CN114558564B - Charcoal @ metal type denitration catalyst based on active algae and preparation method thereof - Google Patents
Charcoal @ metal type denitration catalyst based on active algae and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a biochar @ metal type denitration catalyst based on active algae and a preparation method thereof, belonging to the technical field of sewage treatment and atmospheric pollution treatment. The obtained catalyst can be applied to SCR, and the preparation and application cost of the denitration catalyst can be reduced while the high removal rate of nitrogen oxides is kept. Meanwhile, the active algae and metal ions which are extremely easy to generate harm in the water body can be effectively utilized, the values of the active algae and the metal ions are greatly improved, and the influence and the harm to the water body environment are reduced.
Description
Technical Field
The invention belongs to the technical field of sewage treatment and atmospheric pollution treatment, and particularly relates to a charcoal @ metal type denitration catalyst based on active algae and a preparation method thereof.
Background
In recent years, the phenomenon of active algae pollution in water frequently occurs, the active algae can cause water bloom, meanwhile, algae toxin pollution also occurs, so that the water ecological environment is in crisis, attention of people and national attention are attracted, and how to utilize the active algae in the water as resources becomes a big problem.
Meanwhile, a series of ecological environmental problems are caused by the pollution problem of some metal ions in the water body, including the pollution of metal ions such as manganese (Mn), copper (Cu), iron (Fe) and the like, so that the economic development problem is brought, and the serious influence is brought to the life health of human beings and other organisms; and nitrogen oxides (NOx) brought by smoke emission of fire coal, coking and the like bring great harm to the atmospheric environment, related departments in China also put forward an ultra-low emission policy, the environmental protection requirement is increasingly improved, the denitration technology applied in the industry at present is mainly a selective catalytic reduction technology (SCR), wherein the most key catalyst material has higher cost, is very easy to become solid hazardous waste after being utilized, and can bring harm to the environment while removing the NOx. How to organically combine the three pollutants to realize the efficient utilization of the active algae and the metal ions and reduce the cost of the denitration catalyst and the influence on the environment is a major subject of the next research, and the research on the aspect of simultaneously realizing the resource utilization of the active algae and the metal ions and effectively removing nitrogen oxides (NOx) by utilizing the active algae and the metal ions is relatively less.
At present, articles for adsorbing heavy metal ions by active algae to be applied to sewage treatment are reported in many ways. However, most of the heavy metal ions used for adsorption are Cu 2+ 、Cd 2+ 、Pb 2+ 、Cr 3+ 、Ni + 、Zn 2+ 、Hg 2+ Etc. for Mn, however 2+ The adsorption of (D) has been reported. Active algae processing agentAfter the manganese wastewater is adsorbed and saturated, manganese is not easy to separate from algae, the post-treatment process is complex, dangerous waste is easily formed, and Mn is treated by active algae 2+ And then, the high-value utilization of the composite material has higher research value and application prospect.
Therefore, the method for converting the active algae and the metal ions into the low-cost and low-harm denitration catalyst is developed, the problem of water body pollution caused by the active algae and the metal ions can be solved, the cost of the denitration catalyst and the harm of the waste catalyst can be effectively reduced, and the method has great significance.
Disclosure of Invention
The invention aims to provide a charcoal @ metal type denitration catalyst based on active algae and a preparation method thereof, and aims to solve the technical problems.
Therefore, the invention provides a preparation method of charcoal @ metal type denitration catalyst based on active algae, which comprises the following steps:
s1, adding an ionic compound containing Mn into an active algae solution, and slowly adding the ionic compound while stirring until the ionic compound is completely dissolved;
s2, reacting the mixed solution prepared in the step S1 for 1-30 days in a normal living and growing environment of the active algae, and stirring once at intervals until the active algae are partially or completely coagulated and settled and the concentration of metal ions in the solution is not changed any more, namely the reaction is finished;
s3, carrying out solid-liquid separation on the mixed liquid of the active algae and the ionic compound after the reaction is finished, and collecting solid components;
and S4, carrying out grading drying treatment on the solid component obtained in the S3, and carbonizing the solid component in carbonizing equipment to obtain the denitration catalyst.
Preferably, S1 is added with one or more ionic compounds containing W, co, ni, fe, cu, ce or Cr, and the concentration of each metal ion in the solution is 0.1g/L-10.0g/L.
