CN111298804A - Ozone catalytic oxidation catalyst for treating wastewater and preparation method thereof - Google Patents

Ozone catalytic oxidation catalyst for treating wastewater and preparation method thereof Download PDF

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Publication number
CN111298804A
CN111298804A CN201811519491.5A CN201811519491A CN111298804A CN 111298804 A CN111298804 A CN 111298804A CN 201811519491 A CN201811519491 A CN 201811519491A CN 111298804 A CN111298804 A CN 111298804A
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activated carbon
catalyst
impregnation
impregnation process
product
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CN201811519491.5A
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Inventor
杨琼锋
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Jinfeng Environmental Protection Co ltd
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Jinfeng Environmental Protection Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/889—Manganese, technetium or rhenium
    • B01J23/8892—Manganese
    • C—CHEMISTRY; METALLURGY
    • 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
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
    • C—CHEMISTRY; METALLURGY
    • 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
    • C02F1/72—Treatment of water, waste water, or sewage by oxidation
    • C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds

Abstract

The invention provides an ozone catalytic oxidation catalyst for treating wastewater and a preparation method thereof, wherein the preparation method comprises the following steps: providing an activated carbon carrier; performing a first impregnation process on the activated carbon carrier, and then filtering to obtain an intermediate product, wherein a first impregnation liquid adopted in the first impregnation process comprises a surfactant; performing a second impregnation process on the intermediate product, and then filtering to obtain a filtrate as a pre-product, wherein a second impregnation liquid adopted in the second impregnation process comprises an active component precursor of the catalyst; and drying and roasting the pre-product to obtain the catalyst. By the method, the hydrophobicity of the surface of the activated carbon can be modulated, and the removal capacity of organic matters is improved.

