CN105854900A - Catalytic wet oxidation catalyst applied to harmless treatment of ammonia-nitrogen wastewater and preparation method thereof - Google Patents
Catalytic wet oxidation catalyst applied to harmless treatment of ammonia-nitrogen wastewater and preparation method thereof Download PDFInfo
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- CN105854900A CN105854900A CN201610268998.2A CN201610268998A CN105854900A CN 105854900 A CN105854900 A CN 105854900A CN 201610268998 A CN201610268998 A CN 201610268998A CN 105854900 A CN105854900 A CN 105854900A
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- noble metal
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- sulfur
- wet oxidation
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
- B01J27/045—Platinum group metals
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Catalysts (AREA)
Abstract
The invention discloses a catalytic wet oxidation catalyst applied to harmless treatment of ammonia-nitrogen wastewater and a preparation method thereof. The catalytic wet oxidation catalyst comprises a supporter and an active component supported on the supporter, wherein the supporter is active carbon, and the active component is precious metal sulfide which comprises the following components in percentage by mass: 0.1%-5% of precious metal, 0.5%-8% of sulfur and the balance of active carbon, and the precious metal is Pt, Pd, Ru or Rh. The preparation method comprises the steps of preparing a charcoal supported precious metal catalyst via a chemical reduction method and preparing a charcoal supported precious metal sulfide catalyst via an impregnation method. Compared with a conventional supported precious metal catalyst, the catalytic wet oxidation catalyst has the advantage that the performance, especially the low-temperature performance, of the catalyst is improved greatly as the precious metal sulfide is taken as an active ingredient.
Description
Technical field
Present invention relates particularly to catalytic wet oxidation catalyst of a kind of harmless treatment ammonia nitrogen waste water and preparation method thereof.
Background technology
Ammonia nitrogen is one of major pollutants of causing the whole nation such as the Changjiang river, the Yellow River, Zhujiang River main river Drainage Water Quality to exceed standard, simultaneously
Result also in the water body in lake such as China Taihu Lake, Chaohu, Dian Chi and produce the eutrophication problem such as wawter bloom, cyanophyceae, the ammonia nitrogen of water body
Pollute to have become more than COD (COD) and affect the primary index of China's surface water quality of water environment.Depositing of ammonia nitrogen
Not only cause body eutrophication, causing black and odorous water, destruction water ecology balance, and increase life and water for industrial use
The mankind are even produced toxic action by the difficulty of pre-treatment and cost.Ammonia nitrogen reduces discharging and has become China's water pollution and continue COD
Section 2 binding character Con trolling index afterwards.
CWO technology (CWAO) is a kind of new technique administering waste water grown up the eighties in 20th century,
Under uniform temperature, pressure, with air (or oxygen) as oxidant, by catalyst effect, disposably by ammonia nitrogen
All transfer the nitrogen the most harmless to the mankind and environment to.With other materilization freatment methods (such as: blow-off method, ion exchange,
Absorption method, break point chlorination, chemical precipitation method etc.) compare, it is not necessary to consider ammonia nitrogen after-treatment problem, and will not be because adding
Chemical agent and introduce secondary pollution；Compared with wide variety of biological treatment, CWO technology the most energy-conservation and
Efficiently, and the ammonia nitrogen waste water of high, medium and low variable concentrations be can effectively process, Low Concentration Ammonia Containing Wastewater and biology are especially suitable for
The reluctant poisonous ammonia nitrogen waste water of method, thus economically and technically have more competitive advantage.
