CN106000380A - Activated carbon-loaded nano-zinc oxide ozonation catalyst and preparation and use thereof - Google Patents
Activated carbon-loaded nano-zinc oxide ozonation catalyst and preparation and use thereof Download PDFInfo
- Publication number
- CN106000380A CN106000380A CN201610340041.4A CN201610340041A CN106000380A CN 106000380 A CN106000380 A CN 106000380A CN 201610340041 A CN201610340041 A CN 201610340041A CN 106000380 A CN106000380 A CN 106000380A
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- China
- Prior art keywords
- activated carbon
- zine oxide
- nano zine
- oxidation catalyst
- catalyst
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Classifications
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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
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- 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 relates to an activated carbon-loaded nano-zinc oxide ozonation catalyst and preparation and use thereof. The catalyst is prepared by loading nano-zinc oxide on the surface of modified activated carbon. The modified activated carbon carrier is prepared by cleaning activated carbon with a sodium hydroxide solution, then dipping with dilute nitric acid, cleaning with deionized water and then drying. According to the catalyst disclosed by the invention, active components are prepared by adopting a coprecipitation method and taking zinc nitrate as a precursor; zinc hydroxide precipitate is generated by using a saturated zinc nitrate solution and a saturated urine solution and is attached to the surface of the modified activated carbon, and then the activated carbon the surface of which is attached with the zinc hydroxide is dried and roasted to prepare the oxidization catalyst. That is, the adsorption property of the activated carbon is reserved, and nano-zinc oxide microparticles having ozone catalysis activity are loaded in the activated carbon. Under the synergistic effect of adsorption and activation, organic pollutants in water can be adsorbed at high efficiency, and meanwhile, ozone molecules can be catalyzed and activated to produce free radicals having high oxidizability, thereby obtaining a better catalytic ozonation effect.
Description
Technical field:
The present invention relates to the ozone catalyst field for sewage disposal.
Background technology:
At present, sanitary sewage and the kind of industrial wastewater and discharge capacity are increasing, and composition is more complicated, and it is many difficult wherein to contain
Degradation of organic substances, such as dyestuff, phenol, phenol, pesticide, Polychlorinated biphenyls, polycyclic aromatic hydrocarbon, Nitro-aromatic Compounds in Different, benzene sulfonamide
Acid and humic acid etc..These hardly degraded organic substances use traditional ozonation technology to be difficult to remove.Although ozonation technology exists
Application during water processes is quite varied, also shows that incomparable superiority, but it there is also certain limitation, and one is ozone
Utilization ratio the highest, add that the incurred cost of ozone is high, cause ozone to process costly；But it is as people and manufactures smelly
The raising of oxygen level, the problem that the incurred cost of ozone is high is the most constantly overcome, and oneself has document announcement to show, than routine
Water treatment technology, ozone processing unit operating cost is lower；Two is that ozone has stronger selectivity with organic reaction.Institute
To improve the utilization ratio of ozone the most further and oxidability is the research emphasis of ozonation technology.O3 catalytic oxidation is
Advanced oxidation processes based on ozone, is i.e. converted into the hydroxyl that oxidisability is higher and selectivity is low by adding catalyst by ozone catalytic
Those can be difficult to the oxidation operation individually aoxidizing with ozone or degrading by base free radical, be greatly improved ozone utilization ratio and
Oxidability.
Catalytic ozonation is strong oxidizing property and the absorption of catalyst, the catalysis characteristics of ozone to be combined, and can more have
Effect ground solves the hardly degraded organic substance incomplete problem of degraded.Absorption and catalyzing cooperation effect, can organic dirt in efficient absorption water
Dye thing, simultaneously the most again can catalytic activation ozone molecule, produce the free radical of high oxidative, in the suction of catalyst surface organic pollution
Echo the catalysis synergism of oxidant, more preferable O3 catalytic oxidation effect can be obtained.
