CN107088416A - A kind of catalysis process of co-precipitation Ru Fe Co La Ti composite catalysts - Google Patents
A kind of catalysis process of co-precipitation Ru Fe Co La Ti composite catalysts Download PDFInfo
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Abstract
The invention discloses one kind co-precipitation composite catalyst and its catalysis process, Ru Fe Co La Ti catalyst and its application method prepared by more particularly to a kind of use coprecipitation, the catalyst is a kind of " noble metal-transition metal-rare earth-rare metal " composite catalyst, the Particle Distribution for preparing catalyst using this method is uniform, with nanostructured, its BET is respectively to be more than 50m than surface and pore volume2/ g and more than 0.36cm3/g。
Description
Technical field
The present invention relates to one kind co-precipitation composite catalyst and its catalysis process, more particularly to one kind uses coprecipitation
The Ru-Fe-Co-La-Ti catalyst and its application method of preparation, the catalyst are a kind of " noble metals-transition metal-dilute
Soil-rare metal " composite catalyst, the present invention is used for technical field of waste water processing.
Background technology：
The processing method of organic wastewater includes Physical, chemical method, bioanalysis, ozone or hydrogen peroxide oxidation, photochemistry and urged
Change oxidation and membrane separation process.High concentration hard-degraded organic waste water includes percolate, black liquid, dyeing waste water, sulfur-bearing and given up
One of the characteristics of water, cyanide wastewater, pharmacy waste water etc., this kind of waste water is that pollutant concentration is high, its CODCrValue it is up to tens of thousands of, tens
Ten thousand even mg/L up to a million, the two of feature is containing noxious materials such as dyestuff, sulphur, cyanogen.High concentration hard-degraded organic waste water, with thing
The processing of change method, complex process and is difficult to make each pollution factor qualified discharge；Handled with biochemical process, microorganism is in high pollution thing and has
Growth is suppressed in malicious water body, therefore flow is complicated and waste water is difficult to qualified discharge；Urged with ozone or hydrogen peroxide oxidation, photochemistry
Change oxidative treatment, cost is high and is difficult to make discharged wastewater met the national standard；Handled with membrane separation process, discharged wastewater met the national standard but processing can be made
Cost is too high.It can be seen that, high concentration hard-degraded organic waste water is a kind of intractable high-concentration sewage, so far also without one kind very
Ripe not only can guarantee that standard water discharge but also economically viable processing method.
According to the classification of catalyst, CWO is divided into the homogeneous and class of heterogeneous catalysis wet oxidation two.Although homogeneous
Catalyst it is active it is high, the advantages of reaction speed is fast, still, because catalyst is dissolved in waste water, waste water is caused secondary
Pollution improves the cost of wastewater treatment, it is necessary to the sedimentation for carrying out metal ion is reclaimed, thus technological process is become complicated.
Different from homogeneous catalyst, the advantages of heterogeneous catalyst has easily separated, reusable simplifies the operation stream of wet oxidation
Journey.The catalyst of research efficiently, stable turns into the focus of heterogeneous catalysis wet oxidation.The heterogeneous catalyst studied at present can divide
For three kinds of copper system, composite oxides and noble metal carrier catalyst.Although copper system and composite oxide catalysts have preferably
Catalytic activity, but during the course of the reaction, active component inevitably dissolution causes catalyst activity to reduce, it is impossible to make for a long time
With；Although noble metal catalyst cost is higher, it can still be stabilized under severe reaction conditions, and oxidation activity is very
It is high.
Chinese invention patent publication No. CN103041818A disclose it is a kind of with transition metal Cu, Cr, Mo, Fe,
It is one or more of as catalytic component in one or more in Ni, Co, Mn, and auxiliary agent rare earth element La and Ce, Pr, Nd,
Porous inert material ceramic honey comb, green stone, zeolite molecular sieve or activated carbon are the immersion-type CWAO catalyst of carrier, but catalysis
Agent component is not directed to noble metal in constituting.
Chinese invention patent Authorization Notice No. CN102897895B discloses co-precipitation type cobalt Mn complex oxide catalyst
Preparation, in O3 catalytic oxidation organic matter, wherein be not directed to the doping of noble metal, and co-precipitated catalyst drops in waste water
Solve and be easy to dissolving under the sour environment produced.
