CN102500391A - Catalyst for non-biodegradable wastewater treatment and preparation method thereof - Google Patents
Catalyst for non-biodegradable wastewater treatment and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a catalyst for non-biodegradable wastewater treatment and a preparation method of the catalyst. The catalyst comprises the following components by mass percentage: 0.5-10% of Cu, 0.5-10% of Mn, 0.5-10% of Fe, 0.05-5% of V, 0.1-5% of Ni, 0.1-5% of Ce, 0.1-5% of Co, 0.05-5% of Zn, 0.05-5% of Zr, 0.05-5% of Ti and 0.05-5% of Cr, wherein the activated carbon accounts for 80-95% relative to the total content of the catalyst. The preparation method comprises the following steps of: firstly adopting 0.5-25% of nitric acid to activate activated carbon to prepare carriers and then preparing the catalyst using impregnation-precipitation process, so as to improve the activity and stability of the catalyst. The catalyst prepared by the method in the invention has high activity and good active dispersibility, the active components of the catalyst are hard to lose, and the catalyst can be applied to the treatment of different kinds of wastewater. The catalyst prepared by the invention acts on together with the oxidants to have high COD (chemical oxygen demand) removal rate under the conditions of normal temperature and pressure.
Description
Technical field
The present invention relates to catalyst, relate in particular to a kind of Catalysts and its preparation method that used water difficult to degradate is handled that is used for.
Background technology
The catalytic oxidation technology is a kind of very effective senior chemical oxidize water treatment technology; Be specially adapted to the processing of poisonous and harmful and high concentration, organic wastewater with difficult degradation thereby; The catalytic oxidation technology receives widely with advantages such as its treatment effeciency are high, secondary pollution is low, oxidation rate is fast, equipment volume is little and paying close attention to, and has a good application prospect.
In existing catalytic oxidation technology, heterogeneous catalysis has active high, characteristics such as separation is simple, good stability, life-span length, makes it from the later stage seventies 20th century, becomes the research direction that high-concentration waste water is handled.Through years of development, existing a large amount of achievements are delivered.What research was more at present is precious metal, transition metal-type and terres rares catalyst.Wherein the precious metal catalyst activity is high, the life-span is long, adaptability is strong, and shortcoming is to cost an arm and a leg; Transition-metal catalyst all has catalytic activity preferably, and their shortcoming is to be prone to loss, life-span weak point; And that rare earth metal oxide catalyst has in catalytic reaction is active high, price is low and advantage such as good stability.
Also has Fenton reagent method.Because produce hydroxyl radical free radical ion efficiently, thereby can effectively handle the organic wastewater of some bio-refractories, it uses H
2O
2Be oxidant, Fe
2+Or Fe
3+Be catalyst, Fe
2+Or Fe
3+Can accelerate H
2O
2Be decomposed into OH, make organic matter in the solution by the rapid oxidative degradation of OH.But because catalytic oxidation efficient is low, shortcoming such as the oxidant consumption is big has influenced the industrial applications of this type catalysed oxidation processes.
Now domestic application to Fenton reagent has many patents; But all be to be conceived to Fenton reagent and ultrasonic wave (CN1546395, CN1583587); Little electrolysis (CN1631818); Photocatalysis (CN1699211), and with the improvement technology of bioanalysis associating (CN1611457, CN1736898).This type process is not made improvement to catalyst, and also ubiquity has high input in the application of this type process, the inferior position that processing cost is high.
In sum; Be necessary at present the water treatment catalyst is furtherd investigate; Can further improve activity of such catalysts and stability if on the catalyst of the type, add appropriate ingredients; Make multiple catalyst activity component that cooperative effect can take place, further improve the utilization rate of hydrogen peroxide solution, improving pollutants removal rate will have very important significance.Therefore must study the Preparation of catalysts process; Screen suitable component and definite optimum amount; Optimize some technological parameters in the preparation process, make abundant, active high, the long service life of the catalyst activity uniform component distribution, the specific area that prepare at last.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of Catalysts and its preparation method that used water difficult to degradate is handled that is used for is provided.
Being used for catalyst that used water difficult to degradate handles in the component of quality percentage composition catalyst is:
(1) active carbon content accounts for 80～95% of catalyst total content;
(2) active component: Cu: content accounts for 0.5～10% of catalyst total content;
Mn: content accounts for 0.5～10% of catalyst total content;
Fe: content accounts for 0.5～10% of catalyst total content;
(3) co-catalyst: V: content accounts for 0.05～5% of catalyst total content;
Ni: content accounts for 0.1～5% of catalyst total content;
Ce: content accounts for 0.1～5% of catalyst total content;
Co: content accounts for 0.1～5% of catalyst total content;
Zn: content accounts for 0.05～5% of catalyst total content;
Zr: content accounts for 0.05～5% of catalyst total content;
Ti: content accounts for 0.05～5% of catalyst total content;
Cr: content accounts for 0.05～5% of catalyst total content.
