CN113429617B - Kapok nano-cellulose aerogel and preparation method and application thereof - Google Patents
Kapok nano-cellulose aerogel and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a kapok nano-cellulose aerogel and a preparation method and application thereof. The kapok nano-cellulose aerogel takes nano-cellulose extracted from kapok fibers as a raw material, and is prepared by hydrophobic modification through a silane coupling agent. The method extracts the nano-cellulose from the kapok fiber with rich resources and low price to prepare the oil liquid and the organic solvent adsorption material, can obviously reduce the preparation cost and simplify the production process, and the kapok nano-cellulose aerogel prepared by the method has the excellent performances of low cost, low density, high porosity, degradability and the like, can efficiently adsorb various organic solvents and oil pollutants in sewage, has high adsorption capacity and high speed, can keep the adsorbed oil liquid for a long time without secondary leakage, has good mechanical property, can be repeatedly utilized, and is easy to degrade after being used.
Description
Technical Field
The invention relates to a kapok nano-cellulose aerogel and a preparation method and application thereof, belonging to the technical field of aerogel materials.
Background
In recent years, petroleum pollutants have become one of the main pollutants in water, and cause very serious damage to water areas such as oceans and rivers and surrounding ecological environments. The adsorption method is a main method for treating the oil pollution problem, but the existing commonly used adsorption material still has the problems of high cost, small adsorption quantity, non-recycling, difficult biodegradation, easy secondary pollution and the like. Therefore, the development of an adsorption material which is low in price, simple in preparation process, high in adsorption capacity and capable of being recycled for multiple times is gradually a hot point of research.
Kapok fiber is used as a natural adsorption material, has a unique large hollow structure and excellent adsorption performance, is wide in source, low in price and easy to collect and degrade after being used, is widely applied to the field of oil liquid adsorption, but is still to be improved due to low adsorption capacity (about 20-40 g/g).
The cellulose aerogel has the advantages of high porosity, low density, good adsorption performance and the like, has the characteristics of good biocompatibility, degradability and the like, and is a novel green adsorption material. However, the extraction method of cellulose is complex, the price of raw materials is still relatively high, the environment is easily polluted, the reusability of the cellulose aerogel is poor, the oil liquid recovery step is complex, and secondary pollution is easily caused after adsorption.
Disclosure of Invention
The technical problem solved by the invention is as follows: how to obtain a green adsorption material which has low cost, good adsorption performance, high hydrophobicity and can be recycled.
In order to solve the technical problems, the invention provides a kapok nano-cellulose aerogel, wherein kapok nano-cellulose is extracted by pulping and homogenizing kapok fibers, and is made into aerogel after hydrophobic modification; the density of the aerogel is 2.0-11.0mg/cm3The oil absorption multiplying power is 160-350 g/g, and the contact angle is 150-160 degrees.
The invention also provides a preparation method of the kapok nano cellulose aerogel, which comprises the following steps:
step 1: performing surface treatment on the mechanically crushed kapok fiber by using a NaOH solution, removing wax and other impurities on the surface of the kapok fiber, cleaning the kapok fiber to be neutral by using deionized water, and then putting the kapok fiber into a pulping machine for pulping to obtain kapok pulp; finally, the kapok pulp is put into a high-pressure homogenizer for high-pressure homogenization treatment, and the kapok nano cellulose solution is prepared;
step 2: hydrophobic modification of kapok nanocellulose solution: adding a silane coupling agent into the solution of the ceiba nanocellulose obtained in the step 1, adjusting the pH value, and stirring and reacting at normal temperature to obtain a modified ceiba nanocellulose solution;
and step 3: preparing the kapok nano cellulose aerogel: and (3) placing the modified kapok nano cellulose solution into a mould for freeze forming, and then carrying out freeze drying to obtain the kapok nano cellulose aerogel.
Preferably, the surface treatment in step 1 is specifically: mixing the solution with NaOH solution, and stirring the mixture for 1 to 2 hours at the temperature of 80 ℃, wherein the concentration of the NaOH solution is 10 wt%.
Preferably, the content of the ceiba nanocellulose in the ceiba nanocellulose solution prepared in the step 1 is 0.1-2 wt%.
Preferably, the silane coupling agent in step 2 is vinyltrimethoxysilane; the pH value is adjusted to 3-4 by adopting glacial acetic acid; the adding amount of the silane coupling agent is 0.1-2 mL of the silane coupling agent added in each 100mL of the kapok nano-cellulose solution; the conditions of the stirring reaction are as follows: the stirring speed is 800-1000 rpm, and the time is 3-5 h.