CWO processes the core of ammonia nitrogen waste water technology and is suitable catalyst.Although carried noble metal is catalyzed
Agent has and is preferably catalyzed activity, but its working condition still needs to High Temperature High Pressure.As conventional infusion process prepares Pt/TiO2Catalyst
Will under conditions of 200 DEG C and 3.6MPa, could effectively remove ammonia nitrogen in waste water (Applied Catalysis B:
Environmental,2012,128:64-71).RuPd/CeO prepared by co-impregnation2Catalyst is at 200 DEG C and 2.0MPa
Reaction condition, there is good ammonia nitrogen removal performance (Topics in Catalysis, 2005,33:77-86).Base metal is urged
Agent has more preferable economy, but its ammonia nitrogen catalyzed conversion activity is the lowest, even if in the condition of 230 DEG C He 2.0MPa
Under, the clearance of ammonia nitrogen the most only only has 20% (Water Research, 2004,38:778-782).
Summary of the invention
It is an object of the invention to overcome prior art defect, it is provided that the catalytic wet oxygen of a kind of harmless treatment ammonia nitrogen waste water
Change catalyst.
Another object of the present invention is to provide the preparation of the catalytic wet oxidation catalyst of above-mentioned harmless treatment ammonia nitrogen waste water
Method.
The concrete technical scheme of the present invention is as follows:
A kind of catalytic wet oxidation catalyst of harmless treatment ammonia nitrogen waste water, it is characterised in that:
It includes carrier and the active component being supported on carrier, and carrier is activated carbon, and active component is noble metal sulphide,
Its mass percent is: noble metal 0.1～5%, and sulfur is 0.5～8%, and surplus is activated carbon, wherein noble metal be Pt, Pd,
Ru or Rh；
Its suitable reaction pressure in oxygen or air is 0.1～5MPa, and suitable reaction temperature is 80～230 DEG C, described ammonia
Ammonia-nitrogen content in nitrogen waste water is 100～5000ppm；
Its preparation method includes that chemical reduction method prepares charcoal supported noble metal catalyst and infusion process prepares charcoal supported noble metal sulfur successively
Compound catalyst.
In a preferred embodiment of the invention, its mass percent is: noble metal 0.3～3%, and sulfur is 2～6%, remaining
Amount is activated carbon.
In a preferred embodiment of the invention, its suitable reaction temperature is 100～200 DEG C.
The preparation method of the catalytic wet oxidation catalyst of a kind of above-mentioned harmless treatment ammonia nitrogen waste water, comprises the steps:
(1) weighing each raw material components by mass percentage, each raw material components includes activated carbon, noble metal precursor body and sulfur；
(2) activated carbon is evenly spread in 0.1～0.5mM ammonia, adds isopyknic 1～5% hydrazine hydrate aqueous solution,
Be stirred for 1～3h, be subsequently adding the aqueous solution of noble metal precursor body and stir 6～12h, then sequentially pass through filter, washing and
Described charcoal supported noble metal catalyst is prepared after 50～150 DEG C of vacuum drying；
(3) sulfur is dissolved in CS2, it is subsequently adding above-mentioned charcoal supported noble metal catalyst, after standing 12～24h, in 100～250 DEG C
H2Middle roasting 2～4h, obtains described charcoal supported noble metal sulfide catalyst, is described harmless treatment ammonia nitrogen waste water
Catalytic wet oxidation catalyst.
In a preferred embodiment of the invention, described sulfur is Sublimed Sulfur.
In a preferred embodiment of the invention, described noble metal precursor body is PdCl2、H2PtCl6·6H2O、RuCl3
Or RhCl3·3H2O。
In a preferred embodiment of the invention, the dispersed of described step (1) is specially stirring and supersound process,
Mixing time is 20～40min, and sonication treatment time is 2.5～3.5h.
In a preferred embodiment of the invention, the vacuum drying temperature of described step (2) is 55～65 DEG C.
The invention has the beneficial effects as follows: the catalytic wet oxidation catalyst of the harmless treatment ammonia nitrogen waste water of the present invention is with conventional
Loaded noble metal catalyst is compared, owing to using noble metal sulphide as active component so that the performance of catalyst is (outstanding
It is cryogenic property) it is greatly promoted.