The soluble-salt of described active component and co-catalyst is nitrate, acetate, sulfate or ammonium salt.
The step that is used for the method for preparing catalyst that used water difficult to degradate handles is following:
(1) active carbon being placed mass percent concentration is 0.5～25% salpeter solution activation, reacts 1～5 hour down at 90～100 ℃, through filtration, cleaning, oven dry, obtains catalyst carrier;
(2) catalyst carrier is placed reactor; Adding and containing the quality percentage composition is several kinds of soluble-salt solution among 0.5～10%Cu, 0.5～10%Mn, 0.5～10%Fe, 0.05～5%V, 0.1～5%Ni, 0.1～5%Ce, 0.1～5%Co, 0.05～5%Zn, 0.05～5%Zr, 0.05～5%Ti, the 0.05～5%Cr, floods 12～24 hours;
(3) precipitating reagent is added reactor, reacted 6～12 hours, through after filtration, cleaning 100～115 ℃ dry 8～12 hours down, at last 300～500 ℃ of following activation 3～6 hours, obtain catalyst.
Described precipitating reagent is urea, NH
3H
2O, NaHCO
3Or KOH.
The present invention adopts dipping-precipitation method to come synthetic catalyst shortcoming such as avoided reuniting owing to later stage heat treatment produces active component, crystal grain is grown up voluntarily, and the powder of this method preparation has decentralization, crystal grain component and form is controlled, the reunion degree light, advantage such as few runs off.
Compared with present technology the catalyst of the inventive method preparation has following advantage: the catalyst of the present invention's preparation has very high catalytic activity, and the active material good dispersion is difficult for running off; This catalyst applications is handled operating temperature and the operating cost that reduces traditional handicraft greatly in used water difficult to degradate, and normal temperature and pressure can reach the COD clearance more than 60% down.
The specific embodiment
Being used for catalyst that used water difficult to degradate handles in the component of quality percentage composition catalyst is:
(1) active carbon content accounts for 80～95% of catalyst total content;
(2) active component: Cu: content accounts for 0.5～10% of catalyst total content;
Mn: content accounts for 0.5～10% of catalyst total content;
Fe: content accounts for 0.5～10% of catalyst total content;
(3) co-catalyst: V: content accounts for 0.05～5% of catalyst total content;
Ni: content accounts for 0.1～5% of catalyst total content;
Ce: content accounts for 0.1～5% of catalyst total content;
Co: content accounts for 0.1～5% of catalyst total content;
Zn: content accounts for 0.05～5% of catalyst total content;
Zr: content accounts for 0.05～5% of catalyst total content;
Ti: content accounts for 0.05～5% of catalyst total content;
Cr: content accounts for 0.05～5% of catalyst total content.
The soluble-salt of described active group and co-catalyst is nitrate, acetate, sulfate or ammonium salt.
The step that is used for the method for preparing catalyst that used water difficult to degradate handles is following:
(1) active carbon being placed mass percent concentration is 0.5～25% salpeter solution activation, reacts 1～5 hour down at 90～100 ℃, through filtration, cleaning, oven dry, obtains catalyst carrier;
(2) catalyst carrier is placed reactor; Adding and containing the quality percentage composition is several kinds of soluble-salt solution among 0.5～10%Cu, 0.5～10%Mn, 0.5～10%Fe, 0.05～5%V, 0.1～5%Ni, 0.1～5%Ce, 0.1～5%Co, 0.05～5%Zn, 0.05～5%Zr, 0.05～5%Ti, the 0.05～5%Cr, floods 12～24 hours;
(3) precipitating reagent is added reactor, reacted 6～12 hours, through after filtration, cleaning 100～115 ℃ dry 8～12 hours down, at last 300～500 ℃ of following activation 3～6 hours, obtain catalyst.
Described precipitating reagent is urea, NH
3H
2O, NaHCO
3Or KOH.
Through embodiment the present invention is further specified below.
