CN105170199B - A kind of regeneration method of coal gasification waste water deep oxidation catalyst - Google Patents
A kind of regeneration method of coal gasification waste water deep oxidation catalyst Download PDFInfo
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Abstract
The present invention provides a kind of regeneration method of coal gasification waste water deep oxidation catalyst, include the following steps, 1) catalyst after inactivation is immersed in selected organic solvent, it is ultrasonically treated 5-60min, after filtering separation, by 80~120 DEG C of drying in an oven of processed catalyst；2) catalyst after drying is immersed prepared mass fraction is to be ultrasonically treated 5-60min in 2-10% alkaline solution, be 7-8 with pure water to pH, after drying in an oven, is roasted.Coal gasification waste water deep oxidation catalyst regeneration method of the present invention is simple, and process flow is short, can be to decaying catalyst repeated reproducibility.
Description
Technical field
The invention belongs to coal chemical industrial waste water processing technology fields, and in particular to the waste water advanced oxidation processes of coal gasification course are urged
The regeneration method of agent.
Background technique
China possesses coal resources abundant, how to be cleaned, is efficiently used, and is always scientific research personnel's emphasis
One of research field.Currently, coal gasification is the major way of coal high-efficiency comprehensive utilization, however coal can generate greatly in gasification
High pollution waste water to be measured, phenol, tar, aliphatic and aromatic compound etc. are mainly contained, pollutant concentration is high, complicated component,
Processing difficulty is larger.
Gasification furnace used in Coal Gasification Project mainly has lurgi gasifier, shell furnace, Texaco stove, multiinjector gasification at present
Furnace etc., waste water composition caused by different gasification furnaces be not identical.The processing technological flow of existing coal gasification waste water mainly includes
Three pretreatment, biological treatment and advanced treating steps.Pretreatment generally uses physico-chemical process such as ammonia still process dephenolize, air bearing
Gravity oil-removing, coagulating sedimentation remove ingredient toxic to microorganism in biological treatment or inhibiting effect；Biological treatment is mainly
Waste water is further processed using techniques such as activated sludge, aerobic/anaerobic, SBR；Waste water COD after biochemical treatment,
The indexs such as coloration, ammonia nitrogen are generally extremely difficult to national grade one discharge standard, also need to discharge after further handling.
Recently, country is higher and higher to the environmental requirement of Coal Gasification Project, and many Coal Chemical Engineering Project waste water only reach country
First discharge standard is not enough.In face of shortage of water resources, the environmental carrying capacity real situation such as limited, how research makes coal gasification
Waste water recycles after advanced treating, really realizes the target of Coal Chemical Engineering Project wastewater zero discharge, is industry scientific research personnel
The direction of effort from now on.
The active charcoal absorption of method currently used for coal gasification waste water advanced treating, biofilter, UF membrane, catalysis oxidation
Deng, wherein in activated carbon adsorption method regenerating active carbon energy consumption it is larger, after regeneration adsorption capacity decline；Biofilter is at low cost,
But treatment effeciency is lower, has been easy secondary pollution；UF membrane higher cost, film be easy blocking, and to influent quality require compared with
Height limits the scope of application.Above-mentioned these types method is substantially that pollutant is carried out physical transfer, does not make its disappearance,
Also need subsequent harmless treatment.
Catalysis oxidation can make the organic pollutant in waste water under the effect of the catalyst through being degraded to inorganic matter, from
Organic pollutant is substantially eliminated, there is comprehensive advantage.The oxidation technology reported at present is mainly catalytic ozonation, that is, is existed
In the presence of catalyst, it is passed through ozone into coal gasification waste water, makes organic pollutant degradation carbon dioxide, but this technology needs
A large amount of ozone is expended, the cost is relatively high.
Using effective catalyst, directly to the organic pollutant in waste water after coal gasification biochemical treatment under the action of air
Carrying out degradation rapidly is one of the waste water advanced oxidation technology with bright application prospect.To improve the catalyst market competitiveness,
Reduce catalyst cost, how effectively to catalyst carry out regeneration be determine the technology can Rapid Popularization an important factor for.