On this basis, the application, which provides a kind of high concentration hard-degraded organic waste water that is directed to, has CODCrClearance is high, no
There is biological bacterium poisoning and secondary pollution, the simple Ru-Fe-Co-La-Ti composite catalysts of technological process and its user
Method.
The content of the invention
The object of the invention is achieved through the following technical solutions：
A kind of catalysis process of co-precipitation Ru-Fe-Co-La-Ti composite catalysts, it is characterised in that in terms of parts by weight,
The component of catalyst includes：
(a) 5 parts of RuCl3；
(b) 6 parts of Fe2(SO4)3；
(c) 7 parts of Co (NO3)2·6H2O；
(d) 9 parts of LaCl3·6H2O；
(e) 8 parts of TiO2；
(f) 65 parts of distilled water；
The catalytic wet oxidation catalyst is adopted to be prepared with the following method：
(1) catalytic component, preparing metal salting liquid are weighed according to each component of above-mentioned co-precipitation composite catalyst；
(2) under the conditions of medium-speed magnetic stirring, by 2.0mol/L NH3OH solution instills metal with 5 drops/min speed
In salting liquid, make precipitating reagent NH3OH is well mixed with salting liquid and generates sediment, keeps the pH value 9~10 of mixed liquor；
(3) sediment and solution of step (2) are placed in ultrasonic cleaning machine, ultrasonic disperse, Aging Temperature is 35-95
DEG C, digestion time is 2-5h；
(4) drain well, by the distillation water washing three times of the sediment after ageing, then washs with absolute ethyl alcohol three times, so
Vacuum filtration machine is used afterwards, and suction filtration separation obtains sediment；
(5) sediment for obtaining step (4) is placed in 100~120 DEG C of electric drying oven with forced convections, and drying time 8~
14h；Then it is placed in chamber type electric resistance furnace, 300~750 DEG C, constant temperature calcining 1.5 is warming up to the 6 DEG C/min rate of heat addition
~14h.
(6) sample for being calcined step (5) is ground, and is screened out the powder of 60~80 mesh, is obtained finished catalyst；
CWO device used in the catalysis process of the co-precipitation Ru-Fe-Co-La-Ti composite catalysts
Composition include：Oxygen tank, first pressure table, intake valve, outlet valve, agitating device, autoclave, thermocouple, second pressure table,
Explosive valve, electrothermal furnace, controller.The oxidation steel cylinder is connected by first pressure table and intake valve with autoclave, the high pressure
Kettle includes agitating device, thermocouple and electrothermal furnace, and the thermocouple is connected by second pressure device with explosive valve, described to stir
Mix device and electrothermal furnace is connected with controller.
The catalysis process of described co-precipitation Ru-Fe-Co-La-Ti composite catalysts, it is characterised in that Aging Temperature is
50℃。
The catalysis process of described co-precipitation Ru-Fe-Co-La-Ti composite catalysts, it is characterised in that digestion time is
3h。
The catalysis process of described co-precipitation Ru-Fe-Co-La-Ti composite catalysts, it is characterised in that the drying is
Sample is dried into 12h under 100 DEG C of ventilation conditions.
The catalysis process of described co-precipitation Ru-Fe-Co-La-Ti composite catalysts, it is characterised in that the roasting is
The sample of drying is placed in high temperature box type resistance furnace, 450 DEG C of roastings of design temperature are warming up to the 5 DEG C/min rate of heat addition.
The catalysis process of described co-precipitation Ru-Fe-Co-La-Ti composite catalysts, its CWO device is used
Method is that waste water and catalyst are loaded into reactor, is begun to warm up after sealing, oxygen is passed through when being raised to design temperature and reaches setting
Pressure, while opening agitating device.Now it is set to the zero point of reaction, is sampled at regular intervals by probe tube later, is being taken
During sample, oxygen supply valve is opened constant with the stagnation pressure of maintenance reaction system.
