CN110639473A - Modified activated carbon adsorbent for adsorbing NOx at high temperature and preparation method thereof - Google Patents
Modified activated carbon adsorbent for adsorbing NOx at high temperature and preparation method thereof Download PDFInfo
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- CN110639473A CN110639473A CN201911003202.0A CN201911003202A CN110639473A CN 110639473 A CN110639473 A CN 110639473A CN 201911003202 A CN201911003202 A CN 201911003202A CN 110639473 A CN110639473 A CN 110639473A
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- 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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- 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
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- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/404—Nitrogen oxides other than dinitrogen oxide
Abstract
Used for adsorbing NO at high temperaturexThe invention relates to a modified activated carbon adsorbent and a preparation method thereof, belonging to the technical field of adsorbents, and the modified activated carbon adsorbent is characterized by being prepared from the following raw materials in parts by weight: 15-25 parts of raw material active carbon, 4-5 parts of potassium carbonate, 0.2-1 part of potassium silicate and 45-60 parts of water. Impregnation is carried out first and then calcination is carried out. The invention has simple process and low cost, and can treat NO at normal temperature to 120 DEG CxHas good adsorption effect, and the adsorbent is nontoxic, harmless and easy to regenerate.
Description
Technical Field
The invention relates to a method for adsorbing NO at high temperaturexThe preparation method of the modified activated carbon adsorbent. Belongs to the technical field of adsorbents.
Background
At present, the weather of haze is frequent, the environmental problem is increasingly prominent, and NO isxIs one of the main pollutants in the atmosphere, and NO is strengthened in various countriesxThe treatment strength of (2). The current adsorption method is to treat NOxAs long as it isThe method has the advantages of simple process and low cost. But when the temperature of the flue gas is higher, the active carbon NOxThe adsorption capacity is poor, the improvement of the adsorption capacity of the activated carbon becomes a current research focus, and a scholars can improve the pore structure of the activated carbon to achieve the effects of hole expansion and capacity increase by treating the activated carbon with an oxidant; the researchers also improve the adsorption capacity of the activated carbon by treating the activated carbon with alkali liquor containing potassium or sodium and metal salt solution, improving the types and the number of surface functional groups, introducing metal cations and the like.
CN101480603A discloses a preparation method of a nitrogen oxide adsorbent, which prepares modified activated carbon by combining surface oxidation modification, solution impregnation and metal loading, the activated carbon has excellent adsorption effect under normal temperature and pressure, and has good SO adsorption effect2The VOC has better adsorption effect; CN101879435A discloses a method for preparing a high-adsorption-capacity normal-temperature nitrogen oxide adsorbent, which comprises the steps of pre-oxidizing activated carbon by an oxidizing solution, drying, roasting, soaking by a metal salt solution twice, drying and roasting to obtain the adsorbent suitable for adsorbing NO at normal temperaturexThe adsorbent is NO at 25 DEG CxThe adsorption capacity can reach 80 mg/g; CN101884906A discloses a method for preparing modified activated carbon by using metal oxide and urea through impregnation modification, wherein NO is contained in the activated carbon under the conditions of normal temperature and normal pressurexThe removal effect of (2) is excellent.
In the existing preparation methods of modified activated carbon, some methods need washing after the activated carbon is soaked, a large amount of waste water is generated, and the subsequent treatment process is complex; some methods need harmful modification reagents, thus threatening human health; some methods require multiple times of dipping treatment, so that the production steps are complicated and large-scale production is difficult to realize. The evaluation conditions are single, and SO is not considered2、CO2Influence of water vapor on adsorption performance of the activated carbon; the adsorption performance of the activated carbon was evaluated only under normal temperature and pressure conditions, and the adsorption performance under high temperature conditions was not evaluated. The invention develops a modified activated carbon adsorbent suitable for high temperature conditions aiming at the limit of the scale production and application of the modified activated carbon, and the modified activated carbon adsorbent is prepared at 120℃ and containsWith SO2、CO2Under the condition of water vapor, NO thereofxThe adsorption capacity can reach more than 0.3mmol/g, the adsorption capacity is improved by 40-55 times compared with the original adsorption capacity, the production process of the adsorbent is simple, and the used modification reagent is non-toxic and harmless and is suitable for large-scale production.
