CN106669726A - Ozone catalyst for effectively stabilizing ammonia nitrogen content in iron and steel wastewater and preparation and application - Google Patents
Ozone catalyst for effectively stabilizing ammonia nitrogen content in iron and steel wastewater and preparation and application Download PDFInfo
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- CN106669726A CN106669726A CN201611183906.7A CN201611183906A CN106669726A CN 106669726 A CN106669726 A CN 106669726A CN 201611183906 A CN201611183906 A CN 201611183906A CN 106669726 A CN106669726 A CN 106669726A
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
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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
- C02F1/725—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
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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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- 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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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Abstract
The invention discloses an ozone catalyst for effectively stabilizing ammonia nitrogen content in iron and steel wastewater and preparation and application. Manganese acetate, cobalt acetate and cerous acetate are dissolved into de-ionized water; the concentration of the prepared solution is 1 mol/L and is stored for use; for catalyst carriers, manganese acetate, cobalt acetate and cerous acetate solutions are respectively weighed according to the proportion and are dripped into a beaker containing carriers; the materials are subjected to still standing after being stirred for 2 hours; after the soaking for 24 hours is completed, the catalyst is washed and filtered, catalysts loaded with Mn, Co and Ce are calcined, the calcination time is 4 hours, and the temperature rise speed is controlled to be 5 DEG C/min; finally, the three-ingredient Mn-Co-Ce ozone catalyst is obtained. The ozone catalyst can effectively stabilize the ammonia nitrogen content in iron and steel wastewater, so that the ammonia nitrogen content in iron and steel wastewater can be discharged in a standard reaching manner; the secondary pollution of the catalyst is avoided; the pollution caused on the environment is avoided. The preparation method has the advantages that the process is simple; great popularization and application values are realized.
Description
Technical field
The invention belongs to environmental pollution process for comprehensively treating field, ammonia nitrogen contains in more particularly to a kind of effective stably waste water
The ozone catalyst of amount and preparation and application.
Background technology
Ozone is a kind of gas with strong oxidizing property, with the effect that wide spectrum is killed livestock.Its effect of not only killing livestock is good, kills livestock
Speed is fast（600 ~ 3000 times fast compared with chlorination）, and public hazards and problem of environmental pollution are relatively small, thus become preferably green ring
Guarantor's type oxidant.Ozone has strong oxidizing property, can cut off the unsaturated bond in Organic substance, decomposes pigment, insecticide, cyaniding
The Organic substances such as thing, phenol, eliminate abnormal flavour；Oxidable heavy metal element and water-fast compound, such as ferrum, manganese, aluminum, copper, stannum,
The compound of gold, silver so as to which precipitation is removed, thus ozone has a wide range of applications in water treatment field.At present, it is existing in the world
1000 Duo Zuo water factories are processed using ozone technology, wherein, most popular is heterogeneous ozone catalytic technology, and the technology is with oxygen
It is carrier to change aluminum or molecular sieve, in the different metal of surface impregnation or metal-oxide, while the certain auxiliary agent of addition, with
Improve removal effect of the ozone to particular oxides.
In the exploitation of ozone catalyst, the ozone catalyst with ternary material Mn-Co-Ce as representative is in difficult degradation iron and steel
It is widely used in waste water.The industrialized production of ternary Mn-Co-Ce ozone catalyst is typically by gold such as manganese, cobalt, ceriums
The nitrate of category is impregnated into Al as predecessor2O3Or the surface of molecular sieve carrier, the gold such as manganese, cobalt, cerium are made by calcination processing
Category component is distributed in carrier.To keep the high activity of ozone catalyst, calcination processing general control is in 300 ~ 450 DEG C
Carry out under low temperature.With the development of China's steel and iron industry and in recent years in acid-cleaning plate, heat zinc coating plate, electrolytic tinplate, Coil Coating Products
Adjust Deng the depth on product structure, the harmful substance species of steel wastewater is more and more, will to the advanced treating of steel wastewater
Seek also more and more higher.During actual treatment steel wastewater, although ternary Mn-Co-Ce ozone catalyst being capable of degradation water
Middle organic pollution, effective process COD of sewage, but often there is a problem that ammonia-nitrogen content is exceeded, causes steel saliva is gone out
Iron waste water is unable to qualified discharge, and this hides some dangers in actual applications.Track the exceeded source of ammonia-nitrogen content to show, steel wastewater
The exceeded key factor of ammonia-nitrogen content for catalyst pollution, i.e. the nitrate ion of ternary Mn-Co-Ce ozone catalytic agent material
Caused by residual, and improving calcination processing temperature simply can then substantially reduce the activity of ozone catalyst, therefore develop new
Industrialization ternary Mn-Co-Ce ozone catalyst it is imperative.
