CN108057440B - Method for preparing heterogeneous photo-Fenton catalyst from municipal sludge and red brick waste, product and application - Google Patents
Method for preparing heterogeneous photo-Fenton catalyst from municipal sludge and red brick waste, product and application Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 63
- 239000011449 brick Substances 0.000 title claims abstract description 55
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- 239000010802 sludge Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 34
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- 238000001354 calcination Methods 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
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- 238000006243 chemical reaction Methods 0.000 claims description 5
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 8
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- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 229960003742 phenol Drugs 0.000 description 5
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 5
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- 229910001385 heavy metal Inorganic materials 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
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- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/635—0.5-1.0 ml/g
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- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C02F2101/34—Organic compounds containing oxygen
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Abstract
The method for preparing the heterogeneous light Fenton catalyst from the municipal sludge and the red brick waste provided by the invention has the advantages that the municipal sludge and the red brick waste are used as raw materials, gas released by organic matters in the sludge during high-temperature pyrolysis is used as a catalyst pore-forming agent, minerals formed when inorganic ash in the sludge and the red brick are melted at high temperature are used as a catalyst carrier, and iron in the red brick waste is used as a catalyst active component, so that the method has the advantages of easiness in obtaining the raw materials, low cost, good benefit, high specific surface area of the prepared catalyst, good response capability to visible light, stable product quality and the like. Secondly, the preparation method has the characteristics of simple process, low production cost, easy large-scale production, waste recycling and the like.
Description
Technical Field
The invention relates to the technical field of waste resource utilization and environmental catalysis materials, in particular to a method for preparing a heterogeneous photo-Fenton catalyst from municipal sludge and red brick waste, the heterogeneous photo-Fenton catalyst and application of the heterogeneous photo-Fenton catalyst in a series of reactions initiated by photo-induction in the presence of hydrogen peroxide.
Background
In recent years, with the increase of municipal sewage and industrial sewage treatment capacity in China, the production amount of sludge is gradually increased. The sludge has high water content and contains a large amount of toxic and harmful pathogenic microorganisms and heavy metals, and serious environmental pollution is caused if the sludge is not properly treated.
The red brick is commonly called clay brick, and is a building brick which is formed by mixing and kneading yellow clay, shale, coal gangue and the like which are rich in iron elements, then pressing and molding the materials manually or mechanically, drying the materials and firing the dried materials by oxidizing flame at the temperature of about 900 ℃. Red brick was a building material widely used in 90 s of 20 th century in China. With the improvement of old cities and the acceleration of novel urbanization process in China, a large amount of red brick waste generated after old buildings are dismantled becomes construction waste.
The heterogeneous light Fenton technology refers to a photocatalytic reaction technology for generating a high-activity hydroxyl radical in a solution containing hydrogen peroxide and a solid-phase catalyst under the irradiation of ultraviolet light or visible light. The technology can rapidly degrade refractory organic pollutants in water, and has the characteristics of high reaction speed, simplicity in operation, no toxicity, greenness and the like. The iron oxide photo-Fenton catalyst widely used at present has the problems of low specific surface area, weak adsorption capacity to pollutants in water, poor visible light responsiveness, high price of raw materials and the like.
Disclosure of Invention
The present invention has been made to solve the above problems, and an object of the present invention is to provide a method for preparing a heterogeneous photo-Fenton catalyst from municipal sludge mixed with red brick waste, a heterogeneous photo-Fenton catalyst, and use of the heterogeneous photo-Fenton catalyst in a series of reactions induced by light in the presence of hydrogen peroxide.
The invention provides a method for preparing a heterogeneous photo-Fenton catalyst from municipal sludge and red brick waste, which is characterized by comprising the following steps of:
step 1, placing the dewatered sludge and the red brick waste at 95-105 ℃ for drying for 12-24 hours to obtain dry sludge and dry red brick waste;
step 2, crushing the dry red brick waste obtained in the step 1 by using a mechanical crusher at a preset crushing speed, and screening by using a 60-mesh sieve to obtain dry red brick waste particles;
step 3, mixing the dry sludge obtained in the step 1 and the dry red brick waste particles obtained in the step 2 according to a preset weight ratio, then grinding the mixture by using a ball mill at a preset grinding rotating speed, and screening the mixture by using a 300-mesh sieve to obtain mixed particles;
step 4, placing the mixed particles obtained in the step 3 in a muffle furnace, calcining at 800-1050 ℃, wherein the calcining time is 30-120 min, the heating rate is 10-20 ℃/min, and naturally cooling to room temperature after calcining to obtain calcined particles;
step 5, washing the calcined particles obtained in the step 4 with a hydrochloric acid aqueous solution with the concentration of 1.5-3 moL/L for 1-2 h, then repeatedly washing with deionized water until the pH value of a deionized water washing liquid is stabilized at 6.5-7.0, and then filtering to remove the deionized water to obtain washed particles;
and 6, drying the washed particles obtained in the step 5 at 60 ℃ in vacuum for 12-24 hours to obtain the heterogeneous photo-Fenton catalyst.