Summary of the invention
In view of this, the present invention is directed to propose a kind of regeneration method of coal gasification waste water deep oxidation catalyst.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of regeneration method of coal gasification waste water deep oxidation catalyst, includes the following steps,
1) catalyst after inactivation is immersed in selected organic solvent, is ultrasonically treated 5-60min, it, will after filtering separation
80~120 DEG C of drying in an oven of processed catalyst；Preferably, drying temperature is 100 DEG C；
2) catalyst after drying is immersed prepared mass fraction is to be ultrasonically treated 5- in 2-10% alkaline solution
60min is 7-8 with pure water to pH, in an oven after 80~120 DEG C of drying, is roasted, it is preferred that drying temperature is
100℃。
Preferably, the catalyst in the step 1) is made of being prepared via a method which, a) by metal salt by certain
It is dissolved in solvent after ratio mixing, is prepared into the mixed solution that mass fraction is 1-15%；Mixed solution is stirred at room temperature
Place 6-12h；
B) carrier is immersed in the acid solution that prepared mass fraction is 2-10%, is ultrasonically treated 5-60min, use is pure
Water washing is 6-7 to pH, is dried for standby for 80~120 DEG C in an oven；Preferably, drying temperature is 100 DEG C；
C) by the prepared mixed solution of step 1) and step 2) treated carrier according to mass ratio (0.8~1.2):
(0.8~1.2) it mixes, stands 1-24h, in an oven 80~120 DEG C of drying, then high-temperature roasting；Preferably, in mass ratio for
1:1；Drying temperature is 100 DEG C.
Preferably, it is described a) in soluble metallic salt be zinc, indium, ammonium, iron, copper, manganese, bismuth, nickel, cobalt, molybdenum, tin, ammonium,
One or more of gallium, cerium, antimony, the nitrate of cadmium, sulfate, carbonate, chloride, vanadate, solvent is first
One or more of alcohol, ethyl alcohol, isopropanol, the tert-butyl alcohol, glycerine, ethylene glycol, carbon tetrachloride；In the step b)
Carrier is one of fumed silica, ZSM-5 molecular sieve, S-1 molecular sieve, TS-1 molecular sieve, porous aluminas, and acidity is molten
Liquid is one of sulfuric acid, nitric acid, hydrochloric acid；The temperature of step c) high temperature roasting is 300~800 DEG C, the time is 1~
36h。
Preferably, the organic solvent in the step 1) be methanol, ethyl alcohol, isopropanol, the tert-butyl alcohol, glycerine, ethylene glycol,
One or more of carbon tetrachloride.
Preferably, in the step 1), the mass ratio of the catalyst after the organic solvent and inactivation is (1~10): 1.
Preferably, in the step 2), the alkaline solution is sodium hydroxide, potassium hydroxide, ammonium hydroxide, tetraethyl hydroxide
One or more of ammonium, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, n-butylamine.
Preferably, in the step 2), the maturing temperature is 300~800 DEG C, and calcining time is 1~48h.
Compared with the existing technology, the regeneration method of a kind of coal gasification waste water deep oxidation catalyst of the present invention, tool
There is following advantage:
1) coal gasification waste water deep oxidation catalyst regeneration method of the present invention is simple, and process flow is short, can be catalyzed to inactivation
Agent repeated reproducibility.
2) various solvents can recycle in catalyst regeneration process of the present invention, avoid catalyst regeneration process
Secondary pollution.
Specific embodiment
Below in conjunction with embodiment, the present invention will be described in detail.
Embodiment 1
A kind of preparation method of coal gasification waste water deep oxidation catalyst, includes the following steps:
1) it is dissolved in methanol after mixing zinc nitrate, indium nitrate, ammonium tungstate with molar ratio 0.2:0.4:0.4, is prepared into matter
The mixed solution that score is 1% is measured, mixed solution is stirred at room temperature and places 6h.