Preferably, the specific conditions of the freeze forming in the step 3 are as follows: freezing for 10h at-20-25 deg.C in refrigerator or 5min at-196 deg.C in liquid nitrogen; the conditions of freeze drying are as follows: the temperature is-60 to-70 ℃ and the time is 48 h.
The invention also provides application of the kapok nano cellulose aerogel in oil-water separation and/or oil-water recovery.
Preferably, the application comprises use in the selective adsorption and/or recovery of one or more of mineral oil, vegetable oil, vacuum pump oil, motor oil and organic solvent.
More preferably, the organic solvent includes any one or more of chloroform, DMF, acetone, DMSO, toluene, cyclohexane, isopropanol, and ethanol.
Preferably, the application comprises application in preparing an oil recovery device.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the method, the kapok nano-cellulose is extracted by pulping and homogenizing the cheap and easily-obtained kapok fiber, and the aerogel is prepared, so that the oil absorption capacity of the aerogel can be remarkably improved, the preparation cost is reduced, and the preparation process is simplified;
2. the ceiba nano cellulose aerogel prepared by the invention has good flexibility, and the density of the ceiba nano cellulose aerogel is 2.0-11.0mg/cm3The adsorption material can selectively and efficiently adsorb various oil liquids and organic solvents such as mineral oil, soybean oil, vacuum pump oil, engine oil, chloroform, DMF (dimethyl formamide), ethanol and the like, and the adsorption rate can reach 350g/g at normal temperature; the oil retention performance is excellent and reaches 97 percent; the hydrophobic effect is good, and the contact angle reaches 150-160 degrees;
3. the ceiba nano cellulose aerogel prepared by the invention has ultrahigh porosity and ultralow density, and can be biodegraded; the kapok nano cellulose aerogel can be recycled, the recycling frequency can reach more than 50 times, the aerogel material has good lipophilicity and hydrophobicity, can be used as an oil-water separation or filtering material, can recover oil, and has wide application prospect.
Drawings
Fig. 1 is a schematic view of an oil recovery apparatus in embodiment 3.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Each of the raw materials used in the following examples is a commercially available product.
Example 1
The embodiment provides a preparation method of a kapok nano-cellulose aerogel adsorbing material, wherein the kapok nano-cellulose obtained after microfibrillation and homogenization treatment is prepared into an even suspension, the pH value of the solution is adjusted to be 3-4, a silane coupling agent is added for hydrophobic modification, and the kapok nano-cellulose aerogel is prepared by a freeze-drying method after freezing. The specific operation steps are as follows:
step one, extracting kapok nanocellulose:
putting the kapok fiber into 10 wt% NaOH solution, treating at 80 ℃ for 1h to remove impurities such as wax on the surface layer of the kapok fiber, and then washing off alkali liquor on the fiber by using deionized water; then pulping the kapok fiber by using a pulping machine to obtain kapok fiber pulp; and homogenizing the kapok pulp in a high-pressure homogenizer to obtain the kapok nanocellulose. Putting a cellulose solution with the kapok nano-cellulose content of 0.4 wt% into a beaker, and stirring for 2 hours at normal temperature by using a magnetic stirrer to obtain a uniform solution;
step two, hydrophobic modification of the kapok nano cellulose solution:
adjusting the pH value of the solution obtained in the step one to 3-4 by using glacial acetic acid, sucking 0.2mL of vinyl trimethoxy silane by using a liquid transfer gun, dropwise adding the vinyl trimethoxy silane into the solution, and stirring for 3 hours by using a magnetic stirrer at normal temperature and at the rotating speed of 800 rpm;
step three, preparing the kapok nano cellulose aerogel:
putting the modified solution into a mould, and freezing for 10h at the temperature of-20 to-25 ℃ in a refrigerator (or freezing for 5min at the temperature of liquid nitrogen-196 ℃); and then freeze-drying for 48 hours at the temperature of-60 to-70 ℃ by using a freeze dryer to obtain the kapok nano-cellulose aerogel.
The density of the prepared kapok nano-cellulose aerogel with the size of 2cm multiplied by 1.2cm is 2.6mg/cm3The contact angle is 151 degrees, the aerogel can be put into the mixed solution of water and chloroform, the aerogel can quickly and selectively adsorb the chloroform solution from the mixed solution, and the adsorption rate is 320 g/g.
