CN113244887B - Preparation method of high-functionality graphene diatomite composite material - Google Patents
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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Abstract
The invention discloses a preparation method of a high-functionality graphene diatomite composite material, and belongs to the technical field of preparation of environment-friendly materials. The method mainly comprises the following steps: carrying out composite oxidation treatment on multilayer graphene and secondary-tertiary diatomite, carrying out ultrasonic dispersion, adding auxiliary materials, blending and stirring, defoaming, preparing a sample and the like. The method solves the technical problem that the multi-layer graphene is difficult to separate and extract after oxidation, realizes the integrated preparation of the loading of the graphene on the surface of the diatomite and the purification of the two-stage and three-stage diatomite, has the formaldehyde purification efficiency higher than 95 percent, and can be widely applied to the fields of water body treatment, air purification and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of environment-friendly materials, and particularly relates to preparation and application of a high-functionality graphene diatomite composite material.
Background
Substances such as coatings, paints and adhesives in artificial decorative plates used for indoor decorative materials can release formaldehyde into the air, so that the concentration of the indoor formaldehyde greatly exceeds the national standard, the content of the formaldehyde exceeds the standard, the human body can be induced to generate various diseases by long-term contact, the health of the human body is damaged, how to efficiently remove harmful gases such as formaldehyde and toluene and how to improve the indoor living environment become problems and research focuses to be solved urgently at present.
A large number of nano-pore structures of the diatomite can efficiently adsorb and capture pollutants such as formaldehyde, and the adsorbed and captured pollutants are decomposed into carbon dioxide and water under the condition of visible light by utilizing the photocatalytic effect of the surface-loaded photocatalytic material. Meanwhile, graphene has excellent properties such as high specific surface area and carrier mobility, and thus has received much attention from researchers in various subject fields at home and abroad. However, the application of graphene is limited due to the problems of high cost, difficult material extraction and dispersion, and the like. However, if the excellent performance of graphene is organically combined with diatomite, the respective advantages are fully developed under the condition of using less filler, the cost is reduced, and the comprehensive performance of the product is improved, which inevitably promotes the development and progress of novel air purification materials.
Based on the problems, the method takes multilayer graphene, two-stage and three-stage diatomite, a photocatalytic material and the like as main raw materials, solves the problem of difficult separation and extraction of graphene after oxidation by utilizing the charge effect and the carrier effect of the surface of the diatomite, realizes the integrated preparation of the load of the graphene on the surface of the diatomite and the purification of the diatomite, and simultaneously completes the application of the graphene in the field of diatomite coating, which inevitably promotes the technical development in the field of environmental protection science and technology. The research has not been reported at home and abroad.
Disclosure of Invention
The invention aims to complete the preparation of a high-functionality graphene-diatomite composite material, realize the integrated treatment of two-level and three-level diatomite purification and graphene preparation, apply the graphene composite material in the field of diatomite coatings, solve the problems of difficult extraction and dispersion of multi-layer graphene after oxidation treatment, secondary composite application of diatomite graphene, diatomite purification treatment and the like, and realize the formaldehyde purification efficiency of more than 95% under the visible light catalysis condition.
The technical problem is realized by the following technical scheme:
a preparation method of a high-functionality graphene diatomite composite material comprises the following steps:
1) According to the preparation process of graphene by a hummer method, after the multilayer graphene and secondary-tertiary diatomite are subjected to composite oxidation preparation according to the mass ratio of 1:1-100, a product is washed to be neutral, dried in a forced air drying oven at 45-60 ℃ to obtain a graphene-diatomite composite material, and ground into powder for later use;
2) Ultrasonically dispersing the graphene and diatomite composite material obtained in the step 1) for 20-30 minutes under the condition of 100-200 watts to obtain a graphene and diatomite composite material dispersion liquid;
3) Dispersing 1-2 parts of latex powder, 0.8-1.5 parts of dispersant and 0.5-1.5 parts of cellulose in deionized water by mass, dispersing at high speed for 5 minutes under the condition of 4000-5000 r/min, adding 20-30 parts of the graphene diatomite composite dispersion prepared in the step 2), and blending and stirring for 5 minutes for later use;
4) Adding 40-57 parts of heavy calcium powder, 15-20 parts of ash calcium powder and 2-5 parts of photocatalytic material into the blending liquid obtained in the step 3), dispersing and stirring at a high speed for 10 minutes, standing and defoaming, and preparing a sample to obtain the high-functionality graphene diatomite composite material.
The photocatalytic material in the step 4) is preferably one or a plurality of nano zinc oxide, nano titanium dioxide and tin oxide.