Relative to prior art, the invention has the advantages that：
1) Particle Distribution for preparing catalyst using this method is uniform, and with nanostructured, its BET is than surface and pore volume point
Wei not be more than 50m2/ g and more than 0.36cm3/g；
2) rare-earth elements La and rare metal Ti are as co-catalyst, the function with structural promoter and electronic auxiliary, greatly
It is big to reduce the number of dropouts of active component, and the whole processing procedure of the present invention only needs to a coagulant precipitation pond and a high pressure is anti-
Kettle is answered, compared with conventional materialization, biochemical and other group technologies, its technological process is simple.
3) in the CWAO reactions of percolate, electrical heating is needed in the initial period of reaction；Meeting when system is normally run
Discharge substantial amounts of heat, the heat of system release substantially can be with the condition of high temperature of maintenance reaction system, therefore reaction system energy-saving ring
Protect；
4) under the collective effect of CWAO catalyst, high temperature, high pressure, the percolate component of difficult degradation is thoroughly divided
Solve as CO2、H2O or other small molecule organic compounds, it is to avoid suppression of the toxic pollutant to biological bacterium, will not cause secondary
Pollution.The present invention can be by the landfill leachate treatment of high concentration to being up to state standards.
Embodiment
To more fully understand the present invention, with reference to embodiment, the present invention is further illustrated, but embodiment not structure
The restriction of the paired claimed scope of the invention.
In the present invention, h represents hour, and min represents minute, and CWAO represents CWO.
The preparation of metal salt solution：In terms of parts by weight, Ru-Fe-Co-La-Ti salting liquids in setting metal salt mixture
Constitute：5 parts of RuCl3, 6 parts of Fe2(SO4)3, 7 parts of Co (NO3)2·6H2O, 9 parts of LaCl3·6H2O, 8 parts of TiO2It is dissolved in 65 parts of steamings
Distilled water, obtains metal salt solution；
Under the conditions of medium-speed magnetic stirring, by 6mol/L NH3It is molten that OH solution instills metal salt with 6 drops/min speed
In liquid, make precipitating reagent NH3OH solution is well mixed with salting liquid and generates sediment, and mixed liquor pH value stops when reaching 11
NH3The instillation of OH solution；
Sediment and solution are positioned in ultrasonic cleaning machine, ultrasonic disperse, the precipitation ageing 4h at 60 DEG C；
The aqueous solution is drained, the sediment after ageing is used into distillation water washing three times, then is washed three times with absolute ethyl alcohol, is made clear
Rear pH value of solution is washed between 9-10, then using vacuum filtration machine, suction filtration separation obtains sediment；
Electric drying oven with forced convection is put the precipitate in, 10h is dried at 102 DEG C, is then placed in chamber type electric resistance furnace, with 6
DEG C/the min rate of heat addition is warming up to 450 DEG C, constant temperature calcining 6h.
The roasting sample of step is ground, the powder of 60~80 mesh is screened out, obtains finished catalyst.
By 250mL CODCrFor 2000mg/L stimulated dye wastewater, it is placed in 0.5LGS type reactors, while putting into this
Catalyst 2g/L prepared by embodiment, sets 180 DEG C of reaction temperature, and temperature rises to 180 DEG C and is passed through oxygen to partial pressure of oxygen
1.0MPa, starts timing and terminates to 90min reactions.
【Embodiment 2】
The preparation of metal salt solution：In terms of parts by weight, Ru-Fe-Co-La-Ti salting liquids in setting metal salt mixture
Constitute：5 parts of RuCl3, 6 parts of Fe2(SO4)3, 7 parts of Co (NO3)2·6H2O, 9 parts of LaCl3·6H2O, 8 parts of TiO2It is dissolved in 65 parts of steamings
Distilled water, obtains metal salt solution；
Under the conditions of medium-speed magnetic stirring, by 6mol/L NH3It is molten that OH solution instills metal salt with 6 drops/min speed
In liquid, make precipitating reagent NH3OH solution is well mixed with salting liquid and generates sediment, and mixed liquor pH value stops when reaching 10
NH3The instillation of OH solution；
Sediment and solution are positioned in ultrasonic cleaning machine, ultrasonic disperse, the precipitation ageing 4h at 60 DEG C；
The aqueous solution is drained, the sediment after ageing is used into distillation water washing three times, then is washed three times with absolute ethyl alcohol, is made clear
Rear pH value of solution is washed between 9-10, then using vacuum filtration machine, suction filtration separation obtains sediment；
Electric drying oven with forced convection is put the precipitate in, 10h is dried at 102 DEG C, is then placed in chamber type electric resistance furnace, with 6
DEG C/the min rate of heat addition is warming up to 450 DEG C, constant temperature calcining 6h.