Chinese patent ZL201010229998 discloses a kind of ozonization water treatment method using nano zine oxide as catalyst, and it is to adopt
React with zinc acetate and ammonia and generate white precipitate, white precipitate is cleaned, dry and within 2 hours, obtains 150～300 DEG C of calcinings
Nano zinc oxide material.Then nano zine oxide is joined in ozone oxidation water treatment system as catalyst, starts stirring,
It is passed through ozone, starts organic pollutants of degrading；Ozonation treatment is complete, by standing, be centrifuged or filtering, by nano oxygen
Change zinc to separate, for catalytic process next time.This method there is problems in that (1) this method can be only applied to intermittent
Sewage disposal system；(2) catalyst easily runs off, and causes treatment effect gradually to weaken；(3) zinc oxide catalyst return
Sequence of knocking off is loaded down with trivial details, and operability is the strongest.Another kind of patent ZL201110399282 discloses a kind of using nano ceric oxide as urging
The ozonization water treatment method of agent, by trivalent cerium ion (Ce3+) chemical precipitation under alkaline environment, in air atmosphere under forge
Burning obtains nano ceric oxide sample.The nano ceric oxide sample obtained is joined ozonization water treatment system as catalyst
In, it is passed through ozone, starts stirring, degraded organic pollutants simultaneously；Ozonation treatment is complete, by standing, centrifugal or
Filter, nano ceric oxide sample is separated from aqueous solution, for catalytic process next time.This method and patent
ZL201010229998 is the same, equally exists identical defect.
Summary of the invention:
The technical problem to be solved in the present invention is: after (1) uses activated carbon supported nano zine oxide as catalyst, it is to avoid catalysis
The loss of agent；(2) Supported On Granular Activated Carbon nano zine oxide can apply to the sewage disposal system of continuous processing, and without numerous
Trivial catalyst recovery process.
The preparation method of the present invention activated carbon supported nano zine oxide ozone oxidation catalyst, is to be received by granular active carbon area load
Rice zinc oxide forms.
The preparation method of described activated carbon supported nano zine oxide ozone oxidation catalyst, by granular active carbon with 5～10% hydrogen-oxygen
Change sodium solution to soak after 12～24 hours, clean with distilled water no longer changing to pH value, the most again with 5～10% nitric acid soak
Steep 3～5 hours, then clean with distilled water, dry at a temperature of 80 DEG C～100 DEG C and obtain Pre-Treatment of Activated charcoal；Pretreatment is lived
Property after charcoal mixes with saturated zinc nitrate solution and saturated urea liquid, stirring reaction 6～8 hours under slight fever, product is passed through
Repeatedly after washing, dry 6～10 hours at 80 DEG C～100 DEG C；Dry product roasting under 400 DEG C～600 DEG C and nitrogen atmosphere
3～6 hours prepared end product activated carbon supported nano zine oxide ozone oxidation catalysts.
A kind of activated carbon supported nano zine oxide ozone oxidation catalyst, is prepared by said method.
Described granular active carbon particle diameter is 2～3mm, specific surface area is 1000～1500m2/g。
Described nano zine oxide is to be reacted the zinc hydroxide pyrolysis prepared to form by zinc nitrate saturated solution and urea liquid.
Described zinc nitrate is 1:1～1:3 with the ratio of the amount of carbamide material.
Described urea concentration is 10%～20%.
Described zinc nitrate and quality of activated carbon are than for 1:1～1:3.
The using method of described activated carbon supported nano zine oxide ozone oxidation catalyst, can be individually used for water and process, it is possible to it
He is combined method；Under conditions of not being passed through ozone, also can be used as common adsorbent and use.
The present invention i.e. remains the characterization of adsorption of activated carbon, has loaded again the nano oxygen possessing ozone catalytic activity in this activated carbon
Change zinc microgranule.Under absorption and activation synergism, energy efficient absorption organic pollutants, simultaneously again can catalytic activation ozone
Molecule, produces the free radical of high oxidative, obtains more preferable O3 catalytic oxidation effect.
Accompanying drawing illustrates:
Fig. 1 is the technological process block-diagram of the present invention.
Detailed description of the invention:
Embodiment 1:
Weigh 600g zinc nitrate, be configured to saturated solution；Weigh 350g carbamide, be dissolved in 3150g distilled water；Choose 2～
The activated carbon granule of 3mm soaks 12 hours with the sodium hydroxide solution of 10%, no longer changes to cleanout fluid pH value with distilled water cleaning
Till, then 10% nitric acid dousing 3 hours, then clean with distilled water, dry for standby.First Pre-Treatment of Activated after drying
Charcoal granule adds in above-mentioned zinc nitrate solution, is heated to 400C, then limit adds the urea liquid limit stirring prepared and reacts 8 hours.