According to the preparation method, multilayer graphene, two-third-level diatomite, a photocatalytic material and the like are taken as main raw materials, according to the preparation process of graphene by a hummer method, the two-third-level diatomite and the multilayer graphene are added together in the preparation process of the graphene, the combination of the diatomite and the graphene is realized by utilizing the interaction of the variable effect of the surface charge property of the diatomite (the surface of the diatomite presents positive charge when the pH value is less than 2) and the carrier effect and the graphene with negative charge under different pH values, the separation and extraction difficulty of the oxidized graphene is solved, the integrated preparation of the loading of the graphene on the surface of the diatomite and the purification of the two-third-level diatomite is realized, and the problems of powder falling, cracking, low purification efficiency of the diatomite coating, and the like are solved due to the micro-nano enhanced effect and the adsorption purification effect of the material.
The high-functionality graphene diatomite composite material prepared by the invention can be further processed into materials with different functional attributes and shapes, and can be widely applied to the fields of water treatment, air purification and the like, for example, the composite material can be further processed into ceramsite materials with different shapes and sizes by utilizing the ceramsite manufacturing process, and can be applied to functional materials in other scenes such as sewage treatment, building boards and the like; or household refrigerator deodorant, indoor air purifier filter element, etc.
In conclusion, the invention has the following beneficial effects:
1. by utilizing the surface charge effect of the graphene and the diatomite, the technical effects of mixing and separating the graphene and the diatomite and secondary ultrasonic dispersion are realized. The technical problems that the multi-layer graphene is difficult to separate and extract after oxidation are solved.
2. The integrated preparation of the graphene on the surface of the diatomite and the purification of the second-level diatomite and the third-level diatomite is realized.
3. The graphene-diatomite composite material and the photocatalytic composite material are compounded for use, and the formaldehyde purification efficiency is higher than 95%. Can be widely applied to the fields of water body treatment, air purification and the like.
Description of the drawings:
fig. 1 is a photograph of the oxidized multi-layer graphene-diatomite composite dry powder material obtained in step 1.
Fig. 2 is an electron microscope photograph of the oxidized multilayer graphene-diatomite composite material obtained in step 1.
FIG. 3 is a photograph of the high concentration solution after ultrasonic dispersion in step 2.
FIG. 4 shows the sample mixed in step 4 and applied to a glass plate having a thickness of 6mm and an area of 500mm by 500mm to obtain a sample plate of the final material.
Detailed Description
The invention is described in more detail below by way of example
Example 1:
1) According to the preparation process of graphene by a hummer method, 1g of multilayer graphene and 50g of secondary-tertiary diatomite are subjected to composite oxidation preparation, a product is washed to be neutral, and is dried in a forced air drying oven at 60 ℃, so that the graphene-diatomite composite material is obtained, an optical photo is shown in figure 1, an electron microscope photo is shown in figure 2, and then the graphene-diatomite composite material is ground into powder for later use.
2) Taking 20g of the graphene and diatomite composite material prepared in the step 1), performing ultrasonic dispersion for 30 minutes under the condition of 100 watts to obtain a graphene and diatomite composite material dispersion liquid, as shown in fig. 3.
3) Dispersing 2g of latex powder, 0.8g of dispersing agent and 0.5g of cellulose in deionized water, dispersing at a high speed under the condition of 5000 r/min, stirring for 5 min, and then blending and stirring for 5 min with the graphene diatomite composite dispersion liquid in the step 2) for later use.
4) Adding 40g of heavy calcium powder, 15g of sierozem powder and 2g of nano zinc oxide into the system in the step 3), dispersing and stirring at a high speed for 10 minutes, standing for defoaming, uniformly coating on a glass plate with the thickness of 6mm and the area of 500mm multiplied by 500mm, drying the coating, and standing for 24 hours to obtain a high-functionality graphene diatomite composite material sample, as shown in fig. 4.
Example 2:
1) According to the preparation process of graphene by a hummer method, 1g of multilayer graphene and 40g of secondary-tertiary diatomite are subjected to composite oxidation preparation, the obtained graphene-diatomite composite material is washed to be neutral, dried in a forced air drying oven at 60 ℃, and then ground into powder for later use.
2) Taking 23g of the graphene and diatomite composite material prepared in the step 1), and performing ultrasonic dispersion for 30 minutes under the condition of 100 watts to obtain a graphene and diatomite composite material dispersion liquid.
3) Dispersing 2.5g of latex powder, 1.0g of dispersing agent and 0.8g of cellulose in deionized water, dispersing at a high speed under the condition of 5000 r/min, stirring for 5 min, and then blending and stirring with the graphene dispersion liquid in the step 2 for 5 min for later use.
4) Adding 45g of coarse whiting powder, 18g of sierozem powder and 2.5g of nano zinc oxide into the mixture obtained in the step (3), dispersing and stirring at a high speed for 10 minutes, standing, defoaming and preparing a sample.
Example 3:
1) According to the preparation process of graphene by a hummer method, 1g of multilayer graphene and 30g of secondary-tertiary diatomite are subjected to composite oxidation preparation, the obtained graphene-diatomite composite material is washed to be neutral, dried in a forced air drying oven at 60 ℃, and then ground into powder for later use.
2) Taking 26g of the graphene and diatomite composite material prepared in the step 1), and performing ultrasonic dispersion for 30 minutes under the condition of 100 watts to obtain a graphene and diatomite composite material dispersion liquid.