The roasting sample of step is ground, the powder of 60~80 mesh is screened out, obtains finished catalyst.
By 250mLCODCrFor 2000mg/L stimulated dye wastewater, it is placed in 0.5LGS type reactors, while putting into this reality
The catalyst 2g/L of example preparation is applied, 180 DEG C of reaction temperature is set, temperature rises to 180 DEG C and is passed through oxygen to partial pressure of oxygen 1.0MPa,
Start timing to 90min reactions to terminate.
【Embodiment 3】
The preparation of metal salt solution：In terms of parts by weight, Ru-Fe-Co-La-Ti salting liquids in setting metal salt mixture
Constitute：7 parts of RuCl3, 4 parts of Fe2(SO4)3, 9 parts of Co (NO3)2·6H2O, 8 parts of LaCl3·6H2O, 7 parts of TiO2It is dissolved in 65 parts of steamings
Distilled water, obtains metal salt solution；
Under the conditions of medium-speed magnetic stirring, by 6mol/L NH3It is molten that OH solution instills metal salt with 6 drops/min speed
In liquid, make precipitating reagent NH3OH solution is well mixed with salting liquid and generates sediment, and mixed liquor pH value stops when reaching 11
NH3The instillation of OH solution；
Sediment and solution are positioned in ultrasonic cleaning machine, ultrasonic disperse, the precipitation ageing 4h at 60 DEG C；
The aqueous solution is drained, the sediment after ageing is used into distillation water washing three times, then is washed three times with absolute ethyl alcohol, is made clear
Rear pH value of solution is washed between 9-10, then using vacuum filtration machine, suction filtration separation obtains sediment；
Electric drying oven with forced convection is put the precipitate in, 10h is dried at 102 DEG C, is then placed in chamber type electric resistance furnace, with 6
DEG C/the min rate of heat addition is warming up to 450 DEG C, constant temperature calcining 6h.
The roasting sample of step is ground, the powder of 60~80 mesh is screened out, obtains finished catalyst.
By 250mLCODCrFor 2000mg/L stimulated dye wastewater, it is placed in 0.5LGS type reactors, while putting into this reality
The catalyst 2g/L of example preparation is applied, 180 DEG C of reaction temperature is set, temperature rises to 180 DEG C and is passed through oxygen to partial pressure of oxygen 1.0MPa,
Start timing to 90min reactions to terminate.
【Comparative example 1】
Reaction condition be the same as Example 1, but it is added without catalyst.By 250mLCODCrFor 2000mg/L stimulated dye wastewater,
It is placed in 0.5LGS type reactors, does not put into catalyst, set 180 DEG C of reaction temperature, temperature rises to 180 DEG C and is passed through oxygen to oxygen
Partial pressure 1.0MPa, starts timing and terminates to 90min reactions.
Handle stimulated dye wastewater the results are shown in Table 1.
Table 1
From table 1, the catalyst of embodiment 1~3 is fine to the treatment effect of percolate.Because nothing in comparative example 1
Catalyst, the oxidation efficiency of waste water is very low；Illustrate the work of Ru-Fe-Co-La-Ti composite catalysts prepared using coprecipitation
Property it is high, achieve unexpected effect.