Disclosure of Invention
The invention aims to provide a method for adsorbing NO at high temperaturexThe preparation method of the modified activated carbon adsorbent; the adsorbent has the advantages of large adsorption capacity, simple preparation method, no toxicity and harmlessness of the modifying reagent, and suitability for large-scale production.
The technical scheme of the invention is as follows:
used for adsorbing NO at high temperaturexThe modified activated carbon adsorbent and the preparation method thereof are characterized by being prepared from the following raw materials in parts by weight: raw materials of activated carbon, potassium carbonate, potassium silicate and water, wherein the raw materials of the activated carbon are 15-25%, the potassium carbonate is 4-5%, the potassium silicate is 0.2-1%, and the water is preferably 45-60%.
Used for adsorbing NO at high temperaturexThe preparation method of the modified activated carbon adsorbent comprises the following steps:
(1) weighing raw materials according to the composition of raw materials of the adsorbent, wherein the activated carbon is coal-based activated carbon, fruit-wood-based activated carbon and the like, and the ash content of the activated carbon is 5-13%;
(2) dissolving potassium carbonate in partial water to prepare a solution, adding the prepared potassium silicate aqueous solution, and ultrasonically stirring uniformly for later use;
(3) slowly pouring the prepared solution in the step (2) into active carbon, and continuously shaking until the solution just passes through the active carbon; then stirring once every 10-15 min for 4-6 times, and performing ultrasonic treatment for 2-5 min after each stirring is finished;
(4) soaking activated carbon for 6-12 h, uniformly stirring the activated carbon, discharging residual liquid in the activated carbon, performing microwave treatment on the activated carbon for 2-8 min by using a microwave reactor, and finally continuously drying in an oven;
(5) and (3) placing the dried activated carbon in a tubular furnace, heating to 550-650 ℃ at a heating rate of 3-5 ℃/min under the atmosphere of one or the combination of inert gases such as nitrogen, helium, argon and the like, and roasting for 2h under the temperature condition, wherein the preferred temperature is 600 ℃. And cooling the activated carbon to room temperature, and drying and storing.
The activated carbon adsorbent is used for adsorbing NO at high temperaturexFor example, nitrogen oxide NO is adsorbed under the high temperature condition of 100-120 DEG Cx。
The invention has the following advantages:
(1) has excellent adsorption performance at normal temperature to 120 ℃, and has stronger CO resistance2And the water-mixing capacity is improved by 40-55 times compared with the original capacity when the efficiency reaches 50% at the high temperature of 120 ℃.
(2) No toxicity and harm, and no secondary pollution in the preparation process.
(3) The preparation process is simple, the cost is low, and the method is suitable for large-scale production.
Drawings
FIG. 1 shows NO at 120 deg.C before and after modification with activated carbon (1#, 2#)xAdsorption rate change curve.
FIG. 2 shows NO of modified activated carbon (3#) at 100 deg.CxAdsorption rate change curve.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1:
weighing 5 parts of potassium carbonate in a beaker, adding 50 parts of deionized water, stirring for dissolving, adding 0.5 part of potassium silicate to prepare a solution, uniformly stirring by ultrasound for later use, taking 30 parts of proper coal-based activated carbon (the ash content of the coal-based activated carbon is 12.5%, the same applies below) in a conical flask, adding the prepared solution to just immerse the activated carbon, shaking, stirring once every 10min, stirring for 6 times totally, and performing ultrasound for 4min after each stirring is finished; soaking activated carbon overnight, removing residual liquid, then placing the activated carbon in a microwave reactor for treatment for a certain time, and finally placing the activated carbon in a 110 ℃ oven for complete drying; after the active carbon is dried, the active carbon is placed in a tube furnace, and the reaction is carried out in N2Roasting at 600 deg.C for 2h under atmosphere, cooling to room temperature, and drying and storing the activated carbon adsorbent. The modified activated carbon is marked as No. 2,unmodified activated carbon is noted as 1 #.
Example 2:
weighing 4.5 parts of potassium carbonate into a beaker, adding 50 parts of deionized water, stirring for dissolving, adding 0.95 part of potassium silicate to prepare a solution, uniformly stirring by ultrasound for later use, adding 25 parts of coal-based activated carbon (the ash content of the coal-based activated carbon is 12.5 percent, the same applies below) into a conical flask, adding the prepared solution to just immerse the activated carbon, shaking, stirring once every 10min, stirring for 6 times totally, and performing ultrasound for 5min after each stirring; soaking activated carbon overnight, removing residual liquid, then placing the activated carbon in a microwave reactor for treatment for a certain time, and finally placing the activated carbon in a 110 ℃ oven for complete drying; after the active carbon is dried, the active carbon is placed in a tube furnace, and the reaction is carried out in N2Roasting at 600 deg.C for 2h under atmosphere, cooling to room temperature, and drying and storing the activated carbon adsorbent. The modified activated carbon is marked as # 3.