Example 2
The embodiment provides a preparation method of a kapok nano-cellulose aerogel adsorbing material, wherein the kapok nano-cellulose obtained after microfibrillation and homogenization treatment is prepared into an even suspension, the pH value of the solution is adjusted to be 3-4, a silane coupling agent is added for hydrophobic modification, and the kapok nano-cellulose aerogel is prepared by a freeze-drying method after freezing. The specific operation steps are as follows:
step one, extracting kapok nanocellulose:
putting the kapok fiber into 10 wt% NaOH solution, treating at 80 ℃ for 1h to remove wax on the surface layer of the kapok fiber, and then washing off alkali liquor on the fiber by using deionized water; then pulping the kapok fiber by using a pulping machine to obtain kapok fiber pulp; and homogenizing the kapok pulp in a high-pressure homogenizer to obtain the kapok nanocellulose. Putting a cellulose solution with the kapok nano-cellulose content of 0.8 wt% into a beaker, and stirring for 2 hours at normal temperature by using a magnetic stirrer to obtain a uniform solution;
step two, hydrophobic modification of the kapok nano cellulose solution:
adjusting the pH value of the solution obtained in the step one to 3-4 by using glacial acetic acid, sucking 0.2mL of vinyl trimethoxy silane by using a liquid transfer gun, dropwise adding the vinyl trimethoxy silane into the solution, and stirring for 3 hours by using a magnetic stirrer at normal temperature and at the rotating speed of 800 rpm;
step three, preparing the kapok nano cellulose aerogel:
putting the modified solution into a mould, and freezing for 10h at the temperature of-20 to-25 ℃ in a refrigerator (or freezing for 5min at the temperature of liquid nitrogen-196 ℃); and then freeze-drying for 48 hours at the temperature of-60 to-70 ℃ by using a freeze dryer to obtain the kapok nano-cellulose aerogel.
The density of the prepared ceiba nanometer cellulose aerogel with the size of 4cm multiplied by 4cm is 4.6mg/cm3The contact angle is 160 degrees, the oil-water emulsion is put into a mixed solution of water and mineral oil, and the mineral oil is collected from the oil-water emulsion by adopting a continuous pump suction method, which comprises the following steps: the aerogel is placed at the head end of a pipe of the suction pump and is put into the oil-water mixed solution, and the pump is started to continuously suck the oil liquid, so that the mineral oil in the mixed solution is selectively filtered and recovered.
Example 3
The embodiment provides a preparation method of a kapok nano-cellulose aerogel adsorbing material, wherein the kapok nano-cellulose obtained after microfibrillation and homogenization treatment is prepared into an even suspension, the pH value of the solution is adjusted to be 3-4, a silane coupling agent is added for hydrophobic modification, and the kapok nano-cellulose aerogel is prepared by a freeze-drying method after freezing. The specific operation steps are as follows:
step one, extracting kapok nanocellulose:
putting the kapok fiber into 10 wt% NaOH solution, treating at 80 ℃ for 1h to remove wax on the surface layer of the kapok fiber, and then washing off alkali liquor on the fiber by using deionized water; then pulping the kapok fiber by using a pulping machine to obtain kapok fiber pulp; and homogenizing the kapok pulp in a high-pressure homogenizer to obtain the kapok nanocellulose. Putting a cellulose solution with the kapok nano-cellulose content of 0.5 wt% into a beaker, and stirring for 2 hours at normal temperature by using a magnetic stirrer to obtain a uniform solution;
step two, hydrophobic modification of the kapok nano cellulose solution:
adjusting the pH value of the solution obtained in the step one to 3-4 by using glacial acetic acid, sucking 0.4mL of vinyl trimethoxy silane by using a liquid transfer gun, dropwise adding the vinyl trimethoxy silane into the solution, and stirring for 3 hours by using a magnetic stirrer at normal temperature and at the rotating speed of 800 rpm;
step three, preparing the kapok nano cellulose aerogel:
putting the modified solution into a mould, and freezing for 10h at the temperature of-20 to-25 ℃ in a refrigerator (or freezing for 5min at the temperature of liquid nitrogen-196 ℃); and then freeze-drying for 48 hours at the temperature of-60 to-70 ℃ by using a freeze dryer to obtain the kapok nano-cellulose aerogel.