Preferably, the method of the staged drying treatment in S4 is as follows: drying at 105-115 ℃ for 1-6 h to remove free water, and then freeze-drying at-15 ℃ to-30 ℃ for 2-4 h to remove bound water, so that the water content is lower than 2%.
Preferably, the carbonization temperature in S4 is 350-500 ℃, and the carbonization time is 1-8h.
Preferably, the carbonization temperature in S4 is gradually increased, and the temperature rising rate is 2-5 ℃/min.
Preferably, the liquid component obtained by solid-liquid separation in S3 can be reused according to the concentration of the metal ions.
Preferably, the solid-liquid separation method in S3 is suction filtration by medium-speed or slow-speed filter paper, or centrifugation by a high-speed centrifuge with the rotating speed of more than 3000 r/min.
Preferably, the active algae is chlorella, diatom, oocyst algae with life activities or algae seeds, freeze-dried powder or algae powder capable of recovering life activities in a certain way.
Preferably, the chlorella, diatom or oocyst algae having vital activities can be carbonized in air or inert gas atmosphere after reacting with the ionic compound and drying, and the algae species, freeze-dried powder or algae powder capable of recovering vital activities by a certain way can be carbonized in air or hydrogen atmosphere after reacting with the ionic compound and drying.
In addition, the invention also provides a charcoal @ metal type denitration catalyst based on active algae, which is prepared by the preparation method of the charcoal @ metal type denitration catalyst based on active algae.
Compared with the prior art, the invention has the characteristics and beneficial effects that: according to the invention, a Mn-ion-containing compound is added into an active algae solution for dissolving, and then the solution is cultured for a period of time until the active algae is partially or completely coagulated and settled, meanwhile, the concentration of metal ions in the solution is not changed, the combination of the active algae and the metal ions is completed, and after solid-liquid separation, the denitration catalyst is obtained through grading drying treatment and carbonization. In the synthesis reaction process, metal ions such as manganese are combined with extracellular polymers of algae cells and functional groups on cell walls through coordination, complexation, ion exchange and the like, in addition, the combination of the metal ions combined on the cell surfaces and certain enzymes on the cell surfaces can also be transferred into cells, after drying and carbonization, the metals such as manganese are bonded with carbonized components of the algae cells, and the like, and finally active sites of denitration reaction are formed together, so that efficient denitration is realized. The catalyst prepared by the method can be applied to Selective Catalytic Reduction (SCR) reaction, and can reduce the preparation and application cost of the existing catalyst while maintaining the high removal rate of nitrogen oxides (NOx). Meanwhile, the active algae and metal ions which are extremely easy to generate harm in the water body can be effectively utilized, the values of the active algae and the metal ions are greatly improved, and the influence and the harm to the water body environment are reduced. The preparation method disclosed by the invention is easy to obtain raw materials, simple to operate, good in repeatability and wide in application range, and provides a reliable scheme for realizing the resource efficient utilization of active algae and metal ions and reducing the cost of the denitration catalyst.
Detailed Description
In order to make the technical means, innovative features, objectives and functions realized by the present invention easy to understand, the present invention is further described below.
The embodiments described herein are specific embodiments of the present invention, and are intended to be illustrative and exemplary of the concepts of the present invention and should not be construed as limiting the scope of the embodiments of the present invention. In addition to the embodiments described herein, those skilled in the art will be able to employ other technical solutions which are obvious based on the disclosure of the claims and the specification of the present application, and these technical solutions include technical solutions which make any obvious replacement or modification for the embodiments described herein.
In order to effectively remove NOx in a selective catalytic reduction reaction and fully combine active algae and metal ions, the invention provides a preparation method of a charcoal @ metal type denitration catalyst based on the active algae, which comprises the following steps:
s1, adding an ionic compound containing Mn into the active algae solution, and slowly adding the ionic compound while stirring until the ionic compound is completely dissolved. One or more ionic compounds containing W, co, ni, fe, cu, ce or Cr can be added, and the concentration of each metal ion in the solution is 0.1g/L-10.0g/L. The ionic compounds of different metals can provide active oxygen/acid sites for denitration reaction, promote redox circulation and the like. The active algae is chlorella, diatom, oocyst algae with life activities or algae seed, lyophilized powder or algae powder capable of recovering life activities in a certain way. The vital activities refer to the normal growth, reproduction, metabolism, etc. of algae.
