CN111040254A - Cellulose-based photothermal conversion gel material and preparation method thereof - Google Patents
Cellulose-based photothermal conversion gel material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a cellulose-based photothermal conversion gel material and a preparation method thereof, belonging to the technical field of seawater desalination. The method comprises the following steps: dissolving cellulose in an alkaline urea aqueous solution to obtain a cellulose solution; mixing the cellulose solution with components with photo-thermal conversion performance to obtain a precursor solution; and pouring the cellulose solution into the bottom of a mold, freezing the cellulose solution at a temperature of between 10 ℃ below zero and 15 ℃ below zero for 0.5 hour to serve as a lower layer of gel, taking out the gel, pouring the precursor solution into the top of the mold to serve as an upper layer of the gel, continuously freezing the gel for 0.5 hour, fixing and forming the double-layer gel, heating and curing the gel, and washing the gel to obtain the cellulose-based photothermal conversion gel material. The photothermal conversion gel material and the preparation method thereof have the advantages of simple preparation process, short time, lower cost, good controllability, good biodegradability and greenness and environmental protection, and the prepared gel material can efficiently convert absorbed solar energy into heat energy to accelerate the evaporation of water to be cleaned.
Description
Technical Field
The invention relates to the technical field of seawater desalination, and particularly relates to a preparation method of a cellulose-based photothermal conversion gel material.
Background
With the continuous progress of science and technology, the problems of environmental pollution and energy shortage are increasingly highlighted, and research and development of novel green and environment-friendly materials to obtain required resources are an important way for solving the problems of environment and energy. As is well known, sunlight is the most abundant resource in the world and can in principle meet global energy needs, such as solar steam power generation and solar water evaporation. Solar water evaporation technology is a promising technology for pure water and facilitates the use of sustainable energy for water purification. Seawater is the largest water resource pool at present, but cannot be directly drunk or utilized. At present, the seawater desalination method mainly comprises a freezing method, a distillation method, a reverse osmosis method, an electrodialysis method and the like. The methods are already industrially applied in many areas, but the methods depend on and consume a large amount of fuel or electric power seriously, and the popularization and application of solar seawater desalination are limited seriously.
Therefore, if the solar energy is utilized to desalt the sea water and the biological material which is easily obtained in life is used for solar photo-thermal conversion, the cost is greatly reduced and the solar energy-based solar energy desalination system is rapidly popularized and applied to the aspects of sea water desalination and the like. The solar distillation method has the advantages of clean energy, low operating cost, simple equipment and the like, but the water yield per unit area is low. In order to improve the efficiency and yield of fresh water production, researchers invented and prepared a variety of solar water cleaning materials.
The Self-assembly technique is used to deposit gold particles on an aluminum template to produce a highly efficient solar absorber material in the literature "Self-assembly of high elevation plasma absorber for solar step generation" (Science Advances, 2016, 2 (4): e 1501227.). Chinese patent CN108002366A discloses a method for preparing graphene solar water cleaning foam by reducing graphene oxide and freeze-drying.
Chinese patent CN108455556A discloses a carbon foam material with high nitrogen content obtained by high-temperature treatment, which adopts the technical scheme that formaldehyde-melamine foam is carbonized under inert gas atmosphere or vacuum condition after being dried in vacuum, heated to 150-700 ℃ at the heating rate of 4-10 ℃/min, and kept at constant temperature for 1-3 h; and cooling, washing and drying the product to obtain the carbon foam material with high nitrogen content. The method takes melamine foam with ultrahigh nitrogen content as a raw material, and obtains the carbon foam material after high-temperature carbonization.
According to the existing schemes, graphene or melamine is used as a base material of the solar water cleaning foam material, on one hand, the graphene is high in price, the large-scale production cost with the graphene as a main material is very high, and the income brought by the produced clean water energy is probably far lower than the material cost and the energy cost consumed by the production and preparation; on the other hand, graphene and melamine are both materials which are difficult to naturally degrade in natural environment, and cause environmental pollution if the materials cannot be efficiently utilized after large-scale production or cannot be effectively recycled after being put into use for a certain period of time, and the technical difficulty of recycling the melamine and the graphene is not inferior to the difficulty of preparing solar water cleaning foam materials.
Disclosure of Invention
Problem (A)
In summary, how to provide a solar water cleaning material with higher degradability becomes a technical problem to be solved urgently by those skilled in the art.
(II) technical scheme
The invention aims to provide a cellulose-based photothermal conversion gel material and a preparation method thereof, so as to solve the technical problems.
