CN112427013A - Preparation method and application of flue gas dechlorination material - Google Patents
Preparation method and application of flue gas dechlorination material Download PDFInfo
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- CN112427013A CN112427013A CN202011177269.9A CN202011177269A CN112427013A CN 112427013 A CN112427013 A CN 112427013A CN 202011177269 A CN202011177269 A CN 202011177269A CN 112427013 A CN112427013 A CN 112427013A
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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
- B01J20/20—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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- 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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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- 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
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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Abstract
The invention relates to a preparation method and application of a flue gas dechlorination material, which comprises the steps of carrying out vacuum treatment on a sieve mesh adsorbing material at the temperature of 80-120 ℃ to discharge air in pore channels of the sieve mesh adsorbing material, then impregnating the sieve mesh adsorbing material subjected to vacuum treatment with a silver nitrate impregnation liquid in a vacuum and dark state, adjusting the pH value of the silver nitrate impregnation liquid to 6.0-6.5 by using a nitric acid solution, continuously stirring and mixing for at least 3 hours, separating out the sieve mesh adsorbing material, adsorbing silver ions in the pores of the sieve mesh adsorbing material, and finally washing and drying the separated sieve mesh adsorbing material in sequence to obtain the flue gas dechlorination material.
Description
Technical Field
The invention belongs to the technical field of flue gas purification, and relates to a preparation method and application of a flue gas dechlorination material.
Background
Flue gas discharged from industrial coal, biomass and garbage combustion boilers contains a large amount of chlorine (Cl) elements, and generally exists in the form of ions. The Cl ions existing in the flue gas in large quantity not only corrode a flue gas pipeline, but also have adverse effects on subsequent desulfurization and denitration, and finally the Cl ions discharged into the atmosphere can also affect the atmospheric environment, climate change and human health. The current technology is mainly based on the characteristic that Cl ions have strong water solubility, and Cl in flue gas is dissolved into desulfurization and denitration spray in a spraying mode and then is led out in the form of wastewater. The method has the disadvantage that a large amount of Cl ions in the wastewater cause Na in the wastewater2SO3The recovery is difficult, and the conductivity of the wastewater is too high, which affects the wastewater treatment efficiency. Meanwhile, the stability of Cl ions in water is high, and the problems of pipeline corrosion, treatment cost improvement and the like are also brought to the treatment of desulfurization and denitration wastewater, and the flue gas desulfurization efficiency cannot be effectively improved due to the fact that the existing method is used for directly dechlorinating fresh flue gas.
Disclosure of Invention
The invention aims to provide a preparation method and application of a flue gas dechlorination material, so as to overcome the defects of the prior art
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the flue gas dechlorination material is characterized by comprising the following steps of:
step 1), carrying out vacuum treatment on the sieve pore adsorption material at the temperature of 80-120 ℃;
step 2), soaking the sieve mesh adsorbing material subjected to vacuum treatment by using a silver nitrate soaking solution in a vacuum and dark state, adjusting the pH value of the silver nitrate soaking solution to 6.0-6.5 by using a nitric acid solution, continuously stirring and mixing for at least 3 hours, and separating out the sieve mesh adsorbing material;
and 3) finally, washing and drying the separated sieve pore adsorption materials in sequence to obtain the flue gas dechlorination material.
Furthermore, the sieve pore adsorption material adopts a molecular sieve or an activated carbon material.
Further, the specific surface area of the molecular sieve is 1025m2/g。
Further, the specific surface area of the activated carbon material is 2055m2/g。
Further, the molecular sieve is prepared by the following method:
step 1), taking the following raw materials according to molar ratio: sodium metaaluminate: NaOH: KOH: water glass: water (0.8-1.2), (11-15), (12-16), (2-2.4), (100) and 120);
completely dissolving sodium metaaluminate in water to form sodium metaaluminate dissolving solution, sequentially adding NaOH and KOH into the sodium metaaluminate dissolving solution until the sodium metaaluminate dissolving solution is completely dissolved to obtain mixed solution A, then adding water glass into the mixed solution A, uniformly stirring to obtain mixed solution B,
step 2), sequentially aging and crystallizing the mixed solution B in a reaction kettle, and cooling in cold water after crystallization to obtain a crystallized product; and finally, fully washing the crystallized product in water, and then sequentially drying and grinding to obtain the low-silica-alumina-ratio molecular sieve.
