CN105536813A - Catalytic ozonation catalyst for wastewater treatment and preparation method thereof - Google Patents
Catalytic ozonation catalyst for wastewater treatment and preparation method thereof Download PDFInfo
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- CN105536813A CN105536813A CN201610067238.5A CN201610067238A CN105536813A CN 105536813 A CN105536813 A CN 105536813A CN 201610067238 A CN201610067238 A CN 201610067238A CN 105536813 A CN105536813 A CN 105536813A
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- 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
- B01J23/78—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 alkali- or alkaline earth metals
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- 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
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- 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
- B01J23/83—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 rare earths or actinides
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- 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
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- 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
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- 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
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
The invention belongs to the technical field of water treatment, and in particular relates to a catalytic ozonation catalyst for the wastewater treatment and a preparation method thereof. The catalyst is prepared from an active component, an auxiliary and a carrier, wherein the active component is a transition metal oxide, the auxiliary is an alkali metal oxide, an alkaline earth metal oxide or a lanthanide metal oxide, and the carrier is an aluminum oxide, active carbon or ceramsite. The invention further provides a preparation method of the catalyst. The preparation method comprises the steps: loading the active component, the auxiliary and a dispersing agent on the carrier by utilizing an impregnation method or a dry mixing method, curing, drying and roasting, thereby obtaining the catalyst. According to the catalytic ozonation catalyst for the wastewater treatment and the preparation method thereof, the COD removal rate is higher, and the service life is longer; the preparation process is simple, the costs are low, no secondary pollution exists, and the catalytic ozonation catalyst for the wastewater treatment and the preparation method thereof are very suitable for industrial production.
Description
Technical field
The invention belongs to water-treatment technology field, specifically, relate to a kind of ozone catalytic oxidation catalyst for wastewater treatment and preparation method thereof.
Background technology
Along with the development of society, increasing artificial-synthetic compound enters into water body, and cause in water body and there is some high stabilities, dysoxidizable organic matter, this type organic causes serious destruction to water environment.Remove this kind of persistent organic pollutants in water cost-effectively and become the focus of current water treatment field research and engineer applied.
Recent study exploitation be that the high-level oxidation technology of oxidant can the organic pollution of poisonous in oxidation Decomposition water, difficult degradation with ozone, receive increasing concern.Although simple ozone can degradation of organic substances, have selective, and less with the organic reaction rate of aromatic series, can not by organic matter complete oxidation in a lot of situation.Therefore, people are improved ozone process by the mode of adding catalyst.Catalytic ozonation is divided into two classes according to the difference of used catalyst: a class take metal ion as the homogeneous catalysis ozonation technology of catalyst; Another kind of is the heterogeneous catalysis ozonation technology using solid catalyst.Though it is high and do not have the feature of secondary pollution that existing catalytic ozonation has reaction condition gentleness, oxidation activity, have that Catalyst for CO D clearance is low, catalyst preparation process is complicated, a problem that catalyst service life is short simultaneously, be further improved.
Summary of the invention
The object of this invention is to provide a kind of ozone catalytic oxidation catalyst for wastewater treatment and preparation method thereof, to solve the problem.
The invention provides a kind of ozone catalytic oxidation catalyst for wastewater treatment, this catalyst is made up of active component, auxiliary agent and carrier; Wherein, active component is transition metal oxide, and auxiliary agent is alkali metal oxide, alkaline earth oxide or lanthanide metal oxide; Carrier is aluminium oxide, active carbon or haydite.
Further, in mass, active component is 1.0-15%, and auxiliary agent is 0.1-1.0%, and surplus is carrier.
Further, active component is that one or more are selected from the transition metal oxide of titanium, manganese, iron, cobalt, nickel, copper, zinc.
Further, auxiliary agent is that one or more are selected from sodium, potassium, magnesium, calcium, lanthanum, the alkali metal oxide of cerium, alkaline earth oxide or lanthanide metal oxide.
Present invention also offers a kind of preparation method of the ozone catalytic oxidation catalyst for wastewater treatment, namely adopt infusion process or dry pigmentation by active component, auxiliary agent and dispersant load on carrier, obtained after health, drying, roasting.
