CN111517793A - Graphitized carbonized rice hull foam photothermal material and preparation method thereof - Google Patents

Graphitized carbonized rice hull foam photothermal material and preparation method thereof Download PDF

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CN111517793A
CN111517793A CN202010366444.2A CN202010366444A CN111517793A CN 111517793 A CN111517793 A CN 111517793A CN 202010366444 A CN202010366444 A CN 202010366444A CN 111517793 A CN111517793 A CN 111517793A
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mass
parts
rice hull
solution
foam
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方伟
赵雷
陈辉
何漩
杜星
李薇馨
胡威威
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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Abstract

The invention relates to a graphitized carbonized rice hull foam photothermal material and a preparation method thereof. The technical scheme is as follows: mixing 5-15 parts by mass of rice hull and 100 parts by mass of ZnCl2Mixing the solutions, soaking, drying and grinding to obtain ZnCl2Treating rice hull powder; then, 30-50 parts by mass of ZnCl are added2Treated rice hull powder and 100 parts by mass of Ni (NO)3)2Mixing the solution, dipping and drying to obtain nickel nitrate composite rice hulls; then mixing 10-15 parts by mass of nickel nitrate composite rice hulls with 100 parts by mass of deionized water, adding 1-2 parts by mass of sodium dodecyl sulfate, 1-2 parts by mass of dodecanol and 1-2 parts by mass of resin adhesive after mixing uniformly, and adding 14-21 parts by mass of resin adhesive after low-speed stirring and high-speed stirringEpoxy resin, stirring, molding, freeze drying, and drying at 80-100 ℃; and finally, carrying out heat treatment for 1-3 h at the temperature of 1000-1200 ℃ in nitrogen to obtain the graphitized carbonized rice hull foam photothermal material. The invention has low cost; the prepared product has high graphitization degree, water evaporation efficiency and photo-thermal conversion efficiency.

Description

Graphitized carbonized rice hull foam photothermal material and preparation method thereof
Technical Field
The invention belongs to the technical field of photo-thermal materials. In particular to a graphitized carbonized rice hull foam photo-thermal material and a preparation method thereof.
Background
The Solar-thermal-water vapor Generation system (Solar Steel Generation) is a research hotspot in the field of current photothermal conversion, a photothermal material is used as a core working unit of the Solar Steel Generation system, and the performance of each aspect directly determines the working efficiency of the system. In recent years, most of domestic and foreign researches on solar light-heat energy-water vapor system photothermal materials focus on the aspects of development of new material systems and regulation and control of pore structures, and related material systems comprise plasmons, graphitized porous carbon, biomass morph-genetic carbon and the like. The biomass genetic carbon material has the advantages of wide source, low cost, reproducibility, natural porous structure and the like, and has great application prospect in the field of Solar Stem Generation.
Among the reported biomass morph photothermal Materials are mushrooms (Xu N, Hu X, Xu W, et al, mushrooms as efficient Solar steel Materials-Generation Devices. [ J ]. Advanced Materials,2017,29(28)) and Wood (Xue G, Liu K, Chen Q, et al, robust and Low-cost film-processed good for high-Performance Solar steel Materials Generation. [ J ]. Applied Materials & Interfaces,2017,9(17):15052), which are mainly formed by a carbonization process on the surface to form a layer of amorphous activated carbon, thereby obtaining a large light absorption range and a high light absorption rate, but have a problem of insufficient photothermal conversion efficiency due to Low degree of graphitization of the biomass morph.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a preparation method of a graphitized carbonized rice hull foam photothermal material with low cost; the graphitized carbonized rice hull foam photothermal material prepared by the method has high graphitization degree, water evaporation efficiency and photothermal conversion efficiency.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
step one, adding 5-15 parts by mass of rice hull into 100 parts by mass of ZnCl2Stirring the solution for 10 to 20min, dipping the solution for 24 to 48 hours at normal temperature and normal pressure, and drying the solution for 24 to 36 hours at the temperature of between 90 and 110 ℃ to prepare ZnCl2And (4) processing the rice hulls.
Step two, mixing 30-50 parts by mass of ZnCl2Processing rice hulls, grinding the rice hulls to the particle size of 0.075-0.15 mm, and then grinding the ZnCl2Processing rice hull and adding Ni (NO) 100 weight parts3)2And stirring the solution for 30-60 min, soaking the rice hull for 24-48 h at normal temperature and normal pressure, and drying the rice hull for 24-48 h at 90-110 ℃ to obtain the nickel nitrate composite rice hull.