Further, static aging is carried out in a reaction kettle at 65-75 ℃ for 2.5-3.5h, and then crystallization is carried out at 95-105 ℃ for 1.5-2.5 h.
Further, a magnetic stirrer is adopted to continuously stir for at least 3 hours at the rotating speed of 600r/min-700 r/min.
Further, the concentration of the silver nitrate impregnation liquid is 0.5 mol/L; the concentration of the nitric acid solution is 0.1 mol/L.
A method for dechlorinating flue gas, which comprises the step of placing the flue gas dechlorinating material prepared by the method in a filtering pipeline for filtering the flue gas.
Further, placing the flue gas dechlorination material obtained by filtering the flue gas into a mixed solution of sodium sulfite and ammonia, wherein the mass ratio of the mixed solution of sodium sulfite and ammonia is 1:1, the concentration of sodium sulfite is 2mol/L, and the concentration of ammonia is 1 mol/L; stirring and mixing evenly and fully reacting under the dark vacuum condition to complete the flue gas dechlorination regeneration treatment.
Compared with the prior art, the invention has the following beneficial technical effects:
the utility model provides a flue gas dechlorination material preparation method, through carrying out vacuum treatment with sieve mesh adsorbing material under 80-120 ℃ and discharging the air in the sieve mesh adsorbing material pore canal, then adopt silver nitrate impregnation liquid to impregnate the sieve mesh adsorbing material after the vacuum treatment under the vacuum light-tight state, then adopt nitric acid solution to adjust the pH value of silver nitrate impregnation liquid to 6.0 ~ 6.5, then separate out the sieve mesh adsorbing material after continuously stirring and mixing at least 3h, can make silver ion adsorb in the pore of sieve mesh adsorbing material, wash the sieve mesh adsorbing material who separates out in proper order at last, the flue gas dechlorination material can be obtained in the drying, the flue gas dechlorination material that obtains can pass through anion and Cl ion's specific reaction, reach the direct purpose of dechlorination from the flue gas, high adsorption efficiency, and dechlorination material can be regenerated and repeatedly used.
Further, the specific surface area is 1025m2The molecular sieve has the advantages of optimal adsorption effect and high adsorption efficiency.
According to the flue gas dechlorination method, the porous characteristic of the flue gas dechlorination material is adopted, the wind resistance is low, the energy consumption is reduced, the existing flue gas purification equipment is not required to be changed, and the selective absorption efficiency of HCl can be improved remarkably.
Furthermore, anions in the flue gas dechlorination material which is saturated in the adsorption mode are recycled through regeneration treatment, so that the recycling efficiency is high, and the cost is low.
Drawings
FIG. 1 is a flow chart of a dechlorination module in a flue gas treatment system according to an embodiment of the present invention.
Fig. 2 is a graph of experimental results of the static adsorption of HCl on the silver ion-modified material in the embodiment of the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
a preparation method of a flue gas dechlorination material comprises the following steps:
step 1), carrying out vacuum treatment on the sieve pore adsorption material at 80-120 ℃ to discharge air in a pore channel of the sieve pore adsorption material; vacuum treatment at 80-120 deg.c can raise the thiophanate efficiency without destroying the porous structure.
The sieve pore adsorption material is a molecular sieve or an activated carbon material;
preferably, the specific surface area is 1025m2A molecular sieve per gram.