The density of the prepared kapok nano-cellulose aerogel with the size of 2cm multiplied by 2cm is 4.6mg/cm3The contact angle is 150 degrees, and the oil absorption multiplying power of the oil absorbing agent for vegetable oil is about 180 g/g. The fluid in the saturated aerogel of absorption can be released out with the fluid recovery unit of a self-control and retrieve, and equipment schematic diagram is as shown in figure 1, and concrete process is as follows:
the rotation of the swiveling wheel through the oil recovery device can release oil in the aerogel, the accumulative release rate can reach 90%, after the oil is released, the aerogel can be reused, the repeated adsorption-release use times can reach more than 50 times, and the release rate of the aerogel can not be obviously reduced. Therefore, the prepared ceiba nano cellulose aerogel can achieve efficient recovery and oil liquid separation and realize repeated recycling of the aerogel.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A kapok nano-cellulose aerogel is characterized in that kapok nano-cellulose is extracted by pulping and homogenizing kapok fibers, and is prepared by carrying out hydrophobic modification on the kapok nano-cellulose; the density of the kapok nano cellulose aerogel is 2.0-11.0mg/cm3The oil absorption multiplying power is 160-350 g/g, and the contact angle is 150-160 degrees.
2. The preparation method of the kapok nano cellulose aerogel of claim 1, which is characterized by comprising the following steps of:
step 1: performing surface treatment on the mechanically crushed kapok fiber by using a NaOH solution, removing wax and other impurities on the surface of the kapok fiber, cleaning the kapok fiber to be neutral by using deionized water, and then putting the kapok fiber into a pulping machine for pulping to obtain kapok pulp; finally, the kapok pulp is put into a high-pressure homogenizer for high-pressure homogenization treatment, and the kapok nano cellulose solution is prepared;
and 2, step: hydrophobic modification of kapok nanocellulose solution: adding a silane coupling agent into the solution of the ceiba nanocellulose obtained in the step 1, adjusting the pH value, and stirring and reacting at normal temperature to obtain a modified ceiba nanocellulose solution;
and step 3: preparing the kapok nano-cellulose aerogel: and (3) freezing and forming the modified kapok nano-cellulose solution, and then carrying out freeze drying to obtain the kapok nano-cellulose aerogel.
3. The preparation method of kapok nano-cellulose aerogel according to claim 2, wherein the surface treatment in the step 1 is specifically: mixing the solution with NaOH solution, and stirring the mixture for 1 to 2 hours at the temperature of 80 ℃, wherein the concentration of the NaOH solution is 10 wt%.
4. The preparation method of kapok nano-cellulose aerogel according to claim 2, wherein the content of the kapok nano-cellulose in the kapok nano-cellulose solution prepared in the step 1 is 0.1-2.0 wt%.
5. The method for preparing kapok nano cellulose aerogel according to claim 2, wherein the silane coupling agent in the step 2 is vinyltrimethoxysilane; the pH value is adjusted to 3-4 by adopting glacial acetic acid; the adding amount of the silane coupling agent is 0.1-2 mL of the silane coupling agent added in each 100mL of the kapok nano-cellulose solution; the conditions of the stirring reaction are as follows: the stirring speed is 800-1000 rpm, and the time is 3-5 h.
6. The preparation method of kapok nano-cellulose aerogel according to claim 2, wherein the specific conditions of the freeze forming in the step 3 are as follows: freezing for 10h at-20-25 deg.C or 5min at-196 deg.C in liquid nitrogen; the conditions of freeze drying are as follows: the temperature is-60 to-70 ℃ and the time is 48 h.
7. Use of the kapok nanocellulose aerogel of claim 1 for oil-water separation and/or oil recovery.
8. Use according to claim 7, wherein the use comprises use for selective adsorption and/or recovery of one or more of mineral oil, vegetable oil, vacuum pump oil, motor oil and organic solvents.
9. The use of claim 8, wherein the organic solvent comprises any one or more of chloroform, acetone, DMSO, toluene, cyclohexane, isopropanol, DMF and ethanol.
10. Use according to claim 7, characterised in that it comprises use in a recovery plant for preparation of oil.
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| CN107840988A (en) * | 2017-11-24 | 2018-03-27 | 中国科学技术大学 | The preparation method and heat preserving and insulating material of a kind of nano-cellulose aerogel |
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| CN110437493B (en) * | 2019-07-15 | 2021-08-06 | 苏州大学 | Preparation method of hydrophilic-oleophobic cellulose/silane coupling agent composite aerogel |
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| CN104609394A (en) * | 2015-02-13 | 2015-05-13 | 东北林业大学 | Preparation method of biomass nano cellulose carbon aerogel |
| CN107840988A (en) * | 2017-11-24 | 2018-03-27 | 中国科学技术大学 | The preparation method and heat preserving and insulating material of a kind of nano-cellulose aerogel |
| CN112898625A (en) * | 2021-02-25 | 2021-06-04 | 山东省科学院新材料研究所 | Underwater elastic cellulose aerogel and preparation method and application thereof |
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