CN101259428B - Preparation of catalyst for processing industrial wastewater and using method thereof - Google Patents
Preparation of catalyst for processing industrial wastewater and using method thereof Download PDFInfo
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- CN101259428B CN101259428B CN2008100709578A CN200810070957A CN101259428B CN 101259428 B CN101259428 B CN 101259428B CN 2008100709578 A CN2008100709578 A CN 2008100709578A CN 200810070957 A CN200810070957 A CN 200810070957A CN 101259428 B CN101259428 B CN 101259428B
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Abstract
The present invention provides a preparation and application method for treating a catalyst of industrial waste water. The preparation method of the invention adopts a molecular sieve as a carrier, one or a plurality of P-type semiconductor oxides such as MnO2, CeO2, Ag2O, CuO, etc. is/are loaded on the molecular sieve in a way of ion-exchange and finally a supported catalyst containing the P-type semiconductor oxides is obtained through molding; and the catalyst is used when ozone and light are coexisted. The preparation and application method of the invention aims at the disadvantages of that active constituents of the catalyst and an addition agent in the combination technique of ozone and catalyst are lost easily, active constituents are loaded on the molecular sieve carrier in the way of ion-exchange so as to improve the combination binding capacity of the active constituents and the carrier; and an electronic addition agent can be substituted through a light electro-donating effect, so as to effectively provide electrons in a long term and promote the catalyst and the ozone to generate active matters; the coaction of the catalyst and the ozone can enhance the activity stability of the catalyst and prolong service life, thus being conducive to industrialization of the technologies.
Description
Technical field
The invention belongs to the chemical catalyst field, more specifically relate to a kind of processing industrial wastewater Preparation of catalysts and using method thereof.
Background technology
The improvement of industrial wastewater and to utilize be the main aspect that environmental friendliness is produced again.Present widely used technology for treating industrial waste water is generally conventional methods such as physical absorption, chemical precipitation and microorganism decomposition.These processing methods can't thoroughly be removed pollutants in waste water, and the waste water after it is handled also can't utilize again.For this reason, the waste water that common process was handled must pass through technologies such as catalytic wet oxidation, electrolytic oxidation, ozone oxidation, photocatalysis, constant temperature catalyzing and carry out the deep oxidation processing, with further reduction pollutants in waste water.Yet there is shortcoming separately in these methods: catalytic wet oxidation technology is temperature required higher, and power consumption is big; Electrolysis oxidation process not only consumes energy, and disposal ability is also lower; The ozonation technology disposal ability is stronger, but the cost height; Though photocatalysis advanced treating oxidize contaminants, disposal ability is very limited; Room-temperature catalytic oxidation PROCESS FOR TREATMENT ability a little less than, applicable object is limited.Thereby simple a kind of treatment process often can't really satisfy industrialized demand.On this basis, people further get up these deep oxidation process combination, to improve disposal ability.As, the combination of combination, ozone and catalyst by ultraviolet lighting and ozone all can improve the ability of ozone oxidation contaminated wastewater thing.Yet the combination of ultraviolet lighting and ozone is very high to the dependency degree of ozone, needs a large amount of ozone ability effectively.In the combination of ozone and catalyst, active component has higher degrading activity to ozone in the catalyst, makes it produce a large amount of O
2-, O
2 2-Deng anion active oxygen species and improve the ozone oxidation ability.These active components comprise Ag
2O, NiO, Fe
2O
3, Co
3O
4, CeO
2, MnO
2, P-type semiconductor oxides such as CuO.The ozone degrading activity of P-type semiconductor oxide is higher, and its reason may be the O that reaction produces
2-, O
2 2-Deng the anion oxygen species by Coulomb force and catalyst surface effect and can be on P-type semiconductor stable existence, make its electricity lead increase, thereby strengthened the reactivity of catalyst.Further studies show that, in catalyst, add K
2Electronics auxiliary agents such as O can improve the ozone degrading activity of catalyst.Yet the loss of the catalyst long-term use in solution will causing active component and auxiliary agent causes very easily inactivation and can't realize industrialization of catalyst.Therefore, how to prevent active component in the catalyst loss, to improve activity of such catalysts stability be to influence the principal element that ozone and catalyst combination technology are applied to handle industrial wastewater.The illumination effect is actual to be a process that electronics is provided, thereby if can excite the activity of such catalysts component by illumination, might make its generation electronics and improve activity.The effect that is the electronics auxiliary agent can realize with the illumination of suitable wavelength.And for the load of active component, available special method makes and stronger chemical action takes place in the middle of active component and the carrier, reduces and avoids its leakage.