Specifically, the preparation process of the molecular sieve is as follows:
step 1), completely dissolving sodium metaaluminate in water to form a sodium metaaluminate solution, wherein the solution is transparent or yellowish when the sodium metaaluminate is completely dissolved; sequentially adding NaOH and KOH into the sodium metaaluminate dissolving solution until the NaOH and the KOH are completely dissolved to obtain a mixed solution A, then adding water glass (metasilicic acid) into the mixed solution A, and continuously stirring until the mixture is uniform to obtain a mixed solution B, wherein the molar ratio of the sodium metaaluminate to the NaOH to the KOH to the water glass to the water is as follows: (0.8-1.2): 11-15): 12-16): 2-2.4): 100-120);
preferably, the molar ratio of sodium metaaluminate, NaOH, KOH, water glass and water adopted in the application is as follows: the raw material ratio of 1:13:14:2.2:110 is used for obtaining the molecular sieve with low silica-alumina ratio.
Step 2), aging and crystallizing the mixed solution B in a reaction kettle, and cooling in cold water after crystallization to obtain a crystallized product; and finally, fully washing the crystallized product in water, and then drying and grinding the crystallized product to obtain the molecular sieve with the low silica-alumina ratio.
Specifically, static aging is carried out in a reaction kettle at 65-75 ℃ for 2.5-3.5h, and then crystallization is carried out at 95-105 ℃ for 1.5-2.5 h.
Specifically, the molecular sieve and the active carbon are respectively treated in vacuum at 80-120 ℃, the vacuum degree is-0.095 to-0.090, and the vacuum state is kept for 8-10 hours; the vacuum treatment can evacuate air from the pores of the material.
Step 2), soaking the sieve mesh adsorbing material subjected to vacuum treatment by using a silver nitrate soaking solution in a vacuum and dark state, adjusting the pH value of the silver nitrate soaking solution to 6.0-6.5 by using a nitric acid solution, continuously stirring and mixing for at least 3 hours, and separating out the sieve mesh adsorbing material;
specifically, a magnetic stirrer is adopted to continuously stir for at least 3 hours at the rotating speed of 600r/min-700r/min, so that silver nitrate silver ions are fully adsorbed in gaps of the sieve pore adsorbing material.
Specifically, the concentration of the silver nitrate impregnation liquid is 0.4-0.6 mol/L; the concentration of the nitric acid solution is 0.05-0.15 mol/L.
Preferably, the concentration of the silver nitrate impregnation liquid adopted by the application is 0.5 mol/L; the concentration of the nitric acid solution is 0.1mol/L
The vacuum impregnation condition is used in the stirring process, so that the silver ions are more uniformly distributed on the carrier and can enter active sites in the pore channels, and the loading capacity of the silver ions is improved.
And 3) finally, washing and drying the separated sieve pore adsorption materials in sequence to obtain the flue gas dechlorination material, namely the nano silver modified material.
The flue gas dechlorination method of the flue gas dechlorination material based on the preparation method comprises the following steps:
as shown in fig. 1, the flue gas dechlorination material prepared in the above way is placed in a filtering pipeline, the flue gas dechlorination material adsorbs chloride ions in flue gas passing through the pipeline and then regenerates, the saturated flue gas dechlorination material mainly comprises AgCl, the flue gas dechlorination material adsorbing the chloride ions is placed in a mixed solution of sodium sulfite and ammonia according to the mass ratio of 1:1, the concentration of the sodium sulfite is 2mol/L, and the concentration of the ammonia is 1 mol/L; stirring and mixing evenly under the dark vacuum condition, wherein the temperature is 20-25 ℃; specifically, under the dark condition, the vacuum degree is-0.095 to-0.090, the stirring speed is 600r/min to 700r/min, the stirring is carried out for at least 4 hours, and experiments show that when the concentration of the silver in the leaching solution is 30g/L, the mixed solution of the sodium sulfite and the ammonia water can be circularly leached out of the silver chloride for 11 times. The leached Ag is separated and dried, and then reacts with nitric acid to obtain silver nitrate which can be reused, thereby achieving the purpose of material regeneration.
According to the invention, the flue gas dechlorination material can be made into the modularized adsorption module, and after the flue gas dechlorination material is placed in a dust removal link, due to the porous characteristic of the flue gas dechlorination material, the wind resistance is low, the energy consumption is reduced, the existing flue gas purification equipment is not required to be changed, the anions in the adsorbed saturated flue gas dechlorination material can be recovered through regeneration treatment, the recovery efficiency is high, the cost is low, and the cost problem of dechlorination is solved.
