CN107670641B - Graphene air purification material and preparation method thereof - Google Patents
Graphene air purification material and preparation method thereof Download PDFInfo
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- CN107670641B CN107670641B CN201711162025.1A CN201711162025A CN107670641B CN 107670641 B CN107670641 B CN 107670641B CN 201711162025 A CN201711162025 A CN 201711162025A CN 107670641 B CN107670641 B CN 107670641B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
Abstract
The invention belongs to the field of air purification materials, and particularly relates to a graphene air purification material and a preparation method thereof. The method comprises the following steps: A) mixing the wood activated carbon powder activated by water vapor with alkali, and activating to obtain an activated carbon semi-finished product; B) and mixing the semi-finished product of the activated carbon obtained in the step with the calcium carbonate crystal whisker, the nitrogen source and the graphene solution again, and carrying out reduction reaction to obtain the graphene super air-purifying composite material. The material of the invention has the functions of adsorbing harmful gas and peculiar smell, inhibiting bacteria and sterilizing, and has the advantages of low production cost and no pollution.
Description
Technical Field
The invention belongs to the field of air purification materials, and particularly relates to a graphene air purification material and a preparation method thereof.
Background
In recent years, the problem of air pollution is always a problem to be solved urgently by governments. The flue gas released by burning fossil fuel (coal, petroleum, natural gas, etc.) in energy, chemical, metallurgy, traffic, etc. industries contains a great deal of SO2And NOxCausing serious pollution to the atmosphere. In addition, various dusts generated by human activities, solid suspended particles such as sand dust caused by climate deterioration, and the like pollute the ambient air, and volatile organic pollutants from various decorative materials and oral chemicals increasingly enter residences and public buildings, so that the degree of pollution of human living environment is increased sharply.
Investigation shows that 90% of newly-installed living rooms and 95% of newly-installed office places in China have the phenomenon that VOCs gas pollutants exceed standards. Since most human activities are performed indoors, the harm to human health and population quality caused by indoor environmental pollution is very serious. One statistic of the world health organization shows that the burden of diseases caused by indoor environmental pollution is 6 times more than that caused by outdoor pollution of the same level. In the nineties of the last century, the number of excess deaths caused by indoor environmental pollution in China is 11 million, the number of excess outpatients is 13 million, and the number of excess emergency calls is 150 million, so that the economic loss caused by the excess of the death is over 100 hundred million dollars.
In order to meet the requirements of people on air quality, various types of air purifiers appear on the market, the currently recognized air purification method at home and abroad mainly utilizes an adsorption method and an electrostatic method to remove pollutants, most of the existing air purifiers adopt a filtering material to remove suspended particles in the air, adopt porous materials such as activated carbon and the like to adsorb harmful gases in the air, and are provided with a negative ion generator to generate a certain amount of negative ions. However, the adsorption capacity of the activated carbon is limited, and the contaminant penetration phenomenon occurs after the adsorption is saturated. And the effect of removing main indoor pollutants such as formaldehyde, acetaldehyde, benzene, VOCs and nitrogen oxides is not ideal. At this time, the adsorbing material loses the adsorption property to the pollutant, and when the adsorbed pollutant is a volatile organic compound, the adsorbed harmful pollutant causes secondary pollution, and becomes a new pollution source.
At present, the research on purifying indoor air by utilizing a nano photocatalyst technology is started at home and abroad. The nano photocatalyst is combined with the adsorbent, and the indoor air can be purified by utilizing the adsorption performance of the adsorbent and the characteristic that the nano photocatalyst can decompose harmful gas into harmless gas at normal temperature. Such as: active carbon or active carbon fiber is used as the carrier of photocatalyst to prepare purifying material, etc. However, since such a photocatalytic effect can only be exerted under the irradiation of ultraviolet light, the material manufactured by the method has poor practicability at present, the indoor environment is difficult to meet the use requirement of an ultraviolet illumination strip, and the cost is high.
Disclosure of Invention
The invention aims to provide a graphene air purification composite material and a preparation method thereof aiming at the defects of the prior art; the composite material has strong air purifying capacity, simple preparation method and low cost, and has good application prospect.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the graphene super air purification composite material comprises the following steps:
A) mixing the wood activated carbon powder activated by water vapor with alkali, and activating to obtain an activated carbon semi-finished product; preparing 0.6 wt% graphene aqueous dispersion;
B) and mixing the semi-finished product of the activated carbon obtained in the step with the calcium carbonate crystal whisker, the nitrogen source and the graphene solution again, and carrying out reduction reaction to obtain the graphene super air-purifying composite material.
Preferably, the base comprises one or more of potassium hydroxide, sodium hydroxide and calcium hydroxide;
the mass ratio of the wood activated carbon powder to the alkali is 1: (0.5-2).
Preferably, the activation temperature is 500-800 ℃, and the activation time is 0.5-4 h.