Description

Ozone catalytic oxidation catalyst for treating wastewater and preparation method thereof
Technical Field
The invention belongs to the field of wastewater treatment, and particularly relates to an ozone catalytic oxidation catalyst for treating wastewater and a method for preparing the catalyst.
Background
With the development of industry, the demand for treating industrial wastewater difficult to degrade is increasingly urgent. The nondegradable substances in the industrial wastewater directly determine the standard discharge and stable operation of a sewage treatment plant. The traditional biochemical treatment method cannot remove toxic, harmful and other refractory substances in industrial wastewater, so that an advanced oxidation water treatment technology must be introduced.
In advanced oxidation water treatment technology, the ozone catalytic oxidation method belongs to an important branch. The catalytic ozonation method is a method for oxidizing macromolecular and difficultly biodegradable organic matters into low-toxicity or non-toxic small molecular substances. In the heterogeneous ozone catalytic oxidation reaction process, organic matters in the wastewater are firstly adsorbed on the surface of the catalyst and then are further degraded.
For the catalytic ozonation technology, the key technology is the preparation of the catalyst. However, in the case of the catalyst for catalytic oxidation of ozone in the prior art, the preparation process determines that the catalyst has higher production cost, lower catalytic efficiency and shorter service life, thereby increasing the cost of sewage treatment.
Disclosure of Invention
One aspect of the present invention is to provide a catalyst for improving adsorption of refractory macromolecular organic substances in industrial wastewater and a preparation method thereof.
Another aspect of the present invention is to provide a catalyst having reduced sewage treatment costs and a method for preparing the same.
An exemplary embodiment of the present invention provides a method of preparing a catalyst for treating wastewater, the method including the steps of: providing an activated carbon carrier; performing a first impregnation process on the activated carbon carrier, and then filtering to obtain an intermediate product, wherein a first impregnation liquid adopted in the first impregnation process comprises a surfactant; performing a second impregnation process on the intermediate product, and then filtering to obtain a filtrate as a pre-product, wherein a second impregnation liquid adopted in the second impregnation process comprises an active component precursor of the catalyst; and drying and roasting the pre-product to obtain the catalyst.
According to an exemplary embodiment, the active component of the catalyst may include at least one of Fe, Cu, Ni, Mn.
According to an exemplary embodiment, the active component of the catalyst may include Mn and Cu, and a mass ratio of the Mn element and the Cu element in the second impregnation liquid may be 1:1 to 10: 1.
According to an exemplary embodiment, the contents of the Mn element and the Cu element included in the second impregnation liquid may be configured in a ratio in which 1kg of the activated carbon may support 1g to 100g of the Mn element and 1g to 10g of the Cu element.
According to an exemplary embodiment, the surfactant may include ethylene glycol.
According to an exemplary embodiment, the number of moles of the surfactant may be 0.1 to 10 times the sum of the number of moles of the active components.
According to an exemplary embodiment, in the firing step, the firing temperature may be 300 to 700 ℃ and the firing time may be 2 to 5 hours.
According to an exemplary embodiment, the drying temperature in the drying step is 100 ℃ to 150 ℃ and the drying time is 2h to 10 h.
According to an exemplary embodiment, the impregnation times of the first and second impregnation processes may be not less than 1h, respectively.
Exemplary embodiments of the present invention also provide the ozone catalytic oxidation catalyst prepared by the above method.
The present inventive concept has been described briefly above. Compared with the ozone catalytic oxidation catalyst prepared by the prior art, the preparation method has the following beneficial effects that:
(1) the surface active agent is used for modifying the active carbon, so that the hydrophobicity of the surface of the active carbon can be adjusted, and the removal capacity of the catalyst on organic matters is improved;
(2) the activated carbon carriers with different hydrophobicity can be obtained by modulating the type and the dosage of the surfactant, so that a series of catalysts with proper adsorbability to different water qualities can be further obtained, and the adsorption to the organic matters with weak polarity or nonpolar macromolecules in the industrial wastewater difficult to degrade is enhanced.
Detailed Description
Hereinafter, the inventive concept will be described in detail with reference to specific embodiments, however, the following specific embodiments are only intended to fully convey the inventive concept to those skilled in the art, and do not limit the scope of the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
The organic matters in the wastewater can be roughly divided into two categories of polarity and non-polarity, most of the macromolecular organic matters are non-polarity and hydrophobic organic matters, and the difficultly-degradable organic matters in the industrial wastewater are mainly the macromolecular organic matters.
In the prior art, the key of the catalytic ozonation technology for treating organic matters in industrial wastewater is to decompose ozone into OH through the catalytic action of a catalyst. Because OH has a high potential (E)02.8V), strong reaction capability, fast speed, and can initiate chain reaction, thereby leading to complete degradation of a plurality of organic matters, therefore, OH is 10 of the ozone oxidation reaction speed7-109And (4) doubling.
As a catalyst, the difference of the surface chemical properties of the activated carbon can influence the migration and diffusion speed of organic matters in the pores of the activated carbon and make the activated carbon have certain selectivity on the adsorption of the organic matters. The surface functional groups affect the adsorption capacity of the activated carbon.
Therefore, the present invention is intended to modify an activated carbon support as a catalyst from the following points: the hydrophobicity of the surface of the activated carbon is modulated to enhance the adsorption of macromolecular organic matters. However, it is not the case that the higher the hydrophobicity of the activated carbon surface, the better, because too strong hydrophobicity affects the affinity of the activated carbon for water and thus the adsorption of organic substances in water by the activated carbon. Therefore, modulation of the hydrophobicity of activated carbon is of great importance.