The method for preparing the heterogeneous photo-Fenton catalyst by mixing the municipal sludge with the red brick waste can also have the following characteristics: the dewatered sludge in the step 1 is any one of primary sedimentation tank sludge, secondary sedimentation tank sludge or mixed sludge.
The method for preparing the heterogeneous photo-Fenton catalyst by using the municipal sludge and the red brick waste provided by the invention can also have the following characteristics: the predetermined crushing speed in the step 2 is 1000-2500 rpm/min.
The method for preparing the heterogeneous photo-Fenton catalyst by using the municipal sludge and the red brick waste provided by the invention can also have the following characteristics: the predetermined weight ratio in the step 3 is 3: 2-4: 1.
The method for preparing the heterogeneous photo-Fenton catalyst by using the municipal sludge and the red brick waste provided by the invention can also have the following characteristics: the preset grinding rotating speed in the step 3 is 15-21 rpm/min.
The invention also provides a product prepared by the methodA heterogeneous photo-Fenton catalyst product, characterized in that: the heterogeneous light Fenton catalyst has a mesoporous structure and a specific surface area of 130-270 m2/g。
The invention also provides an application of the heterogeneous light Fenton catalyst product in a series of reactions initiated by light induction in the presence of hydrogen peroxide.
The heterogeneous light Fenton catalyst product provided by the invention can be applied to a series of reactions initiated by light induction in the presence of hydrogen peroxide and a solid-phase catalyst, and also has the following characteristics: the light induction is any one of visible light, ultraviolet light or sunlight.
Action and Effect of the invention
The method for preparing the heterogeneous light Fenton catalyst by mixing the municipal sludge and the red brick waste, provided by the invention, has the advantages that the municipal sludge and the red brick waste are used as raw materials, gas released by organic matters in the sludge during high-temperature pyrolysis is used as a catalyst pore-forming agent, mineral formed by sludge and inorganic ash in the red brick during high-temperature melting is used as a catalyst carrier, and iron in the red brick waste is used as a catalyst active component, so that the method has the advantages of easiness in obtaining the raw materials, low cost, good benefit, high specific surface area of the prepared catalyst, good response capability to visible light, stable product quality and the like. Secondly, the preparation method has the characteristics of simple process, low production cost, easy large-scale production, waste recycling and the like.
Drawings
FIG. 1 is a nitrogen adsorption-desorption graph of the heterogeneous photo-Fenton catalyst obtained in example 1;
FIG. 2 is a graph of the UV-visible diffuse reflectance spectrum of the heterogeneous photo-Fenton catalyst obtained in example 1; and
FIG. 3 shows the photo-Fenton catalytic degradation efficiency of the heterogeneous photo-Fenton catalyst obtained in example 1 on rhodamine B, methylene blue, phenol and nitrobenzene.
Detailed Description
The method for preparing the heterogeneous photo-Fenton catalyst by using the municipal sludge and the red brick waste according to the invention is further described below with reference to the accompanying drawings.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; the raw materials, containers, apparatuses and the like used are commercially available unless otherwise specified.
< example one >
The embodiment is a method for preparing a heterogeneous photo-Fenton catalyst from municipal sludge and red brick waste, and the method comprises the following steps:
step 1, placing the dewatered sludge and the red brick waste at 105 ℃ for drying for 24 hours to obtain dry sludge and dry red brick waste;
step 2, crushing the dry red brick waste obtained in the step 1 by using a mechanical crusher at the rotation speed of 2500rpm/min, and screening by using a 60-mesh sieve to obtain dry red brick waste particles;
step 3, mixing 3Kg of the dry sludge obtained in the step 1 with 2Kg of the dry red brick waste particles obtained in the step 2, then grinding the mixture by using a ball mill at the rotating speed of 15rpm/min, and screening the ground mixture by using a 300-mesh sieve to obtain mixed particles;
step 4, placing the mixed particles obtained in the step 3 in a muffle furnace, calcining at 950 ℃, wherein the calcining time is 60min, the heating rate is 10 ℃/min, and naturally cooling to room temperature after calcining to obtain calcined particles;
step 5, washing the calcined particles obtained in the step 4 for 1 hour by using a hydrochloric acid aqueous solution with the concentration of 1.5moL/L, then repeatedly washing by using deionized water until the pH of a deionized water washing liquid is stabilized at 6.8, and then filtering to remove the deionized water to obtain washed particles;
and 6, drying the washed particles obtained in the step 5 at 60 ℃ in vacuum for 24 hours to obtain the heterogeneous photo-Fenton catalyst.