Embodiment 1
1) 0.5% salpeter solution is joined in the active carbon, 100 ℃ of reactions 5 hours, through filtration, clean, oven dry, obtain catalyst carrier;
2) catalyst carrier is placed reactor; Add and contain the soluble-salt solution that the quality percentage composition is 5%Cu, 5%Mn, 5%Fe, 0.05%V, 0.1%Ni, 0.1%Ce, 0.1%Co, 0.05% Zn, 0.05%Zr, 0.05%Ti, 0.05%Cr; Flooded 24 hours; Add ammoniacal liquor again, reaction 12 was as a child taken out active carbon, through filtration, clean, 100 ℃ dry 12 hours down; At 300 ℃ of temperature lower calcination 6h hours, obtain being used for the catalyst of catalytic oxidation treatment organic wastewater with difficult degradation thereby again.
The catalyst oxidation processes organic additive factory waste water that makes
COD value of waste water is 6452.4mg/L, mainly contains cyanic acid benzyl chloride, tricresyl phosphite second fat, terephthalaldehyde, DMF, Cyanuric Chloride etc.Waste water transfers to 3.5 with sour pH value with waste water earlier; With peristaltic pump waste water is squeezed in the reactor then, the control flow is 100 ml/h, in reactor, adds catalyst and oxidant (containing hydrogen peroxidase 10 .1ml/L) simultaneously; The bubbling air aeration; The catalytic reaction certain hour, after the present invention's processing, the COD clearance is 73.8%.
Embodiment 2
1)) 25% salpeter solution is joined in the active carbon, 90 ℃ of reactions 1 hour, through filtration, clean, oven dry, obtain catalyst carrier;
2) catalyst carrier is placed reactor, add and contain the soluble-salt solution that the quality percentage composition is 10%Cu, 10%Mn, 10%Fe, 2%V, 2%Ni, 2%Cer, flooded 12 hours; Urea is added reactor, reacted 6 hours, through after filtration, cleaning 115 ℃ dry 8 hours down, at last 500 ℃ of following activation 3～6 hours, obtain catalyst.
The catalyst oxidation processes Organic Chemical Plant waste water that makes
Organic Chemical Plant's COD value of waste water is 5674mg/L, mainly contains cyanic acid benzyl chloride, monoethanolamine, DSD acid, DMF, Cyanuric Chloride etc.Transfer to 3.5 with sour pH value earlier with waste water; With peristaltic pump waste water is squeezed in the reactor then, the control flow is 800ml/h, in reactor, adds catalyst and oxidant (containing hydrogen peroxidase 10 .1ml/L) simultaneously; The bubbling air aeration; The catalytic reaction certain hour, after the present invention's processing, the COD clearance is 72.2%.
Embodiment 3
1) 15% salpeter solution is joined in the active carbon, 100 ℃ of reactions 5 hours, through filtration, clean, oven dry, obtain catalyst carrier;
2) catalyst carrier is placed reactor; Add and contain the soluble-salt solution that the quality percentage composition is 0.5%Cu, 0.5%Mn, 0.5%Fe, 5%Co, 5% Zn, 5%Zr, 5%Ti, 5%Cr, flooded 24 hours, add KOH again; Active carbon was as a child taken out in reaction 12; Through filtration, clean, 100 ℃ dry 12 hours down, again at 350 ℃ of temperature lower calcination 4h hours, obtain being used for catalyst.
The catalyst method for oxidation that makes is handled Chemical Manufacture waste water
Chemical Manufacture factory composite waste COD value is 18677.3mg/L, mainly contains a large amount of phenolic compounds, halogenated aliphatic compound, aromatic hydrocarbon, halogenated aromatic compound etc.Waste water transfers to 4 with sour pH value with waste water earlier; With peristaltic pump it is squeezed in the reactor then, the control flow is 500ml/h, in reactor, adds catalyst and oxidant (containing hydrogen peroxidase 10 .5ml/L) simultaneously; Bubbling air; The catalytic reaction certain hour, after the present invention's processing, the COD clearance is 63.7%.
Embodiment 4
1) 20% salpeter solution is joined in the active carbon, 100 ℃ of reactions 3 hours, through filtration, clean, oven dry, obtain catalyst carrier;
2) catalyst carrier is placed reactor; Add and contain the soluble-salt solution that the quality percentage composition is 7%Cu, 7%Mn, 7%Fe, 5%V, 5%Ni, 5%Ce, flooded 24 hours, add ammoniacal liquor again; Active carbon was as a child taken out in reaction 12; Through filtration, clean, 100 ℃ dry 12 hours down, again at 350 ℃ of temperature lower calcination 4h hours, obtain being used for the catalyst of catalytic oxidation treatment organic wastewater with difficult degradation thereby.The catalyst method for oxidation that makes is handled Chemical Manufacture waste water
The former water COD of chemical plant factory effluent value is 5718.7mg/L, mainly contains a large amount of nitrated aromatics, heteroaromatic compounds, cyanogen, acid imide etc.COD value of waste water reaches 2197.1mg/L after the preliminary biochemical treatment, then the waste water after the biochemical treatment is transferred to 3.5 with acid with the pH value, with peristaltic pump it is squeezed in the reactor then; The control flow is 500ml/h; In reactor, add catalyst and oxidant (containing hydrogen peroxidase 10 .6ml/L), bubbling air aeration, catalytic reaction certain hour simultaneously; After the present invention's processing, the COD clearance is 78.4%.