Detailed description of the invention
Below by way of detailed description of the invention technical scheme it is further detailed and describes.
The formula of catalyst prepared by following embodiment is M-S/C, during in formula, M represents precious metals pt, Pd, Ru, Rh
One.
Embodiment 1
(1) 0.5g activated carbon is joined ammonia (6mL NH3·H2O joins in 94mL deionized water, stirs 30min
Complete preparation) and ultrasonic 3h, add isopyknic 4% (percent by volume) hydrazine hydrate aqueous solution, be stirred for 3h, so
Rear addition 4.2ml 1g/500mL PdCl2Solution & stir 12h, after then sequentially passing through filter, washing and 60 DEG C of vacuum drying
Prepare Pd/C catalyst；
(2) 0.0040g Sublimed Sulfur is dissolved in 1.5mL CS2, it is subsequently adding 0.4g above-mentioned Pd/C catalyst, stands 12h
After, in the H of 200 DEG C2Middle roasting 4h, obtains Pd-S/C catalyst.
Examination condition: react in autoclave, catalyst amount 0.4g, ammonia-nitrogen content 2000ppm in waste water,
Reaction temperature 180 DEG C, reaction pressure 0.5MPa, react 4h.Na's reagent detection ammonia nitrogen, liquid chromatographic detection nitric acid
Salt, nitrite.Appraisal result is shown in Table 1.
Embodiment 2
By PdCl2Solution changes makees 6.6mL 1g/500mL H2PtCl6·6H2O solution, remaining is with embodiment 1, prepares Pt-S/C
Catalyst.Examination condition is with embodiment 1, and appraisal result is shown in Table 1.
Embodiment 3
By PdCl2Solution changes makees 5.2mL 1g/500mL RuCl3Solution, remaining is with embodiment 1, prepares Ru-S/C catalysis
Agent.Examination condition is with embodiment 1, and appraisal result is shown in Table 1.
Embodiment 4
By PdCl2Solution changes makees 6.4ml 1g/500mL RhCl3·3H2O solution, remaining is with embodiment 1, prepares Rh-S/C
Catalyst.Examination condition is with embodiment 1, and appraisal result is shown in Table 1.
The ammonia nitrogen catalyzed conversion performance of the catalyst obtained by table 1 embodiment 1 to 4
Embodiment 5
Reaction temperature in examination condition is changed 100 DEG C of work, and remaining is with embodiment 1, and appraisal result is shown in Table 2.
Embodiment 6
Reaction temperature in examination condition is changed 120 DEG C of work, and remaining is with embodiment 1, and appraisal result is shown in Table 2.
Embodiment 7
Reaction temperature in examination condition is changed 150 DEG C of work, and remaining is with embodiment 1, and appraisal result is shown in Table 2.
The impact on the ammonia nitrogen catalyzed conversion performance of Pd-S/C catalyst of table 2 reaction temperature
Comparative example 1～4
Only carry out the step (1) of embodiment 1, prepare Pd/C catalyst, the reaction temperature in examination condition is become respectively
100 DEG C, 120 DEG C, 150 DEG C and 180 DEG C, remaining examination condition is with embodiment 1, and appraisal result is shown in Table 3.
The impact on the ammonia nitrogen catalyzed conversion performance of Pd/C catalyst of table 3 reaction temperature
Those of ordinary skill in the art understand, when technical scheme change in following ranges, remain able to obtain and
The technique effect that above-described embodiment is same or like:
A kind of catalytic wet oxidation catalyst of harmless treatment ammonia nitrogen waste water,
It includes carrier and the active component being supported on carrier, and carrier is activated carbon, and active component is noble metal sulphide,
Its mass percent is: noble metal 0.1～5%, and sulfur is 0.5～8%, and surplus is activated carbon, wherein noble metal be Pt, Pd,
Ru or Rh, it is preferred that its mass percent is: noble metal 0.3～3%, sulfur is 2～6%, and surplus is activated carbon；
Its suitable reaction pressure in oxygen or air is 0.1～5MPa, and suitable reaction temperature is 80～230 DEG C, described ammonia
Ammonia-nitrogen content in nitrogen waste water is 100～5000ppm；
Its preparation method includes that chemical reduction method prepares charcoal supported noble metal catalyst and infusion process prepares charcoal supported noble metal sulfur successively
Compound catalyst.