Further, in mass, described active component is 1.0-15%, and auxiliary agent is 0.1-1.0%, and surplus is carrier.
Further, the method specifically comprises:
Mixed impregnant liquor A is mixed with by active component and auxiliary agent;
In mixed impregnant liquor A, add dispersant make mixed impregnant liquor B;
By mixed impregnant liquor B load on carrier, then obtain this catalyst through health, drying, roasting.
Further, the mass concentration of mixed impregnant liquor A is 1%-15%.
Further, the addition of dispersant is 100-1000g/L.
Further, sintering temperature is 400-800 DEG C, and roasting time is 2-6h.
Compared with prior art the invention has the beneficial effects as follows: make that COD clearance is higher, longer service life, and preparation technology is simple, with low cost, non-secondary pollution, is very applicable to suitability for industrialized production.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described in detail, but is not limited to this.Those skilled in the art can use for reference content of the present invention, the links such as suitable change material, parameter, technique realize other objects corresponding, its relevant change does not all depart from content of the present invention, all similar replacements and change will become apparent to those skilled in the art that and all should be deemed to be included within scope of the present invention.
The embodiment provides a kind of ozone catalytic oxidation catalyst, this catalyst is made up of active component, auxiliary agent and carrier; In mass, active component is 1.0-15%, and auxiliary agent is 0.1-1.0%, and surplus is carrier; Wherein, active component is transition metal oxide, and auxiliary agent is alkali metal oxide, alkaline earth oxide or lanthanide metal oxide; Carrier is aluminium oxide, active carbon or haydite.
In an embodiment of the present invention, active component is that one or more are selected from the transition metal oxide of titanium, manganese, iron, cobalt, nickel, copper, zinc.
In an embodiment of the present invention, auxiliary agent is that one or more are selected from sodium, potassium, magnesium, calcium, lanthanum, the alkali metal oxide of cerium, alkaline earth oxide or lanthanide metal oxide.
Embodiments of the invention additionally provide a kind of preparation method of the ozone catalytic oxidation catalyst for wastewater treatment, the method adopts infusion process or dry pigmentation by active component, auxiliary agent and dispersant load on carrier, obtained catalyst after health, drying, roasting.The preferred infusion process of this preparation method.
In an embodiment of the present invention, in mass, active component is 1.0-15%, and auxiliary agent is 0.1-1.0%, and surplus is carrier; Wherein, active component is transition metal oxide, and auxiliary agent is alkali metal oxide, alkaline earth oxide or lanthanide metal oxide; Dispersant is the compound of phosphorus, silicon, boron, nitrogen, sulphur or halogen; Carrier is aluminium oxide, active carbon or haydite.
In an embodiment of the present invention, the method specifically comprises:
Mixed impregnant liquor A is mixed with by active component and auxiliary agent;
In mixed impregnant liquor A, add dispersant make mixed impregnant liquor B;
With dipping or the method that is dry mixed by described mixed impregnant liquor B load on carrier, then obtain described catalyst through health, drying, roasting.The preferred infusion process of the preparation method of catalyst in an embodiment of the present invention, further preferred equi-volume impregnating.
In an embodiment of the present invention, the mass concentration of mixed impregnant liquor A is 1%-15%, and namely the mass concentration of transition metal ions, alkali metal ion or alkaline-earth metal ions or lanthanide metal ion solution is all 1%-15%.
In an embodiment of the present invention, the addition of dispersant is 100-1000g/L, and preferred addition is 100-800g/L.
In an embodiment of the present invention, sintering temperature is 400-800 DEG C, and roasting time is 2-6h.
Embodiments of the invention can make catalyst have good Active components distribution state by adding dispersant in the preparation process of catalyst.Dispersant in the embodiment of the present invention is a kind of surfactant with good dispersion performance and wettability, have and make various metals salt be homodisperse function on the surface of carrier pore, the ozone catalytic oxidation catalyst that embodiments of the invention provide, COD clearance is higher, longer service life, and preparation technology is simple.After catalytic ozonation process, the COD clearance in refinery reverse osmosis concentrated water can reach more than 60%, and the biodegradability BOD/COD of waste water brings up to more than 0.30; COD clearance in phenol wastewater can reach about 90%.And non-secondary pollution, with low cost, be very applicable to suitability for industrialized production.