3) Dispersing 3g of latex powder, 1.1g of dispersing agent and 1.0g of cellulose in deionized water, dispersing at a high speed under the condition of 5000 r/min, stirring for 5 min, and then blending and stirring with the graphene dispersion liquid in the step 2 for 5 min for later use.
4) Adding 50g of coarse whiting powder, 18g of sierozem powder and 3g of nano zinc oxide into the mixture obtained in the step (3), dispersing and stirring at a high speed for 10 minutes, standing, defoaming and preparing a sample.
Example 4:
1) According to the preparation process of graphene by the hummer method, 1g of multilayer graphene and 20g of secondary-tertiary diatomite are subjected to composite oxidation preparation, the obtained graphene-diatomite composite material is washed to be neutral, dried in a forced air drying oven at 60 ℃, and then ground into powder for later use.
2) Taking 30g of the graphene and diatomite composite material prepared in the step 1), and performing ultrasonic dispersion for 30 minutes under the condition of 100 watts to obtain a graphene and diatomite composite material dispersion liquid.
3) Dispersing 2.5g of latex powder, 1.0g of dispersing agent and 0.8g of cellulose in deionized water, dispersing at a high speed under the condition of 5000 revolutions per minute, stirring for 5 minutes, and then blending and stirring with the graphene dispersion liquid in the step 2 for 5 minutes for later use.
4) Adding 50g of coarse whiting powder, 18g of sierozem powder and 3.5g of nano zinc oxide into the mixture obtained in the step (3), dispersing and stirring at a high speed for 10 minutes, standing, defoaming and preparing a sample.
Example 5:
1) According to the preparation process of graphene by a hummer method, 1g of multilayer graphene and 10g of secondary-tertiary diatomite are subjected to composite oxidation preparation, the obtained graphene-diatomite composite material is washed to be neutral, dried in a forced air drying oven at 60 ℃, and then ground into powder for later use.
2) Taking 35g of the graphene and diatomite composite material prepared in the step 1), and performing ultrasonic dispersion for 30 minutes under the condition of 100 watts to obtain a graphene and diatomite composite material dispersion liquid.
3) Dispersing 2.5g of latex powder, 1.0g of dispersing agent and 0.8g of cellulose in deionized water, dispersing at a high speed under the condition of 5000 r/min, stirring for 5 min, and then blending and stirring with the graphene dispersion liquid in the step 2 for 5 min for later use.
4) 49g of heavy calcium powder, 18g of ash calcium powder and 4g of nano zinc oxide are added into the mixture obtained in the step 3, dispersed and stirred at a high speed for 10 minutes, and stood still for defoaming to prepare a sample.
Example 6
According to the test requirements of the building material industry standard JC/T2177-2013, the samples prepared in the examples 1-5 are subjected to a 48-hour formaldehyde purification efficiency test in a GDYJ-201MF full-automatic multifunctional formaldehyde and ammonia tester. The results are shown in Table 1.
TABLE 1 Formaldehyde purification efficiency test results
| Serial number | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Efficiency of formaldehyde purification | 95.33％ | 98.99％ | 96.98％ | 97.89％ | 98.96％ |
The test results show that the product of the invention has excellent formaldehyde purification performance, and the purification efficiency is more than 95%. Meanwhile, the method is simple and efficient in process, can greatly improve the formaldehyde purification rate in the air under the condition of visible light irradiation, is easy for industrial application, has high practical application value, and widens the application range of the method in the technical field of environmental protection.
Claims (2)
1. A preparation method of a high-functionality graphene diatomite composite material comprises the following steps:
1) According to the preparation process of graphene by a hummer method, after the multilayer graphene and secondary-tertiary diatomite are subjected to composite oxidation preparation according to the mass ratio of 1:1-100, a product is washed to be neutral, dried in a forced air drying oven at 45-60 ℃ to obtain a graphene-diatomite composite material, and ground into powder for later use;
2) Ultrasonically dispersing the graphene and diatomite composite material obtained in the step 1) for 20-30 minutes under the condition of 100-200 watts to obtain a graphene and diatomite composite material dispersion liquid;
3) Dispersing 1-2 parts of latex powder, 0.8-1.5 parts of dispersant and 0.5-1.5 parts of cellulose in deionized water by mass, dispersing at high speed for 5 minutes under the condition of 4000-5000 r/min, adding 20-30 parts of the graphene diatomite composite dispersion prepared in the step 2), and blending and stirring for 5 minutes for later use;
4) Adding 40-57 parts of heavy calcium powder, 15-20 parts of ash calcium powder and 2-5 parts of photocatalytic material into the blending liquid obtained in the step 3), dispersing and stirring at a high speed for 10 minutes, standing and defoaming, and preparing a sample to obtain the high-functionality graphene diatomite composite material.
2. The method for preparing the highly functional graphene-diatomite composite material according to claim 1, wherein the photocatalytic material in the step 4) is one or more of nano zinc oxide, nano titanium dioxide and tin oxide.
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