Step three, adding 10-15 parts by mass of the nickel nitrate composite rice hulls into 100 parts by mass of deionized water, and uniformly mixing to obtain a mixed solution I; then adding 1-2 parts by mass of sodium dodecyl sulfate, 1-2 parts by mass of dodecanol and 1-2 parts by mass of resin adhesive into the mixed solution I, and stirring for 10-20 min at 40-60 ℃ and 100-200 r/min to obtain a mixed solution II; and stirring the mixed solution II for 15-20 min at the rotating speed of 1500-2000 r/min to obtain a high-speed stirring mixed solution, and adding 14-21 parts by mass of epoxy resin into the high-speed stirring mixed solution to obtain the nickel nitrate composite rice hull foam slurry.
Step four, casting and molding the nickel nitrate composite rice hull foam slurry, freeze-drying for 24-48 h at the temperature of-50 to-45 ℃, and drying for 18-24 h at the temperature of 80-100 ℃ to obtain nickel nitrate composite rice hull foam; and (3) carrying out heat treatment on the nickel nitrate composite rice hull foam for 1-3 h under the conditions of nitrogen atmosphere and 1000-1200 ℃ to prepare the graphitized carbonized rice hull foam photo-thermal material.
The ZnCl2The concentration of the solution is 10-15wt％。
The Ni (NO)3)2The concentration of the solution is 0.2-1 wt%.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following advantages:
(1) the main raw materials required by the invention are rice hull, sodium dodecyl sulfate, dodecanol, resin adhesive, zinc chloride and nickel nitrate, and the raw materials have wide sources and low cost.
(2) Aiming at the problems of low graphitization degree and low photothermal conversion efficiency of biomass morph-genetic photothermal materials, the invention improves the graphitization degree of the carbonized rice hulls in the high-temperature heat treatment process by introducing nickel nitrate into the rice hulls, thereby improving the water evaporation efficiency and the photothermal conversion efficiency of the graphitized carbonized rice hull foam photothermal materials.
The graphitized carbonized rice hull foam photothermal material prepared by the invention is detected as follows: the ratio of the Raman spectrum D peak to the Raman spectrum G peak (I)D/IG) 0.7 to 0.8; at 1KW/m2The water evaporation efficiency under the sunlight intensity is 1.01-1.12 kg.m-2·h-1The photothermal conversion efficiency is 69.5-77.1%; the graphitization degree, the water evaporation efficiency and the photothermal conversion efficiency are high.
Therefore, the cost is low, and the prepared graphitized carbonized rice hull foam photothermal material has high graphitization degree, water evaporation efficiency and photothermal conversion efficiency.
Drawings
FIG. 1 is a Raman spectrum of a graphitized carbonized rice hull foam photothermal material prepared by the invention.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope.
Example 1
A graphitized carbonized rice hull foam photo-thermal material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, adding 5 parts by mass of rice hull to 100 parts by mass of ZnCl2Stirring for 15min, and soaking at room temperature and normal pressure for 30h, and then dried for 36h at the temperature of 90 ℃ to prepare ZnCl2And (4) processing the rice hulls.
Step two, 36 parts by mass of ZnCl2Processing rice hulls, grinding the rice hulls to the particle size of 0.075-0.15 mm, and then grinding the ZnCl2Processing rice hull and adding Ni (NO) 100 weight parts3)2Stirring the solution for 30min, soaking the solution for 24h at normal temperature and pressure, and drying the solution for 30h at 100 ℃ to obtain the nickel nitrate composite rice hull.
Step three, adding 12 parts by mass of the nickel nitrate composite rice hulls into 100 parts by mass of deionized water, and uniformly mixing to obtain a mixed solution I; then adding 1 part by mass of sodium dodecyl sulfate, 1 part by mass of dodecanol and 1 part by mass of resin adhesive into the mixed solution I, and stirring for 10min at 40 ℃ and 150r/min to obtain a mixed solution II; and stirring the mixed solution II for 15min at the rotating speed of 1500r/min to obtain a high-speed stirring mixed solution, and adding 14 parts by mass of epoxy resin into the high-speed stirring mixed solution to obtain the nickel nitrate composite rice hull foam slurry.