2) fumed silica is immersed in the sulfuric acid solution that prepared mass fraction is 2%, is ultrasonically treated 5min, used
Pure water is 6-7 to pH, is dried for standby at 100 DEG C in an oven.
3) the prepared mixed solution of step 1) and step 2) treated carrier are mixed according to mass ratio 1:1, is stood
1h is dried at 100 DEG C, then 300 DEG C of roasting 1h in Muffle furnace in an oven.
A kind of regeneration method of the coal gasification waste water deep oxidation catalyst of method preparation as above, includes the following steps,
1) the catalyst 20g after inactivation is immersed in 20g methanol, is ultrasonically treated 5min, it, will be processed after filtering separation
Catalyst 100 DEG C of drying in an oven；
2) the 20g catalyst after drying is immersed prepared 20g mass fraction is ultrasound in 2% sodium hydroxide solution
Handle 5min, be 7-8 with pure water to pH, in an oven 100 DEG C drying after, in Muffle furnace at 300 DEG C calcining time
For 1h.
Embodiment 2
A kind of preparation method of coal gasification waste water deep oxidation catalyst, includes the following steps:
1) it is dissolved in ethyl alcohol after mixing copper nitrate, cadmium nitrate, chromic nitrate with molar ratio 0.4:0.3:0.3, is prepared into matter
The mixed solution that score is 15% is measured, mixed solution is stirred at room temperature and places 12h.
2) ZSM-5 molecular sieve is immersed in the hydrochloric acid solution that prepared mass fraction is 10%, is ultrasonically treated 60min,
It is 6-7 with pure water to pH, is dried for standby at 100 DEG C in an oven.
3) the prepared mixed solution of step 1) and step 2) treated carrier are mixed according to mass ratio 1:1, is stood
For 24 hours, it dries at 100 DEG C in an oven, then 800 DEG C of roasting 36h in Muffle furnace.
A kind of regeneration method of the coal gasification waste water deep oxidation catalyst of method preparation as above, includes the following steps,
1) the catalyst 20g after inactivation is immersed in 200g ethyl alcohol, is ultrasonically treated 60min, after filtering separation, will processed
Catalyst in an oven 100 DEG C drying；
2) the 20g catalyst after drying is immersed prepared 200g mass fraction is to surpass in 10% sodium hydroxide solution
Sonication 60min is 7-8 with pure water to pH, in an oven after 100 DEG C of drying, when roasting at 800 DEG C in Muffle furnace
Between be 48h.
Embodiment 3
A kind of preparation method of coal gasification waste water deep oxidation catalyst, includes the following steps:
1) isopropyl is dissolved in after mixing nitric acid molybdenum, manganese nitrate, nitric acid antimony, ferric nitrate with molar ratio 0.4:0.4:0.1:0.1
In alcohol, it is prepared into the mixed solution that mass fraction is 10%, mixed solution is stirred at room temperature and places 6h.
2) TS-1 molecular sieve is immersed in the hydrochloric acid solution that prepared mass fraction is 5%, is ultrasonically treated 30min, used
Pure water is 6-7 to pH, is dried for standby for 95 DEG C in an oven.
3) the prepared mixed solution of step 1) and step 2) treated carrier are mixed according to mass ratio 1:1, is stood
12h, in an oven 105 DEG C drying, then in Muffle furnace 600 DEG C roasting for 24 hours.
A kind of regeneration method of the coal gasification waste water deep oxidation catalyst of method preparation as above, includes the following steps,
1) the catalyst 20g after inactivation is immersed in 100g ethyl alcohol, is ultrasonically treated 30min, after filtering separation, will processed
Catalyst in an oven 100 DEG C drying；
2) the 20g catalyst after drying is immersed prepared 100g mass fraction is ultrasonic treatment in 5% ammonia spirit
30min is 7-8 with pure water to pH, and in an oven after 100 DEG C of drying, calcining time is at 600 DEG C in Muffle furnace
24h。
Embodiment 4
A kind of preparation method of coal gasification waste water deep oxidation catalyst, includes the following steps:
1) it is dissolved in methanol after mixing cobalt nitrate, nickel nitrate with molar ratio 0.4:0.6, being prepared into mass fraction is 10%
Mixed solution, by mixed solution be stirred at room temperature place 6h.
