CN101766999B - Nd2O3-ACF catalyst, preparation method and application - Google Patents

Nd2O3-ACF catalyst, preparation method and application Download PDF

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CN101766999B
CN101766999B CN 200910155904 CN200910155904A CN101766999B CN 101766999 B CN101766999 B CN 101766999B CN 200910155904 CN200910155904 CN 200910155904 CN 200910155904 A CN200910155904 A CN 200910155904A CN 101766999 B CN101766999 B CN 101766999B
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acf
catalyst
activated carbon
carbon fiber
waste gas
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宋爽
屠锦军
何志桥
杨岳平
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Zhejiang University of Technology ZJUT
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Abstract

The invention provides an Nd2O3-ACF catalyst, a preparation method and an application in treating dimethyldisulfide (C2H6S2) odor waste gas. The preparation method of the catalyst comprises the following steps of: preparing impregnation liquid by using activated carbon fibers (ACF) as carriers, neodymium nitrate as a precursor and water as a solvent; loading neodymium into the activated carbon fibers (ACF) by adopting an initial wet method and an immersion method; and roasting to obtain the Nd2O3-ACF catalyst. The invention has simple treatment process, low treatment cost and obvious effect on removing the odor waste gas and particularly the dimethyldisulfide, and has the characteristics of easy reaction control, easy operation, convenient maintenance, and the like, thus the invention is an effective method for treating odor organic waste gas of sewage treatment plants (stations) and has quite wide market development prospect.

Description

Nd 2O 3-ACF catalyst and preparation method and application
(1) technical field
The present invention relates to a kind of Nd 2O 3-ACF catalyst, and use Nd 2O 3-ACF catalyst coupling catalytic ozonation is processed DMDS (C 2H 6S 2) application of foul waste gas.
(2) background technology
The discharging of foul gas not only endangers ecological environment, and the infringement health.Odorant is by osmophore, stimulates olfactory cell as sulfenyl, carboxyl etc., makes the people feel to detest and unhappiness.A lot of odorants can cause human central nervous to produce obstacle, pathology, cause chronic disease and acute disease.The pollution sources multiaspect of foul gas is wide, relates to multiple industry.Due to the general lower and complicated component of concentration, and be difficult to administer.At present, with regard to sewage treatment plant's (station), the main generating source of its foul gas is aeration tank, grille well, storage basin, sludge concentration tank and sludge dewatering machine room etc., mainly comprises hydrogen sulfide (H 2S), methyl mercaptan (CH 3SH), ammonia (NH 3), methyl sulfide (C 2H 6S), DMDS (C 2H 6S 2), front three ammonia (C 3H 9Six kinds of compositions such as N).
Conventional rotten exhaust organic gas treatment process mainly contains: absorption process, Production by Catalytic Combustion Process, biological treatment, absorption method, oxidizing process, plasma method etc.Although these methods all can be used for the processing of rotten exhaust organic gas, certain application is also arranged on engineering, every kind of method all has certain limitation and the scope of application.For sewage treatment plant's (station) foul waste gas of low odor threshold, processing requirements is high, and difficulty is very big, adopts monotechnics to be difficult to reach processing requirements, needs to adopt coupling processing technique.Coupling technique commonly used has absorption/absorption method, biology/absorption method, absorption/oxidizing process etc.In these three kinds of coupling processing techniques, absorption/oxidizing process has obvious advantage for the processing of sewage treatment plant's (station) foul waste gas of low concentration.It is concentrated that absorption method is applicable to the enrichment of low concentration odorant pollutant, and oxidation rule can decompose pollutant more up hill and dale, has avoided the generation of secondary pollution, is therefore a kind of foul waste gas treatment technology that has application prospect.