Step four, casting and molding the nickel nitrate composite rice hull foam slurry, freeze-drying for 24 hours at the temperature of-50 ℃, and drying for 24 hours at the temperature of 80 ℃ to obtain nickel nitrate composite rice hull foam; and (3) carrying out heat treatment on the nickel nitrate composite rice hull foam for 2h under the conditions of nitrogen atmosphere and 1000 ℃ to prepare the graphitized carbonized rice hull foam photo-thermal material.
ZnCl described in this example2The concentration of the solution was 10 wt%; the Ni (NO)3)2The concentration of the solution was 0.2 wt%.
The graphitized carbonized rice hull foam photothermal material prepared by the embodiment is detected as follows: the ratio of the Raman spectrum D peak to the Raman spectrum G peak (I)D/IG) Is 0.8; at 1KW/m2The water evaporation efficiency under the sunlight intensity is 1.01 kg.m-2·h-1The photothermal conversion efficiency was 69.5%.
Example 2
A graphitized carbonized rice hull foam photo-thermal material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step (ii) ofFirstly, 10 parts by mass of rice hull is added into 100 parts by mass of ZnCl2Stirring the solution for 10min, soaking the solution for 24h at normal temperature and pressure, and drying the solution for 24h at 110 ℃ to obtain ZnCl2And (4) processing the rice hulls.
Step two, adding 40 parts by mass of ZnCl2Processing rice hulls, grinding the rice hulls to the particle size of 0.075-0.15 mm, and then grinding the ZnCl2Processing rice hull and adding Ni (NO) 100 weight parts3)2Stirring the solution for 42min, soaking the solution for 36h at normal temperature and pressure, and drying the solution for 24h at 90 ℃ to obtain the nickel nitrate composite rice hull.
Step three, adding 14 parts by mass of the nickel nitrate composite rice hulls into 100 parts by mass of deionized water, and uniformly mixing to obtain a mixed solution I; then adding 1.2 parts by mass of sodium dodecyl sulfate, 1.2 parts by mass of dodecanol and 1.2 parts by mass of resin adhesive into the mixed solution I, and stirring for 12min at 50 ℃ and 100r/min to obtain a mixed solution II; and stirring the mixed solution II for 17min at the rotating speed of 1600r/min to obtain a high-speed stirring mixed solution, and adding 17 parts by mass of epoxy resin into the high-speed stirring mixed solution to obtain the nickel nitrate composite rice hull foam slurry.
Step four, casting and molding the nickel nitrate composite rice hull foam slurry, freeze-drying for 32 hours at the temperature of-48 ℃, and drying for 24 hours at the temperature of 85 ℃ to obtain nickel nitrate composite rice hull foam; and (3) carrying out heat treatment on the nickel nitrate composite rice hull foam for 1h under the conditions of nitrogen atmosphere and 1100 ℃, thus preparing the graphitized carbonized rice hull foam photo-thermal material.
ZnCl described in this example2The concentration of the solution was 12 wt%; the Ni (NO)3)2The concentration of the solution was 0.5 wt%.
The graphitized carbonized rice hull foam photothermal material prepared by the embodiment is detected as follows: the ratio of the Raman spectrum D peak to the Raman spectrum G peak (I)D/IG) Is 0.73; at 1KW/m2The water evaporation efficiency under the sunlight intensity is 1.08 kg.m-2·h-1The photothermal conversion efficiency was 74.3%.
Example 3
A graphitized carbonized rice hull foam photo-thermal material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, adding 15 parts by mass of rice hull into 100 parts by mass of ZnCl2Stirring the solution for 18min, soaking the solution for 48h at normal temperature and pressure, and drying the solution for 36h at 110 ℃ to obtain ZnCl2And (4) processing the rice hulls.
Step two, 50 parts by mass of ZnCl2Processing rice hulls, grinding the rice hulls to the particle size of 0.075-0.15 mm, and then grinding the ZnCl2Processing rice hull and adding Ni (NO) 100 weight parts3)2Stirring the solution for 50min, soaking the solution for 48h at normal temperature and pressure, and drying the solution for 48h at 110 ℃ to obtain the nickel nitrate composite rice hull.