Example 1:
step 1), taking the following raw materials according to molar ratio: sodium metaaluminate: NaOH: KOH: water glass: water 1:13:14:2.2: 110; completely dissolving sodium metaaluminate in water to form sodium metaaluminate dissolving solution, sequentially adding NaOH and KOH into the sodium metaaluminate dissolving solution until the sodium metaaluminate dissolving solution is completely dissolved to obtain mixed solution A, then adding water glass into the mixed solution A, uniformly stirring to obtain mixed solution B,
step 2), sequentially aging and crystallizing the mixed solution B in a reaction kettle, and cooling in cold water after crystallization to obtain a crystallized product; finally, fully washing the crystallized product in water, and then sequentially drying and grinding to obtain the molecular sieve with the low silica-alumina ratio;
step 3), carrying out vacuum treatment on the obtained low-silicon-aluminum ratio molecular sieve at 100 ℃;
step 2), soaking the sieve mesh adsorption material subjected to vacuum treatment by using a silver nitrate impregnation liquid in a vacuum and dark state, adjusting the pH value of the silver nitrate impregnation liquid to 6.3 by using a nitric acid solution, continuously stirring and mixing for 3 hours, and separating out the sieve mesh adsorption material;
and 3) finally, washing and drying the separated sieve pore adsorption materials in sequence to obtain the flue gas dechlorination material.
The same preparation method steps as the embodiment are adopted, sodium metaaluminate, NaOH, KOH, water glass and water are taken according to different molar ratios to prepare the low silica alumina ratio molecular sieve material, then the obtained low silica alumina ratio molecular sieve material is subjected to silver ion modification treatment to obtain different flue gas dechlorination materials, finally flue gas treatment is carried out to obtain different Cl adsorption efficiencies, and the specific results are shown in Table 1:
the specific surface area to be obtained in the present application from the above-mentioned example 1 was 1025m2The specific surface area of the molecular sieve (molecular sieve-1)/g is 702m compared with that of the existing molecular sieve directly purchased2Molecular sieve (molecular sieve-2) and a specific surface area of 2055 m/g2The active carbon per gram is respectively subjected to silver ion modification treatment and then subjected to smoke treatmentThe specific flue gas and filtering structure of the dechlorination treatment are shown in Table 2, and it can be seen from Table 2 that the specific surface area of the material modified by adding silver is 1025m2The silver attached amount in the/g molecular sieve can reach 25.6 percent, and the specific surface area is 702m2The silver content of the molecular sieve per gram reaches 12.2 percent, and the specific surface area is 2055m2The silver attached amount in the active carbon per gram reaches 15.5 percent, and the specific surface area is 1025m2The silver ion loading effect in the/g molecular sieve is best.
Table 2 shows the molecular sieves synthesized in the present application and the existing specific surface area of 702m2A molecular sieve per gram and a specific surface area of 2055m2Result data of flue gas treatment with activated carbon per gram (X-ray fluorescence spectrum characterization result)
As can be seen from FIG. 2, the molecular sieve material modified by silver ions is obviously superior to the material without modification in the HCl static adsorption experiment, wherein the modified molecular sieve-1 can reach adsorption balance within 5 hours, the adsorption efficiency is up to more than 25%, and is more than 2 times higher than that of the modified molecular sieve-2, which indicates that the low-silica-alumina ratio molecular sieve prepared by the invention has better matching property with Ag ions. The modified activated carbon can reach adsorption balance within 5h, the Cl adsorption efficiency reaches more than 15 percent, but the effect is still obviously lower than that of the modified molecular sieve-1. Compared with the original form of the three porous materials modified by silver ions, the three porous materials modified by silver ions show extremely high HCl adsorption efficiency, and the average efficiency is higher than 5 times. The result shows that the adsorption material modified by silver ions has a remarkable effect of improving the selective absorption efficiency of HCl. Has extremely high selective adsorption and adsorption efficiency, and is suitable for being used as a material for directly dechlorinating flue gas. The low silica alumina ratio molecular sieve of the invention has the highest efficiency after being improved.
