CN110773114A - Preparation method of modified fly ash adsorbent for VOCs (volatile organic chemicals) - Google Patents
Preparation method of modified fly ash adsorbent for VOCs (volatile organic chemicals) Download PDFInfo
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- CN110773114A CN110773114A CN201911057138.4A CN201911057138A CN110773114A CN 110773114 A CN110773114 A CN 110773114A CN 201911057138 A CN201911057138 A CN 201911057138A CN 110773114 A CN110773114 A CN 110773114A
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
Abstract
The invention discloses a preparation method of a modified fly ash adsorbent for VOCs. The preparation method comprises the following steps: 1) sieving the fly ash raw ash with a 80-mesh sieve, and taking the sieved ash; 2) using HCl with the mass fraction of 20% to perform acid modification on the fly ash at the temperature of 80 ℃; 3) cleaning and drying the acid modified fly ash, mixing the acid modified fly ash with NaOH with a certain concentration and the fly ash, and performing microwave irradiation modification under a set condition; 4) and removing water in the fly ash by using a vacuum drying oven to obtain the modified fly ash. The fly ash prepared by the method can adsorb various organic waste gases with higher efficiency, has simple and easy desorption operation, can recover valuable components in the organic waste gases, and can also destroy useless components cleanly and efficiently.
Description
Technical Field
The invention relates to a preparation method of a material for eliminating VOCs, in particular to a preparation method of fly ash capable of eliminating VOCs discharged in the coating industry and printing.
Technical Field
VOCs are a general name of a class of organic compounds, have high evaporation rate at normal temperature and are volatile. VOCs have great harm to the environment and the human body: they are important precursors for ozone generation and therefore become the main control factor for photochemical smog generation in many cities; the concentration of PM2.5 in the atmosphere can be increased by secondary organic aerosol generated by converting VOCs; VOCs containing halogen enter the stratosphere and then can consume ozone under the irradiation of ultraviolet rays, so that ozone layer cavities are formed; VOCs can cause skin irritation, and are particularly likely to cause various diseases after being inhaled by a human body, and even to increase the probability of cancer. Therefore, the prevention and control and treatment of VOCs are very important.
Organic solvents and chemical raw materials used by industrial enterprises can volatilize in workshops and are discharged to the outside through a ventilation system. The discharged VOCs can cause serious harm to the environment and can cause pollution to the air, water environment and water source. At present, VOCs in workshops are treated by various methods at home and abroad, and the methods are summarized as follows: adsorption technology, catalytic oxidation technology, plasma degradation technology, biodegradation technology and condensation method. Each of these processing techniques has its own advantages and short board. Such as biodegradation, which is a relatively efficient and clean process for treating VOCs, but requires equipment with a significant footprint. The condensation technology has good effect when treating high-concentration organic waste gas, is beneficial to recycling gas, but has the problem of high energy consumption. The adsorption technology is economical, occupies less land, is beneficial to gas recycling, but the adsorption efficiency changes along with the change of the adsorbent. The main means for improving the technical effect of adsorption is to develop more efficient and more appropriate adsorbent. The VOCs adsorbent commonly used at present is activated carbon, but in the coating and printing industries, organic waste gas often contains more solid particles. In order to prevent the adsorbent from being blocked and failed, water spraying treatment is often required in advance, which increases the humidity of the organic waste gas. However, the adsorption efficiency of activated carbon in a high humidity environment is not ideal. The fly ash particles have loose and porous surfaces and large specific surface area, contain more active alumina and silicon oxide and have certain adsorption capacity. The untreated fly ash has low adsorption capacity, so that the fly ash needs to be modified.
Disclosure of Invention
Aiming at the problem of treatment of industrial organic waste gas at present, in particular to the problem that the adsorption efficiency is not improved aiming at the characteristics of the organic waste gas, the invention provides a preparation method of modified fly ash.
A preparation method of an adsorbent capable of adsorbing VOCs adopts fly ash as an adsorbing material, and comprises the following steps:
calcining the power plant fly ash in a high-temperature furnace at 850 ℃ for 2 hours, sieving, and taking a 80-mesh sieve.