It is adsorbent that present Chinese scholars mainly adopts active carbon to the research of absorption/oxidization combination technique, and oxidant mainly contains airborne oxygen and O 3Compare with active carbon, activated carbon fiber (ACF) has better absorption property, is a kind of more superior adsorbent, large several times to tens times than granular activated charcoal of its adsorption capacities, adsorption rate is exceedingly fast, and the rate of adsorption exceeds 2-3 the order of magnitude, and desorption rate is also very fast.In addition, in order further to improve ACF to the absorption property of extraordinary material, work out at present multiple method of modifying, introduced nitrogen-containing functional group, oxidation processes introducing oxygen-containing functional group, chemical vapour deposition (CVD) and carried metal etc. comprising heat treatment, ammonia treatment.But use Nd 2O 3Modified ACFs and and O 3Coupling (Nd 2O 3-ACF/O 3) the catalytic oxidation treatment odorant pollutant has no report.Nd 2O 3-ACF catalysis and O 3Oxidation technology can form cooperative effect, and ACF absorption has improved the reaction density of pollutant, Nd 2O 3Accelerated O as catalyst 3Decomposition produce OH.Pollution control to sewage treatment plant's (station) rotten exhaust organic gas has far-reaching theory significance and potential using value, and its technology is used the new trend that has represented absorption and high-level oxidation technology combined removal sewage treatment plant (station) rotten exhaust organic gas.
(3) summary of the invention
The present invention will solve the deficiencies in the prior art, provide a kind of adsorption efficiency high, can and O 3The catalyst n d of the rotten exhaust organic gas of sewage treatment plant's (station) generation is effectively removed in the coupling and catalyzing oxidation 2O 3-ACF.The present invention is with C 2H 6S 2Be representative pollutant, carry out Nd 2O 3-ACF and O 3The coupling and catalyzing oxidation processes is removed C 2H 6S 2Waste gas.
In order to reach the object of the invention, technical scheme of the present invention is:
A kind of Nd 2O 3-ACF catalyst is take activated carbon fiber ACF as carrier, and take neodymium nitrate as presoma, water is that solvent is made into maceration extract, adopts initial wet method infusion process that neodymium is carried in described activated carbon fiber ACF, and roasting namely gets described Nd 2O 3-ACF catalyst.
Nd of the present invention 2O 3The preparation method of-ACF catalyst carries out as follows: with Nd (NO 3) 3Be made into Nd (NO take water as solvent for presoma 3) 3The aqueous solution as maceration extract, add activated carbon fiber ACF, stir, make fully moisteningly, get roasting after the sample vacuum drying of dipping, namely get described Nd 2O 3-ACF catalyst, described maceration extract are unsaturated solution or saturated solution, the pore volume coupling of described dipping solution cumulative volume and activated carbon fiber ACF.
Further, Nd (NO of the present invention 3) 3The concentration of the aqueous solution be 75～225mmol/L.
Further, activated carbon fiber ACF of the present invention is that viscose base activated carbon fiber is sticking.
Further, Nd of the present invention 2O 3Be 5%～15% for the loading of neodymium in-ACF catalyst.
Further, vacuum drying of the present invention is-0.1MPa, 80 ℃ of insulations 2 hours.
Further again, Nd of the present invention 2O 3In the preparation method of-ACF catalyst, described roasting is 600～800 ℃ of insulation calcinings 2 hours.
Roasting of the present invention be under the High Purity Nitrogen atmosphere in Muffle furnace, be warming up to 600～800 ℃ with the heating rate of 3～5 ℃/min, insulation calcining 2 hours.
Nd of the present invention 2O 3-ACF catalyst is used for and O 3The application of coupling and catalyzing oxidation processes foul waste gas, described foul waste gas is for containing following one or more gases: methyl mercaptan, methyl sulfide or DMDS.The present invention is the most applicable to containing DMDS (C 2H 6S 2) removal of waste gas.