Preferably, the particle size of the wood activated carbon powder is 8-12 μm; the length of the calcium carbonate whisker is 20-30 μm; the diameter is 1-2 μm; the average sheet diameter of the graphene is 1-50 mu m;
the mass of the graphene in the graphene aqueous dispersion liquid accounts for 0.1-10% of the mass of the wood activated carbon powder.
The mass of the calcium carbonate whiskers accounts for 0.1-10% of the mass of the wood activated carbon powder.
Preferably, the reduction reaction is specifically: carrying out reduction reaction under the condition of protective gas;
the protective gas comprises one or more of hydrogen, ammonia and nitrogen;
the temperature of the reduction reaction is 650-800 ℃, and the time of the reduction reaction is 1-6 h.
Preferably, the nitrogen source is a small molecule nitrogen-containing compound (nitrogen-containing small molecule), more preferably melamine and/or urea;
the mass of the nitrogen source accounts for 1-3% of the mass of the activated carbon powder.
The invention has the following remarkable advantages:
(1) according to the invention, the graphene is attached to the surface of the calcium carbonate whisker by adding the calcium carbonate whisker, so that the graphene is dispersed more uniformly, the specific surface area is increased, and the functions of adsorbing pollution gas and purifying air of the graphene are optimized and improved.
(2) The material of the invention has the functions of adsorbing harmful gas and peculiar smell, inhibiting bacteria and sterilizing, and has the advantages of low production cost and no pollution.
Detailed Description
For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.
Example 1
Taking 100g of wood charcoal and crushing the wood charcoal to 8-12 mu m; dissolving 50g of sodium hydroxide in 50mL of water, uniformly mixing with the wood charcoal, and drying under vacuum; then adding the materials into an activation furnace protected by nitrogen, heating to 780 ℃ at the speed of 5 ℃/min and keeping for 2 hours; cooling to room temperature, washing the activated product to be neutral, adding 6M hydrochloric acid, refluxing for 2h, and washing with deionized water again to be neutral; adding 4g of calcium carbonate whiskers and 300 mL0.6wt% graphene aqueous dispersion, adding 2g of melamine, ultrasonically stirring for 1h, and then spray-drying; placing the materials in a reduction furnace, heating to 800 ℃ at a speed of 10 ℃/min under the protection of hydrogen, and keeping for 2 hours; and cooling to room temperature to obtain the graphene super air purification composite material.
Example 2
Taking 100g of wood charcoal and crushing the wood charcoal to 8-12 um; dissolving 100g of sodium hydroxide in 100mL of water, uniformly mixing with the wood charcoal, and drying under vacuum; then adding the materials into an activation furnace protected by nitrogen, heating to 780 ℃ at the speed of 5 ℃/min and keeping for 2 hours; cooling to room temperature, washing the activated product to be neutral, adding 6M hydrochloric acid, refluxing for 2h, and washing with deionized water again to be neutral; adding 4g of calcium carbonate whiskers and 300 mL0.6wt% graphene aqueous dispersion, adding 2g of melamine, ultrasonically stirring for 1h, and then spray-drying; placing the materials in a reduction furnace, heating to 800 ℃ at a speed of 10 ℃/min under the protection of hydrogen, and keeping for 2 hours; and cooling to room temperature to obtain the graphene super air purification composite material.
Example 3
Taking 100g of wood charcoal and crushing the wood charcoal to 8-12 mu m; dissolving 50g of potassium hydroxide in 50mL of water, uniformly mixing with the wood charcoal, and drying under vacuum; then adding the materials into an activation furnace protected by nitrogen, heating to 780 ℃ at the speed of 5 ℃/min and keeping for 2 hours; cooling to room temperature, washing the activated product to be neutral, adding 6M hydrochloric acid, refluxing for 2h, and washing with deionized water again to be neutral; adding 4g of calcium carbonate whiskers and 300 mL0.6wt% graphene aqueous dispersion, adding 2g of melamine, ultrasonically stirring for 1h, and then spray-drying; placing the materials in a reduction furnace, heating to 800 ℃ at a speed of 10 ℃/min under the protection of hydrogen, and keeping for 2 hours; and cooling to room temperature to obtain the graphene super air purification composite material.
Example 4
Taking 100g of wood charcoal and crushing the wood charcoal to 8-12 um; dissolving 100g of potassium hydroxide in 100mL of water, uniformly mixing with the wood charcoal, and drying under vacuum; then adding the materials into an activation furnace protected by nitrogen, heating to 780 ℃ at the speed of 5 ℃/min and keeping for 2 hours; cooling to room temperature, washing the activated product to be neutral, adding 6M hydrochloric acid, refluxing for 2h, and washing with deionized water again to be neutral; adding 4g of calcium carbonate whiskers and 300 mL0.6wt% graphene aqueous dispersion, adding 2g of melamine, ultrasonically stirring for 1h, and then spray-drying; placing the materials in a reduction furnace, heating to 800 ℃ at a speed of 10 ℃/min under the protection of hydrogen, and keeping for 2 hours; and cooling to room temperature to obtain the graphene super air purification composite material.
