CN111204829B - Solar sewage purification aerogel based on waste paper and graphite and preparation method thereof - Google Patents
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- C02F1/02—Treatment of water, waste water, or sewage by heating
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Abstract
The invention discloses a preparation method of solar sewage purification aerogel based on waste paper and ball-milled graphite, which comprises the following steps: (1) adding graphite powder, N-methyl pyrrolidone (NMP) and ball milling balls into a ball milling tank, and obtaining ball milling graphite by adopting a ball milling method; (2) adding the obtained ball-milled graphite and concentrated sulfuric acid into a container, heating and carrying out acid treatment to obtain acidified ball-milled graphite; (3) adding waste paper scraps into a mixed solution of water, NaOH and thiourea, and carrying out ball milling and freeze drying to obtain ball-milled cellulose; (4) adding cellulose and alcohol into the acid-treated ball-milled graphite dispersion liquid, carrying out ultrasonic treatment, and carrying out freeze casting and freeze drying to obtain the ball-milled graphite/cellulose composite aerogel. The ball-milled graphite/cellulose aerogel prepared by the invention has excellent hydrophilic property, extremely low density, extremely high porosity and extremely low thermal conductivity, and the size and thickness of the aerogel are controllable, so that the aerogel can be used as an efficient light and hot water treatment material for purifying sewage and desalinating seawater.
Description
Technical Field
The invention belongs to the field of solar energy hot water evaporation materials, and particularly relates to a solar sewage purification aerogel based on waste paper and graphite and a preparation method thereof.
Background
With the rapid development of nanotechnology, solar energy has become an indispensable clean renewable natural resource in industrial manufacturing and daily life of residents. At the same time, the world is facing the crisis of shortage of clean water due to the growing pollution and explosive population growth. In the solar water-heating-water-evaporating technology, harmful chemical substances are not involved, and artificial energy sources such as fuel, electric power and the like are not consumed, so that the solar water-heating-water-evaporating technology is considered to be one of the most promising sewage purification and seawater desalination methods at present. The development of efficient photothermal conversion materials by directly converting solar radiation into heat energy to generate steam is a major challenge in realizing sustainable and large-scale application of solar evaporation technology in the fields of water purification, desalination and the like.
Recently, a plasma absorber and noble metal nanoparticles have been widely studied as a photothermal material. However, these photothermal materials involve either expensive raw materials or complicated synthetic processes, which hinders their industrial manufacture and scale-up applications. Further, photo-thermal materials based on carbon materials, polymer-derived materials, carbonized materials, biomimetic materials, and the like have recently received much attention. These photothermal materials are typically fabricated as sheets or films that float on the surface of water. The gas-water interface is then heated by solar energy to produce steam. However, in the case of sheet-like or film-like photothermal, when they float on water (direct contact), a large amount of heat is lost to water, resulting in low photothermal conversion efficiency.
Three-dimensional porous photothermal materials such as polymer hydrogel, sponge, carbon aerogel and the like are widely concerned in solar hot water treatment due to the advantages of low volume density, high porosity, low heat conduction and the like. Graphene aerogel is emerging as a three-dimensional photo-thermal material for solar steam generation. However, in previous studies, the graphene sheets used to make aerogels were generally derived from graphene oxide, which required a complex series of preparation steps involving expensive and toxic chemicals and huge energy consumption. In addition, the solar water evaporation rate of the developed porous photothermal materials, such as graphene aerogel and the like, is 1.4kgm-2h-1The following. In summary, the rare and expensive materials, sophisticated processes and low solar evaporation rates have hindered the practical application of photothermal materials in solar water purification.
The method for preparing the few-layer graphite has the advantages that the waste paper is used for preparing the cellulose, the waste recycling is realized, the acidified ball-milled graphite is obtained through ball milling and acid treatment, the novel method for preparing the few-layer graphite is provided, a large amount of pollution caused by preparation of graphene through a graphene oxide approach is avoided, the material preparation cost is greatly reduced, and the large-batch industrial production is easy to realize.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the technical problems in the prior art, the invention provides a solar sewage purification aerogel based on waste paper and graphite and a preparation method thereof.
