an oriented structure comprises the following specific steps:
(1) adding oxidized nano-cellulose into water, and performing ultrasonic treatment to obtain cellulose nano-fiber dispersion liquid;
(2) adding a cross-linking agent and montmorillonite into the cellulose nano-fiber dispersion liquid, and performing ultrasonic dispersion to obtain a cellulose nano-fiber montmorillonite mixed liquid;
(3) placing the cellulose nano-fiber montmorillonite mixed solution into a refrigerator for precooling, then carrying out liquid nitrogen directional freezing treatment, and finally carrying out freeze drying to obtain cellulose montmorillonite aerogel;
(4) the cellulose montmorillonite aerogel is subjected to hydrophobic treatment by chemical vapor deposition, and the aerogel, a hydrophobic modifier and water are placed in an oven for treatment, so that the hydrophobic oil absorption type cellulose montmorillonite aerogel is obtained.
Preferably, the mass ratio of the oxidized nano-cellulose to water in the step (1) is 1-5: 200; the ultrasonic power is 800-1000W, the ultrasonic frequency is 10-30 KHz, and the ultrasonic temperature is 25-45 ℃; the ultrasonic treatment time is 45-240 min.
Preferably, the ultrasonic power in the step (2) is 100-500W, and the ultrasonic frequency is 20-60 KHz; the ultrasonic temperature is 60-90 ℃; the ultrasonic time is 30-120 min; the cross-linking agent is one of polyvinyl alcohol and glutaraldehyde, and the cellulose nano-fiber: a crosslinking agent: the mass ratio of the montmorillonite is 1: 0.1-0.6: 0.4-1.
Preferably, the pre-cooling temperature of the refrigerator in the step (3) is 2-6 ℃, and the pre-cooling time of the refrigerator is 6-24 h.
Preferably, the time of the liquid nitrogen directional freezing treatment in the step (3) is 3-7 minutes; the temperature of the freeze drying is-60 to-80 ℃, and the time of the freeze drying is 24 to 72 hours.
Preferably, the hydrophobic modifier in the step (4) is methyltrimethoxysilane or heptadecafluorodecyltriethoxysilane; the mass ratio of the aerogel to the hydrophobic modifier to the water is 1 (0.5-2) to 0.5-1.
Preferably, the temperature of the oven treatment in the step (4) is 50-80 ℃; the treatment time is 6-12 h.
Has the advantages that:
(1) compared with the traditional preparation of the cellulose aerogel material, the preparation method has the advantages of simple preparation process, convenient operation and high success rate;
(2) compared with other nano-cellulose aerogel materials, the oriented nano-cellulose/polyvinyl alcohol/montmorillonite aerogel material prepared by the method has an ordered structure, has the characteristics of high specific surface area, high porosity and the like, and can provide a faster transmission channel for oil-water separation.
Drawings
FIG. 1 is a scanning electron micrograph of the hydrophobic CNF/MMT aerogel prepared in example 1; (a) pore characterization map (b) oriented structure;
FIG. 2 is a graph of the adsorption effect of the hydrophobic CNF/MMT aerogel prepared in example 1; (a) floating oil on water (b) the aerogel completely adsorbs the floating oil;
FIG. 3 is a water contact angle test plot of the hydrophobic CNF/MMT aerogel prepared in example 1.
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of protection.
Example 1
(1) Placing 2g of oxidized nano-cellulose in 200g of water to obtain cellulose nano-fiber dispersion, and performing ultrasonic treatment at 45 ℃ for 90min, wherein the ultrasonic power is 1000W, and the ultrasonic frequency is 30 KHz.
(2) Uniformly dispersing cellulose nano-fibers in deionized water, adding cross-linking agent polyvinyl alcohol and montmorillonite into oxidized nano-fibers, cross-linking agent and montmorillonite according to the mass ratio of 1:0.5:1, keeping the water temperature at 85 ℃, the ultrasonic frequency at 50KHz and the ultrasonic power at 400W, and continuing to perform ultrasonic dispersion for 60min until the mixture is uniformly dispersed;
(3) pouring the uniformly dispersed mixture into a specific mould, placing the mould in a refrigerator for precooling for 12h at 4 ℃, then placing the mould in liquid nitrogen for freezing for 5min for orientation, and after freezing, carrying out freeze drying for 48h at-80 ℃ to obtain the dried cellulose nanofiber crosslinked aerogel;
(4) preparing methyltrimethoxysilane silane solution as a hydrophobic treatment agent, placing 4g of methyltrimethoxysilane, 1g of water and 2g of prepared aerogel sample into a 500ml sealed container, and placing at 70 ℃ for 12 hours to obtain the hydrophobic CNF/MMT aerogel. The cellulose-based aerogel sample has remarkable hydrophobic property, which shows that the composite aerogel treated by the methyltrimethoxysilane silane has excellent hydrophobic property, the oil adsorption capacity of the composite aerogel is 54g/g, and the water contact angle of the composite aerogel is 115 degrees. The surface structure of the cellulose nanofiber/montmorillonite aerogel is shown in figure 1, wherein a chart shows that the cellulose nanofiber/montmorillonite aerogel has three-dimensional structures with different pore diameters, the sizes of ice crystals are different, the large ice crystals extrude the inner wall of cellulose to form the orientation of a chart b, and the liquid nitrogen cooling speed of the ice crystals further determines that the occurrence frequency of the ice crystals at partial positions is extremely high, so that the orientation of the large-scale CNF aerogel is consistent. The obstruction of the oil transport by the disordered structure of the aerogel can be weakened. The directional channel of the aerogel tends to be uniform, the curvature is gradually reduced, the capillary effect is increased, and the transmission distance and the transmission speed are improved. Figure 2 shows the oil absorption capacity of the hydrophobic oil absorption type cellulose montmorillonite aerogel, floating oil is put into water, the aerogel is put into water, the adsorption is completed within 2min, and the shape of the aerogel is not deformed. Fig. 3 shows that the water contact angle of the material is 115 degrees, which shows that the hydrophobic modification makes the network structure of the cellulose aerogel become more compact, and the surface of the cellulose aerogel also becomes more rough and uneven, so that the hydrophobic angle becomes larger and larger.