Example 5
Taking 100g of wood charcoal and crushing the wood charcoal to 8-12 mu m; dissolving 50g of calcium hydroxide in 50mL of water, uniformly mixing with the wood charcoal, and drying under vacuum; then adding the materials into an activation furnace protected by nitrogen, heating to 780 ℃ at the speed of 5 ℃/min and keeping for 2 hours; cooling to room temperature, washing the activated product to be neutral, adding 6M hydrochloric acid, refluxing for 2h, and washing with deionized water again to be neutral; adding 4g of calcium carbonate whiskers and 300 mL0.6wt% graphene aqueous dispersion, adding 2g of melamine, ultrasonically stirring for 1h, and then spray-drying; placing the materials in a reduction furnace, heating to 800 ℃ at a speed of 10 ℃/min under the protection of hydrogen, and keeping for 2 hours; and cooling to room temperature to obtain the graphene super air purification composite material.
Example 6
Taking 100g of wood charcoal and crushing the wood charcoal to 8-12 um; dissolving 100g of calcium hydroxide in 100mL of water, uniformly mixing with the wood charcoal, and drying under vacuum; then adding the materials into an activation furnace protected by nitrogen, heating to 780 ℃ at the speed of 5 ℃/min and keeping for 2 hours; cooling to room temperature, washing the activated product to be neutral, adding 6M hydrochloric acid, refluxing for 2h, and washing with deionized water again to be neutral; adding 4g of calcium carbonate whiskers and 300 mL0.6wt% graphene aqueous dispersion, adding 2g of melamine, ultrasonically stirring for 1h, and then spray-drying; placing the materials in a reduction furnace, heating to 800 ℃ at a speed of 10 ℃/min under the protection of hydrogen, and keeping for 2 hours; and cooling to room temperature to obtain the graphene super air purification composite material.
The performance test of the purification material of the invention comprises the following steps: 3.5 mg of formaldehyde and 3.5 mg of toluene were added to a closed space of 1 cubic meter. The volatile matter is evenly volatilized by micro ventilation. 50g of the sample is uniformly spread at four corners of a space, formaldehyde in the space is detected every 1 hour after 6 hours, the content of toluene is 0.048 mg of formaldehyde, the content of toluene is 0.107 mg of toluene, the contents of toluene and toluene are respectively lower than 0.10 mg of formaldehyde and 0.20 mg of toluene, the removal rates of the toluene and the formaldehyde are respectively 98.6 percent and 96.9 percent.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (8)
1. A preparation method of a graphene air purification composite material is characterized by comprising the following steps: the method comprises the following steps:
A) mixing the wood activated carbon powder activated by water vapor with alkali, and heating and activating under the condition of nitrogen to obtain a semi-finished product of activated carbon; preparing 0.6 wt% graphene aqueous dispersion;
B) mixing the activated carbon semi-finished product obtained in the step with the calcium carbonate whisker, the nitrogen source and the graphene solution again, and then carrying out heating reduction reaction under protective gas to obtain a graphene air-purifying composite material;
the mass of the calcium carbonate whiskers accounts for 0.1-10% of the mass of the wood activated carbon powder; the particle size of the wood activated carbon powder is 8-12 mu m; the length of the calcium carbonate whisker is 20-30 μm; the diameter is 1-2 μm; the average sheet diameter of graphene in the graphene aqueous dispersion is 1-50 mu m;
the protective gas is one or more of hydrogen, ammonia, and nitrogen.
2. The preparation method of the graphene air-purifying composite material according to claim 1, characterized by comprising the following steps:
the base comprises one or more of potassium hydroxide, sodium hydroxide and calcium hydroxide.
3. The preparation method of the graphene air-purifying composite material according to claim 1, characterized by comprising the following steps:
the mass ratio of the wood activated carbon powder to the alkali is 1: 0.5 to 2.
4. The preparation method of the graphene air-purifying composite material according to claim 1, characterized by comprising the following steps:
the activation temperature is 500-800 ℃, and the activation time is 0.5-4 h.
5. The preparation method of the graphene air-purifying composite material according to claim 1, characterized by comprising the following steps:
the graphene in the graphene aqueous dispersion liquid accounts for 0.1-10% of the mass of the wood activated carbon powder.
6. The preparation method of the graphene air-purifying composite material according to claim 1, characterized by comprising the following steps:
the temperature of the reduction reaction is 650-800 ℃, and the time of the reduction reaction is 1-6 h.
7. The preparation method of the graphene air-purifying composite material according to claim 1, characterized by comprising the following steps:
the nitrogen source is a small molecular nitrogen-containing compound, and the mass of the nitrogen source accounts for 1-3% of the mass of the activated carbon powder.
8. The preparation method of the graphene air-purifying composite material according to claim 7, characterized in that:
the nitrogen source is melamine and/or urea.
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