The technical scheme is as follows: the invention relates to a preparation method of waste paper and graphite-based solar sewage purification aerogel, which comprises the following steps:
(1) ball milling of graphite powder: taking stone ink powder, N-methyl pyrrolidone (NMP) and zirconia balls, performing ball milling, filtering and drying to obtain ball-milled graphite powder;
(2) acidifying ball-milling graphite powder: mixing the ball-milled graphite powder obtained in the step (1) with concentrated sulfuric acid, stirring in a water bath at 60-80 ℃ to obtain acidified ball-milled graphite, repeatedly filtering and washing with deionized water, and freeze-drying to obtain acidified ball-milled graphite powder;
(3) preparing cellulose by using waste paper: mixing water, NaOH and thiourea to obtain a mixed solution, adding waste paper scraps into the mixed solution, stirring for 2-3h, freezing for 12-24h, and then carrying out ball milling for 4-6 h; centrifuging the obtained solution, repeatedly centrifuging and washing with deionized water until the pH of the supernatant is 8-9, and freeze-drying the centrifuged product to obtain cellulose;
(4) ball-milling graphite cellulose composite aerogel: dispersing the acidified ball-milled graphite powder obtained in the step (2) in water to prepare 6-21 mg/mL-1Adding the cellulose and alcohol obtained in the step (3) into the acidified ball-milled graphite dispersion liquid, and performing ultrasonic treatment; and pouring the ultrasonic solution into a mold, freezing the mold in a liquid nitrogen environment for 5-10min, and then putting the mold into a freeze drying box for drying to obtain the ball-milled graphite cellulose composite aerogel.
In the step (1), 0.4-0.8g of graphite powder, 15-25mL of N-methylpyrrolidone and 180g of zirconia balls 120-. Wherein the zirconia balls have two sizes, the diameters are 0.1-0.3mm and 1-3mm respectively, and the mass ratio is 1: 1.
In the step (1), the drying after ball milling filtration means ball milling for 4-8h, filtering the obtained mixed solution, and then drying at 60-80 ℃ for 1.5-2.5 h.
In the step (2), 3-5g of the ball-milled graphite powder obtained in the step (1) is mixed with 30-50mL of concentrated sulfuric acid.
In the step (2), continuously stirring for 4-6h in a water bath at 60-80 ℃.
In the step (2), repeatedly filtering and washing with deionized water until the pH value of the supernatant is 5-6.
In the step (3), 1-2g of waste paper scraps are added into a mixed solution of 50-150ml of water, 1-3g of NaOH and 5-15g of thiourea. And centrifuging the solution obtained by ball milling at the rotating speed of 3000-.
And (4) taking 40ml of acidified ball-milled graphite dispersion liquid, adding 30-105mg of cellulose obtained in the step (3) and 1-2ml of alcohol, and carrying out ultrasonic treatment for 20-40 min. Preferably, the mass ratio of the acidified ball-milled graphite to the cellulose is 6:1, and the composite aerogel prepared by the method has the most excellent mechanical properties.
In the step (4), the mold is a mold having a metal bottom and a polypropylene (PP) wall surface, and preferably a polypropylene mold having an aluminum metal bottom. The polypropylene material has good low temperature resistance and low thermal conductivity, the metal has low temperature resistance and high thermal conductivity, and the mould can realize the directional freezing of the solution into ice.
Further, the mold was placed on a metal platform in liquid nitrogen so that the liquid nitrogen contacted the bottom of the mold.
The ball-milled graphite cellulose aerogel prepared according to the method is also within the protection scope of the invention. The thickness of the ball-milling graphite cellulose aerogel is 5-10 mm.
The ball-milled graphite/cellulose aerogel prepared by the method has excellent hydrophilic performance, can quickly transmit water to an interface of the ball-milled graphite flake and cellulose, and realizes quick photo-thermal water evaporation; the density is very low and is 15mg/cm3The density of the ball-milled graphite/cellulose aerogel can be reduced as required, and the subsequent evaporation and condensation device is light; the material has extremely high porosity (99 percent), and is beneficial to the transmission of liquid water and the diffusion of water vapor; has extremely low thermal conductivity (0.042W/mK), is beneficial to heat accumulation in the aerogel, thereby realizing higher water evaporation rate andthe light-heat conversion efficiency; the size and thickness are controllable, and different application occasions can be met.