Nd of the present invention 2O 3-ACF catalyst application process is as follows: will contain C 2H 6S 2Waste gas and O 3After fully mixing in surge flask, by being equipped with Nd 2O 3The catalytic oxidation post of-ACF catalyst is controlled temperature at 65～75 ℃, carries out the catalytic oxidation coupling processing 5～50 hours, effectively removes C 2H 6S 2, the described C that contains 2H 6S 2Waste gas and O 3By 150～200: 1 volume flow ratio mixes, described Nd 2O 3-ACF catalyst is loaded with ratio of height to diameter at 4: 1.The connotation of the ratio of height to diameter here be the catalyst inserted in the catalytic oxidation post height and the ratio of the diameter of catalytic oxidation post be 4: 1.
Beneficial effect of the present invention is mainly reflected in: treatment process is simple, and processing cost is low, removes foul waste gas, particularly processes to contain C 2H 6S 2The successful of waste gas has the characteristics such as reaction is easy to control, easy to operate, easy to maintenance, is one of the effective ways for the treatment of plant's (station) rotten exhaust organic gas of disposing of sewage, and has the boundless prospect of marketing.
(4) description of drawings:
Accompanying drawing 1: the Nd that Application Example is used 2O 3-ACF coupling catalytic ozonation is processed C 2H 6S 2The experimental provision flow chart;
Accompanying drawing 2:Nd 2O 3-ACF catalyst coupling catalytic ozonation is processed C 2H 6S 2The practical implementation flow chart.
(5) specific embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this.
Embodiment 1:
Nd 2O 3-ACF method for preparing catalyst is:
Get the viscose base activated carbon fiber of the ACF-1300 model of Nantong City Yong Tong Environmental Protection Technology Co., Ltd production, distribution of pores rate 〉=90%, pore volume 0.8-1.2mg/L.
Get 1g gram viscose base activated carbon fiber, with Nd (NO 3) 3Be made into the Nd (NO of 150mmol/L take water as solvent for presoma 3) 3The aqueous solution, get the Nd (NO of the 150mmol/L of 1mL 3) 3The aqueous solution as maceration extract, be added drop-wise on viscose base activated carbon fiber, stir, flooded 2 hours, take out the activated carbon fiber ACF of infiltration in 80 ℃ of vacuum drying 2h, the gained presoma under the High Purity Nitrogen atmosphere, is warming up to 600 ℃ of design temperatures and is incubated 2h with the heating rate of 5 ℃/min in Muffle furnace, namely gets required Nd after naturally cooling to room temperature 2O 3-ACF catalyst 1.1g, the Nd that obtains 2O 3Nd in-ACF 2O 3Load capacity be 10%.
Embodiment 2
Except Nd 2O 3-ACF preparation method middle and later periods calcining heat is 700 ℃, and all the other operations are all identical with embodiment 1.Obtain Nd 2O 3-ACF catalyst 1.08g.
Embodiment 3
Except Nd 2O 3-ACF preparation method middle and later periods calcining heat is 800 ℃, and all the other operations are all identical with embodiment 1.Obtain Nd 2O 3-ACF catalyst 1.06g.
Embodiment 4
Except Nd 2O 3Nd (NO in-ACF preparation method 3) 3Concentration of aqueous solution be 75mmol/L, all the other operations are all identical with embodiment 1.Obtain Nd 2O 3-ACF catalyst 1.05g, the Nd that obtains 2O 3Nd in-ACF 2O 3Load capacity be 5%.
Embodiment 5
Except Nd 2O 3Nd (NO in-ACF preparation method 3) 3Concentration of aqueous solution be 225mmol/L, all the other operations are all identical with embodiment 1.Obtain Nd 2O 3-ACF catalyst 1.15g, the Nd that obtains 2O 3Nd in-ACF 2O 3Load capacity be 15%.