Test example 1:
the testing device is shown in fig. 1, and comprises the following specific steps: the gas is distributed by using the gas in the steel cylinder, the concentration of NO is controlled to be about 200ppm, and SO is controlled2Concentration of about 25ppm, CO2About 4.5% of O2The content is about 15 percent, the water vapor content is 1.5 percent, the gas flow is 1.7L/min, the gas velocity in the adsorption column is 0.1m/s, the temperature of an adsorbent bed layer is 120 ℃, the dosage of an adsorbent is 15g, the thickness of the bed layer is about 10cm, and a flue gas analyzer is used for continuously monitoring NO at an outletxConcentration until the outlet NO concentration reaches 50% of the inlet concentration. The modified active carbon NO can be obtained by calculationxThe adsorption capacity of the adsorbent # (2#) to NO can reach more than 0.335mmol/g, which is 55.8 times higher than that of the activated carbon sample # (1 #).
Test example 2:
the testing device is shown in fig. 1, and comprises the following specific steps: the gas is distributed by using the gas in the steel cylinder, the concentration of NO is controlled to be about 200ppm, and SO is controlled2Concentration of about 25ppm, CO2About 4.5% of O2The content is about 15 percent, the water vapor content is 1.5 percent, the gas flow is 1.7L/min, the gas velocity in the adsorption column is 0.1m/s, the temperature of an adsorbent bed layer is 100 ℃, the dosage of an adsorbent is 15g, the thickness of the bed layer is about 10cm, and a flue gas analyzer is used for continuously monitoring NO at an outletxIn a concentration ofThe outlet NO concentration reached 50% of the inlet concentration. The modified active carbon NO can be obtained by calculationx Adsorbent # 3 to NOxThe adsorption capacity of the adsorbent can reach more than 0.307 mmol/g.
TABLE 1 NO before and after modification of activated carbon under different temperature conditionsxComparison of adsorption amount
Claims (4)
1. Used for adsorbing NO at high temperaturexThe preparation method of the modified activated carbon adsorbent is characterized by being prepared from the following raw materials in parts by weight: raw materials of activated carbon, potassium carbonate, potassium silicate and water, wherein the raw materials of the activated carbon are 15-25%, the potassium carbonate is 4-5%, the potassium silicate is 0.2-1%, and the water is preferably 45-60%;
the preparation method comprises the following steps:
(1) weighing raw materials according to the composition of raw materials of the adsorbent, wherein the activated carbon is coal-based activated carbon, fruit-wood-based activated carbon and the like, and the ash content of the activated carbon is 5-13%;
(2) dissolving potassium carbonate in partial water to prepare a solution, adding the prepared potassium silicate aqueous solution, and ultrasonically stirring uniformly for later use;
(3) slowly pouring the prepared solution in the step (2) into active carbon, and continuously shaking until the solution just passes through the active carbon; then stirring once every 10-15 min for 4-6 times, and performing ultrasonic treatment for 2-5 min after each stirring is finished;
(4) soaking activated carbon for 6-12 h, uniformly stirring the activated carbon, discharging residual liquid in the activated carbon, performing microwave treatment on the activated carbon for 2-8 min by using a microwave reactor, and finally continuously drying in an oven;
(5) and (3) placing the dried activated carbon in a tubular furnace, heating to 550-650 ℃ at a heating rate of 3-5 ℃/min under the atmosphere of one or a combination of inert gases such as nitrogen, helium, argon and the like, roasting for 2h under the temperature condition, cooling the activated carbon to room temperature, and drying and storing.
2. The method of claim 1, wherein the temperature of the calcination in step (5) is 600 ℃.
3. The modified activated carbon adsorbent prepared according to the method of claim 1 or 2.
4. Use of the modified activated carbon adsorbent prepared according to the method of claim 1 or 2 for high temperature adsorption of NOxAdsorbing nitrogen oxide NO at 100-120 deg.cx。
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