In addition, the catalyst that the embodiment of the present invention provides is not limited to catalytic oxidation treatment refinery reverse osmosis concentrated water, is also applicable to the reverse osmosis concentrated water processing other systems such as Coal Chemical Industry reverse osmosis concentrated water, oil recovery reverse osmosis concentrated water.Meanwhile, be also applicable to the wastewater treatment of other systems, such as Phenol-Containing Wastewater Treatment, the waste water etc. of ester-contaning compounds, compound fragrant hydrocarbon and Small molecular acid.
The preparation method of catalyst is described in detail below by instantiation.
Embodiment 1 prepares Fe-Mn-Na/ aluminium oxide catalyst
(1) Fe (NO of 1wt.% is measured respectively
3)
3, Mn (NO
3)
2, NaNO
3solution 170ml, 43ml and 17ml are mixed with mixed impregnant liquor A.
(2) in above-mentioned mixed impregnant liquor A, add 100g Cetyltrimethylammonium bromide and be mixed with mixed impregnant liquor B.
(3) by the method for incipient impregnation, above-mentioned mixed impregnant liquor B is sprayed on 500g shaped alumina alumina supporter, then seal health 4h, then in 100 DEG C of dry 5h, finally obtain catalyst A in 400 DEG C of roasting 4h.
Embodiment 2 prepares Fe-Cu-K/ activated-carbon catalyst
(1) Fe (NO of 15wt.% is measured respectively
3)
3, Cu (NO
3)
2, KNO
3solution 170ml, 80ml and 10ml are mixed with mixed impregnant liquor A.
(2) in above-mentioned mixed impregnant liquor A, add 260g fourth octyl group phosphorodithioate and be mixed with mixed impregnant liquor B.
(3) by the method for incipient impregnation, above-mentioned mixed impregnant liquor B is sprayed on 500g Constitutive active high-area carbon, then health 12h in atmosphere, then in 120 DEG C of dry 4h, finally obtain catalyst B in 600 DEG C of roasting 4h.
Embodiment 3 prepares Cu-Mn-Ce/ ceramsite catalyst
(1) Cu (NO of 6wt.% is measured respectively
3)
2, Mn (NO
3)
2, Ce (NO
3)
3solution 170ml, 80ml and 30ml are mixed with mixed impregnant liquor A.
(2) in above-mentioned mixed impregnant liquor A, add 200g myristyl tributyl ammonium chloride and be mixed with mixed impregnant liquor B.
(3) above-mentioned mixed impregnant liquor B and 500g haydite materials are mixed, then carry out rolling granulation, and control granulation diameter.
(4) particle that step (3) obtains is carried out sealing health 8h, then in 120 DEG C of dry 5h, finally obtain catalyst C in 500 DEG C of roasting 5h.
Embodiment 4 prepares Mn-Fe-Ni-La/ aluminium oxide catalyst
(1) Mn (NO of 8wt.% is measured respectively
3)
2, Fe (NO
3)
3, Ni (NO
3)
2, La (NO
3)
3solution 150ml, 30ml, 30ml and 20ml are mixed with mixed impregnant liquor A.
(2) in above-mentioned mixed impregnant liquor A, add 100g myristyl benzyl dimethyl ammonium chloride and be mixed with mixed impregnant liquor B.
(3) by the method for incipient impregnation, above-mentioned mixed impregnant liquor B is sprayed on 500g shaped alumina alumina supporter, then health 16h in atmosphere, then in 100 DEG C of dry 5h, finally obtain catalyst D in 400 DEG C of roasting 4h.