In a first aspect of an embodiment of the present invention, a method for preparing a cellulose-based photothermal conversion gel material is provided, the method including the steps of:
preparing an alkaline aqueous solution, and dissolving cellulose in the alkaline aqueous solution at 0-5 ℃ to obtain a cellulose solution;
mixing the cellulose solution with components with photo-thermal conversion performance to obtain a precursor solution;
and pouring the cellulose solution into the bottom of the mold, freezing the cellulose solution at a temperature of between 10 ℃ below zero and 15 ℃ below zero for 25 to 35 minutes to form a lower layer of gel, taking out the lower layer of gel, pouring the precursor solution into the top of the mold to form an upper layer of gel, continuously freezing the upper layer of gel for 25 to 35 minutes to obtain fixed and formed double-layer gel, heating and curing the fixed and formed double-layer gel, and washing the fixed and formed double-layer gel to obtain the cellulose-based photothermal conversion.
Optionally, the cellulose comprises:
one or more of cotton linters, bamboo fibers, straw fibers, poplar pulp boards, cotton pulp boards, microcrystalline cellulose or α -cellulose.
Optionally, the cellulose is dissolved in an alkaline aqueous solution, and the method further comprises the following steps: the cellulose is dried in an oven at 58-62 ℃.
Optionally, the alkaline aqueous solution comprises:
hydroxide, one or two of urea and thiourea, and deionized water;
wherein, the hydroxide comprises one or more of sodium hydroxide, potassium hydroxide and lithium hydroxide; the mass fraction of the hydroxide is 5-10%, the mass fraction of the urea or thiourea is 5-15%, and the mass fraction of the deionized water is 90-75%.
Optionally, the mass fraction of cellulose in the cellulose solution is 3-20%.
Optionally, the lower layer of the double-layer gel is a cellulose solution, the upper layer of the double-layer gel is a precursor solution, and the mass ratio of the cellulose solution to the precursor solution is 2: 8-8: 2.
optionally, the components with photothermal conversion performance include:
one or more of graphene oxide, reduced graphene oxide, graphene, carbon nanotubes, graphite powder, carbon black and carbon nanofibers.
Optionally, the mass fraction of the components with the photothermal conversion performance in the precursor solution is 0.1-3%.
Optionally, the heating temperature for heating and curing is 30-80 ℃, and the curing time is 1-24 h.
In a second aspect of the embodiments of the present invention, a cellulose-based photothermal conversion gel material is further provided, which is prepared by the preparation method of the cellulose-based photothermal conversion gel material of the present invention.
(III) technical effects
The invention uses cellulose as a base material, and prepares the cellulose-based gel material with higher photothermal conversion efficiency by doping photothermal conversion material and gelatinizing the mixed solution through simple and short-time operation, the cellulose has strong hydrophilicity, wide sources and relatively low cost, compared with the prior art, the gel material obtained by the photothermal conversion material provided by the invention has higher hydrophilicity, porosity and high-efficiency photothermal conversion efficiency, and the cellulose as the base material can be completely and naturally degraded and is environment-friendly; and the preparation method is simple, the cost is lower, and the large-scale production is facilitated.
Furthermore, the porous structure of the gel material can be regulated and controlled by regulating the quantity and the ratio of the cellulose and the photothermal conversion material, and the photothermal conversion efficiency, the strength and the elasticity of the gel are regulated, so that the water evaporation speed is controlled.
Drawings
Fig. 1 is a graph comparing the change curves of the mass of water in a container under sunlight which is not covered with and covered with the cellulose-based photothermal conversion gel material of example 1 of the present invention.
Detailed Description
For a further understanding of the present invention, reference will now be made in detail to the embodiments illustrated in the drawings. The examples are given solely for the purpose of illustration and are not intended to limit the scope of the invention. Therefore, it is within the scope of the present invention to design the structure and the embodiments similar to the technical solutions without various inventive changes or modifications without departing from the spirit of the present invention.