Putting 20% hydrochloric acid into a flask according to the mass ratio of 10: 1 of the fly ash in the volume of the hydrochloric acid, and stirring for 2h in a 80-DEG water bath kettle
After cooling and precipitation, pouring off acid liquor, and filtering the treated fly ash for multiple times by using deionized water washing paint until the pH value of the filtrate is 7. And (3) drying the filter on the filter paper in a constant-temperature air-blast drying oven at 105 ℃ for 12h, and grinding the filter until all the filter is sieved by a 80-mesh sieve after drying.
Respectively and uniformly mixing the fly ash subjected to acid treatment and a sodium hydroxide solution according to the solid-liquid mass ratio of 1: 10.
And performing microwave irradiation for 15min under the conditions of microwave temperature of 60 ℃ and microwave power of 600W. And after cooling and precipitation, pouring out the alkali liquor, and filtering the fly ash subjected to mixed alkali treatment for multiple times by using deionized water washing paint until the pH value of the filtrate is neutral.
Drying the filtrate in a constant temperature air-blast drying oven at 105 deg.C for 12 hr, and grinding for use.
The acid-base modification and microwave crystallization operations used in the invention can effectively increase the specific surface area of the fly ash particles, enlarge the pore volume of the pore diameter, reduce the polarity, and effectively improve the hydrophobicity and the adsorption efficiency of the fly ash.
The method has the advantages of simple operation, simple process and low cost. The prepared modified fly ash has high toluene adsorption efficiency, longer penetration time and lasting effect compared with the currently common activated carbon. In addition, the heat resistance of the modified fly ash is far better than that of a conventional adsorbent, so that the modified fly ash has a wider application range than other adsorbents, and VOCs (volatile organic compounds) are more easily desorbed and recovered.
The invention provides a new possibility of comprehensive utilization of the fly ash, provides a new approach for treating the fly ash in a power plant, saves the cost for preparing the activated carbon, and is lower-carbon, environment-friendly and more economic.
Detailed Description
The technical solution described in this application is specifically described below by referring to some examples. This technical solution is only illustrated in order to understand, not to limit, the present application, which can be implemented in many different ways, as defined and covered by the claims.
Example 1
10 g of power plant fly ash calcined at high temperature is taken and sieved, 80-mesh undersize is taken and mixed with hydrochloric acid with the mass fraction of 20 percent according to the mass ratio of 10: 1 of the fly ash by the volume of the hydrochloric acid, and the mixture is stirred and treated for 2 hours in a water bath kettle with the temperature of 80 ℃. After cooling and precipitation, pouring off acid liquor, washing paint with deionized water and filtering for multiple times until the pH value of the filtrate is neutral. Drying the filtrate in a constant temperature air-blast drying oven at 105 deg.C for 12 hr, and grinding. The mixture is evenly mixed with 10 percent sodium hydroxide solution according to the solid-to-liquid ratio of 1: 10. And performing microwave irradiation for 15min under the conditions of microwave temperature of 60 ℃ and microwave power of 600W. And after cooling and precipitation, pouring out the alkali liquor, and filtering the fly ash subjected to mixed alkali treatment for multiple times by using deionized water washing paint until the pH value of the filtrate is neutral. The filtrate was dried in a constant temperature forced air drying oven at 105 ℃ for 12 h. The fly ash capable of adsorbing VOCs is prepared.
Example 2
Sieving 10 g of fly ash from a power plant, mixing the undersize of 80 meshes with 20% hydrochloric acid according to the mass ratio of 10: 1 of the fly ash by the volume of the hydrochloric acid, and stirring for 2 hours in a water bath kettle at 80 ℃. After cooling and precipitation, pouring off acid liquor, washing paint with deionized water and filtering for multiple times until the pH value of the filtrate is neutral. Drying the filtrate in a constant temperature air-blast drying oven at 105 deg.C for 12 hr, and grinding. The mixture is evenly mixed with sodium hydroxide solution with the concentration of 7.5mol/L according to the solid-to-liquid ratio of 1: 10. And performing microwave irradiation for 15min under the conditions of microwave temperature of 60 ℃ and microwave power of 600W. And after cooling and precipitation, pouring out the alkali liquor, and filtering the fly ash subjected to mixed alkali treatment for multiple times by using deionized water washing paint until the pH value of the filtrate is neutral. The filtrate was dried in a constant temperature forced air drying oven at 105 ℃ for 12 h. The fly ash capable of adsorbing VOCs is prepared.