Has the advantages that: the application relates to a preparation method of solar sewage purification aerogel based on waste paper and graphite, which comprises the following steps: (1) the few-layer graphite flake is prepared by ball milling and acid treatment, so that large-scale and low-cost production of acidified ball-milled graphite can be realized, the few-layer graphite has physical and chemical properties which are comparable to those of graphene, and the method is simple and pollution-free; (2) the cellulose is prepared from the waste paper, so that the waste utilization is realized, the raw material cost is reduced, and the environment is protected; (3) by using a liquid nitrogen freezing method and a special die, large-area ball-milled graphite/cellulose aerogel can be quickly prepared in a large scale, the energy consumption is reduced, and the mass production is possible; (4) compared with other methods, the method has the advantages of simpler process, lower cost and more environment-friendly materials. The ball-milled graphite/cellulose aerogel prepared by the method has excellent performance and wide application range.
Drawings
FIG. 1 is a scanning electron microscope image of the cross section and the side surface of the ball-milled graphite/cellulose aerogel obtained by the present invention with different magnifications;
FIG. 2 is an X-ray diffraction pattern (a) and a Raman pattern (b) of crystalline flake graphite and acidified ball milled graphite (BG);
fig. 3(a) - (b) are water evaporation rate and temperature rise comparison under one sunlight irradiation for ball-milled graphite cellulose aerogel BGCA prepared in step (4) with ball-milled graphite/cellulose mass ratio of 1:1, 4:1, and 8:1, respectively;
FIGS. 3(c) - (d) are respectively a comparison of the water evaporation rate and the temperature of the ball-milled graphite cellulose aerogel with the thickness of 5-10mm under the irradiation of sunlight, wherein the mass ratio of the ball-milled graphite to the cellulose is fixed to 6:1 in the step (4);
fig. 4 is a comparison of the evaporation rate and the photothermal efficiency of the graphene-fiber aerogel prepared according to the present invention with those of the prior art.
Detailed Description
The present application will be described in detail with reference to specific examples.
Example 1
A preparation method of solar sewage purification aerogel based on waste paper and graphite comprises the following steps:
(1) adding 0.4g of graphite powder, 15mL of N-methylpyrrolidone (NMP) and 120g of two zirconia balls into a zirconia ball milling tank, carrying out ball milling for 4 hours, filtering the obtained mixed solution, drying at 60 ℃ for 1.5 hours, and grinding to obtain ball-milled graphite powder;
(2) 3g of ball-milled graphite powder and 30mL of concentrated sulfuric acid were added to a vessel and stirred continuously in a water bath at 80 ℃ for 4 hours. Repeatedly filtering and washing the obtained acidified ball-milled graphite by using deionized water until the pH value of the supernatant is 6, and obtaining acidified ball-milled graphite powder by adopting a freeze-drying method;
(3) adding 1g of waste paper scraps into a mixed solution of 50ml of water, 1g of NaOH and 5g of thiourea, stirring for 2 hours, putting the mixture into a refrigerator, freezing for 12 hours, and then ball-milling for 4 hours; centrifuging the obtained solution at 4000rpm for 5min, repeatedly centrifuging and washing with deionized water until the pH of the supernatant is 9, and freeze-drying the centrifuged product to obtain cellulose;
(4) weighing the acidified ball-milled graphite obtained in the step (2), and dispersing the acidified ball-milled graphite in water to prepare 6mg mL-1Adding 30g of cellulose and 2ml of alcohol into 40ml of acidified ball-milled graphite dispersion liquid, and carrying out ultrasonic treatment for 20 min; pouring the ultrasonic solution into a mold with a metal bottom and a polypropylene (PP) wall surface, placing the mold on a metal platform placed in liquid nitrogen to enable the liquid nitrogen to contact the bottom of the mold, freezing for 5min, and then placing the mold into a freeze drying box for drying to obtain the ball-milled graphite cellulose composite aerogel.
(5) When the mass ratio of the ball-milled graphite to the cellulose is 6:1, the composite aerogel obtains a regular pore structure, the ball-milled graphite sheets are arranged in an oriented manner, and the cellulose bridges the graphite sheets to form a three-dimensional network structure, as shown in fig. 1.