And S2, reacting the mixed solution prepared in the step S1 for 1-30 days in a normal living and growing environment of the active algae, and stirring once at intervals until the active algae are partially or completely coagulated and settled and the concentration of metal ions in the solution is not changed any more, namely the reaction is finished. And concretely, stirring the mixture every day at an interval of 12 hours for 5-20 minutes, and stirring the mixture evenly.
And S3, carrying out solid-liquid separation on the mixed liquid of the active algae and the ionic compound after the reaction is finished, and collecting solid components. The liquid component obtained by solid-liquid separation can be reused according to the concentration condition of the metal ions. The solid-liquid separation method is to use medium-speed or slow-speed filter paper to carry out suction filtration or to use a high-speed centrifuge with the rotating speed of more than 3000r/min to carry out centrifugation.
And S4, carrying out grading drying treatment on the solid component obtained in the S3, and carbonizing the solid component in carbonizing equipment to obtain the denitration catalyst. The method for the grading drying treatment comprises the following steps: drying at 105-115 ℃ for 1-6 h to remove free water, and then freeze-drying at-15 ℃ to-30 ℃ for 2-4 h to remove bound water, so that the water content is lower than 2%. In S4, the carbonization temperature is 350-500 ℃, and the carbonization time is 1-8h. The carbonization temperature is gradually increased, and the heating rate is 2-5 ℃/min. Active algae such as chlorella, diatom and oocyst algae can be carbonized in air or inert gas atmosphere such as nitrogen and helium after reacting with ionic compounds and drying, and other algae species, freeze-dried powder or algae powder which can recover life activities by a certain mode can be carbonized in air or hydrogen after reacting with ionic compounds and drying.
When the denitration catalyst prepared by the method is applied to removing NOx, a reducing agent needs to participate, wherein the related reducing agent comprises NH 3 Components with strong reducing property such as liquid ammonia, ammonia water, urea, etc., CO, propylene, etc.
The present invention is further illustrated in detail by the following specific examples, it being understood that the specific examples described herein are for the purpose of illustration only and are not intended to limit the invention, and that various changes may be made within the scope of the invention as defined by the claims.
Example 1
(a) Manganese acetate is added into 2000 ten thousand/ml diatom solution and slowly added with stirring until the manganese acetate is completely dissolved, so that the concentration of manganese ions in the solution is 0.5g/L.
(b) And (c) stirring the mixed solution prepared in the step (a) under the normal living condition of the diatom every day for 12 hours, wherein the stirring time is 10 minutes, reacting for 3 days, partially settling the diatom, and detecting that the concentration of manganese ions is not changed any more, so that the reaction is finished.
(c) And centrifuging the mixed solution after the reaction is finished at the rotating speed of 4000r/min, and after solid-liquid separation, collecting solid components, wherein the concentration of manganese ions in the liquid components is 0.3g/L for repeated use.
(d) Drying the solid component obtained in the step (c) at 110 ℃ for 3h, then freeze-drying the solid component at-15 ℃ for 2h, finally heating the solid component in carbonization equipment according to the heating rate of 5 ℃/min, finally carbonizing the solid component at 450 ℃ for 3h in air atmosphere, and obtaining the catalyst for removing NOx after carbonization.
The sample of the NOx removing catalyst obtained in the embodiment has a space velocity of 32000h -1 、175℃、 [NO] = [NH 3 ] =500 ppm、[O 2 ] =5 vol.%、N 2 The denitration activity was tested under the condition of the equilibrium gas, and the conversion rate of nitrogen oxides (NOx) was 96%.
Example 2
(a) Adding manganese acetate into 1 hundred million/milliliter of chlorella solution, and slowly adding while stirring until the manganese acetate is completely dissolved to ensure that the concentration of manganese ions in the solution is 0.8g/L.
(b) Stirring the mixed solution prepared in the step (a) every day at an interval of 12 hours for 5 minutes, reacting for 1 day, completely settling chlorella, and detecting that the concentration of manganese ions is not changed any more, thus finishing the reaction.
(c) And (3) carrying out suction filtration on the mixed solution after the reaction is finished by using slow filter paper, carrying out solid-liquid separation, and collecting solid components, wherein the concentration of manganese ions in the suction filtration solution is 0.4g/L, so that the manganese ions can be repeatedly utilized.
(d) Drying the solid component obtained in (c) at 110 deg.C for 2h, freeze drying at-25 deg.C for 3h, heating in carbonization equipment at 2 deg.C/min, and heating at 350 deg.C with nitrogen (N) 2 ) Carbonizing for 2h under the atmosphere condition, and obtaining the catalyst for removing NOx after carbonization.