Embodiment 5
1) 20% salpeter solution is joined in the active carbon, 100 ℃ of reactions 2 hours, through filtration, clean, oven dry, obtain catalyst carrier;
2) catalyst carrier is placed reactor, add and contain the soluble-salt solution that the quality percentage composition is 5%Cu, 5%Fe, 0.2%V, 5%Ni, 4%Ce, flooded 24 hours, add NaHCO again
3, reaction 12 was as a child taken out active carbon, through filtration, clean, 100 ℃ dry 12 hours down, again at 400 ℃ of temperature lower calcination 4h hours, obtain being used for the catalyst of catalytic oxidation treatment organic wastewater with difficult degradation thereby.
The catalyst method for oxidation that makes is handled Chemical Manufacture waste water, and Chemical Manufacture factory composite waste COD value is 18677.3mg/L, mainly contains a large amount of phenolic compounds, halogenated aliphatic compound, aromatic hydrocarbon, halogenated aromatic compound etc.Waste water transfers to 4 with sour pH value with waste water earlier; With peristaltic pump it is squeezed in the reactor then, the control flow is 500ml/h, in reactor, adds catalyst and oxidant (containing hydrogen peroxidase 10 .5ml/L) simultaneously; Bubbling air; The catalytic reaction certain hour, after the present invention's processing, the COD clearance is 63.7%.
Embodiment 6
Step by embodiment 4 prepares; Just in dipping process, adjust component; Adding and containing the quality percentage composition is that other operations of soluble-salt solution of 5%Cu, 5%Fe, 0.2%V, 5%Ni, 4%Ce are all undertaken by embodiment 4, obtains being used for the catalyst of treating high-concentration organic wastewater through catalytic oxidation.
The catalyst method for oxidation that makes is handled Chemical Manufacture waste water, and sewage quality is identical with embodiment 4, and the catalytic reaction process peace is carried out according to embodiment 4, and the COD clearance is 88.7%.
Embodiment 7
Step by embodiment 4 prepares; Just in dipping process, adjust component; Adding and containing the quality percentage composition is that other operations of soluble-salt solution of 2%Cu, 2%Mn, 2%Fe, 2%Ce, 0.5%Co, 0.5% Zn are all undertaken by embodiment 4, obtains being used for the catalyst of treating high-concentration organic wastewater through catalytic oxidation.
The catalyst method for oxidation that makes is handled Chemical Manufacture waste water, and sewage quality is identical with embodiment 4, and the catalytic reaction process peace is carried out according to embodiment 4, and the COD clearance is 68.2%.
Embodiment 8
Step by embodiment 4 prepares; Just in dipping process, adjust component; Adding and containing the quality percentage composition is that other operations of soluble-salt solution of 8%Cu, 4%Mn, 8%Fe, 2%Ni, 2%Ce, 0.5%Cr are all undertaken by embodiment 4, obtains being used for the catalyst of treating high-concentration organic wastewater through catalytic oxidation.The catalyst method for oxidation that makes is handled Chemical Manufacture waste water, and sewage quality is identical with embodiment 4, and the catalytic reaction process peace is carried out according to embodiment 4, and the COD clearance is 75.8%.
Embodiment 9
Step by embodiment 4 prepares; Just in dipping process, adjust component; Adding and containing the quality percentage composition is that other operations of soluble-salt solution of 4%Cu, 4%Mn, 4%Fe, 0.5%Co, 0.5% Zn, 0.5%Zr, 0.5%Ti are all undertaken by embodiment 4, obtains being used for the catalyst of treating high-concentration organic wastewater through catalytic oxidation.
The catalyst method for oxidation that makes is handled Chemical Manufacture waste water, and sewage quality is identical with embodiment 4, and the catalytic reaction process peace is carried out according to embodiment 4, and the COD clearance is 63.8%.