2) S-1 molecular sieve is immersed in the nitric acid solution that prepared mass fraction is 5%, is ultrasonically treated 30min, use is pure
Water washing is 6-7 to pH, is dried for standby for 100 DEG C in an oven.
3) the prepared mixed solution of step 1) and step 2) treated carrier are mixed according to mass ratio 1:1, is stood
12h, in an oven 100 DEG C drying, then in Muffle furnace 600 DEG C roasting for 24 hours.
A kind of regeneration method of the coal gasification waste water deep oxidation catalyst of method preparation as above, includes the following steps,
1) the catalyst 20g after inactivation is immersed in 100g isopropanol, is ultrasonically treated 30min, after filtering separation, will located
The catalyst managed 100 DEG C of drying in an oven；
2) the 20g catalyst after drying is immersed prepared 100g mass fraction is 8% tetrapropylammonium hydroxide solution
In, it is ultrasonically treated 30min, is 7-8 with pure water to pH, in an oven after 100 DEG C of drying, in Muffle furnace at 600 DEG C
Calcining time is for 24 hours.
Embodiment 5
A kind of preparation method of coal gasification waste water deep oxidation catalyst, includes the following steps:
1) copper nitrate is dissolved in glycerine, the mixed solution that mass fraction is 8% is prepared into, by mixed solution in room temperature
10h is placed in lower stirring.
2) fumed silica is immersed in the hydrochloric acid solution that prepared mass fraction is 10%, is ultrasonically treated 30min,
It is 6-7 with pure water to pH, is dried for standby for 105 DEG C in an oven.
3) the prepared mixed solution of step 1) and step 2) treated carrier are mixed according to mass ratio 1:1, is stood
10h is dried for 105 DEG C, then 400 DEG C of roasting 10h in Muffle furnace in an oven.
A kind of regeneration method of the coal gasification waste water deep oxidation catalyst of method preparation as above, includes the following steps,
1) the catalyst 20g after inactivation is immersed in 100g glycerine, is ultrasonically treated 30min, after filtering separation, will handled
The catalyst crossed 100 DEG C of drying in an oven；
2) the 20g catalyst after drying is immersed prepared 50g mass fraction is 10% tetrabutylammonium hydroxide solution
In, it is ultrasonically treated 30min, is 7-8 with pure water to pH, after drying in an oven, when being roasted at 400 DEG C in Muffle furnace
Between be 12h.
It is in 400ml tubular reactor that coal gasification waste water deep oxidation catalyst 50g, which is placed in volume, and being pumped into COD is
Waste water after the coal gasification biochemical treatment of 300ppm, flow 200ml/min are passed through air, air velocity 30ml/ into waste water
Min starts to react under normal temperature and pressure, and the COD value of detection reactor water outlet stops reaction when COD value is higher than 100ppm, determines
For inactivation, the service life of fresh catalyst is recorded.Inactivation records the catalyst after the 10th regeneration repeatedly after regenerating 10 times
Service life, the results are shown in Table 1.