Application Example:
Nd 2O 3-ACF coupling catalytic ozonation is processed foul gas: adopt the described experimental provision of accompanying drawing 1, pure nitrogen gas by steel cylinder out after, after mass flowmenter (D07-11A, Beijing Qixing Huachuang Electronics Co., Ltd), C flows through 2H 6S 2The stripping bottle arrives blender (1); O 3Pass through ozone generator by oxygen
Figure G2009101559040D00051
Health CHYF-3A) produce, after mass flowmenter (D07-11A, Beijing Qixing Huachuang Electronics Co., Ltd), arrive blender.Mist passes to Nd through after heater 2O 3-ACF catalytic bed (2) is established programmed temperature control instrument (3) on described catalytic bed, it is 70 ℃ that peripheral hardware temperature control chuck keeps reaction temperature.Obtain Nd by online detection of gas chromatograph-hydrogen sungpan monkshood root detector (GC-FID) (4) after reaction 2O 3-ACF processes C 2H 6S 2Time of break-through and exit concentration.Described Nd 2O 3-ACF catalytic bed is: (this catalytic bed is made by the column type quartz glass tube, internal diameter 8mm, external diameter 10mm divides into air distribution plate, places the 0.4g catalyst on air distribution plate, presses ratio of height to diameter and loads at 4: 1).
Application examples 1
Adopt the described experimental provision of accompanying drawing 1, will implement 1 Nd that makes 2O 3-ACF catalyst is packed in catalytic bed, O 3Be 6mL/min by oxygen by the ozone generator flow, C 2H 6S 2Be the High Purity Nitrogen load (C of 1L/min by flow 2H 6S 2Inlet concentration 100ppmv), follow O by 1000: 6 volume flow ratios 3Fully mix in surge flask, through passing to the 0.4gNd of said method preparation after heater 2O 3-ACF catalytic bed, it is 70 ℃ that peripheral hardware temperature control chuck keeps reaction temperature, to C 2H 6S 2Carried out the catalytic oxidation coupling processing 50 hours.Import and export C 2H 6S 2Detect by gas chromatograph-flame ionization ditector (GC-FID) is online, obtain Nd 2O 3-ACF processes C 2H 6S 2Time of break-through to be 46h and exit concentration be～0ppmv.
Application examples 2:
Adopt the described experimental provision of accompanying drawing 1, the Nd that makes with embodiment 2 2O 3-ACF catalyst is packed in catalytic bed, and its application operating is identical with Application Example 1.Import and export C 2H 6S 2Detect by gas chromatograph-flame ionization ditector (GC-FID) is online, obtain Nd 2O 3-ACF processes C 2H 6S 2Time of break-through to be 22h and exit concentration be～5ppmv.
Application examples 3:
Adopt the described experimental provision of accompanying drawing 1, the Nd that makes with embodiment 3 2O 3-ACF catalyst is packed in catalytic bed, and its application operating is identical with Application Example 1.Import and export C 2H 6S 2Detect by gas chromatograph-flame ionization ditector (GC-FID) is online, obtain Nd 2O 3-ACF processes C 2H 6S 2Time of break-through to be 5h and exit concentration be～31ppmv.
Application examples 4:
Adopt the described experimental provision of accompanying drawing 1, the Nd that makes with embodiment 4 2O 3-ACF catalyst is packed in catalytic bed, and its application operating is identical with Application Example 1.Import and export C 2H 6S 2Detect by gas chromatograph-flame ionization ditector (GC-FID) is online, obtain Nd 2O 3-ACF processes C 2H 6S 2Time of break-through to be 30h and exit concentration be～5ppmv.
Application examples 5:
Adopt the described experimental provision of accompanying drawing 1, the Nd that makes with embodiment 5 2O 3-ACF catalyst is packed in catalytic bed, and its application operating is identical with Application Example 1.Import and export C 2H 6S 2Detect by gas chromatograph-flame ionization ditector (GC-FID) is online, obtain Nd 2O 3-ACF processes C 2H 6S 2Time of break-through to be 33h and exit concentration be～6ppmv.