Step three, adding 15 parts by mass of the nickel nitrate composite rice hulls into 100 parts by mass of deionized water, and uniformly mixing to obtain a mixed solution I; then adding 2 parts by mass of sodium dodecyl sulfate, 2 parts by mass of dodecanol and 2 parts by mass of resin adhesive into the mixed solution I, and stirring for 20min at the temperature of 60 ℃ and at the speed of 180r/min to obtain a mixed solution II; and stirring the mixed solution II for 20min at the rotating speed of 1800r/min to obtain a high-speed stirring mixed solution, and adding 21 parts by mass of epoxy resin into the high-speed stirring mixed solution to obtain the nickel nitrate composite rice hull foam slurry.
Step four, casting and molding the nickel nitrate composite rice hull foam slurry, freeze-drying for 48 hours at the temperature of minus 45 ℃, and drying for 18 hours at the temperature of 100 ℃ to obtain nickel nitrate composite rice hull foam; and (3) carrying out heat treatment on the nickel nitrate composite rice hull foam for 3h under the conditions of nitrogen atmosphere and 1200 ℃ to prepare the graphitized carbonized rice hull foam photo-thermal material.
ZnCl described in this example2The concentration of the solution was 15 wt%; the Ni (NO)3)2The concentration of the solution was 1 wt%.
The graphitized carbonized rice hull foam photothermal material prepared by the embodiment is detected as follows: the ratio of the Raman spectrum D peak to the Raman spectrum G peak (I)D/IG) Is 0.7; at 1KW/m2The water evaporation efficiency under the sunlight intensity is 1.12 kg.m-2·h-1Photo-thermal conversionThe conversion efficiency was 77.1%.
Example 4
A graphitized carbonized rice hull foam photo-thermal material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, adding 13 parts by mass of rice hull into 100 parts by mass of ZnCl2Stirring the solution for 20min, soaking the solution for 40h at normal temperature and pressure, and drying the solution for 30h at 110 ℃ to obtain ZnCl2And (4) processing the rice hulls.
Step two, 30 parts by mass of ZnCl2Processing rice hulls, grinding the rice hulls to the particle size of 0.075-0.15 mm, and then grinding the ZnCl2Processing rice hull and adding Ni (NO) 100 weight parts3)2Stirring the solution for 60min, soaking the solution for 48h at normal temperature and pressure, and drying the solution for 36h at 100 ℃ to obtain the nickel nitrate composite rice hull.
Step three, adding 10 parts by mass of the nickel nitrate composite rice hulls into 100 parts by mass of deionized water, and uniformly mixing to obtain a mixed solution I; then adding 1.5 parts by mass of sodium dodecyl sulfate, 1.5 parts by mass of dodecanol and 1.5 parts by mass of resin adhesive into the mixed solution I, and stirring for 16min at 45 ℃ and 200r/min to obtain a mixed solution II; and stirring the mixed solution II for 18min at the rotating speed of 2000r/min to obtain a high-speed stirring mixed solution, and adding 15 parts by mass of epoxy resin into the high-speed stirring mixed solution to obtain the nickel nitrate composite rice hull foam slurry.
Step four, casting and molding the nickel nitrate composite rice hull foam slurry, freeze-drying for 30 hours at the temperature of minus 45 ℃, and drying for 22 hours at the temperature of 95 ℃ to obtain nickel nitrate composite rice hull foam; and (3) carrying out heat treatment on the nickel nitrate composite rice hull foam for 2h under the conditions of nitrogen atmosphere and 1000 ℃ to prepare the graphitized carbonized rice hull foam photo-thermal material.
ZnCl described in this example2The concentration of the solution was 12 wt%; the Ni (NO)3)2The concentration of the solution was 0.8 wt%.
The graphitized carbonized rice hull foam photothermal material prepared by the embodiment is detected as follows: the ratio of the Raman spectrum D peak to the Raman spectrum G peak (I)D/IG) Is 0.78; at 1KW/m2The water evaporation efficiency under the sunlight intensity is 1.03 kg.m-2·h-1The photothermal conversion efficiency was 70.8%.
Compared with the prior art, the specific implementation mode has the following advantages:
(1) the main raw materials required by the specific embodiment are rice husk, sodium dodecyl sulfate, dodecanol, resin adhesive, zinc chloride and nickel nitrate, and the raw materials are wide in source and low in cost.
(2) Aiming at the problems of low graphitization degree and low photothermal conversion efficiency of biomass morph-genetic photothermal materials, the specific embodiment improves the graphitization degree of the carbonized rice hulls in the high-temperature heat treatment process by introducing nickel nitrate into the rice hulls, and further improves the water evaporation efficiency and the photothermal conversion efficiency of the graphitized carbonized rice hull foam photothermal materials.