Summary of the invention:
The invention provides a kind of processing industrial wastewater Preparation of catalysts and using method, the present invention is directed to catalyst activity component and the easy shortcoming that runs off of auxiliary agent in ozone and the catalyzed combination technology, by ion-exchange method with active constituent loading on molecular sieve carrier, to improve the binding ability of active component and carrier; The preparation method is simple, and raw material sources are extensive, and by illumination replace the electronics auxiliary agent so that electronics to be provided long-term effectively to electronic action, promote catalyst and ozone generating active specy; Both actings in conjunction will improve activity of such catalysts stability and service life, and then help the industrialization of this type of technology.
Processing industrial wastewater Preparation of catalysts method of the present invention is characterized in that: described Preparation of catalysts method is to be carrier with the molecular sieve, with ion-exchange method with MnO
2, CeO
2, Ag
2In P-type semiconductor such as O, the CuO oxide one or more load on the molecular sieve, make the loaded catalyst that contains the P-type semiconductor oxide by moulding at last.
The using method of processing industrial wastewater catalyst of the present invention is characterized in that: described catalyst uses in the presence of ozone and illumination jointly.
Remarkable advantage of the present invention is:
(1) on the one hand, the present invention has improved the bond strength between active component and carrier with the ion-exchange method load active component, can reduce the loss of active component; On the other hand, the present invention utilizes the electronics promoter effect in the illumination alternative catalysts, can avoid the activity decline of running off and being caused because of the electronics auxiliary agent.
(2) technology of catalyst elder generation load active component aftershaping can improve the ability of catalyst cupport active component effectively, and the use of moulding catalyst also can reduce catalyst separation and the recovery problem of being brought in the fine catalyst use.
(3) catalyst of the present invention is easy to use, can handle the organic pollution in the industrial wastewater long-term effectively.
The specific embodiment
The present invention is that mode with ion-exchange is at molecular sieve carrier area load MnO
2, CeO
2, Ag
2In P-type semiconductor such as O, the CuO oxide one or more are by making the loaded catalyst that weight content is 0.5～10.0%P type semiconductor oxide after the moulding.
Preparation process of the present invention is as follows:
(1) but place pyrolytic to become the water-soluble metal salting liquid of P-type semiconductor oxide molecular sieve powder, both weight ratios are 1: 5～1: 50, under 10～95 ℃ of temperature conditions, fully stirred 8～48 hours, leave standstill back elimination redundant solution, the oven dry back contains the fine catalyst that weight content is 0.5～10%P type semiconductor oxide 300～800 ℃ of roastings 2～6 hours to make under 60～200 ℃ of low temperature;
(2) moulding of catalyst: in percentage by weight is the fine catalyst of step (1) preparation of 77～94wt%, add the adhesive of 5～20wt%, the expanding agent of 1～3wt% mixes, in described mixture, add the concentration account for mixture weight 30～50wt% and be 2～10% dilute nitric acid solution, utilize banded extruder to be squeezed into strip after fully mixing, 400～600 ℃ of oven dry 2～4 hours, obtain the strip catalyst of side pressure strength after 80～150 ℃ of oven dry greater than 20N/cm.
It is that cation is Mn that but pyrolytic becomes the water-soluble metal salting liquid of P-type semiconductor oxide
2+, Ce
4+, Ag
+Or Cu
2+Sulfate solution, nitrate aqueous solution or acetate aqueous solution in a kind of, the cation concn of described water-soluble metal salting liquid is 0.005～0.5M.
Adhesive is a hydrated alumina.
Expanding agent is organic expanding agent.
The catalyst that technology of the present invention makes uses under ozone and illumination acting in conjunction; Light wavelength is 180～800nm during illumination.
Below in conjunction with embodiment the present invention is specifically described, but the present invention not only is confined to this.
Embodiment 1
Ion-exchange prepares MnO
2/ ZSM-5 catalyst
Taking by weighing 50 gram silica alumina ratios is that 25 H-ZSM-5 molecular sieve is in beaker, adding 1.0L contains the aqueous solution of 6.0 gram manganese sulfates, stirred 24 hours down at 80 ℃, leave standstill the supernatant liquor that inclines, the oven dry back rises to 300 ℃ of constant temperature calcinings 4 hours by the speed of 2 ℃/min under 120 ℃.The catalyst that roasting is made is crushed into powder, add hydrated alumina (boehmite) 15 grams, organic expanding agent 3 grams, mixing back adding concentration is the dilute nitric acid solution 40mL of 5.0V%, continuing to be kneaded into bulk, then is the clover shape of φ=2.0mm with the banded extruder extrusion modling.100 ℃ of oven dry rose to 500 ℃ of constant temperature 4 hours by the speed of 2 ℃/min after 2 hours, made the MnO of trifolium-shaped strip after the cooling
2/ ZSM-5 catalyst.MnO in this catalyst
2Content is about 3.0w%.