In order to solve the technical problem, the technical scheme adopted by the invention is as follows: and adding the photo-thermal conversion material powder or dispersion into a cellulose solution, and curing and forming to prepare the hydrophilic porous gel material. The gel material not only can effectively convert absorbed sunlight into heat energy to accelerate the evaporation of water to be cleaned, but also has good biodegradability. As an implementation, the method specifically includes the following steps:
(1) preparation of cellulose solution: dissolving cellulose in an alkaline aqueous solution at 0-5 ℃ to obtain a cellulose solution;
(2) preparing a precursor solution: dispersing components with the photo-thermal conversion performance into the cellulose solution, and uniformly mixing to obtain a precursor solution;
(3) curing and molding the gel: pouring the cellulose solution obtained in the step (1) into the bottom of a mould, freezing the cellulose solution at a temperature of between 10 ℃ below zero and 15 ℃ below zero for 25 to 35 minutes (preferably 30 minutes) to serve as a lower layer of gel, taking out the gel, pouring the precursor solution obtained in the step (2) into the top of the mould to serve as an upper layer of gel, wherein the mass ratio of the cellulose solution to the precursor solution is 8: 2, continuously freezing the gel for 25-35 minutes (preferably 30 minutes), fixing and forming the double-layer gel, heating and curing, and washing to obtain the cellulose-based photothermal conversion gel material;
(4) and (3) cleaning the gel: and repeatedly washing with deionized water for many times to remove residual reagents, thereby obtaining the cellulose-based photothermal conversion gel material.
In the embodiment of the invention, cellulose refers to a raw material with a high cellulose content, and can be one or more of cotton linters, bamboo fibers, straw fibers, poplar pulp boards, cotton pulp boards, microcrystalline cellulose, α -cellulose and the like, preferably, the cellulose raw material is dried in an oven at 58-62 ℃ before being dissolved until the quality is stable, namely, the difference of the measured quality change in a preset time is within a preset threshold range.
To further illustrate the invention, several specific examples are listed below:
example 1
S11, preparation of cellulose solution: the mass fraction of sodium hydroxide, the mass fraction of urea and the mass fraction of deionized water in the alkaline aqueous solution are respectively 5%, 5% and 90%. Weighing microcrystalline cellulose with the mass fraction of 5.5%, dissolving the microcrystalline cellulose in an alkaline aqueous solution with the mass fraction of 92% at 5 ℃, and fully stirring for 0.5h until the solution is transparent;
s12, preparation of precursor solution: weighing 2.5% by mass of the carbon nanotube aqueous dispersion, adding the aqueous dispersion into the fiber solution which is fully dissolved, and fully and uniformly stirring at low temperature;
s13, curing and molding the gel: pouring the cellulose solution into the bottom of a mold, freezing the cellulose solution at-10 ℃ for 0.5 hour to serve as a lower layer of gel, taking out the gel, pouring the precursor solution into the top of the mold to serve as an upper layer of gel, wherein the mass ratio of the cellulose solution to the precursor solution is 4: continuously freezing the gel for 0.5 hour, fixing and forming the upper layer gel and the lower layer gel, and then placing the gel into a 60 ℃ oven for curing for 3 hours;
s14, washing gel: and taking the gel out of the mold, and repeatedly washing the gel with deionized water for many times to remove residual reagents to obtain the cellulose photothermal conversion gel material gel.
Tests prove that the cellulose-based photothermal conversion gel material prepared in the embodiment can improve the evaporation speed of water in a container by 3.1 times under sunlight, and the salt removal rate of the cellulose-based photothermal conversion gel material prepared in the embodiment is more than 99.5%.
Example 2
S21, preparation of cellulose solution: the mass fraction of lithium hydroxide, the mass fraction of urea and the mass fraction of deionized water in the alkaline aqueous solution are respectively 10%, 15% and 75%. Weighing microcrystalline cellulose with the mass fraction of 15.5%, dissolving the microcrystalline cellulose in 84% of alkaline aqueous solution with the mass fraction at 0 ℃, and fully stirring for 1h until the solution is transparent;
s22, preparation of precursor solution: weighing 0.5 mass percent of carbon nano tube water dispersion, adding the water dispersion into the fiber solution which is fully dissolved, and fully and uniformly stirring at low temperature;
s23, curing and molding the gel: pouring the cellulose solution into the bottom of a mold, freezing the cellulose solution at-10 ℃ for 0.5 hour to serve as a lower layer of gel, taking out the gel, pouring the precursor solution into the top of the mold to serve as an upper layer of gel, wherein the mass ratio of the cellulose solution to the precursor solution is 6: 4, continuously freezing the gel for 0.5 hour, fixing and forming the upper layer gel and the lower layer gel, and then placing the gel into a 65 ℃ oven for curing for 3 hours;
s24, washing gel: and taking the gel out of the mold, and repeatedly washing the gel with deionized water for many times to remove residual reagents to obtain the cellulose photothermal conversion gel material gel.
The cellulose-based photothermal conversion gel material prepared in this example can increase the evaporation rate of water in the container by 1.9 times under the same sunlight irradiation conditions.