The Raman spectrum of the graphitized carbonized rice hull foam photothermal material prepared by the specific embodiment is shown in fig. 1, fig. 1 is a Raman spectrum of the graphitized carbonized rice hull foam photothermal material prepared in example 4, and as can be seen from fig. 1: the prepared graphitized carbonized rice hull foam photothermal material has clear carbon material characteristic D peak and G peak, and the ratio (I) of the D peak to the G peakD/IG) 0.78, high graphitization degree; the prepared graphitized carbonized rice hull foam photo-thermal material is 2800cm-1Clear graphene characteristic 2D peaks appear nearby, and further shows that the graphitized carbonized rice hull foam photothermal material has high graphitization degree.
The graphitized carbonized rice hull foam photothermal material prepared by the specific embodiment is detected as follows: the ratio of the Raman spectrum D peak to the Raman spectrum G peak (I)D/IG) 0.7 to 0.8; at 1KW/m2The water evaporation efficiency under the sunlight intensity is 1.01-1.12 kg.m-2·h-1The photothermal conversion efficiency is 69.5-77.1%; the graphitization degree, the water evaporation efficiency and the photothermal conversion efficiency are high.
Therefore, the cost of the embodiment is low, and the prepared graphitized carbonized rice hull foam photothermal material has high graphitization degree, water evaporation efficiency and photothermal conversion efficiency.

Claims (4)

1. A preparation method of a graphitized carbonized rice hull foam photo-thermal material is characterized by comprising the following steps:
step one, adding 5-15 parts by mass of rice hull into 100 parts by mass of ZnCl2Stirring the solution for 10 to 20min, dipping the solution for 24 to 48 hours at normal temperature and normal pressure, and drying the solution for 24 to 36 hours at the temperature of between 90 and 110 ℃ to prepare ZnCl2Treating rice hulls;
step two, mixing 30-50 parts by mass of ZnCl2Processing rice hulls, grinding the rice hulls to the particle size of 0.075-0.15 mm, and then grinding the ZnCl2Processing rice hull and adding Ni (NO) 100 weight parts3)2Stirring the solution for 30-60 min, soaking the solution for 24-48 h at normal temperature and pressure, and drying the solution for 24-48 h at 90-110 ℃ to obtain nickel nitrate composite rice hulls;
step three, adding 10-15 parts by mass of the nickel nitrate composite rice hulls into 100 parts by mass of deionized water, and uniformly mixing to obtain a mixed solution I; then adding 1-2 parts by mass of sodium dodecyl sulfate, 1-2 parts by mass of dodecanol and 1-2 parts by mass of resin adhesive into the mixed solution I, and stirring for 10-20 min at 40-60 ℃ and 100-200 r/min to obtain a mixed solution II; stirring the mixed solution II for 15-20 min at the rotating speed of 1500-2000 r/min to obtain a high-speed stirring mixed solution, and adding 14-21 parts by mass of epoxy resin into the high-speed stirring mixed solution to obtain nickel nitrate composite rice hull foam slurry;
step four, casting and molding the nickel nitrate composite rice hull foam slurry, freeze-drying for 24-48 h at the temperature of-50 to-45 ℃, and drying for 18-24 h at the temperature of 80-100 ℃ to obtain nickel nitrate composite rice hull foam; and (3) carrying out heat treatment on the nickel nitrate composite rice hull foam for 1-3 h under the conditions of nitrogen atmosphere and 1000-1200 ℃ to prepare the graphitized carbonized rice hull foam photo-thermal material.
2. The method for preparing the graphitized carbonized rice hull foam photothermal material according to claim 1, characterized in that the ZnCl is used as a material for preparing the graphitized carbonized rice hull foam photothermal material2The concentration of the solution is 10-15 wt%.
3. The method for preparing graphitized carbonized rice hull foam photothermal material according to claim 1, characterized in that said Ni (NO) is3)2The concentration of the solution is 0.2-1 wt%.
4. A graphitized carbonized rice hull foam photothermal material, which is characterized in that the graphitized carbonized rice hull foam photothermal material is prepared by the preparation method of the graphitized carbonized rice hull foam photothermal material according to any one of claims 1 to 3.
CN202010366444.2A 2020-04-30 2020-04-30 Graphitized carbonized rice hull foam photothermal material and preparation method thereof Pending CN111517793A (en)

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