For the nitrate ion residual that the preparation of industrialization of ternary Mn-Co-Ce ozone catalyst is produced, patent of the present invention is adopted
The method that nitrate prepares ozone catalyst is replaced in whole or in part with a kind of use acetate, and the method can be effectively steady
Determine the ammonia-nitrogen content in steel wastewater, make steel wastewater qualified discharge, it is to avoid the secondary pollution of catalyst.Due to manganese acetate,
Cobalt acetate, the boiling point of Cerium triacetate are respectively 80 DEG C, 298 DEG C, 308 DEG C, the boiling point of corresponding acetate are below, in chemistry
Also there is similarity with acetate in performance, causing nitrate precursor to substitute nitrate carries out ternary Mn-Co-Ce ozone
It is prepared by Catalystization.Manganese acetate, cobalt acetate, Cerium triacetate are configured to certain density aqueous solution by the present invention first, then
Manganese acetate, cobalt acetate, Cerium triacetate are added in molecular sieve solution according to different mass percents, be sufficiently impregnated with 24 hours with
On, it is to be adsorbed completely after fully washing, drying, the calcining under 350 ~ 400 DEG C of medium and low temperatures obtains the industry of ternary Mn-Co-Ce
Change ozone catalyst.
The content of the invention
To overcome the deficiencies in the prior art, the present invention to propose that a kind of ozone for effectively stablizing ammonia-nitrogen content in steel wastewater is urged
Agent and preparation and application.The method does not change existing process conditions, only changes or replace the kind of catalyst precursor
Class, prepared ternary Mn-Co-Ce ozone catalyst can keep stablizing for ammonia-nitrogen content in steel wastewater.On realizing
Purpose is stated, the present invention is adopted the following technical scheme that：
A kind of preparation method for effectively stablizing the ozone catalyst of ammonia-nitrogen content in steel wastewater, it is characterised in that comprising following
Step：
（1）Quantitative manganese acetate, cobalt acetate, Cerium triacetate are weighed, in being dissolved in deionized water, the solution concentration of preparation is 1 mol/
L, stays with standby；
（2）Catalyst carrier is weighed, manganese acetate, cobalt acetate and Cerium triacetate solution are proportionally measured respectively, be added drop-wise to equipped with load
In the beaker of body, stirring stands after 2 hours；After the completion of 24 hours to be impregnated, catalyst is washed and filtered；
（3）The catalyst of Supported Manganese, cobalt, cerium is calcined under medium and low temperature scope, calcination time is 4 hours, heat up speed
Rate is controlled in 5 DEG C/min, finally gives ternary Mn-Co-Ce ozone catalyst.
Described manganese, cobalt, cerium molar ratio are (60 ~ 79):(9~11):(5~7).
Described catalyst carrier is respectively molecular sieve, aluminium oxide, silicon dioxide.
Described medium and low temperature calcining scope refers to 300 ~ 400 DEG C.
A kind of ozone catalyst for effectively stablizing ammonia-nitrogen content in steel wastewater, it is characterised in that according to any of the above-described institute
The method of stating is prepared.
A kind of ozone catalyst for effectively stablizing ammonia-nitrogen content in steel wastewater ammonia-nitrogen content in steel wastewater is stablized
Using.
The present invention proposes a kind of preparation side for effectively stablizing the industrial ozone catalyst of ammonia-nitrogen content in steel wastewater
Method, possesses advantages below：Solvent contamination used by preparing is little, and building-up process is not high to equipment requirements；Synthesized ternary Mn-
Co-Ce ozone catalysts are waited do not change existing technique when in use, will not introduce the pollution of catalyst, and iron and steel can be kept to give up
Ammonia-nitrogen content stablizes in water.Preparation process is simple of the present invention, can be applied not only to the process of wastewater of steel industry, can be with
For the process of other industrial wastewaters and contaminated natural water, with larger application value.
Description of the drawings
Fig. 1 is the scanning electron microscope spectrogram of the ternary Mn-Co-Ce ozone catalyst prepared by the embodiment of the present invention 1.
Specific embodiment
The present invention is described in detail below by instantiation, gives detailed embodiment and specific operation
Process, but protection scope of the present invention is not only restricted to these examples of implementation.