Example 3
S31, preparation of cellulose solution: the mass fraction of potassium hydroxide, the mass fraction of urea and the mass fraction of deionized water in the alkaline aqueous solution are respectively 8%, 10% and 82%. Weighing 4.6% by mass of cotton linters, dissolving the cotton linters in 95% by mass of alkaline aqueous solution at 0 ℃, and fully stirring for 0.5h until the solution is transparent;
s32, preparation of precursor solution: weighing reduced graphene oxide aqueous dispersion with the mass fraction of 0.4%, adding the reduced graphene oxide aqueous dispersion into the fiber solution which is fully dissolved, and fully and uniformly stirring at low temperature;
s33, curing and molding the gel: pouring the cellulose solution into the bottom of a mold, freezing the cellulose solution at-10 ℃ for 0.5 hour to serve as a lower layer of gel, taking out the gel, pouring the precursor solution into the top of the mold to serve as an upper layer of the gel, wherein the mass ratio of the cellulose solution to the precursor solution is 5: 5, continuously freezing the gel for 0.5 hour, fixing and forming the upper layer gel and the lower layer gel, and then placing the gel into a 70 ℃ oven for curing for 2 hours;
s34, washing gel: and taking the gel out of the mold, and repeatedly washing the gel with deionized water for many times to remove residual reagents to obtain the cellulose photothermal conversion gel material gel.
Example 4
S41, preparation of cellulose solution: the mass fraction of sodium hydroxide, thiourea and deionized water in the alkaline aqueous solution is 8%, 12% and 80%, respectively. Weighing a cotton pulp plate with the mass fraction of 6%, dissolving the cotton pulp plate in an alkaline aqueous solution with the mass fraction of 90% at 5 ℃, and fully stirring for 1h until the solution is transparent;
s42, preparation of precursor solution: weighing 3% by mass of the carbon nanotube aqueous dispersion, adding the carbon nanotube aqueous dispersion into the fiber solution which is fully dissolved, and fully and uniformly stirring at a low temperature;
s43, curing and molding the gel: pouring the cellulose solution into the bottom of a mold, freezing the cellulose solution at-15 ℃ for 0.5 hour to serve as a lower layer of gel, taking out the gel, pouring the precursor solution into the top of the mold to serve as an upper layer of gel, wherein the mass ratio of the cellulose solution to the precursor solution is 2: 8, continuously freezing the gel for 0.5 hour, fixing and forming the upper layer gel and the lower layer gel, and then placing the gel into a 70 ℃ oven for curing for 2 hours;
and S44, taking the gel out of the mold, and repeatedly washing the gel with deionized water for multiple times to remove residual reagents to obtain the cellulose photothermal conversion gel material gel.
The cellulose-based photothermal conversion gel material prepared in the embodiment can increase the evaporation rate of water in the container by 2.8 times under the same sunlight irradiation condition.
Example 5
S51, preparation of cellulose solution: the mass fraction of sodium hydroxide, thiourea and deionized water in the alkaline aqueous solution is 6%, 8% and 86%. Weighing microcrystalline cellulose with the mass fraction of 7%, dissolving the microcrystalline cellulose in 88% of alkaline aqueous solution with the mass fraction at the temperature of 3 ℃, and fully stirring for 0.5h until the solution is transparent;
s52, preparation of precursor solution: weighing 2.6 mass percent of carbon nano tube water dispersion, adding the water dispersion into the fiber solution which is fully dissolved, and fully and uniformly stirring at low temperature;
s53, curing and molding the gel: pouring the cellulose solution into the bottom of a mold, freezing the cellulose solution at-10 ℃ for 0.5 hour to serve as a lower layer of gel, taking out the gel, pouring the precursor solution into the top of the mold to serve as an upper layer of gel, wherein the mass ratio of the cellulose solution to the precursor solution is 4: continuously freezing the gel for 0.5 hour, fixing and forming the upper layer gel and the lower layer gel, and then placing the gel into a 50 ℃ oven for curing for 3 hours;
s54, washing gel: and taking the gel out of the mold, and repeatedly washing the gel with deionized water for many times to remove residual reagents to obtain the cellulose photothermal conversion gel material gel.
The cellulose-based photothermal conversion gel material prepared in the embodiment can increase the evaporation rate of water in the container by 2.3 times under the same sunlight irradiation condition.