As described above, the surface functional group may affect adsorption of the activated carbon to the macromolecular organic substance with weak polarity, and therefore, the present invention contemplates modifying the surface of the activated carbon with a surfactant such as ethylene glycol, so as to modulate the hydrophobicity of the surface of the activated carbon and improve the removal capability of the hydrophobic organic substance. In addition, the invention also obtains the activated carbon carriers with different hydrophobicity by modulating the type and the dosage of the surfactant, thereby further obtaining a series of catalysts with proper adsorbability to different water qualities.
Hereinafter, detailed steps of a method for preparing an ozone catalytic oxidation catalyst for treating wastewater according to an exemplary embodiment of the present invention will be described in detail.
A method of preparing an ozone catalytic oxidation catalyst for treating wastewater according to an exemplary embodiment of the present invention includes the steps of: providing an activated carbon carrier; performing a first impregnation process on the activated carbon carrier, and then filtering to obtain an intermediate product; performing a second impregnation process on the intermediate product, and then filtering to obtain a filtrate as a pre-product; and drying and roasting the pre-product to obtain the catalyst.
The catalyst according to an exemplary embodiment of the present invention includes activated carbon as a carrier, and thus, it is required to have a small particle size to have a large specific surface area in order to provide adsorption of organic substances to a large extent and promote ozonolysis, thereby enabling efficient treatment of wastewater. According to an exemplary embodiment, the activated carbon as the support may be a columnar particle having 3mm to 4 mm. However, the inventive concept is not limited to the shape and specific size of the activated carbon, and one skilled in the art can adaptively select physical characteristics of the activated carbon according to the inventive concept.
After the activated carbon carrier is selected, the activated carbon carrier is immersed into a first immersion liquid to perform a first immersion process on the activated carbon carrier. The first impregnation liquid employed in the first impregnation process includes a surfactant, which may include a surfactant used in the prior art for treating sewage, and may include, but is not limited to, ethylene glycol. However, the inventive concept is not limited thereto. That is, one skilled in the art can select at least one of any surfactants in the prior art as the surfactant contemplated by the present invention. The surface of the activated carbon is treated by the surfactant, so that the hydrophobicity of the surface of the activated carbon can be modulated by the surfactant. However, too strong hydrophobicity may affect the affinity of activated carbon for water. Therefore, the amount of the surfactant to be used needs to be controlled. According to exemplary embodiments of the inventive concept, the number of moles of the surfactant is 0.1 to 10 times the sum of the number of moles of the active components to be described below.
After the activated carbon support is impregnated into the first impregnation liquid, the activated carbon support may be maintained in the first impregnation liquid for a predetermined time to facilitate the attachment of the surfactant to the activated carbon support. According to exemplary embodiments of the inventive concept, the impregnation time of the activated carbon support into the first impregnation liquid may be not less than one hour (e.g., 3h to 24h), but exemplary embodiments of the inventive concept are not limited thereto. Thereafter, the impregnation liquor comprising the activated carbon support may be filtered to obtain an intermediate product.
Then, the intermediate product may be immersed into a second immersion liquid to perform a second immersion process. Here, the second impregnation liquid used in the second impregnation process includes an active component precursor of the catalyst. The active component may be an active component known in the art for treating wastewater. For example, the active component according to an exemplary embodiment of the inventive concept may include at least one of Fe, Cu, Ni, Mn. When the active component includes Mn and Cu, the precursor of Mn in the second impregnation liquid may be a soluble manganese salt and the precursor of Cu may be a soluble copper salt, and the mass ratio of the Mn element and the Cu element in the second impregnation liquid may be 1:1 to 10: 1. Further, when Mn and Cu are included as the active components in the second impregnation liquid, the Mn element and the Cu element included in the second impregnation liquid may be formulated in a ratio of 1g to 100g of the Mn element and 1g to 10g of the Cu element supported by 1kg of the activated carbon with respect to the activated carbon support, so that the active components may be sufficiently attached to the activated carbon support.
After the activated carbon support is impregnated into the second impregnation liquid, the activated carbon support may be maintained in the second impregnation liquid for a predetermined time to facilitate the attachment of the active component to the activated carbon support. According to exemplary embodiments of the inventive concept, the duration of impregnation of the activated carbon support into the second impregnation liquid may be not less than one hour (e.g., 3h to 24h), but exemplary embodiments of the inventive concept are not limited thereto. Thereafter, the second impregnation liquor comprising the activated carbon support may be filtered to obtain filtrate as a pre-product.
Thereafter, the pre-product may be dried and calcined to obtain the catalyst. Here, the respective components attached to the activated carbon support may be firmly fixed on the activated carbon support through a roasting process. According to a specific example, the pre-product may be roasted at a temperature of 300 to 700 ℃ for 2 to 5 hours, however, exemplary embodiments of the inventive concept are not limited thereto. Furthermore, the intermediate product may be dried at a temperature lower than the calcination temperature before the calcination step, in order to prevent cracking of the catalyst induced by too rapid evaporation of the water adhering to the intermediate product due to the relatively high temperature of calcination. According to a specific example, the drying temperature may be from 100 ℃ to 150 ℃ and the drying time may last from 2h to 10 h.
The method of preparing the catalytic oxidation catalyst for ozone for treating wastewater according to the exemplary embodiments of the inventive concept is described above in detail with reference to the exemplary embodiments. Wherein descriptions of well-known techniques are avoided in order to more fully convey the concept of the invention to those skilled in the art. For example, the skilled person in the art can additionally increase the dispersibility and adhesion and improve the impregnation efficiency of the activated carbon support for the first impregnation liquid and/or the intermediate product for the second impregnation liquid by reasonably controlling the impregnation temperature, increasing the stirring operation, and other process steps under the teaching of the inventive concept.