Embodiment 2
Ion-exchange prepares Ag
2The O/Y catalyst
Take by weighing 50 gram H-Y molecular sieves in beaker, add the aqueous solution that 1.0L contains 3.0 gram silver nitrates, then make Ag by the method among the embodiment 1
2O content is about the Ag of 3.0w%
2The O/Y catalyst.
Embodiment 3
Ion-exchange prepares the CuO/ZSM-5 catalyst
Take by weighing 50 gram silica alumina ratios and be 25 H-ZSM-5 molecular sieve in beaker, add 1.0L and contain the aqueous solution of 5.0 gram Schweinfurt greens then by make the CuO/ZSM-5 catalyst that contains CuO 3.5w% by the method among the embodiment 1.
Embodiment 4
Ion-exchange prepares MnO
2-CeO
2/ ZSM-5 catalyst
Take by weighing 50 gram silica alumina ratios and be 25 H-ZSM-5 molecular sieve in beaker, add the aqueous solution that 1.0L contains manganese nitrate 4.0 grams and cerous nitrate 3.0 grams, then make MnO by the method among the embodiment 1
2Content is 2.0w%, CeO
2Content is the MnO of 2.0w%
2-CeO
2/ ZSM-5 catalyst.
Embodiment 5
Immersion process for preparing MnO
2/ ZSM-5 catalyst
Taking by weighing 50 gram silica alumina ratios is 25 H-ZSM-5 type molecular sieve powder, add boehmite 15 grams, organic expanding agent 3 grams, mixing back adding concentration is the dilute nitric acid solution 40mL of 5.0V%, continue to be kneaded into bulk, extruding then becomes the trifolium-shaped of φ=2.0mm.100 ℃ of oven dry rose to 500 ℃ of constant temperature 4 hours by the speed of 2 ℃/min after 2 hours, made trifolium-shaped strip ZSM-5 carrier.Then take by weighing 50 gram shaping carriers and be immersed in the aqueous solution that 200mL contains 5.0 gram manganese sulfates, room temperature dipping 8 hours, then rotary evaporation drying.100 ℃ of oven dry rose to 500 ℃ of constant temperature 4 hours by the speed of 2 ℃/min after 2 hours, made the MnO of trifolium-shaped strip after the cooling
2/ ZSM-5 catalyst.MnO in this catalyst
2Content is about 3.0w%.
Embodiment 6
Immersion process for preparing Ag
2The O/Y catalyst
To be immersed into the aqueous solution that 200mL contains 2.0 gram silver nitrates, room temperature dipping 8 hours, then rotary evaporation drying by trifolium-shaped strip H-Y type molecular sieve carrier 50 grams that embodiment 5 makes.100 ℃ of oven dry rose to 500 ℃ of constant temperature 4 hours by the speed of 2 ℃/min after 2 hours, made the Ag of trifolium-shaped strip after the cooling
2The O/Y catalyst.Ag in this catalyst
2O content is about 3.0w%.
Embodiment 7
Immersion process for preparing Ag
2O-K
2The O/Y catalyst
For the relatively effect of electronics auxiliary agent, the Ag that will make by embodiment 6
2O/Y catalyst 50 grams are immersed into the aqueous solution that 100mL contains 1.0 gram potassium nitrate, room temperature dipping 8 hours, then rotary evaporation drying.100 ℃ of oven dry rose to 500 ℃ of constant temperature 4 hours by the speed of 2 ℃/min after 2 hours, made the Ag of trifolium-shaped strip after the cooling
2O-K
2The O/Y catalyst.Ag in this catalyst
2O content is about 3.0w%, K
2O content is 1.0w%.