Application examples 6:
Based on experimental study, design one cover practical implementation scheme, flow process is seen accompanying drawing 2, the Nd that gets by embodiment 1 method 2O 3-ACF catalyst is packed in catalytic tower (6).As at actual 10000m 3In/h foul gas processing procedure, odorant pollutant is introduced Nd by air-introduced machine (5) after collecting 2O 3-ACF catalytic tower, the O that (CF-G-2-800g) is occured by the medium-sized ozone generator of air-source (7) simultaneously 3Also blasted catalytic tower, O 3Flow is 20m 3/ h, foul gas (C 2H 6S 2) and O 3Discharge after by aiutage by 1000: 2 abundant hybrid reactions of volume flow ratio, tail gas is detected by GC-FID, at Nd 2O 3Be qualified discharge before-ACF is not penetrated, time of break-through is 42h.Nd 2O 3The design parameter of-ACF catalytic tower is: catalytic bed ratio of height to diameter 4: 1, air speed are 30000h -1, catalytic tower peripheral hardware temperature is controlled.The air-source of described ozone generator is originated as follows: air compressor machine (10) is introduced air and is entered cooling driers (9) by air purifier (11-1) again, pass through again air purifier (11-2), then enter the living O of ozone generator after passing into again drier (8) drying 3
Application examples 7:
Adopt the described experimental provision of accompanying drawing 2, the Nd that makes by embodiment 2 methods 2O 3-ACF catalyst is packed in catalytic tower, and other operations are identical with application examples 6.Tail gas is detected by GC-FID, at Nd 2O 3Be qualified discharge before-ACF is not penetrated, time of break-through is 17h.
Application examples 8:
Adopt the described experimental provision of accompanying drawing 2, the Nd that makes by embodiment 3 methods 2O 3-ACF catalyst is packed in catalytic tower, and other operations are identical with application examples 6.Tail gas is detected by GC-FID, at Nd 2O 3Be qualified discharge before-ACF is not penetrated, time of break-through is 3h.
Application examples 9:
Adopt the described experimental provision of accompanying drawing 2, the Nd that makes by embodiment 4 methods 2O 3-ACF catalyst is packed in catalytic tower, and other operations are identical with application examples 6.Tail gas is detected by GC-FID, at Nd 2O 3Be qualified discharge before-ACF is not penetrated, time of break-through is 26h.
Application examples 10:
Adopt the described experimental provision of accompanying drawing 2, the Nd that makes by embodiment 5 methods 2O 3-ACF catalyst is packed in catalytic tower, and other operations are identical with application examples 6.Tail gas is detected by GC-FID, at Nd 2O 3Be qualified discharge before-ACF is not penetrated, time of break-through is 31h.
Comparative Examples 1
Adopt the described experimental provision of accompanying drawing 1, adopt separately ACF, namely adopt separately viscose base activated carbon fiber catalytic oxidation adsorption treatment C 2H 6S 2Waste gas is packed the ACF catalyst in catalytic bed into, C 2H 6S 2Be the High Purity Nitrogen load (C of 1L/min by flow 2H 6S 2Inlet concentration 100ppmv), pass to 0.4g ACF catalytic bed through after heater, it is 70 ℃ that peripheral hardware temperature control chuck keeps reaction temperature, to C 2H 6S 2Carried out the adsoption catalysis oxidation processes 25 hours.Import and export C 2H 6S 2Detect by gas chromatograph-flame ionization ditector (GC-FID) is online, to obtain Nd 2O 3-ACF processes C 2H 6S 2Time of break-through to be 20h and exit concentration be～12ppmv.
Comparative Examples 2
Adopt the described experimental provision of accompanying drawing 1, adopt independent O 3Oxidation processes C 2H 6S 2Waste gas, catalytic bed is not filled, O 3Be 6mL/min by oxygen by the ozone generator flow, C 2H 6S 2Be the High Purity Nitrogen load (C of 1L/min by flow 2H 6S 2Inlet concentration 100ppmv), follow O by 1000: 6 volume flow ratios 3Fully mix in surge flask, pass to catalytic bed through after heater, it is 70 ℃ that peripheral hardware temperature control chuck keeps reaction temperature, to C 2H 6S 2Carried out oxidation processes 25 hours.Import and export C 2H 6S 2Detect by gas chromatograph-flame ionization ditector (GC-FID) is online, obtain C after oxidation processes 2H 6S 2Exit concentration be～83ppmv.