Reacted product is by filtering, wash, sending into muffle furnace after drying, and in 6000C environment, roasting 3 is little under nitrogen atmosphere
Time prepare finished catalyst.
Embodiment 2:
Weigh 300g zinc nitrate, be configured to saturated solution；Weigh 200g carbamide, be dissolved in 800g distilled water；Choose 2～
The activated carbon granule of 3mm soaks 20 hours with the sodium hydroxide solution of 5%, no longer changes to cleanout fluid pH value with distilled water cleaning
Till, then 10% nitric acid dousing 4 hours, then clean with distilled water, dry for standby.First Pre-Treatment of Activated after drying
Charcoal granule adds in above-mentioned zinc nitrate solution, is heated to 500C, then limit adds the urea liquid limit stirring prepared and reacts 6 hours.
Reacted product is by filtering, wash, sending into muffle furnace after drying, and in 5000C environment, roasting 3 is little under nitrogen atmosphere
Time prepare finished catalyst.
Embodiment 3:
Weigh 900g zinc nitrate, be configured to saturated solution；Weigh 600g carbamide, be dissolved in 2400g distilled water；Choose 2～
The activated carbon granule of 3mm soaks 16 hours with the sodium hydroxide solution of 10%, no longer changes to cleanout fluid pH value with distilled water cleaning
Till, then 8% nitric acid dousing 5 hours, then clean with distilled water, dry for standby.First the Pre-Treatment of Activated charcoal after drying
Granule adds in above-mentioned zinc nitrate solution, is heated to 400C, then limit adds the urea liquid limit stirring prepared and reacts 8 hours.Instead
Product after should is by filtering, wash, sending into muffle furnace, under nitrogen atmosphere roasting 4 hours in 6000C environment after drying
Prepare finished catalyst.
Embodiment 4:
Weigh 500g zinc nitrate, be configured to saturated solution；Weigh 300g carbamide, be dissolved in 2700g distilled water；Choose 2～
The activated carbon granule of 3mm soaks 12 hours with the sodium hydroxide solution of 8%, no longer changes to cleanout fluid pH value with distilled water cleaning
Till, then 5% nitric acid dousing 5 hours, then clean with distilled water, dry for standby.First the Pre-Treatment of Activated charcoal after drying
Granule adds in above-mentioned zinc nitrate solution, is heated to 400C, then limit adds the urea liquid limit stirring prepared and reacts 8 hours.Instead
Product after should is by filtering, wash, sending into muffle furnace, under nitrogen atmosphere roasting 6 hours in 4500C environment after drying
Prepare finished catalyst.
Embodiment 5
The catalyst that embodiment 4 prepares is for certain Mechanical Processing Industry garden sewage disposal, and this sewage by COD after pretreatment is
138mg/L, using the COD after ozone advanced treating before not adding catalyst is 107.6mg/L.After adding catalyst,
Under equal ozone dosage, COD reduces to 73.8mg/L, and treatment effeciency improves 24.5%.
Activated carbon supported nano zine oxide ozone oxidation catalyst in above-described embodiment is to add to carry out ozone to ozone reaction device and urge
Change oxidation.This ozone reaction device is to be made by the U-PVC pipe of diameter 110mm, high 2 meters.Device by ozone air dispelling device,
Pre-reaction zone, catalyst contact area and rear reaction zone composition.Sewage is entered by reaction unit top, sequentially pass through pre-reaction zone,
By lower end water outlet behind catalyst contact area and rear reaction zone.Ozone is entered by bottom reaction unit, is uniformly expanded by ozone air dispelling device
Dissipating, after being fully contacted reaction with sewage, tail gas is discharged from upper end.The tail gas that Practical Project is discharged in using need to destroy through tail gas
High altitude discharge after device decomposition, has prevented ozone effusion from polluting.
Claims (9)
1. the preparation method of an activated carbon supported nano zine oxide ozone oxidation catalyst, it is characterised in that this catalyst
It is to be formed by granular active carbon area load nano zine oxide.