Embodiment 1：
（1）Weigh 110.7 g manganese acetates respectively to be dissolved in 640 mL deionized waters；23.9 g cobalt acetates are dissolved in 96 mL
In deionized water；20.3 g Cerium triacetates are dissolved in 64 mL deionized waters, have configured precursor solution with standby.
（2）The 13X molecular sieves of 50g are weighed as carrier, in molecular sieve carrier distinguish the mL acetic acid manganese solutions of Deca 64,
9.6 mL cobalt acetates and 6.4 mL Cerium triacetate solution, stand after stirring 2 as a child under room temperature.Through 24 hours be sufficiently impregnated with
Afterwards, it is washed with deionized, finally calcining obtains ternary Mn-Co-Ce ozone catalyst in 4 hours at 350 DEG C.Figure one is made
The scanning electron microscope spectrogram of standby ternary Mn-Co-Ce ozone catalyst, it is seen that catalyst keeps preferable graininess.
（2）The evaluation of catalytic ozonation is carried out in ozone catalytic tower, and ternary Mn-Co-Ce ozone catalyst is thrown
Enter in ozone catalytic tower, the ozonation aerated time is 30 min, the flow for adjusting the steel wastewater of ozone catalytic tower is 6 g/ h,
Depth degradation is carried out to it, the COD clearances for finally measuring steel wastewater reach 38 %, and waste water nitrogen oxygen content remains within one
Individual extremely low concentration, does not find the pollution of ozone catalyst.
Embodiment 2：
（1）The configuration of precursor solution is with the step in embodiment 1（1）；
（2）Weigh the Al of 50 g2O3As carrier, the mL acetic acid manganese solutions of Deca 79,9.6 mL second are distinguished in molecular sieve carrier
Sour cobalt and 7 mL Cerium triacetate solution, stand after stirring 2 as a child under room temperature.After 24 hours be sufficiently impregnated with, deionization is used
Water washing, finally calcining obtains ternary Mn-Co-Ce ozone catalyst in 4 hours at 400 DEG C.
（3）The evaluation of catalytic ozonation is carried out in ozone catalytic tower, and ternary Mn-Co-Ce ozone catalyst is thrown
Enter in ozone catalytic tower, the ozonation aerated time is 30 min, the flow for adjusting the steel wastewater of ozone catalytic tower is 5 g/ h,
Depth degradation is carried out to it, the COD clearances for finally measuring steel wastewater reach 36 %, the ammonia-nitrogen content in waste water keeps not
Become, do not find the pollution of ozone catalyst.
Embodiment 3：
（1）The configuration of precursor solution is with the step in embodiment 1（1）；
（2）The NaY molecular sieve of 50 g is weighed as carrier, the mL acetic acid manganese solutions of Deca 60,9 mL are distinguished in molecular sieve carrier
Cobalt acetate and 5 mL Cerium triacetate solution, stand after stirring 2 as a child under room temperature.After 24 hours be sufficiently impregnated with, spend from
Sub- water washing, finally calcining obtains ternary Mn-Co-Ce ozone catalyst in 4 hours at 350 DEG C.
（3）The evaluation of catalytic ozonation is carried out in ozone catalytic tower, and ternary Mn-Co-Ce ozone catalyst is thrown
Enter in ozone catalytic tower, the ozonation aerated time is 30 min, the flow for adjusting the steel wastewater of ozone catalytic tower is 5 g/ h,
Depth degradation is carried out to it, the COD clearances for finally measuring steel wastewater reach 32 %, the ammonia-nitrogen content in waste water keeps not
Become, do not find the pollution of ozone catalyst.
Claims (6)
1. a kind of preparation method for effectively stablizing the ozone catalyst of ammonia-nitrogen content in steel wastewater, it is characterised in that comprising with
Lower step：
（1）Quantitative manganese acetate, cobalt acetate, Cerium triacetate are weighed, in being dissolved in deionized water, the solution concentration of preparation is 1 mol/
L, stays with standby；
（2）Catalyst carrier is weighed, manganese acetate, cobalt acetate and Cerium triacetate solution are proportionally measured respectively, be added drop-wise to equipped with load
In the beaker of body, stirring stands after 2 hours；After the completion of 24 hours to be impregnated, catalyst is washed and filtered；
（3）The catalyst of Supported Manganese, cobalt, cerium is calcined under medium and low temperature scope, calcination time is 4 hours, heat up speed
Rate is controlled in 5 DEG C/min, finally gives ternary Mn-Co-Ce ozone catalyst.