< example two >
The embodiment is a method for preparing a heterogeneous photo-Fenton catalyst from municipal sludge and red brick waste, and the method comprises the following steps:
step 1, placing the dewatered sludge and the red brick waste at 100 ℃ for drying for 18h to obtain dry sludge and dry red brick waste;
step 2, crushing the dry red brick waste obtained in the step 1 by using a mechanical crusher at the rotation degree of 1500rpm/min, and screening by using a 60-mesh sieve to obtain dry red brick waste particles;
step 3, mixing 4Kg of the dry sludge obtained in the step 1 with 2Kg of the dry red brick waste particles obtained in the step 2, then grinding the mixture by using a ball mill at the rotating speed of 18rpm/min, and screening the ground mixture by using a 300-mesh sieve to obtain mixed particles;
step 4, placing the mixed particles obtained in the step 3 in a muffle furnace, calcining at 800 ℃, wherein the calcining time is 30min, the heating rate is 15 ℃/min, and naturally cooling to room temperature after calcining to obtain calcined particles;
step 5, washing the calcined particles obtained in the step 4 for 1.5h by using a hydrochloric acid aqueous solution with the concentration of 2moL/L, then repeatedly washing by using deionized water until the pH of a deionized water washing liquid is stabilized at 6.5, and then filtering to remove the deionized water to obtain washed particles;
and 6, drying the washed particles obtained in the step 5 at 60 ℃ for 18h in vacuum to obtain the heterogeneous photo-Fenton catalyst.
< example three >
The embodiment is a method for preparing a heterogeneous photo-Fenton catalyst from municipal sludge and red brick waste, and the method comprises the following steps:
step 1, placing the dewatered sludge and the red brick waste at 95 ℃ for drying for 12 hours to obtain dry sludge and dry red brick waste;
step 2, crushing the dry red brick waste obtained in the step 1 by using a mechanical crusher at the rotation degree of 1000rpm/min, and screening by using a 60-mesh sieve to obtain dry red brick waste particles;
step 3, mixing 4Kg of the dry sludge obtained in the step 1 with 1Kg of the dry red brick waste particles obtained in the step 2, then grinding the mixture by using a ball mill at the rotating speed of 21rpm/min, and screening the ground mixture by using a 300-mesh sieve to obtain mixed particles;
step 4, placing the mixed particles obtained in the step 3 in a muffle furnace, calcining at 1050 ℃, wherein the calcining time is 120min, the heating rate is 20 ℃/min, and naturally cooling to room temperature after calcining to obtain calcined particles;
step 5, washing the calcined particles obtained in the step 4 for 2 hours by using a hydrochloric acid aqueous solution with the concentration of 3moL/L, then repeatedly washing by using deionized water until the pH value of a deionized water washing liquid is stabilized at 7, and then filtering to remove the deionized water to obtain washed particles;
and 6, drying the washed particles obtained in the step 5 at 60 ℃ in vacuum for 12 hours to obtain the heterogeneous photo-Fenton catalyst.
Examples analysis
Nitrogen adsorption-desorption test analysis:
FIG. 1 is a graph showing nitrogen adsorption-desorption of the heterogeneous photo-Fenton catalyst obtained in example 1.
As shown in FIG. 1, the heterogeneous photo-Fenton catalyst obtained in example 1 was used at a relative pressure (p/p)0) Capillary condensation phenomenon occurs above 0.43, adsorption and desorption branches do not coincide to generate a loop, and the typical mesoporous material is in a sphere-like shape.
The specific surface area, total pore volume and average pore diameter data of the heterogeneous photo-Fenton catalysts obtained in examples 1 to 3 calculated by the BJH model are shown in Table 1.
TABLE 1
| Example 1 | Example 2 | Example 3 | |
| Specific surface area (m)2/g) | 270 | 204 | 130 |
| Total pore volume (cm)3/g) | 0.850 | 0.634 | 0.607 |
| Average pore diameter (nm) | 15.00 | 18.03 | 17.56 |
Ultraviolet-visible spectrophotometer test analysis:
FIG. 2 is a UV-visible diffuse reflectance spectrum of the heterogeneous photo-Fenton catalyst obtained in example 1.
The heterogeneous photo-Fenton catalyst obtained in example 1 is detected by an ultraviolet-visible spectrophotometer to obtain an ultraviolet-visible light diffuse reflection spectrogram as shown in FIG. 2, and the forbidden bandwidth of the heterogeneous photo-Fenton catalyst is calculated by a Tauplot method to be 2.6eV, and the maximum wavelength of response is 477 nm.