TABLE 3 characterization results of X-ray fluorescence spectra of porous materials after desorption
Table 3 shows the elemental composition of the porous material after equilibrium of adsorbed Cl and recovery of Ag from a mixed solution of sodium sulfite and ammonia for 4 hours. The results show that the recovery rates of the Ag loaded in the molecular sieve-1, the molecular sieve-2 and the activated carbon are 93.67%, 90.20% and 92.06% respectively, so that higher recovery rate levels are achieved, and the recycling of the Ag is basically completed.
Claims (10)
1. The preparation method of the flue gas dechlorination material is characterized by comprising the following steps of:
step 1), carrying out vacuum treatment on the sieve pore adsorption material at the temperature of 80-120 ℃;
step 2), soaking the sieve mesh adsorbing material subjected to vacuum treatment by using a silver nitrate soaking solution in a vacuum and dark state, adjusting the pH value of the silver nitrate soaking solution to 6.0-6.5 by using a nitric acid solution, continuously stirring and mixing for at least 3 hours, and separating out the sieve mesh adsorbing material;
and 3) finally, washing and drying the separated sieve pore adsorption materials in sequence to obtain the flue gas dechlorination material.
2. The method for preparing the flue gas dechlorination material according to claim 1, wherein the sieve pore adsorption material is a molecular sieve or an activated carbon material.
3. The method for preparing the flue gas dechlorination material according to claim 1, wherein the specific surface area of the molecular sieve is 1025m2/g。
4. The method for preparing the flue gas dechlorination material according to claim 1, wherein the specific surface area of the activated carbon material is 2055m2/g。
5. The method for preparing the flue gas dechlorination material according to the claim 2 or 3, characterized in that the molecular sieve is prepared by the following method:
step 1), taking the following raw materials according to molar ratio: sodium metaaluminate: NaOH: KOH: water glass: water (0.8-1.2), (11-15), (12-16), (2-2.4), (100) and 120);
completely dissolving sodium metaaluminate in water to form sodium metaaluminate dissolving solution, sequentially adding NaOH and KOH into the sodium metaaluminate dissolving solution until the sodium metaaluminate dissolving solution is completely dissolved to obtain mixed solution A, then adding water glass into the mixed solution A, uniformly stirring to obtain mixed solution B,
step 2), sequentially aging and crystallizing the mixed solution B in a reaction kettle, and cooling in cold water after crystallization to obtain a crystallized product; and finally, fully washing the crystallized product in water, and then sequentially drying and grinding to obtain the low-silica-alumina-ratio molecular sieve.
6. The preparation method of the flue gas dechlorinated material according to claim 5, wherein the material is statically aged for 2.5-3.5 hours at 65-75 ℃ in a reaction kettle, and then crystallized for 1.5-2.5 hours at 95-105 ℃.
7. The method for preparing the flue gas dechlorinated material according to claim 1, wherein the magnetic stirrer is used for stirring at a speed of 600r/min-700r/min for at least 3 h.
8. The method for preparing the flue gas dechlorination material according to claim 1, wherein the concentration of the silver nitrate impregnation liquid is 0.5 mol/L; the concentration of the nitric acid solution is 0.1 mol/L.
9. A flue gas dechlorination method, characterized in that the flue gas dechlorination material prepared by the method in claim 1 is placed in a filtering pipeline for flue gas filtration.
10. The flue gas dechlorination method according to claim 9, characterized in that the flue gas dechlorination material obtained by filtering the flue gas is placed in a mixed solution of sodium sulfite and ammonia in a mass ratio of 1:1, the concentration of sodium sulfite is 2mol/L, and the concentration of ammonia is 1 mol/L; stirring and mixing evenly and fully reacting under the dark vacuum condition to complete the flue gas dechlorination regeneration treatment.
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