Example 2
(1) Placing 5g of oxidized nano-cellulose in 200g of water to obtain cellulose nano-fiber dispersion, and performing ultrasonic treatment at 35 ℃ for 240min, wherein the ultrasonic power is 900W, and the ultrasonic frequency is 20 KHz.
(2) Uniformly dispersing cellulose nano-fibers in deionized water, adding glutaraldehyde and montmorillonite as crosslinking agents into oxidized nano-fibers, namely the montmorillonite according to the mass ratio of 1:0.4:0.8, maintaining the water temperature at 90 ℃, the ultrasonic frequency at 30KHz and the ultrasonic power at 500W, and continuing to perform ultrasonic dispersion for 120min until the mixture is uniformly dispersed;
(3) pouring the uniformly dispersed mixture into a specific mould, placing the mould in a refrigerator for precooling for 24h at 6 ℃, then placing the mould in liquid nitrogen for freezing for 7 min for orientation, and after freezing, carrying out freeze drying for 72h at-70 ℃ to obtain the dried cellulose nanofiber crosslinked aerogel;
(4) a heptadecafluorodecyltriethoxysilane solution was prepared as a hydrophobic treatment agent, and two glass vials, 1g of heptadecafluorodecyltriethoxysilane, 1g of water, and 2g of the prepared aerogel sample were placed in a 500ml sealed container to obtain a hydrophobic CNF/MMT aerogel, and placed at a temperature of 80 ℃ for 8 hours. The cellulose-based aerogel sample has remarkable hydrophobic property, which shows that the composite aerogel treated by the methyltrimethoxysilane silane has excellent hydrophobic property, the oil adsorption capacity of the composite aerogel is 36g/g, and the water contact angle of the composite aerogel is 112 degrees.
Example 3
(1) Placing 1g of oxidized nano-cellulose in 200g of water to obtain cellulose nano-fiber dispersion, and performing ultrasonic treatment at 25 ℃ for 45min, wherein the ultrasonic power is 800W and the ultrasonic frequency is 10 KHz.
(2) Uniformly dispersing cellulose nano-fibers in deionized water, adding glutaraldehyde and montmorillonite as crosslinking agents into oxidized nano-fibers, namely montmorillonite according to the mass ratio of 1:0.2:0.4, maintaining the water temperature at 60 ℃, the ultrasonic frequency at 20KHz and the ultrasonic power at 200W, and continuing to perform ultrasonic dispersion for 30min until the mixture is uniformly dispersed;
(3) pouring the uniformly dispersed mixture into a specific mould, placing the mould in a refrigerator for precooling for 6h at the temperature of 2 ℃, then placing the mould in liquid nitrogen for freezing for 4 min for orientation, and after freezing, carrying out freeze drying for 24h at the temperature of-60 ℃ to obtain the dried cellulose nanofiber crosslinked aerogel;
(4) a heptadecafluorodecyltriethoxysilane solution was prepared as a hydrophobic treatment agent, and two glass vials, 2g of heptadecafluorodecyltriethoxysilane, 2g of water and 2g of the prepared aerogel sample were placed in a 500ml sealed container to obtain a hydrophobic CNF/MMT aerogel, and placed at a temperature of 50 ℃ for 10 hours. The cellulose-based aerogel sample has remarkable hydrophobic property, which shows that the composite aerogel treated by the methyltrimethoxysilane silane has excellent hydrophobic property, the adsorption capacity to oil is 30g/g, and the water contact angle is 108 degrees.
Example 4
(1) Placing 4g of oxidized nano-cellulose in 200g of water to obtain cellulose nano-fiber dispersion, and performing ultrasonic treatment at 40 ℃ for 60min, wherein the ultrasonic power is 950W, and the ultrasonic frequency is 15 KHz.