Comparative example 1
Sieving 10 g of fly ash from a power plant, mixing the undersize of 80 meshes with 20% hydrochloric acid according to the mass ratio of 10: 1 of the fly ash by the volume of the hydrochloric acid, and stirring for 2 hours in a water bath kettle at 80 ℃. After cooling and precipitation, pouring off acid liquor, washing paint with deionized water and filtering for multiple times until the pH value of the filtrate is neutral. Drying the filtrate in a constant temperature air-blast drying oven at 105 deg.C for 12 hr, and grinding. The mixture is evenly mixed with sodium hydroxide solution with the mass fraction of 5 percent according to the solid-to-liquid ratio of 1: 10. And performing microwave irradiation for 15min under the conditions of microwave temperature of 60 ℃ and microwave power of 600W. And after cooling and precipitation, pouring out the alkali liquor, and filtering the fly ash subjected to mixed alkali treatment for multiple times by using deionized water washing paint until the pH value of the filtrate is neutral. The filtrate was dried in a constant temperature forced air drying oven at 105 ℃ for 12 h. The fly ash capable of adsorbing VOCs is prepared.
Comparative example 2
Sieving 10 g of fly ash from a power plant, mixing the undersize of 80 meshes with 20% hydrochloric acid according to the mass ratio of 10: 1 of the fly ash by the volume of the hydrochloric acid, and stirring for 2 hours in a water bath kettle at 80 ℃. After cooling and precipitation, pouring off acid liquor, washing paint with deionized water and filtering for multiple times until the pH value of the filtrate is neutral. Drying the filtrate in a constant temperature air-blast drying oven at 105 deg.C for 12 hr, and grinding. The mixture is evenly mixed with 15 percent sodium hydroxide solution according to the solid-to-liquid ratio of 1: 10. And performing microwave irradiation for 15min under the conditions of microwave temperature of 60 ℃ and microwave power of 600W. And after cooling and precipitation, pouring out the alkali liquor, and filtering the fly ash subjected to mixed alkali treatment for multiple times by using deionized water washing paint until the pH value of the filtrate is neutral. The filtrate was dried in a constant temperature forced air drying oven at 105 ℃ for 12 h. The fly ash capable of adsorbing VOCs is prepared.
Comparative example 3
Sieving 10 g of fly ash from a power plant, mixing the undersize of 80 meshes with 20% hydrochloric acid according to the mass ratio of 10: 1 of the fly ash by the volume of the hydrochloric acid, and stirring for 2 hours in a water bath kettle at 80 ℃. After cooling and precipitation, pouring off acid liquor, washing paint with deionized water and filtering for multiple times until the pH value of the filtrate is neutral. Drying the filtrate in a constant temperature air-blast drying oven at 105 deg.C for 12 hr, and grinding. The mixture is evenly mixed with sodium hydroxide solution with the concentration of 7mol/L according to the solid-to-liquid ratio of 1: 10. And performing microwave irradiation for 15min under the conditions of microwave temperature of 60 ℃ and microwave power of 600W. And after cooling and precipitation, pouring out the alkali liquor, and filtering the fly ash subjected to mixed alkali treatment for multiple times by using deionized water washing paint until the pH value of the filtrate is neutral. The filtrate was dried in a constant temperature forced air drying oven at 105 ℃ for 12 h. The fly ash capable of adsorbing VOCs is prepared.