The heterogeneous photo-Fenton catalyst obtained in example 2 had a forbidden band width of 2.7eV and a maximum wavelength at which a response occurred of 459 nm.
The heterogeneous photo-Fenton catalyst obtained in example 3 had a forbidden band width of 2.7eV and a maximum wavelength at which a response occurred was 459 nm.
And (3) analyzing photocatalytic degradation efficiency:
FIG. 3 shows the photo-Fenton catalytic degradation efficiency of the heterogeneous photo-Fenton catalyst obtained in example 1 on rhodamine B, methylene blue, phenol and nitrobenzene.
As shown in FIG. 3, the degradation efficiency of the heterogeneous photo-Fenton catalyst on rhodamine B, methylene blue, phenol and nitrobenzene in water for 480min can reach 81.4%, 90.8%, 74.0% and 78.5% respectively.
The degradation efficiency of the heterogeneous light Fenton catalyst obtained in the example 2 to rhodamine B, methylene blue, phenol and nitrobenzene in water for 480min can reach 80.9%, 89.2%, 73.2% and 74.1% respectively.
The degradation efficiency of the heterogeneous light Fenton catalyst obtained in the embodiment 3 to rhodamine B, methylene blue, phenol and nitrobenzene in water for 480min can reach 80.0%, 85.4%, 78.1% and 79.1% respectively.
Advantageous effects and effects of the embodiments
The method for preparing the heterogeneous light Fenton catalyst from the municipal sludge and the red brick waste provided by the invention has the advantages that the municipal sludge and the red brick waste are used as raw materials, gas released by organic matters in the sludge during high-temperature pyrolysis is used as a catalyst pore-forming agent, minerals formed when inorganic ash in the sludge and the red brick are melted at high temperature are used as a catalyst carrier, and iron in the red brick waste is used as a catalyst active component, so that the method has the advantages of easiness in obtaining the raw materials, low cost, good benefit, high specific surface area of the prepared catalyst, good response capability to visible light, stable product quality and the like. Secondly, the preparation method has the characteristics of simple process, low production cost, easy large-scale production, waste recycling and the like.
The above description is only a basic description of the present invention, and any equivalent changes made according to the technical solution of the present invention belong to the protection scope of the present invention.
Claims (8)
1. A method for preparing a heterogeneous photo-Fenton catalyst from municipal sludge and red brick waste is characterized by comprising the following steps:
step 1, placing the dewatered sludge and the red brick waste at 95-105 ℃ for drying for 12-24 hours to obtain dry sludge and dry red brick waste;
step 2, crushing the dry red brick waste obtained in the step 1 by using a mechanical crusher at a preset crushing speed, and screening by using a 60-mesh sieve to obtain dry red brick waste particles;
step 3, mixing the dry sludge obtained in the step 1 and the dry red brick waste particles obtained in the step 2 according to a preset weight ratio, then grinding the mixture by using a ball mill at a preset grinding rotating speed, and screening the ground mixture by using a 300-mesh sieve to obtain mixed particles;
step 4, placing the mixed particles obtained in the step 3 in a muffle furnace, calcining at 800-1050 ℃, wherein the calcining time is 30-120 min, the heating rate is 10-20 ℃/min, and naturally cooling to room temperature after calcining to obtain calcined particles;
step 5, washing the calcined particles obtained in the step 4 with 1.5-3 mol/L hydrochloric acid aqueous solution for 1-2 h, then repeatedly washing with deionized water until the pH value of a deionized water washing liquid is stabilized at 6.5-7.0, and then filtering to remove the deionized water to obtain washed particles;
and 6, drying the washed particles obtained in the step 5 at 60 ℃ in vacuum for 12-24 hours to obtain the heterogeneous photo-Fenton catalyst.
2. The method of claim 1, wherein:
wherein the dewatered sludge in the step 1 is any one of primary sedimentation tank sludge, secondary sedimentation tank sludge or mixed sludge.
3. The method of claim 1, wherein:
wherein the predetermined pulverizing speed in the step 2 is 1000-2500 rpm/min.
4. The method of claim 1, wherein:
wherein the predetermined weight ratio in the step 3 is 3: 2-4: 1.
5. The method of claim 1, wherein:
wherein the predetermined grinding speed in the step 3 is 15-21 rpm/min.
6. The heterogeneous photo-Fenton catalyst prepared by the method of any one of claims 1 to 5, wherein:
the heterogeneous light Fenton catalyst has a mesoporous structure, and the specific surface area is 130-270 m2/g。
7. Use of the heterogeneous photo-Fenton catalyst prepared by the method according to any one of claims 1 to 5 in a series of reactions initiated by photo-induction in the presence of hydrogen peroxide.
8. Use according to claim 7, characterized in that:
wherein the light induction is any one of visible light, ultraviolet light or sunlight.
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