Embodiment 8
The performance evaluation of catalyst treatment waste water
The catalyst that embodiment 1-7 is made is seated in a caliber 5cm respectively, volume is in the quartz tube reactor of 20L, estimates its handling property to petrochemical wastewater.The uviol lamp that it is 254nm that reactor is equipped with 2 30W dominant wavelengths on every side, COD content is about 110mg/L in the waste water raw material, and charging rate is 20L/h; Ozone and O
2The mode of mixing adds, and wherein ozone content is 30v%, and the gaseous mixture input amount is 100L/h.The handling property of evaluate catalysts under the situation of turning on light, turning off the light respectively.The content of COD in the outlet waste water of test reaction after 2 hours according to the clearance of the change calculations COD that imports and exports waste water COD concentration, compares the performance of catalyst with this.
Table 1 different catalysts is handled petrochemical wastewater under different condition performance compares
Show in the table 1 that (1) ion-exchange has higher removal COD performance than infusion process; (2) under the unglazed photograph, electronics auxiliary agent K
2Introducing (the Ag of O
2O-K
2O/Y (infusion process)) helps Ag
2The raising that O/Y (infusion process) is active; (3) ultraviolet lighting obviously improves activity of such catalysts, and its facilitation is much remarkable than the electronics auxiliary agent.As seen, ion-exchange has higher removal COD activity than infusion process, and illumination can replace the facilitation of electronics auxiliary agent to activity.
Embodiment 9
The stability evaluation of catalyst
Press the method among the embodiment 8, relatively different catalysts is handled the variation of 7 days process middle outlet waste water COD concentration continuously under the different disposal condition.It the results are shown in Table 2.
Table 2 different catalysts is handled in the waste water COD concentration over time under the different disposal condition
Table 2 result shows, (1) along with the carrying out in reaction time, the Ag of immersion process for preparing under the unglazed photograph
2O-K
2The O/Y catalyst sharply descends to the removal ability of COD; (2) Ag of ion-exchange preparation under the illumination
2The O/Y catalyst not only has good initial activity, and has good active stability; (3) but for the Ag of immersion process for preparing
2O/Y, along with the prolongation in reaction time, catalytic activity is also descending under the illumination effect.This result shows, active component A g
2O and electronics auxiliary agent K
2The loss of O will cause catalyst activity progressively to descend.And the illumination effect can replace the electronics promoter effect, and has good long-term effectiveness.But because the Ag of immersion process for preparing
2Active component A g in the O/Y catalyst
2The loss of O, the illumination effect also can't be kept initial activity.
Claims (3)
1. using method of handling the industrial wastewater catalyst is characterized in that: described Preparation of catalysts method is that mode with ion-exchange is at molecular sieve carrier area load MnO
2, CeO
2, Ag
2In O or the CuO P-type semiconductor oxide one or more are by making the loaded catalyst that weight content is 0.5～10.0%P type semiconductor oxide after the moulding; Preparation process is:
(1) but place pyrolytic to become the water-soluble metal salting liquid of P-type semiconductor oxide molecular sieve powder, both weight ratios are 1: 5～1: 50, under 10～95 ℃ of temperature conditions, fully stirred 8～48 hours, leave standstill back elimination redundant solution, the oven dry back contains the fine catalyst that weight content is 0.5～10%P type semiconductor oxide 300～800 ℃ of roastings 2～6 hours to make under 60～200 ℃ of low temperature;
(2) moulding of catalyst: in percentage by weight is the fine catalyst of step (1) preparation of 77～94wt%, add the adhesive of 5～20wt%, the expanding agent of 1～3wt% mixes, in described mixture, add the concentration account for mixture weight 30～50wt% and be 2～10% dilute nitric acid solution, utilize banded extruder to be squeezed into strip after fully mixing, 400～600 ℃ of oven dry 2～4 hours, obtain the strip catalyst of side pressure strength after 80～150 ℃ of oven dry greater than 20N/cm;
It is that cation is Mn that but described pyrolytic becomes the water-soluble metal salting liquid of P-type semiconductor oxide
2+, Ce
4+, Ag
+Or Cu
2+Sulfate solution, nitrate aqueous solution or acetate aqueous solution in a kind of, the cation concn of described water-soluble metal salting liquid is 0.005～0.5M; Described adhesive is a hydrated alumina; Described expanding agent is organic expanding agent; The use in the presence of illumination and ozone are common of described catalyst.
2. the using method of processing industrial wastewater catalyst according to claim 1 is characterized in that: the using method of this catalyst is installed uviol lamp for catalyst is seated in the reactor around reactor, wastewater feed speed is 20L/h, ozone and O
2The mode of mixing adds, and the gaseous mixture input amount is 100L/h.
3. the using method of processing industrial wastewater catalyst according to claim 1 and 2 is characterized in that: light wavelength is 180～800nm during described illumination.
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