2. a preparation method for activated carbon supported nano zine oxide ozone oxidation catalyst as claimed in claim 1, its
Be characterised by, by granular active carbon with 5～10% sodium hydroxide solution soak after 12～24 hours, clean to PH with distilled water
Till value no longer change, the most again with 5～10% nitric acid dousing 3～5 hours more clean with distilled water, at 80 DEG C～100 DEG C
At a temperature of dry obtain Pre-Treatment of Activated charcoal；Pre-Treatment of Activated charcoal is mixed with saturated zinc nitrate solution and saturated urea liquid
After, under slight fever stirring reaction 6～8 hours, product through repeatedly washing after, at 80 DEG C～100 DEG C dry 6～
10 hours；Dry product roasting 3～6 hours prepared end products under 400 DEG C～600 DEG C and nitrogen atmosphere activated carbon supported
Nano zine oxide ozone oxidation catalyst.
3. a preparation method for activated carbon supported nano zine oxide ozone oxidation catalyst as claimed in claim 2, its
Being characterised by, described granular active carbon particle diameter is 2～3mm, specific surface area is 1000～1500m2/g。
4. a preparation method for activated carbon supported nano zine oxide ozone oxidation catalyst as claimed in claim 2, its
Being characterised by, nano zine oxide is to be reacted the zinc hydroxide pyrolysis prepared to form by zinc nitrate saturated solution and urea liquid.
5. an activated carbon supported nano zine oxide ozone oxidation catalyst as claimed in claim 4, it is characterised in that nitric acid
Zinc is 1:1～1:3 with the ratio of the amount of carbamide material.
6. an activated carbon supported nano zine oxide ozone oxidation catalyst as claimed in claim 4, it is characterised in that carbamide
Solution concentration is 10%～20%.
7. an activated carbon supported nano zine oxide ozone oxidation catalyst as claimed in claim 2, it is characterised in that nitric acid
Zinc and quality of activated carbon are than for 1:1～1:3.
8. an activated carbon supported nano zine oxide ozone oxidation catalyst, is prepared by method described in claim 1.
9. a using method for activated carbon supported nano zine oxide ozone oxidation catalyst according to claim 1,
It is characterized in that, it is possible to be individually used for water and process, or be combined with additive method；Under conditions of not being passed through ozone, as
Common adsorbent uses.
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| CN201610340041.4A CN106000380A (en) | 2016-05-19 | 2016-05-19 | Activated carbon-loaded nano-zinc oxide ozonation catalyst and preparation and use thereof |
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| CN201610340041.4A CN106000380A (en) | 2016-05-19 | 2016-05-19 | Activated carbon-loaded nano-zinc oxide ozonation catalyst and preparation and use thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107876062A (en) * | 2017-11-06 | 2018-04-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Ozone catalyst preparation method and products thereof and application |
| CN108545823A (en) * | 2018-03-12 | 2018-09-18 | 江苏蓝必盛化工环保股份有限公司 | A kind of bio-carrier charcoal and preparation method thereof containing various trace elements |
| CN108927212A (en) * | 2017-05-22 | 2018-12-04 | 暨南大学 | For controlling the iron silver oxide zeolite catalyst that bromate generates during ozone oxidation |
| CN109319850A (en) * | 2018-09-21 | 2019-02-12 | 广东工业大学 | A kind of preparation method of the composite modified filtrate of graphene-based-iron chloride and its modified filter material of preparation |
| CN109499563A (en) * | 2017-09-15 | 2019-03-22 | 张家港市沐和新材料技术开发有限公司 | A kind of preparation method of zinc oxide-active carbon composite catalyst |
| CN111659376A (en) * | 2020-06-05 | 2020-09-15 | 北京化工大学 | Preparation method of ozone catalytic oxidation catalyst and ozone catalytic oxidation catalyst prepared by same |