Below the performance of catalyst is evaluated:
The catalyst that embodiment 1-4 is prepared and commercially available, industrial used being carrier with aluminium oxide and active carbon, being that the catalyst of active component (its catalyst numbering is respectively E and F) carries out the test evaluation of waste water by ozone catalytic oxidation with transition metal respectively, test condition and test result as follows:
Test condition: catalyst of the present invention is used for processing waste water in fixed bed reactors.Waste water is reverse osmosis concentrated water, take from the dense water of petro-chemical corporation of PetroChina Company Limited. wastewater reusing device reverse osmosis units scene discharge, it forms complexity, organic pollution containing bio-refractories such as higher aliphatic hydrocarbon, polycyclic aromatic hydrocarbon, poly-ring aromatic compoundses, the mass concentration of its COD is about 200mg/L after measured, pH value is 7.5-8.5, and chlorine ions concentration is about 2500mg/L.
Catalyst bed volume is 377ml, wastewater volume air speed is 2h
-1(namely the time of staying is 30min), O
3concentration is 8.1mg/L, O
3volume flow rate is 80L/h; When at room temperature running 3h, 4h and 5h continuously, the COD clearance of reverse osmosis concentrated water and BOD/COD ratio are listed in and are shown in-1.
Table-1 catalyst treatment reverse osmosis concentrated water performance evaluation test result
A series of detailed description listed is above only illustrating for feasibility embodiment of the present invention; they are also not used to limit the scope of the invention, all do not depart from the skill of the present invention equivalent implementations done of spirit or change all should be included within protection scope of the present invention.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
Claims (10)
1. for an ozone catalytic oxidation catalyst for wastewater treatment, it is characterized in that, be made up of active component, auxiliary agent and carrier; Wherein, described active component is transition metal oxide, and auxiliary agent is alkali metal oxide, alkaline earth oxide or lanthanide metal oxide; Described carrier is aluminium oxide, active carbon or haydite.
2. the ozone catalytic oxidation catalyst for wastewater treatment according to claim 1, is characterized in that, described active component is that one or more are selected from the transition metal oxide of titanium, manganese, iron, cobalt, nickel, copper, zinc.
3. the ozone catalytic oxidation catalyst for wastewater treatment according to claim 1, is characterized in that, described auxiliary agent is that one or more are selected from sodium, potassium, magnesium, calcium, lanthanum, the alkali metal oxide of cerium, alkaline earth oxide or lanthanide metal oxide.
4. for a preparation method for the ozone catalytic oxidation catalyst of wastewater treatment, it is characterized in that, adopt infusion process or dry pigmentation by active component, auxiliary agent and dispersant load on carrier, obtained after health, drying, roasting.
5. the preparation method of the ozone catalytic oxidation catalyst for wastewater treatment according to claim 4, is characterized in that, in mass, described active component is 1.0-15%, and auxiliary agent is 0.1-1.0%, and surplus is carrier.
6. the preparation method of the ozone catalytic oxidation catalyst for wastewater treatment according to claim 4, is characterized in that, specifically comprise:
Mixed impregnant liquor A is mixed with by active component and auxiliary agent;
In mixed impregnant liquor A, add dispersant make mixed impregnant liquor B;
By described mixed impregnant liquor B load on carrier, then obtain described catalyst through health, drying, roasting.
7. the preparation method of the ozone catalytic oxidation catalyst for wastewater treatment according to claim 6, is characterized in that, the mass concentration of described mixed impregnant liquor A is 1%-15%.
8. the preparation method of the ozone catalytic oxidation catalyst for wastewater treatment according to claim 6, is characterized in that, described dispersant is the compound of phosphorus, silicon, boron, nitrogen, sulphur or halogen.
9. the preparation method of the ozone catalytic oxidation catalyst for wastewater treatment according to claim 6, is characterized in that, the addition of described dispersant is 100-1000g/L.