After the above method, the catalytic ozonation catalyst for treating wastewater according to the present inventive concept can be prepared. The catalytic ozonation catalyst for treating wastewater has proper hydrophobicity through the process so as to be beneficial to adsorbing macromolecular organic matters which are difficult to degrade, and meanwhile, the active components are loaded on the surface of the active carbon, so that the active carbon can be used for degrading the organic matters after adsorbing the organic matters, the removal rate of COD is greatly improved, and the investment cost and the operation cost are further reduced.
Hereinafter, specific examples of the inventive concept and comparative examples of the prior art will be described.
Example 1
First-step impregnation: putting the columnar activated carbon carrier with the diameter of 3-4 mm into the aqueous solution of ethylene glycol, uniformly stirring, soaking for 3h, and filtering to obtain an intermediate product. Here, the amount of ethylene glycol added was 0.1 times the sum of the moles of the active components used in the second impregnation.
Second step dipping: putting the intermediate product subjected to the first-step impregnation into a mixed solution (active component precursor solution) composed of Mn metal elements and Cu metal elements in a mass ratio of 1:1, mixing and impregnating an active carbon carrier and the mixed solution for 3 hours according to the proportion that 1kg of active carbon can load 1g of Mn metal elements and 1g of Cu metal elements, and then filtering to obtain a pre-product. Here, the manganese precursor used in the second impregnation solution was a commercially available 50% manganese nitrate solution, and the copper precursor used was copper nitrate.
Thereafter, the pre-product was dried at 100 ℃ for 10 hours and then calcined at 300 ℃ for 5 hours, thereby obtaining catalyst A.
Example 2
First-step impregnation: putting the columnar activated carbon carrier with the diameter of 3mm-4mm into the aqueous solution of ethylene glycol, uniformly stirring, and soaking for 4h to obtain an intermediate product. Here, the amount of ethylene glycol added was 10 times the sum of the moles of the active components used in the second impregnation.
Second step dipping: putting the intermediate product subjected to the first-step impregnation into a mixed solution (active component solution) composed of Mn metal elements and Cu metal elements in a mass ratio of 10:1, mixing and impregnating an activated carbon carrier and the mixed solution for 24 hours according to the proportion that 1kg of activated carbon can load 100g of Mn metal elements and 10g of Cu metal elements, and then filtering to obtain a pre-product. Here, the manganese precursor used in the second impregnation solution was a commercially available 50% manganese nitrate solution, and the copper precursor used was copper nitrate.
Thereafter, the preliminary product was dried at 150 ℃ for 2 hours and then calcined at 700 ℃ for 2 hours, thereby obtaining catalyst B.
Example 3
First-step impregnation: putting the columnar activated carbon carrier with the diameter of 3mm-4mm into the aqueous solution of ethylene glycol, uniformly stirring, soaking for 4h, and filtering to obtain an intermediate product. Here, the amount of ethylene glycol added was 2 times the sum of the moles of the active components used in the second impregnation.
Second step dipping: putting the intermediate product subjected to the first-step impregnation into a mixed solution (active component solution) composed of Mn metal elements and Cu metal elements in a mass ratio of 5:1, mixing and impregnating an activated carbon carrier and the mixed solution for 4 hours according to the proportion that 1kg of activated carbon can load 50g of Mn metal elements and 10g of Cu metal elements, and then filtering to obtain a pre-product. Here, the manganese precursor used in the second impregnation solution was a commercially available 50% manganese nitrate solution, and the copper precursor used was copper nitrate.
Thereafter, the pre-product was dried at 120 ℃ for 3 hours and then calcined at 400 ℃ for 3 hours, thereby preparing catalyst C.
Comparative example
A columnar activated carbon carrier with a diameter of 3mm to 4mm is placed in a mixed solution with a mass ratio of Mn metal element to Cu metal element of 2:1 so that 1kg of activated carbon is loaded with 20g of Mn metal element and 10g of Cu metal element, and then impregnated for 4 hours. Then, the impregnation solution was filtered off, and dried at 120 ℃ for 3 hours, and then calcined at 600 ℃ for 3 hours, thereby obtaining catalyst D.
The catalysts a to C prepared in examples 1 to 3 and the catalyst D prepared in comparative example were subjected to evaluation of the ozone catalytic oxidation test for wastewater under the following evaluation conditions and test results: the catalyst is used for treating wastewater in a fixed bed reactor, the wastewater is wastewater of a certain industrial park, the wastewater of the industrial park comprises medicine, pesticide, pigment, chemical fertilizer and spice wastewater, and the pigment wastewater is mainly used. Wherein the COD content is about 100mg/L, and the chloride ion content is lower than 2000 mg/L.
The volume of the catalyst bed layer is 2L, and the space velocity of the wastewater volume is 1h-1The ozone concentration is 100mg/L, and the ozone adding amount is 70 mg/L. The COD removal rate of the wastewater and the dissolution rate of the manganese metal ions of the catalyst at room temperature for 3h, 4h and 5h of continuous operation are shown in Table 1.
TABLE 1 evaluation test result of catalyst for treating wastewater of certain industrial park
Figure BDA0001902866460000071
As can be seen from table 1, the COD removal rate using the catalysts according to the exemplary embodiments of the inventive concept was significantly higher than that using the catalysts according to the comparative examples of the related art.
By summarizing and reviewing, the invention conception modifies the surface of the activated carbon by using the surfactant, thereby modulating the hydrophobicity of the surface of the activated carbon and improving the removal capacity of hydrophobic organic matters. In addition, the activated carbon carriers with different hydrophobicity can be obtained by adjusting the type and the dosage of the surfactant, so that a series of catalysts with proper adsorbability to different water qualities can be further obtained. In addition, because the active component is attached to the surface of the active carbon, the COD removing capability can be improved by degrading the macromolecular organic matters through the active component after the active carbon adsorbs the macromolecular organic matters.