Claims (6)
1. a kind of catalysis process of co-precipitation Ru-Fe-Co-La-Ti composite catalysts, it is characterised in that in terms of parts by weight, urge
The component of agent includes：
(a) 5 parts of RuCl3；
(b) 6 parts of Fe2(SO4)3；
(c) 7 parts of Co (NO3)2·6H2O；
(d) 9 parts of LaCl3·6H2O；
(e) 8 parts of TiO2；
(f) 65 parts of distilled water；
The catalytic wet oxidation catalyst is adopted to be prepared with the following method：
(1) catalytic component, preparing metal salting liquid are weighed according to each component of above-mentioned co-precipitation composite catalyst；
(2) under the conditions of medium-speed magnetic stirring, by 2.0mol/L NH3It is molten that OH solution instills metal salt with 5 drops/min speed
In liquid, make precipitating reagent NH3OH is well mixed with salting liquid and generates sediment, keeps the pH value 9~10 of mixed liquor；
(3) sediment and solution of step (2) are placed in ultrasonic cleaning machine, ultrasonic disperse, Aging Temperature is 35-95 DEG C, old
The change time is 2-5h；
(4) drain well, distillation water washing is used three times by the sediment after ageing, then is washed three times with absolute ethyl alcohol, is then made
With vacuum filtration machine, suction filtration separation obtains sediment；
(5) sediment for obtaining step (4) is placed in 100~120 DEG C of electric drying oven with forced convections, 8~14h of drying time；So
After be placed in chamber type electric resistance furnace, 300~750 DEG C, 1.5~14h of constant temperature calcining are warming up to the 6 DEG C/min rate of heat addition.
(6) sample for being calcined step (5) is ground, and is screened out the powder of 60~80 mesh, is obtained finished catalyst；
The composition of CWO device includes used in the co-precipitation composite catalyst：Oxygen tank, first pressure table,
Intake valve, outlet valve, agitating device, autoclave, thermocouple, second pressure table, explosive valve, electrothermal furnace, controller.The oxidation
Steel cylinder is connected by first pressure table and intake valve with autoclave, and the autoclave includes agitating device, thermocouple and electric heating
Stove, the thermocouple is connected by second pressure device with explosive valve, and the agitating device and electrothermal furnace are connected with controller.
2. the catalysis process of the co-precipitation Ru-Fe-Co-La-Ti composite catalysts according to claim 1, its feature exists
In Aging Temperature is 50 DEG C.
3. the catalysis process of the co-precipitation Ru-Fe-Co-La-Ti composite catalysts according to claim 1, its feature exists
In digestion time is 3h.
4. the catalysis process of the co-precipitation Ru-Fe-Co-La-Ti composite catalysts according to claim 1, its feature exists
In the drying is that sample is dried into 12h under 100 DEG C of ventilation conditions.
5. the catalysis process of the co-precipitation Ru-Fe-Co-La-Ti composite catalysts according to claim 1, its feature exists
In the roasting is that the sample of drying is placed in high temperature box type resistance furnace, and setting temperature is warming up to the 5 DEG C/min rate of heat addition
450 DEG C of roastings of degree.
6. the catalysis process of the co-precipitation Ru-Fe-Co-La-Ti composite catalysts according to claim 1, its catalysis is wet
Formula oxidation unit application method is that waste water and catalyst are loaded into reactor, begun to warm up after sealing, is raised to logical during design temperature
Enter oxygen and reach setting pressure, while opening agitating device.Now it is set to the zero point of reaction, later at regular intervals by taking
Sample pipe is sampled, during sampling, and opens oxygen supply valve constant with the stagnation pressure of maintenance reaction system.
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| CN112678940A (en) * | 2020-12-02 | 2021-04-20 | 厦门大学 | Method for treating wastewater |
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| CN112337472A (en) * | 2020-11-27 | 2021-02-09 | 湖南湘牛环保实业有限公司 | Catalyst for removing COD (chemical oxygen demand) in wastewater by Fenton oxidation method, preparation method and application |
| CN112337472B (en) * | 2020-11-27 | 2023-08-11 | 湖南湘牛环保实业有限公司 | Catalyst for removing COD in wastewater by Fenton oxidation method, preparation method and application |
| CN112371115A (en) * | 2020-12-02 | 2021-02-19 | 厦门大学 | Catalyst for treating wastewater and preparation method thereof |
| CN112678940A (en) * | 2020-12-02 | 2021-04-20 | 厦门大学 | Method for treating wastewater |
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