2. the preparation method for effectively stablizing the ozone catalyst of ammonia-nitrogen content in steel wastewater according to claim 1, its
It is characterised by, described manganese, cobalt, cerium molar ratio are (60 ~ 79):(9~11):(5~7).
3. the preparation method for effectively stablizing the ozone catalyst of ammonia-nitrogen content in steel wastewater according to claim 1, its
It is characterised by, described catalyst carrier is respectively molecular sieve, aluminium oxide, silicon dioxide.
4. the preparation method for effectively stablizing the ozone catalyst of ammonia-nitrogen content in steel wastewater according to claim 1, its
It is characterised by, described medium and low temperature calcining scope refers to 300 ~ 400 DEG C.
5. a kind of ozone catalyst for effectively stablizing ammonia-nitrogen content in steel wastewater, it is characterised in that appointed according to claim 1-4
One methods described is prepared.
6. according to claim 5 effectively stablize steel wastewater in ammonia-nitrogen content ozone catalyst in steel wastewater is stablized
The application of ammonia-nitrogen content.
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| CN201611183906.7A CN106669726A (en) | 2016-12-20 | 2016-12-20 | Ozone catalyst for effectively stabilizing ammonia nitrogen content in iron and steel wastewater and preparation and application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110694637A (en) * | 2019-10-14 | 2020-01-17 | 大连第一有机化工有限公司 | Preparation method of supported multi-element metal oxide oxidation catalyst |
| CN111841659A (en) * | 2020-07-28 | 2020-10-30 | 福建省农业科学院农业工程技术研究所 | Preparation of magnetic suspended 3D microspheres and application thereof in catalyzing ozone to mineralize refractory organic matters |
| CN113371941A (en) * | 2021-06-23 | 2021-09-10 | 中南大学 | Application of microbial carbon-loaded metal ammonia nitrogen oxidation ozone catalyst in degradation of high-concentration ammonia nitrogen wastewater |
| CN114054029A (en) * | 2020-08-05 | 2022-02-18 | 万华化学集团股份有限公司 | Catalyst for catalytic oxidation treatment of wastewater and preparation method and application thereof |
| CN114471585A (en) * | 2022-02-28 | 2022-05-13 | 山东华特环保科技有限公司 | Ozone catalyst with acetate as precursor and preparation method and application thereof |
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| CN104307534A (en) * | 2014-10-31 | 2015-01-28 | 天津市联合环保工程设计有限公司 | Preparation method for MnO2-CeO2-CoO/AC ternary supported catalyst for treatment of phenolic wastewater |
| CN105381797A (en) * | 2015-10-16 | 2016-03-09 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of catalytic ozonation supported catalyst used for treating sewage and doped with dual rare earth elements |
| CN105688928A (en) * | 2014-11-27 | 2016-06-22 | 中国海洋石油总公司 | Ozone catalytic oxidation catalyst and preparation method and application thereof |
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| CN103586026A (en) * | 2013-11-26 | 2014-02-19 | 北京碧水源科技股份有限公司 | Carbon supported catalyst for ozone oxidation, and preparation method and use thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110694637A (en) * | 2019-10-14 | 2020-01-17 | 大连第一有机化工有限公司 | Preparation method of supported multi-element metal oxide oxidation catalyst |
| CN111841659A (en) * | 2020-07-28 | 2020-10-30 | 福建省农业科学院农业工程技术研究所 | Preparation of magnetic suspended 3D microspheres and application thereof in catalyzing ozone to mineralize refractory organic matters |
| CN114054029A (en) * | 2020-08-05 | 2022-02-18 | 万华化学集团股份有限公司 | Catalyst for catalytic oxidation treatment of wastewater and preparation method and application thereof |
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| CN113371941A (en) * | 2021-06-23 | 2021-09-10 | 中南大学 | Application of microbial carbon-loaded metal ammonia nitrogen oxidation ozone catalyst in degradation of high-concentration ammonia nitrogen wastewater |
| CN114471585A (en) * | 2022-02-28 | 2022-05-13 | 山东华特环保科技有限公司 | Ozone catalyst with acetate as precursor and preparation method and application thereof |
| CN114471585B (en) * | 2022-02-28 | 2024-05-07 | 山东华特环保科技有限公司 | Ozone catalyst with acetate as precursor and preparation method and application thereof |
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Application publication date: 20170517 |