Claims (10)

1. A method of preparing an ozone catalytic oxidation catalyst for treating wastewater, the method comprising the steps of:
providing an activated carbon carrier;
performing a first impregnation process on the activated carbon carrier, and then filtering to obtain an intermediate product, wherein a first impregnation liquid adopted in the first impregnation process comprises a surfactant;
performing a second impregnation process on the intermediate product, and then filtering to obtain a filtrate as a pre-product, wherein a second impregnation liquid adopted in the second impregnation process comprises an active component precursor of the catalyst;
and drying and roasting the pre-product to obtain the catalyst.
2. The method of claim 1, wherein the active component of the catalyst comprises at least one of Fe, Cu, Ni, Mn.
3. The method of claim 2, wherein the active component of the catalyst comprises Mn and Cu, and a mass ratio of the Mn element to the Cu element in the second impregnation solution is 1:1 to 10: 1.
4. The method according to claim 3, wherein the contents of the Mn element and the Cu element included in the second impregnation liquid are set in such a manner that 1kg of the activated carbon supports 1g to 100g of the Mn element and 1g to 10g of the Cu element.
5. The method of claim 1, wherein the surfactant comprises ethylene glycol.
6. The method of claim 1, wherein the number of moles of the surfactant is from 0.1 times to 10 times the sum of the number of moles of the active components.
7. The method of claim 1, wherein in the roasting step, the roasting temperature is 300 ℃ to 700 ℃ and the roasting time is 2h to 5 h.
8. The method of claim 7, wherein the drying temperature in the drying step is from 100 ℃ to 150 ℃ and the drying time is from 2h to 10 h.
9. The method according to claim 1, wherein the first impregnation process and the second impregnation process are each impregnated for not less than 1 hour.
10. A catalytic ozonation catalyst for treating wastewater, characterized in that the catalytic ozonation catalyst is prepared by the method of any one of claims 1 to 9.
CN201811519491.5A 2018-12-12 2018-12-12 Ozone catalytic oxidation catalyst for treating wastewater and preparation method thereof Pending CN111298804A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113788524A (en) * 2021-09-27 2021-12-14 金风环保有限公司 Method for treating papermaking wastewater and wastewater treatment apparatus

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113788524A (en) * 2021-09-27 2021-12-14 金风环保有限公司 Method for treating papermaking wastewater and wastewater treatment apparatus
CN113788524B (en) * 2021-09-27 2023-06-02 金风环保有限公司 Method for treating papermaking wastewater and wastewater treatment device

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