(2) Uniformly dispersing cellulose nano-fibers in deionized water, adding cross-linking agent polyvinyl alcohol and montmorillonite into oxidized nano-fibers, cross-linking agent and montmorillonite according to the mass ratio of 1:0.5:1, keeping the water temperature at 65 ℃, the ultrasonic frequency at 30KHz and the ultrasonic power at 200W, and continuing to perform ultrasonic dispersion for 60min until the mixture is uniformly dispersed;
(3) pouring the uniformly dispersed mixture into a specific mould, placing the mould in a refrigerator for precooling for 16h at 3 ℃, then placing the mould in liquid nitrogen for freezing for 7 min for orientation, and after freezing, carrying out freeze drying for 28h at-70 ℃ to obtain the dried cellulose nanofiber crosslinked aerogel;
(4) preparing methyltrimethoxysilane silane solution as a hydrophobic treatment agent, placing 3g of methyltrimethoxysilane, 1.6g of water and 2g of prepared aerogel sample into a 500ml sealed container, and placing at 60 ℃ for 7 hours to obtain the hydrophobic CNF/MMT aerogel. The cellulose-based aerogel sample has remarkable hydrophobic property, which shows that the composite aerogel treated by the methyltrimethoxysilane silane has excellent hydrophobic property, the oil adsorption capacity of the composite aerogel is 41g/g, and the water contact angle of the composite aerogel is 111 degrees.
Claims (7)
1. A preparation method of nano-cellulose montmorillonite aerogel with an oriented structure comprises the following specific steps:
(1) adding oxidized nano-cellulose into water, and performing ultrasonic treatment to obtain cellulose nano-fiber dispersion liquid;
(2) adding a cross-linking agent and montmorillonite into the cellulose nano-fiber dispersion liquid, and performing ultrasonic dispersion to obtain a cellulose nano-fiber montmorillonite mixed liquid;
(3) placing the cellulose nano-fiber montmorillonite mixed solution into a refrigerator for precooling, then carrying out liquid nitrogen directional freezing treatment, and finally carrying out freeze drying to obtain cellulose montmorillonite aerogel;
(4) the cellulose montmorillonite aerogel is subjected to hydrophobic treatment by chemical vapor deposition, and the aerogel, a hydrophobic modifier and water are placed in an oven for treatment, so that the hydrophobic oil absorption type cellulose montmorillonite aerogel is obtained.
2. The preparation method according to claim 1, wherein the mass ratio of the oxidized nanocellulose to the water in the step (1) is 1-5: 200; the ultrasonic power is 800-1000W, the ultrasonic frequency is 10-30 KHz, and the ultrasonic temperature is 25-45 ℃; the ultrasonic treatment time is 45-240 min.
3. The preparation method according to claim 1, wherein the ultrasonic power in the step (2) is 100-500W, and the ultrasonic frequency is 20-60 KHz; the ultrasonic temperature is 60-90 ℃; the ultrasonic time is 30-120 min; the cross-linking agent is one of polyvinyl alcohol and glutaraldehyde, and the cellulose nano-fiber: a crosslinking agent: the mass ratio of the montmorillonite is 1: 0.1-0.6: 0.4-1.
4. The preparation method according to claim 1, wherein the temperature for precooling in the refrigerator in the step (3) is 2-6 ℃, and the time for precooling in the refrigerator is 6-24 h.
5. The preparation method according to claim 1, wherein the time of the liquid nitrogen directional freezing treatment in the step (3) is 3 to 7 minutes; the temperature of the freeze drying is-60 to-80 ℃, and the time of the freeze drying is 24 to 72 hours.
6. The method according to claim 1, wherein the hydrophobic modifier in the step (4) is methyltrimethoxysilane or heptadecafluorodecyltriethoxysilane; the mass ratio of the aerogel to the hydrophobic modifier to the water is 1 (0.5-2) to 0.5-1.
7. The preparation method according to claim 1, wherein the temperature of the oven treatment in the step (4) is 50-80 ℃; the treatment time is 6-12 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805914A (en) * | 2022-05-19 | 2022-07-29 | 武汉纺织大学 | Magnetic nanofiber aerogel for thick oil separation |
| CN114989499A (en) * | 2022-05-24 | 2022-09-02 | 西北农林科技大学 | Super-hydrophobic nano cellulose membrane and preparation method thereof |
| CN115260573A (en) * | 2022-07-25 | 2022-11-01 | 天津工业大学 | Oriented PVA (polyvinyl alcohol) -doped magnesium hydroxide composite cellulose aerogel and preparation method thereof |
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| 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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| 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805914A (en) * | 2022-05-19 | 2022-07-29 | 武汉纺织大学 | Magnetic nanofiber aerogel for thick oil separation |
| CN114989499A (en) * | 2022-05-24 | 2022-09-02 | 西北农林科技大学 | Super-hydrophobic nano cellulose membrane and preparation method thereof |
| CN115260573A (en) * | 2022-07-25 | 2022-11-01 | 天津工业大学 | Oriented PVA (polyvinyl alcohol) -doped magnesium hydroxide composite cellulose aerogel and preparation method thereof |
| CN115260573B (en) * | 2022-07-25 | 2023-10-13 | 天津工业大学 | Directional PVA doped magnesium hydroxide composite cellulose aerogel and preparation method thereof |
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