Comparative Examples 3
Adopt the described experimental provision of accompanying drawing 1, ACF is packed in catalytic bed, O 3Be 6mL/min by oxygen by the ozone generator flow, C 2H 6S 2Be the High Purity Nitrogen load (C of 1L/min by flow 2H 6S 2Inlet concentration 100ppmv), follow O by 1000: 6 volume flow ratios 3Fully mix in surge flask, through passing to the 0.4g ACF catalytic bed of said method preparation after heater, it is 70 ℃ that peripheral hardware temperature control chuck keeps reaction temperature, to C 2H 6S 2Processed 30 hours.Import and export C 2H 6S 2Detect by gas chromatograph-flame ionization ditector (GC-FID) is online, obtain ACF and process C 2H 6S 2Time of break-through to be 25h and exit concentration be～11ppmv.

Claims (6)

1. Nd 2O 3-ACF catalyst is characterized in that described catalyst is take activated carbon fiber ACF as carrier, and take neodymium nitrate as presoma, water is that solvent is made into maceration extract, adopts initial wet method infusion process that neodymium is carried in described activated carbon fiber ACF, and roasting namely gets described Nd 2O 3-ACF catalyst; Described activated carbon fiber ACF is viscose base activated carbon fiber; Described Nd 2O 3The preparation method of-ACF catalyst carries out as follows: with Nd (NO 3) 3Be made into Nd (NO take water as solvent for presoma 3) 3The aqueous solution as maceration extract, add activated carbon fiber ACF, stir, make fully moisteningly, get roasting after the sample vacuum drying of dipping, namely get described Nd 2O 3-ACF catalyst, described maceration extract are unsaturated solution or saturated solution, the pore volume coupling of described dipping solution cumulative volume and activated carbon fiber ACF; Described Nd (NO 3) 3The concentration of the aqueous solution be 75～225mmol/L, described Nd 2O 3In-ACF catalyst, the loading of neodymium is 5%～15%.
2. Nd as claimed in claim 1 2O 3-ACF catalyst is characterized in that described vacuum drying is-0.1MPa, 80 ℃ of insulations 2 hours.
3. Nd as claimed in claim 1 2O 3-ACF catalyst is characterized in that described roasting is 600～800 ℃ of insulation calcinings 2 hours.
4. Nd as claimed in claim 3 2O 3-ACF catalyst, it is characterized in that described roasting be under the High Purity Nitrogen atmosphere in Muffle furnace, be warming up to 600～800 ℃ with the heating rate of 3～5 ℃/min, insulation calcining 2 hours.
5. Nd as claimed in claim 1 2O 3-ACF catalyst is used for and O 3The coupling and catalyzing oxidation processes contains the application of the waste gas of DMDS.
6. application as claimed in claim 5, described application process is as follows: waste gas and the O that will contain DMDS 3After fully mixing in surge flask, by being equipped with Nd 2O 3The catalytic oxidation post of-ACF catalyst is controlled temperature at 65～75 ℃, carries out the catalytic oxidation coupling processing 5～50 hours, effectively removes C 2H 6S 2, the described C that contains 2H 6S 2Waste gas and O 3By 150～200: 1 volume flow ratio mixes, described Nd 2O 3-ACF catalyst is loaded with ratio of height to diameter at 4: 1.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1129146A (en) * 1995-02-17 1996-08-21 段忠善 Catalyst for purifying waste industrial gas and exhausted gas of automobile
CN1745036A (en) * 2003-12-05 2006-03-08 三菱重工业株式会社 Carbon material and flue gas treatment apparatus

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1129146A (en) * 1995-02-17 1996-08-21 段忠善 Catalyst for purifying waste industrial gas and exhausted gas of automobile
CN1745036A (en) * 2003-12-05 2006-03-08 三菱重工业株式会社 Carbon material and flue gas treatment apparatus

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