Example 2
A preparation method of solar sewage purification aerogel based on waste paper and graphite comprises the following steps:
(1) adding 0.6g of graphite powder, 20mL of N-methylpyrrolidone (NMP) and 150g of two zirconia balls into a zirconia ball milling tank, carrying out ball milling for 6 hours, filtering the obtained mixed solution, drying at 80 ℃ for 2 hours, and grinding to obtain ball-milled graphite powder;
(2) 4g of ball-milled graphite powder and 40mL of concentrated sulfuric acid were added to the vessel and stirred continuously in a water bath at 80 ℃ for 5 hours. Repeatedly filtering and washing the obtained acidified ball-milled graphite by using deionized water until the pH of a supernatant is 5-6, and obtaining acidified ball-milled graphite powder by adopting a freeze-drying method; compared with the flake graphite raw material (graphite) (Guangdong Tianrun electronic materials Co., Ltd.), the prepared ball-milled graphite flake (BG) has greatly reduced peak intensity (26 ℃) of X-ray diffraction peak and enlarged peak width, which indicates that the flake graphite is ball-milled into a tiny nanosheet structure, as shown in FIG. 2 a; in addition, the flake graphite after ball milling introduces a large number of defects into the ball milled graphite, and the intensity of D/G in Raman spectrum increases, as shown in FIG. 2 b.
(3) Adding 2g of waste paper scraps into a mixed solution of 100ml of water, 2g of NaOH and 10g of thiourea, stirring for 3 hours, putting the mixture into a refrigerator, freezing for 18 hours, and then carrying out ball milling for 6 hours; centrifuging the obtained solution at 5000rpm for 10min, repeatedly centrifuging and washing with deionized water until the pH of the supernatant is 8-9, and freeze drying the centrifuged product to obtain cellulose.
(4) Weighing the acidified ball-milled graphite obtained in the step (2), and dispersing the acidified ball-milled graphite in water to prepare 12mg mL-1Adding 60mg of cellulose and 2ml of alcohol into 50ml of acidified ball-milled graphite dispersion liquid, and carrying out ultrasonic treatment for 30 min; pouring the ultrasonic solution into a mold with a metal bottom and a polypropylene (PP) wall surface, placing the mold on a metal platform placed in liquid nitrogen to enable the liquid nitrogen to contact the bottom of the mold, freezing for 8min, and then placing the mold into a freeze drying box for drying to obtain the ball-milled graphite cellulose composite aerogel.
(5) When the prepared composite aerogel is used as a light hot water evaporation material, compared with pure water, the water evaporation rate in the ball-milled graphite/cellulose aerogel is greatly increased, as shown in fig. 3 a; as the concentration of the ball-milled graphite/cellulose increases, the evaporation rate of water in the composite aerogel increases with the temperature, as shown in fig. 3 b. When the ball-milled graphite/cellulose ratio is 8:1, the water evaporation rate and temperature in the composite aerogel are highest.
(6) Preparing a composite aerogel with a thickness of 5-10mm when the ratio of the fixed ball-milled graphite to the cellulose is 6:1, and having the fastest water evaporation rate when the aerogel thickness is 7mm, as shown in fig. 3 c; when the composite aerogel had a thickness of 5mm, it had the highest surface temperature, as shown in fig. 3 d.