Embodiment 10
Step by embodiment 4 prepares; Just in dipping process, adjust component; Add contain the quality percentage composition be 8%Cu, 4%Mn, 8%Fe, 0.2%V, 4%Ni, 1%Ce, 0.5%Ti, 0.5%Cr, other operations of soluble-salt solution all undertaken by embodiment 4, obtain being used for the catalyst of treating high-concentration organic wastewater through catalytic oxidation.
The catalyst method for oxidation that makes is handled Chemical Manufacture waste water, and sewage quality is identical with embodiment 4, and the catalytic reaction process peace is carried out according to embodiment 4, and the COD clearance is 72.1%.
Claims (4)
1. one kind is used for the catalyst that used water difficult to degradate is handled, and it is characterized in that in the component of quality percentage composition catalyst being:
(1) active carbon content accounts for 80～95% of catalyst total content;
(2) active component: Cu: content accounts for 0.5～10% of catalyst total content;
Mn: content accounts for 0.5～10% of catalyst total content;
Fe: content accounts for 0.5～10% of catalyst total content;
(3) co-catalyst: V: content accounts for 0.05～5% of catalyst total content;
Ni: content accounts for 0.1～5% of catalyst total content;
Ce: content accounts for 0.1～5% of catalyst total content;
Co: content accounts for 0.1～5% of catalyst total content;
Zn: content accounts for 0.05～5% of catalyst total content;
Zr: content accounts for 0.05～5% of catalyst total content;
Ti: content accounts for 0.05～5% of catalyst total content;
Cr: content accounts for 0.05～5% of catalyst total content.
2. a kind of used water difficult to degradate that is used for as claimed in claim 1 is handled catalyst, and it is characterized in that: the soluble-salt of described active component and co-catalyst is nitrate, acetate, sulfate or ammonium salt.
3. one kind is used for the method for preparing catalyst that used water difficult to degradate is handled according to claim 1, it is characterized in that its step is following:
(1) active carbon being placed mass percent concentration is 0.5～25% salpeter solution activation, reacts 1～5 hour down at 90～100 ℃, through filtration, cleaning, oven dry, obtains catalyst carrier;
(2) catalyst carrier is placed reactor; Adding and containing the quality percentage composition is several kinds of soluble-salt solution among 0.5～10%Cu, 0.5～10%Mn, 0.5～10%Fe, 0.05～5%V, 0.1～5%Ni, 0.1～5%Ce, 0.1～5%Co, 0.05～5%Zn, 0.05～5%Zr, 0.05～5%Ti, the 0.05～5%Cr, floods 12～24 hours;
(3) precipitating reagent is added reactor, reacted 6～12 hours, through after filtration, cleaning 100～115 ℃ dry 8～12 hours down, at last 300～500 ℃ of following activation 3～6 hours, obtain catalyst.
4. a kind of used water difficult to degradate that is used for as claimed in claim 3 is handled the Preparation of catalysts method, and it is characterized in that: described precipitating reagent is urea, NH
3H
2O, NaHCO
3Or KOH.
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| CN104923238A (en) * | 2015-05-25 | 2015-09-23 | 北京铸盟科技有限公司 | Oxidization catalyst used for advanced oxidation, preparation method thereof and application thereof |
| CN105363465A (en) * | 2015-07-07 | 2016-03-02 | 博天环境集团股份有限公司 | Preparation method of ozone oxidation catalyst loaded with polymetallic oxide |
| 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 |
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| CN106345485B (en) * | 2016-08-25 | 2018-12-07 | 万华化学集团股份有限公司 | A kind of catalyst and its preparation method and application for catalytic oxidation treatment organic wastewater |
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| CN111203179A (en) * | 2020-01-15 | 2020-05-29 | 清创人和生态工程技术有限公司 | Preparation method and application of renewable phenol-containing organic wastewater catalytic adsorption material |
| CN113856691A (en) * | 2021-09-27 | 2021-12-31 | 金风环保有限公司 | Ozone catalyst and preparation method thereof |
| CN113856691B (en) * | 2021-09-27 | 2024-05-14 | 达斯玛环境科技（北京）有限公司 | Ozone catalyst and preparation method thereof |
| CN114453007A (en) * | 2022-02-23 | 2022-05-10 | 南京合一环境集团有限公司 | Preparation and application method of Ce-Zr/molecular sieve Fenton heterogeneous catalyst |
| CN117065759A (en) * | 2023-05-12 | 2023-11-17 | 扬州优境环境工程有限公司 | Activated carbon supported metal catalyst for treating industrial wastewater or waste gas and preparation method thereof |
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