| CN112323304A (en) * | 2020-11-06 | 2021-02-05 | 江苏泰慕士针纺科技股份有限公司 | Zero-emission pretreatment process for cotton knitted fabric |
| CN112657463A (en) * | 2020-11-13 | 2021-04-16 | 深圳市净万嘉环保科技有限公司 | Manganese-zinc-carbon composite material and preparation method thereof |
| CN113262787A (en) * | 2021-05-27 | 2021-08-17 | 煤炭科学技术研究院有限公司 | Preparation method of iron-based composite catalyst for catalytic ozonation treatment of coal chemical wastewater |
| CN114632525A (en) * | 2022-05-18 | 2022-06-17 | 中国环境科学研究院 | Petrochemical wastewater treatment method based on heterogeneous catalytic ozonation |
| CN114797890A (en) * | 2022-04-22 | 2022-07-29 | 浙江大学 | High-stability ortho-position bifunctional catalyst and preparation method and application thereof |
| CN114804906A (en) * | 2022-05-27 | 2022-07-29 | 陕西美兰德炭素有限责任公司 | High-purity carbon/carbon composite material and preparation method and application thereof |
| CN114917908A (en) * | 2022-04-21 | 2022-08-19 | 山东亮剑环保新材料有限公司 | Preparation method of supported modified activated carbon ozone catalyst |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108927212A (en) * | 2017-05-22 | 2018-12-04 | 暨南大学 | For controlling the iron silver oxide zeolite catalyst that bromate generates during ozone oxidation |
| CN109499563A (en) * | 2017-09-15 | 2019-03-22 | 张家港市沐和新材料技术开发有限公司 | A kind of preparation method of zinc oxide-active carbon composite catalyst |
| CN107876062A (en) * | 2017-11-06 | 2018-04-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Ozone catalyst preparation method and products thereof and application |
| CN108545823A (en) * | 2018-03-12 | 2018-09-18 | 江苏蓝必盛化工环保股份有限公司 | A kind of bio-carrier charcoal and preparation method thereof containing various trace elements |
| CN109319850A (en) * | 2018-09-21 | 2019-02-12 | 广东工业大学 | A kind of preparation method of the composite modified filtrate of graphene-based-iron chloride and its modified filter material of preparation |
| CN109319850B (en) * | 2018-09-21 | 2022-02-11 | 广东工业大学 | Graphene-based iron chloride composite modified filter material and preparation method and application thereof |
| CN111659376B (en) * | 2020-06-05 | 2021-05-04 | 北京化工大学 | Preparation method of ozone catalytic oxidation catalyst and ozone catalytic oxidation catalyst prepared by same |
| CN111659376A (en) * | 2020-06-05 | 2020-09-15 | 北京化工大学 | Preparation method of ozone catalytic oxidation catalyst and ozone catalytic oxidation catalyst prepared by same |
| CN112323304A (en) * | 2020-11-06 | 2021-02-05 | 江苏泰慕士针纺科技股份有限公司 | Zero-emission pretreatment process for cotton knitted fabric |
| CN112657463A (en) * | 2020-11-13 | 2021-04-16 | 深圳市净万嘉环保科技有限公司 | Manganese-zinc-carbon composite material and preparation method thereof |
| CN113262787A (en) * | 2021-05-27 | 2021-08-17 | 煤炭科学技术研究院有限公司 | Preparation method of iron-based composite catalyst for catalytic ozonation treatment of coal chemical wastewater |
| CN114917908A (en) * | 2022-04-21 | 2022-08-19 | 山东亮剑环保新材料有限公司 | Preparation method of supported modified activated carbon ozone catalyst |
| CN114797890A (en) * | 2022-04-22 | 2022-07-29 | 浙江大学 | High-stability ortho-position bifunctional catalyst and preparation method and application thereof |
| CN114632525A (en) * | 2022-05-18 | 2022-06-17 | 中国环境科学研究院 | Petrochemical wastewater treatment method based on heterogeneous catalytic ozonation |
| CN114632525B (en) * | 2022-05-18 | 2022-07-19 | 中国环境科学研究院 | Petrochemical wastewater treatment method based on heterogeneous catalytic ozonation |
| CN114804906A (en) * | 2022-05-27 | 2022-07-29 | 陕西美兰德炭素有限责任公司 | High-purity carbon/carbon composite material and preparation method and application thereof |
| CN114804906B (en) * | 2022-05-27 | 2023-02-14 | 陕西美兰德炭素有限责任公司 | High-purity carbon/carbon composite material and preparation method and application thereof |
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