Example 6
S61, preparation of cellulose solution: in the alkaline aqueous solution, the mass fraction of sodium hydroxide is 8%, the mass fraction of urea is 5%, the mass fraction of thiourea is 5%, and the mass fraction of deionized water is 82%. Weighing a cotton pulp plate with the mass fraction of 5.5%, dissolving the cotton pulp plate in an alkaline aqueous solution with the mass fraction of 92% at the temperature of 3 ℃, and fully stirring for 0.5h until the solution is transparent;
s62, preparation of precursor solution: weighing 1.5 mass percent of graphene oxide aqueous dispersion, adding the graphene oxide aqueous dispersion into the fiber solution which is fully dissolved, and fully and uniformly stirring at low temperature;
s63, curing and molding the gel: pouring the cellulose solution into the bottom of a mold, freezing the cellulose solution at-10 ℃ for 0.5 hour to serve as a lower layer of gel, taking out the gel, pouring the precursor solution into the top of the mold to serve as an upper layer of gel, wherein the mass ratio of the cellulose solution to the precursor solution is 4: continuously freezing the gel for 0.5 hour, fixing and forming the upper layer gel and the lower layer gel, and then placing the gel into a 50 ℃ oven for curing for 6 hours;
s64, washing gel: and taking the gel out of the mold, and repeatedly washing the gel with deionized water for many times to remove residual reagents to obtain the cellulose photothermal conversion gel material gel.
The cellulose-based photothermal conversion gel material prepared in the embodiment can increase the evaporation rate of water in the container by 2.5 times under the same sunlight irradiation condition.
In conclusion, compared with the prior art, the preparation method provided by the embodiment of the invention has the advantages that the process is simple, the preparation time is short, the cost is lower, the controllability is good, the prepared gel material can efficiently convert absorbed solar energy into heat energy to accelerate the evaporation of water to be cleaned, the main material is cellulose which is easier to degrade in the natural environment, and the preparation method is more environment-friendly. The restriction factors for large-scale production are fewer, and the realization is easier.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In summary, this summary should not be construed to limit the present invention.
Claims (10)
1. A preparation method of a cellulose-based photothermal conversion gel material is characterized by comprising the following steps:
preparing an alkaline aqueous solution, and dissolving cellulose in the alkaline aqueous solution at 0-5 ℃ to obtain a cellulose solution;
mixing the cellulose solution with components with photo-thermal conversion performance to obtain a precursor solution;
and pouring the cellulose solution into the bottom of a mold, freezing the cellulose solution at the temperature of between 10 ℃ below zero and 15 ℃ below zero for 25 to 35 minutes to serve as a lower layer of gel, taking out the gel, pouring the precursor solution into the top of the mold to serve as an upper layer of the gel, continuously freezing the gel for 25 to 35 minutes to obtain fixed and formed double-layer gel, heating and curing the gel, and washing the gel to obtain the cellulose-based photothermal conversion gel material.
2. The method of preparing a cellulose-based photothermal conversion gel material according to claim 1, wherein the cellulose comprises:
one or more of cotton linters, bamboo fibers, straw fibers, poplar pulp boards, cotton pulp boards, microcrystalline cellulose or α -cellulose.
3. The method for preparing a cellulose-based photothermal conversion gel material according to claim 1, wherein the cellulose is dissolved in an alkaline aqueous solution, and the method further comprises the following steps: the cellulose is dried in an oven at 58-62 ℃.
4. The method of preparing a cellulose-based photothermal conversion gel material according to claim 1, wherein the composition of the alkaline aqueous solution comprises:
hydroxide, one or two of urea and thiourea, and deionized water;
wherein the hydroxide comprises one or more of sodium hydroxide, potassium hydroxide and lithium hydroxide; the mass fraction of the hydroxide is 5-10%, the mass fraction of the urea or thiourea is 5-15%, and the mass fraction of the deionized water is 75-90%.
5. The method for preparing a cellulose-based photothermal conversion gel material according to claim 1, wherein the mass fraction of the cellulose in the cellulose solution is 3% to 20%.
6. The method for preparing the cellulose-based photothermal conversion gel material according to claim 1, wherein the lower layer of the double-layer gel is the cellulose solution, and the upper layer is the precursor solution, wherein the mass ratio of the cellulose solution to the precursor solution is 2: 8-8: 2.
7. the method for preparing a cellulose-based photothermal conversion gel material according to claim 1, wherein the components having photothermal conversion properties comprise:
one or more of graphene oxide, reduced graphene oxide, graphene, carbon nanotubes, graphite powder, carbon black and carbon nanofibers.
8. The method for preparing a cellulose-based photothermal conversion gel material according to claim 1, wherein the mass fraction of the component having photothermal conversion performance in the precursor solution is 0.1-3%.
9. The method of preparing a cellulose-based photothermal conversion gel material according to any one of claims 1 to 8, wherein the heating temperature for the heat curing is 30 to 80 ℃ and the curing time is 1 to 24 hours.
10. A cellulose-based photothermal conversion gel material prepared by the method of any one of claims 1 to 9.
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