Concrete preparation method is:
(1) weighing each raw material components by mass percentage, each raw material components includes activated carbon, noble metal precursor body and sulfur；
(2) activated carbon is evenly spread in 0.1～0.5mM ammonia, adds isopyknic 1～5% hydrazine hydrate aqueous solution,
Be stirred for 1～3h, be subsequently adding the aqueous solution of noble metal precursor body and stir 6～12h, then sequentially pass through filter, washing and
Described charcoal supported noble metal catalyst is prepared after 50～150 DEG C of vacuum drying；
(3) sulfur is dissolved in CS2, it is subsequently adding above-mentioned charcoal supported noble metal catalyst, after standing 12～24h, in 100～250 DEG C
H2Middle roasting 2～4h, obtains described charcoal supported noble metal sulfide catalyst, is described harmless treatment ammonia nitrogen waste water
Catalytic wet oxidation catalyst.
The above, only presently preferred embodiments of the present invention, therefore the scope that the present invention implements can not be limited according to this, i.e. depend on
The equivalence change that the scope of the claims of the present invention and description are made with modify, all should still belong in the range of the present invention contains.
Claims (8)
1. the catalytic wet oxidation catalyst of a harmless treatment ammonia nitrogen waste water, it is characterised in that:
It includes carrier and the active component being supported on carrier, and carrier is activated carbon, and active component is noble metal sulphide,
Its mass percent is: noble metal 0.1～5%, and sulfur is 0.5～8%, and surplus is activated carbon, wherein noble metal be Pt, Pd,
Ru or Rh；
Its suitable reaction pressure in oxygen or air is 0.1～5MPa, and suitable reaction temperature is 80～230 DEG C, described ammonia
Ammonia-nitrogen content in nitrogen waste water is 100～5000ppm；
Its preparation method includes that chemical reduction method prepares charcoal supported noble metal catalyst and infusion process prepares charcoal supported noble metal sulfur successively
Compound catalyst.
The catalytic wet oxidation catalyst of a kind of harmless treatment ammonia nitrogen waste water the most as claimed in claim 1, its feature exists
In: its mass percent is: noble metal 0.3～3%, and sulfur is 2～6%, and surplus is activated carbon.
The catalytic wet oxidation catalyst of a kind of harmless treatment ammonia nitrogen waste water the most as claimed in claim 1, its feature exists
In: its suitable reaction temperature is 100～200 DEG C.
4. the CWO of the harmless treatment ammonia nitrogen waste water as described in any claim in claims 1 to 3 is urged
The preparation method of agent, it is characterised in that: comprise the steps:
(1) weighing each raw material components by mass percentage, each raw material components includes activated carbon, noble metal precursor body and sulfur；
(2) activated carbon is evenly spread in 0.1～0.5mM ammonia, adds isopyknic 1～5% hydrazine hydrate aqueous solution,
Be stirred for 1～3h, be subsequently adding the aqueous solution of noble metal precursor body and stir 6～12h, then sequentially pass through filter, washing and
Described charcoal supported noble metal catalyst is prepared after 50～150 DEG C of vacuum drying；
(3) sulfur is dissolved in CS2, it is subsequently adding above-mentioned charcoal supported noble metal catalyst, after standing 12～24h, in 100～250 DEG C
H2Middle roasting 2～4h, obtains described charcoal supported noble metal sulfide catalyst, is described harmless treatment ammonia nitrogen waste water
Catalytic wet oxidation catalyst.