10. the preparation method of the ozone catalytic oxidation catalyst for wastewater treatment according to claim 6, is characterized in that, sintering temperature is 400-800 DEG C, and roasting time is 2-6h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610067238.5A CN105536813A (en) | 2016-01-30 | 2016-01-30 | Catalytic ozonation catalyst for wastewater treatment and preparation method thereof |
| PCT/CN2016/086231 WO2017128600A1 (en) | 2016-01-30 | 2016-06-17 | Ozone catalytic oxidation catalyst for wastewater treatment and preparation method therefor |
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|---|---|---|---|
| CN201610067238.5A CN105536813A (en) | 2016-01-30 | 2016-01-30 | Catalytic ozonation catalyst for wastewater treatment and preparation method thereof |
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Cited By (27)
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| CN106345485A (en) * | 2016-08-25 | 2017-01-25 | 万华化学集团股份有限公司 | Catalyst for catalytic oxidation treatment of organic waste water, and preparation method and purpose thereof |
| CN106391034A (en) * | 2016-10-27 | 2017-02-15 | 上海纳米技术及应用国家工程研究中心有限公司 | Ceramic membrane based ferric oxide-nickel oxide-cerium oxide ozone catalyst and preparation and application thereof |
| WO2017128600A1 (en) * | 2016-01-30 | 2017-08-03 | 北京纬纶华业环保科技股份有限公司 | Ozone catalytic oxidation catalyst for wastewater treatment and preparation method therefor |
| CN108114711A (en) * | 2016-11-30 | 2018-06-05 | 中国科学院大连化学物理研究所 | A kind of catalyst of transition metal oxide and preparation method of catalytic eliminating ozone |
| CN108579755A (en) * | 2018-04-09 | 2018-09-28 | 北京天地人环保科技有限公司 | A kind of wastewater treatment catalyst and its application |
| CN109012658A (en) * | 2018-09-06 | 2018-12-18 | 杭州恒畅环保科技有限公司 | A kind of ozone oxidation catalyst and preparation method thereof |
| CN109225225A (en) * | 2018-10-31 | 2019-01-18 | 北京师范大学 | A kind of composition metal absorbent charcoal based catalyst and preparation method thereof of catalytic electrochemical-ozone-potentiometric titrations oxidation |
| CN109382092A (en) * | 2017-08-07 | 2019-02-26 | 光大水务（深圳）有限公司 | Ozone oxidation catalyst and preparation method thereof based on the balloon borne body of active gama-alumina |
| CN109718803A (en) * | 2018-06-29 | 2019-05-07 | 光大水务（深圳）有限公司 | A kind of catalyst and its preparation, application method for handling waste water nbsCOD |
| CN109794260A (en) * | 2019-02-22 | 2019-05-24 | 上海电气集团股份有限公司 | A kind of preparation method and ozone oxidation catalyst of ozone oxidation catalyst |
| CN110115999A (en) * | 2018-02-06 | 2019-08-13 | 浙江中凯瑞普环境工程股份有限公司 | Ozone catalytic oxidation catalyst and preparation method thereof for degradation of organic waste water |
| CN110538655A (en) * | 2018-05-29 | 2019-12-06 | 中国石油天然气股份有限公司 | Ozone oxidation catalyst and preparation method thereof |
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| CN111468106A (en) * | 2020-04-28 | 2020-07-31 | 光大水务科技发展（南京）有限公司 | Ceramsite catalyst for sewage treatment and preparation and application methods thereof |
| CN111744492A (en) * | 2019-03-26 | 2020-10-09 | 中国石油化工股份有限公司 | Catalytic ozonation catalyst, preparation method thereof and sewage treatment method |
| CN112121813A (en) * | 2020-09-15 | 2020-12-25 | 北京山美水美臭氧高科技有限公司 | Alkaline earth metal modified Mn-based ozone oxidation catalyst and application thereof |
| CN112390472A (en) * | 2020-11-23 | 2021-02-23 | 广东佳德环保科技有限公司 | Device system and method for treating coking wastewater |
| CN112403457A (en) * | 2020-12-09 | 2021-02-26 | 北京化工大学 | Method for oxidizing organic matters in wastewater by using activated carbon structured catalyst ozone |
| CN112547088A (en) * | 2020-12-23 | 2021-03-26 | 安道麦安邦(江苏)有限公司 | Ozone catalyst for high-concentration organic phosphorus conversion treatment in pesticide wastewater, and preparation method and application thereof |
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