The sample of the NOx removal catalyst obtained in the example was at a space velocity of 32000h -1 、175℃、 [NO] = [NH 3 ] =500 ppm、[O 2 ] =5 vol.%、N 2 The denitration activity was tested under the condition of the equilibrium gas, and the conversion of nitrogen oxides (NOx) was obtained to be 98%.
Example 3
(a) Adding manganese acetate and ammonium metatungstate into the chlorella solution of 5000 ten thousand/ml, and slowly adding while stirring until the manganese acetate and the ammonium metatungstate are completely dissolved, so that the manganese ion concentration in the solution is 0.4g/L and the tungsten ion concentration is 0.2g/L.
(b) And (c) stirring the mixed solution prepared in the step (a) under the normal survival condition of the chlorella every day, wherein the stirring interval is 12 hours, the stirring time is 8 minutes, the reaction time is 15 days, the chlorella is completely settled, and meanwhile, the reaction is finished when the concentration of manganese ions and tungsten ions is detected to be not changed any more.
(c) And centrifuging the mixed solution after the reaction is finished at the rotating speed of 5000r/min, after solid-liquid separation, collecting solid components, wherein the concentration of manganese ions in the centrifuged supernatant is 0.08g/L and the concentration of tungsten ions is 0.05g/L, and the centrifuged supernatant does not meet the requirement of preparing the catalyst, so the mixed solution is not reused.
(d) And (c) conventionally drying the solid component obtained in the step (c) at 105 ℃ for 6h, then carrying out freeze drying at-20 ℃ for 2h, finally heating the solid component in carbonization equipment according to the heating rate of 3 ℃/min, finally carrying out carbonization for 3h at 400 ℃ under the air atmosphere condition, and obtaining the catalyst for removing NOx after carbonization.
The NOx removing catalyst obtained in this exampleThe space velocity of the sample is 32000h -1 、175℃、 [NO] = [NH 3 ] =500 ppm、[O 2 ] =5 vol.%、N 2 The denitration activity was tested under the condition of the equilibrium gas, and the conversion rate of nitrogen oxides (NOx) was obtained to be 92%.
Example 4
(a) Adding manganese acetate and chromium nitrate into the oocyst algae solution with the concentration of 4000 ten thousand per milliliter, and slowly adding the manganese acetate and the chromium nitrate while stirring until the manganese acetate and the chromium nitrate are completely dissolved, so that the concentration of manganese ions in the solution is 1.0g/L and the concentration of chromium ions is 0.2g/L.
(b) Stirring the mixed solution prepared in the step (a) under the normal survival condition of the chlorella every day, wherein the stirring interval is 12 hours, the stirring time is 15 minutes, the reaction time is 10 days, the chlorella partially settles, and meanwhile, the ion concentration is detected to be not changed any more, and the reaction is finished.
(c) And centrifuging the mixed solution after the reaction is finished at the rotating speed of 6000r/min, and after solid-liquid separation, collecting solid components, wherein the concentration of manganese ions in the centrifuged supernatant is 0.6g/L, but the concentration of chromium ions is 0.09g/L, so that the mixed solution does not meet the requirement of preparing the catalyst, and the mixed solution is not reused.
(d) And (c) conventionally drying the solid component obtained in the step (c) at 115 ℃ for 4h, then freeze-drying the solid component at-25 ℃ for 2.5h, finally heating the solid component in carbonization equipment at a heating rate of 4 ℃/min, finally carbonizing the solid component for 3h at 450 ℃ under the condition of helium (He) atmosphere, and obtaining the catalyst for removing NOx after carbonization.
The sample of the NOx removal catalyst obtained in the example was at a space velocity of 32000h -1 、175℃、 [NO] = [NH 3 ] =500 ppm、[O 2 ] =5 vol.%、N 2 The denitration activity was tested under the condition of the equilibrium gas, and the conversion rate of nitrogen oxides (NOx) was obtained to be 94%.
Comparative example 1
In the comparative example, the active algae is replaced by the algae powder with the same amount, and the algae powder is carbonized to obtain the carbon carrier; soaking the carbon carrier in 0.5g/L manganese acetate solution, performing solid-liquid separation, and drying; and then calcining the dried material to obtain the denitration catalyst.