The catalyst service life of the different embodiments of table 1
| Number | The fresh catalyst service life (h) | Regenerate 10 rear catalyst service life (h) |
| Embodiment 1 | 82 | 40 |
| Embodiment 2 | 78 | 65 |
| Embodiment 3 | 81 | 63 |
| Embodiment 4 | 79 | 57 |
| Embodiment 5 | 80 | 46 |
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of regeneration method of coal gasification waste water deep oxidation catalyst, it is characterised in that: include the following steps,
1) catalyst after inactivation is immersed in selected organic solvent, is ultrasonically treated 5-60min, after filtering separation, will handled
The catalyst crossed 80~120 DEG C of drying in an oven；The organic solvent be methanol, ethyl alcohol, isopropanol, the tert-butyl alcohol, glycerine,
One or more of ethylene glycol, carbon tetrachloride；The organic solvent and inactivation after catalyst mass ratio be (1~
10): 1；
2) catalyst after drying is immersed prepared mass fraction is to be ultrasonically treated 5-60min in 2-10% alkaline solution,
It is 7-8 with pure water to pH, in an oven after 80~120 DEG C of drying, is roasted；The alkaline solution be sodium hydroxide,
One of potassium hydroxide, ammonium hydroxide, tetraethyl ammonium hydroxide, tetrapropylammonium hydroxide, tetrabutylammonium hydroxide, n-butylamine or two
Kind or more；The temperature of the roasting is 300~800 DEG C, and calcining time is 1~48h；
Catalyst in the step 1) is made of being prepared via a method which,
A) it is dissolved in after being mixed in a certain ratio metal salt or ammonium salt in solvent, it is molten to be prepared into the mixing that mass fraction is 1-15%
Liquid；Mixed solution is stirred at room temperature and places 6-12h；The solvent be methanol, ethyl alcohol, isopropanol, the tert-butyl alcohol, glycerine,
One or more of ethylene glycol, carbon tetrachloride；The ammonium salt is ammonium nitrate, ammonium sulfate, ammonium carbonate, ammonium chloride, vanadic acid
One or more of ammonium；
B) carrier is immersed in the acid solution that prepared mass fraction is 2-10%, is ultrasonically treated 5-60min, is washed with pure water
Washing to pH is 6-7, is dried for standby for 80~120 DEG C in an oven；Acid solution is one of sulfuric acid, nitric acid, hydrochloric acid；
C) by the prepared mixed solution of step a) and step b) treated carrier according to mass ratio (0.8~1.2): (0.8~
1.2) it mixes, stands 1-24h, in an oven 80~120 DEG C of drying, then high-temperature roasting.
2. the regeneration method of coal gasification waste water deep oxidation catalyst according to claim 1, it is characterised in that: it is described a)
In metal salt be zinc, indium, iron, copper, manganese, bismuth, nickel, cobalt, molybdenum, tin, gallium, cerium, antimony, the nitrate of cadmium, sulfate, carbonate,
One or more of chloride, vanadate, and metal salt is soluble；Carrier in the step b) is gas phase two
One of silica, ZSM-5 molecular sieve, S-1 molecular sieve, TS-1 molecular sieve, porous aluminas；Step c) the high temperature roasting
The temperature of burning is 300~800 DEG C, and the time is 1~36h.
3. the regeneration method of coal gasification waste water deep oxidation catalyst according to claim 1, it is characterised in that: step 1)
In drying temperature be 100 DEG C；Drying temperature in step 2) is 100 DEG C；Drying temperature in step b) is 100 DEG C；Step
C) in, treated that carrier is mixed according to mass ratio 1:1 by the prepared mixed solution of step a) and step b), stands 1-24h,
100 DEG C of drying in baking oven.
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| CN106391140B (en) * | 2016-10-21 | 2019-01-22 | 中国天辰工程有限公司 | A kind of regeneration method of laughing gas low-temperature decomposition catalyst |
| CN107115867A (en) * | 2017-06-22 | 2017-09-01 | 中国天辰工程有限公司 | A kind of preparation method of the catalyst of ozone oxidation organic exhaust gas |
| CN112221489A (en) * | 2020-11-18 | 2021-01-15 | 西安凯立新材料股份有限公司 | Regeneration method of gold carbon catalyst for preparing VCM |
| CN115945228A (en) * | 2022-12-12 | 2023-04-11 | 巴斯夫公司 | Regeneration method for preparing 1,4-butynediol catalyst through alkyne hydroformylation reaction |
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| JPS60102943A (en) * | 1983-11-08 | 1985-06-07 | Daido Steel Co Ltd | Catalyst regenerating method |
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