Comparative example 4
Sieving 10 g of fly ash from a power plant, mixing the undersize of 80 meshes with 20% hydrochloric acid according to the mass ratio of 10: 1 of the fly ash by the volume of the hydrochloric acid, and stirring for 2 hours in a water bath kettle at 80 ℃. After cooling and precipitation, pouring off acid liquor, washing paint with deionized water and filtering for multiple times until the pH value of the filtrate is neutral. Drying the filtrate in a constant temperature air-blast drying oven at 105 deg.C for 12 hr, and grinding. The mixture is evenly mixed with sodium hydroxide solution with the concentration of 8mol/L according to the solid-to-liquid ratio of 1: 10. And performing microwave irradiation for 15min under the conditions of microwave temperature of 60 ℃ and microwave power of 600W. And after cooling and precipitation, pouring out the alkali liquor, and filtering the fly ash subjected to mixed alkali treatment for multiple times by using deionized water washing paint until the pH value of the filtrate is neutral. The filtrate was dried in a constant temperature forced air drying oven at 105 ℃ for 12 h. The fly ash capable of adsorbing VOCs is prepared.
Comparative example 5
Sieving the fly ash of the power plant, and taking the 80-mesh screen underflow for later use.
The modified fly ash products prepared in examples 1-2 and comparative examples 1-5 were tested for performance. The method comprises the steps of preparing VOCs with stable concentration by using a bubbling method, then adding a certain mass of fly ash into a gas path, measuring the concentration of organic matters before and after the product is connected and the penetration time of adsorption by using a gas chromatograph, and calculating the adsorption rate and the adsorption quantity.
The following are the experimental results of the product for adsorbing two representative VOCs of toluene and ethyl acetate:
as can be seen from the adsorption experiment results of example 1 and comparative example 1/2/5, under the same test conditions, the modified fly ash prepared by the method has a significantly better toluene adsorption effect than untreated raw ash, and a specific value for optimizing the adsorption efficiency exists within the concentration range of NaOH involved in the method. As can be seen from the adsorption test results of example 2 and comparative example 3/4/5, under the same test conditions, the modified fly ash prepared by the method has a significantly better adsorption effect on ethyl acetate than untreated raw ash, and a specific value for optimizing the adsorption efficiency exists within the concentration range of NaOH involved in the method.
The above are merely examples of the method and do not limit the scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. A preparation method of a modified fly ash adsorbent for VOCs is characterized by comprising the following steps:
1) putting the fly ash calcined in a high-temperature furnace into a hydrochloric acid solution with the mass fraction of 20% according to the mass ratio of 1: 10, stirring and treating for 2 hours in a water bath kettle at the temperature of 80 ℃, pouring off the acid solution after the solution is cooled and precipitated, washing and filtering the fly ash modified by acid by using deionized water until the pH value of the filtrate is about 7, drying the filtrate on the filter paper in a constant-temperature air-blast drying oven at the temperature of 105 ℃ for 12 hours, and grinding after drying;
2) uniformly mixing the acid modified fly ash and a sodium hydroxide solution according to the solid-liquid mass ratio of 1: 10, placing the mixture in a microwave oven, performing microwave irradiation for 15min at the microwave temperature of 60 ℃ and the microwave power of 600W, pouring out alkali liquor after cooling and precipitating, washing the fly ash modified by alkali and microwave by deionized water, and filtering until the pH value of a filtrate is about 7;
3) and (3) drying the filtrate in a constant-temperature air-blast drying oven at 105 ℃ for 12h to obtain the modified fly ash for adsorbing VOCs.
2. The method for preparing the modified fly ash adsorbent for VOCs according to claim 1, wherein the calcination temperature of the high temperature furnace in the step 1) is 850 ℃, and the calcination time is 2 h; the acid modified fly ash is ground into powder and is sieved by a 80-mesh sieve after being modified.
3. The method according to claim 1, wherein the concentration of the sodium hydroxide solution in step 2) is 5% to 25%, preferably 8% to 12%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210346838A1 (en) * | 2020-05-11 | 2021-11-11 | Wisconsin Alumni Research Foundation | Method for sulfur removal from coal fly ash |
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