Example 3
A preparation method of solar sewage purification aerogel based on waste paper and graphite comprises the following steps:
(1) adding 0.8g of graphite powder, 25mL of N-methylpyrrolidone (NMP) and 180g of two zirconia balls into a zirconia ball milling tank, carrying out ball milling for 8 hours, filtering the obtained mixed solution, drying at 80 ℃ for 2.5 hours, and grinding to obtain ball-milled graphite powder;
(2) 5g of ball-milled graphite powder and 50mL of concentrated sulfuric acid were added to a vessel and stirred continuously in a water bath at 80 ℃ for 6 hours. Repeatedly filtering and washing the obtained acidified ball-milled graphite by using deionized water until the pH of a supernatant is 5-6, and obtaining acidified ball-milled graphite powder by adopting a freeze-drying method;
(3) adding 2g of waste paper scraps into a mixed solution of 150ml of water, 3g of NaOH and 10g of thiourea, stirring for 3 hours, putting the mixture into a refrigerator, freezing for 24 hours, and then carrying out ball milling for 6 hours; centrifuging the obtained solution at 5000rpm for 5-10min, repeatedly centrifuging and washing with deionized water until the pH of the supernatant is 8-9, and freeze drying the centrifuged product to obtain cellulose;
(4) weighing the acidified ball-milled graphite obtained in the step (2), and dispersing the acidified ball-milled graphite in water to prepare 21mg mL-1Adding 105mg of cellulose and 2ml of alcohol into 40ml of the acidified ball-milled graphite dispersion liquid, and carrying out ultrasonic treatment for 40 min; pouring the ultrasonic solution into a mold with a metal bottom and a polypropylene (PP) wall surface, placing the mold on a metal platform placed in liquid nitrogen to enable the liquid nitrogen to contact the bottom of the mold, freezing for 10min, and then placing the mold into a freeze drying box for drying to obtain the ball-milled graphite cellulose composite aerogel.
(5) When the mass ratio of the ball-milled graphite to the cellulose in the prepared composite aerogel is controlled to be 8:1 and the thickness of the aerogel is 7mm, the obtained photo-thermal water evaporation rate is superior to that of most reported photo-thermal water evaporation materials, as shown in figure 4.
Claims (6)
1. A preparation method of solar sewage purification aerogel based on waste paper and graphite is characterized by comprising the following steps:
(1) ball milling of graphite powder: taking 0.4-0.8g of graphite powder, 15-25mL of N-methylpyrrolidone and 120-180g of zirconia balls, carrying out ball milling for 4-8h, filtering the obtained mixed solution, and then drying at 60-80 ℃ for 1.5-2.5h to obtain ball-milled graphite powder;
(2) acidifying ball-milling graphite powder: mixing 3-5g of ball-milled graphite powder obtained in the step (1) with 30-50mL of concentrated sulfuric acid, heating and acidifying to obtain acidified ball-milled graphite, repeatedly filtering and washing with deionized water until the pH value of supernatant is 5-6, and then freeze-drying to obtain acidified ball-milled graphite powder;
(3) preparing cellulose by using waste paper: mixing water, NaOH and thiourea to obtain a mixed solution, adding waste paper scraps into the mixed solution, stirring for 2-3h, freezing for 12-24h, and then carrying out ball milling for 4-6 h; centrifuging the obtained solution, repeatedly centrifuging and washing with deionized water until the pH of the supernatant is 8-9, and freeze-drying the centrifuged product to obtain cellulose;
(4) ball-milling graphite cellulose composite aerogel: dispersing the acidified ball-milled graphite powder obtained in the step (2) in water to prepare 6-21 mg/mL-1Adding the cellulose and alcohol obtained in the step (3) into the acidified ball-milled graphite dispersion liquid, and performing ultrasonic treatment; and pouring the ultrasonic solution into a mold, placing the mold in a liquid nitrogen environment for freezing, and then placing the mold into a freeze drying box for drying to obtain the ball-milled graphite cellulose composite aerogel.
2. The method of claim 1, wherein the zirconia balls have two sizes, the diameters of which are 0.1-0.3mm and 1-3mm, respectively, and the mass ratio is 1: 1.
3. The method for preparing waste paper and graphite-based solar sewage purifying aerogel according to claim 1, wherein 1-2g of waste paper scrap is added to a mixed solution of 50-150ml of water, 1-3g of NaOH and 5-15g of thiourea in step (3).
4. The method for preparing waste paper and graphite-based solar sewage purification aerogel according to claim 1, wherein in step (4), 30-105mg of the cellulose of step (3) and 1-2ml of alcohol are added to 40ml of acidified ball-milled graphite dispersion, and the mixture is subjected to ultrasonic treatment for 20-40 min.
5. The method for preparing waste paper and graphite-based solar sewage purifying aerogel according to claim 1, wherein in step (4), the molds are molds having a metal bottom and a polypropylene wall surface.
6. The ball-milled graphitic cellulose aerogel prepared by the method of any one of claims 1-5.
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