The catalyst obtained in the present comparative exampleThe space velocity of the sample of the NOx removal catalyst is 32000h -1 、175℃、 [NO] = [NH 3 ] =500 ppm、[O 2 ] =5 vol.%、N 2 The denitration activity was tested under the condition of the equilibrium gas, and the conversion rate of nitrogen oxides (NOx) was obtained to be 43%.
The method comprises the steps of carbonizing the active algae to obtain the carbon carrier, and then combining the carbon carrier with the manganese ions, wherein only the physical characteristics of the carbon carrier, such as specific surface area, pore channels and the like, are utilized, and the living activities of the active algae are not participated, so that the manganese ions are not fully complexed with functional groups on the surface of the active algae, and finally, the combination amount of manganese is relatively less, so that the active sites in the denitration reaction process are fewer, the denitration effect is relatively poor, and the conversion rate of nitrogen oxides (NOx) is relatively low.
The above embodiments are merely illustrative and not intended to limit the scope of the claims, and other alternatives that may be suggested to one skilled in the art in light of the disclosure of this disclosure are to be included within the scope of the appended claims.
Claims (10)
1. A preparation method of charcoal @ metal type denitration catalyst based on active algae is characterized in that the active algae are algae with life activities or algae species capable of recovering the life activities in a certain mode, and the preparation method comprises the following steps:
s1, adding an ionic compound containing Mn into an active algae solution, and slowly adding the ionic compound while stirring until the ionic compound is completely dissolved;
s2, reacting the mixed solution prepared in the step S1 for 1-30 days in a normal living and growing environment of the active algae, and stirring once at intervals until the active algae are partially or completely coagulated and settled and the concentration of metal ions in the solution is not changed any more, namely the reaction is finished;
s3, carrying out solid-liquid separation on the mixed liquid of the active algae and the ionic compound after the reaction is finished, and collecting solid components;
and S4, carrying out grading drying treatment on the solid component obtained in the S3, and carbonizing treatment in carbonizing equipment to obtain the denitration catalyst.
2. The preparation method of the activated algae-based biochar @ metal type denitration catalyst as claimed in claim 1, wherein: s1 is also added with one or more ionic compounds containing W, co, ni, fe, cu, ce or Cr, and the concentration of each metal ion in the solution is 0.1g/L-10.0g/L.
3. The preparation method of activated algae-based biochar @ metal type denitration catalyst as claimed in claim 1, wherein the step S4 is implemented by a staged drying treatment method comprising the following steps: drying at 105-115 ℃ for 1-6 h to remove free water, and then freeze-drying at-15 ℃ to-30 ℃ for 2-4 h to remove bound water, so that the water content is lower than 2%.
4. The preparation method of the activated algae-based biochar @ metal type denitration catalyst as claimed in claim 1, wherein: in S4, the carbonization temperature is 350-500 ℃, and the carbonization time is 1-8h.
5. The preparation method of the charcoal @ metal type denitration catalyst based on activated algae as claimed in claim 4, characterized in that: in the S4, the carbonization temperature is gradually increased, and the heating rate is 2-5 ℃/min.
6. The preparation method of the activated algae-based biochar @ metal type denitration catalyst as claimed in claim 1, wherein: the liquid component obtained by solid-liquid separation in S3 can be reused according to the concentration condition of metal ions.
7. The preparation method of the activated algae-based biochar @ metal type denitration catalyst as claimed in claim 1, wherein: and the solid-liquid separation method in the S3 is to use medium-speed or slow-speed filter paper for suction filtration or use a high-speed centrifuge with the rotating speed of more than 3000r/min for centrifugation.
8. The preparation method of the activated algae-based biochar @ metal type denitration catalyst as claimed in claim 1, wherein: the algae with life activities is Chlorella, diatom or oocyst algae.
9. The preparation method of activated algae-based biochar @ metal type denitration catalyst as claimed in claim 8, wherein: chlorella, diatom or oocyst algae with vital activities are reacted with ionic compounds, dried and carbonized in air or inert gas atmosphere, and algae species capable of recovering vital activities are reacted with ionic compounds, dried and carbonized in air or hydrogen atmosphere.
10. A charcoal @ metal type denitration catalyst based on active algae is characterized in that: the activated algae-based biochar @ metal type denitration catalyst is prepared by the preparation method of the activated algae-based biochar @ metal type denitration catalyst as claimed in any one of claims 1 to 9.
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