5. preparation method as claimed in claim 4, it is characterised in that: described sulfur is Sublimed Sulfur.
6. preparation method as claimed in claim 4, it is characterised in that: described noble metal precursor body is PdCl2、
H2PtCl6·6H2O、RuCl3Or RhCl3·3H2O。
7. preparation method as claimed in claim 4, it is characterised in that: dispersed specially the stirring of described step (1)
Mixing and stirring supersound process, mixing time is 20～40min, and sonication treatment time is 2.5～3.5h.
8. preparation method as claimed in claim 4, it is characterised in that: the vacuum drying temperature of described step (2) is
55～65 DEG C.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109775837A (en) * | 2019-01-21 | 2019-05-21 | 中石化上海工程有限公司 | The treatment by catalytic oxidation of nitrogen-containing wastewater |
| CN109796073A (en) * | 2019-01-21 | 2019-05-24 | 中石化上海工程有限公司 | Nitrogen-containing wastewater processing method |
| CN109867418A (en) * | 2019-04-12 | 2019-06-11 | 鲁东大学 | A kind of method for innocent treatment of the industrial wastewater containing brominated bisphenol-A |
| CN109908935A (en) * | 2019-02-19 | 2019-06-21 | 江苏海普功能材料有限公司 | A kind of Pt-Ru bimetal nano catalyst and preparation method thereof for organic wastewater with high concentration catalytic wet oxidation |
| CN112034027A (en) * | 2020-08-29 | 2020-12-04 | 南京航空航天大学 | Electrochemical sensing electrode for measuring ammonia nitrogen ions in wastewater and preparation method thereof |
| CN112387277A (en) * | 2020-12-11 | 2021-02-23 | 南京大学 | Method for catalytic hydrogenation reduction of algal toxins in water based on supported noble metal catalyst |
| CN112607924A (en) * | 2020-12-14 | 2021-04-06 | 浙江奇彩环境科技股份有限公司 | Method for removing total nitrogen from wastewater containing nitrogen organic matters |
| CN115970680A (en) * | 2022-12-28 | 2023-04-18 | 厦门大学 | Wet oxidation catalyst and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109775837A (en) * | 2019-01-21 | 2019-05-21 | 中石化上海工程有限公司 | The treatment by catalytic oxidation of nitrogen-containing wastewater |
| CN109796073A (en) * | 2019-01-21 | 2019-05-24 | 中石化上海工程有限公司 | Nitrogen-containing wastewater processing method |
| CN109908935A (en) * | 2019-02-19 | 2019-06-21 | 江苏海普功能材料有限公司 | A kind of Pt-Ru bimetal nano catalyst and preparation method thereof for organic wastewater with high concentration catalytic wet oxidation |
| CN109867418A (en) * | 2019-04-12 | 2019-06-11 | 鲁东大学 | A kind of method for innocent treatment of the industrial wastewater containing brominated bisphenol-A |
| CN112034027A (en) * | 2020-08-29 | 2020-12-04 | 南京航空航天大学 | Electrochemical sensing electrode for measuring ammonia nitrogen ions in wastewater and preparation method thereof |
| CN112034027B (en) * | 2020-08-29 | 2021-12-14 | 南京航空航天大学 | Electrochemical sensing electrode for measuring ammonia nitrogen ions in wastewater and preparation method thereof |
| CN112387277A (en) * | 2020-12-11 | 2021-02-23 | 南京大学 | Method for catalytic hydrogenation reduction of algal toxins in water based on supported noble metal catalyst |
| CN112607924A (en) * | 2020-12-14 | 2021-04-06 | 浙江奇彩环境科技股份有限公司 | Method for removing total nitrogen from wastewater containing nitrogen organic matters |
| CN115970680A (en) * | 2022-12-28 | 2023-04-18 | 厦门大学 | Wet oxidation catalyst and preparation method and application thereof |
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Application publication date: 20160817 |