CN103920494B - The application of the catalyst of catalytic wet oxidation method for preparing catalyst and preparation - Google Patents
The application of the catalyst of catalytic wet oxidation method for preparing catalyst and preparation Download PDFInfo
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- CN103920494B CN103920494B CN201410135952.4A CN201410135952A CN103920494B CN 103920494 B CN103920494 B CN 103920494B CN 201410135952 A CN201410135952 A CN 201410135952A CN 103920494 B CN103920494 B CN 103920494B
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Abstract
The invention discloses a kind of catalytic wet oxidation method for preparing catalyst, described preparation method comprises the following steps: 1. the natural crystal with catalytic wet oxidation catalyst activity component is obtained natural minerals concentrate after Mineral separation enrichment; 2. the concentrate of step 1 gained is passed through washing, filtration step, put into drying box, dry under 50-100 DEG C of condition; 3. step 2 gained concentrate is after drying put into calciner, at the roasting temperature 2-5 hour of 400-700 DEG C; 4. take out from calciner after the concentrate cooling after roasting, through grinding, obtain catalytic wet oxidation catalyst.The present invention directly adopts natural crystal separation and concentration gained concentrate gained catalyst after simple process, compared to the catalytic wet oxidation catalyst preparation mode of carrier+active component in the past, has started a kind of new thoughtcast.The preparation method of catalyst is convenient and simple, with the obvious advantage economically, obvious to the organic treatment effect in water.
Description
Technical field
The present invention relates to a kind of preparation of catalyst and the application of catalyst, be specifically related to the application of the catalyst of a kind of catalytic wet oxidation method for preparing catalyst and preparation.
Background technology
Wet raw noodles (catalyticwetairoxidation, be called for short CWAO) be by means of catalyst, under certain pressure and temperature, high concentration, difficult degradation and poisonous organic wastewater are oxidized to a kind of oxidation technology of carbon dioxide, water and small organic molecule.Wet Catalytic Oxidation Method is the advanced technology of a kind of efficient process high concentration hard-degraded organic waste water that nearly 2O years development is got up.This method is the improvement of traditional chemical oxidizing process, and application prospect is very wide.The key of wet raw noodles is greater activity, the preparation of the effective catalyst of universality, durability and effectively using.Adding of catalyst, the activation energy of reaction can be reduced, thus reduce the temperature and pressure of reaction, reaction is carried out in relatively mild condition with in the shorter time, improve oxidative decomposition capacity, reduce costs, for its industrial applications creates essential condition.
In prior art, adopt Fe
2o
3/ CNT(CNT) catalyst is under phenol and hydrogen peroxide initial mass concentration are respectively 350 and 1500mg/L, catalyst amounts are 1.0g/L, temperature 80 DEG C of conditions, and through the reaction of 240min, phenol clearance reaches 100%.It is too high to there is reaction temperature demand in the method, and the reaction time is also partially long, is unfavorable for applying.
Adopt flyash catalyst at 30 DEG C, pH=2, the initial concentration of hydrogen peroxide and phenol is respectively 0.60mol/L and 0.15mol/L, reaction time is 100min, flyash consumption is 6.0%, and mixing speed is under the condition of 1000r/min, and flyash has good catalytic activity, can catalyzing hydrogen peroxide oxidation of phenol effectively, the clearance of phenol can reach about 83%.The defects such as it is more complicated that the method exists treatment conditions, and treatment effect is not ideal enough.
Patent " a kind of activated charcoal carried copper oxide catalyst and preparation method thereof " (application number 200610089575.0) adopts activated charcoal carried copper oxide to make catalyst and H
2o
2acting in conjunction catalytic oxidation treatment coking chemical waste water.
Patent " a kind of preparation method of catalyst of CWO organic pollutants " (application number 201310117329.1).Adopt SBA-15 molecular sieve to be carrier, CuO is that active component is oxidized Organic substance in water as catalyst.
Patent " application of a kind of complex function nano-sphere catalyst with recyclable function of carried noble metal and the reduction of catalysis p-nitrophenol thereof " (application number 201310091252.5) adopts and is coated in polymer by noble metal nano particles and magnetic nanoparticle, obtains the complex function nano-sphere catalyst of carried noble metal in polar solvent.
The catalyst that uses in prior art exist can reusing not good, catalyst preparation process is complicated, the high deficiency of catalytic reaction condition, have impact on the application of this technology.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, the application of the catalyst of a kind of catalytic wet oxidation method for preparing catalyst of solving the problem and preparation is provided.
For solving above-mentioned technical problem, the present invention by the following technical solutions:
A kind of catalytic wet oxidation method for preparing catalyst, described preparation method comprises the following steps:
1. the natural crystal with catalytic wet oxidation catalyst activity component is obtained natural minerals concentrate after Mineral separation enrichment;
2. the concentrate of step 1 gained is passed through washing, filtration step, put into drying box, dry under 50-100 DEG C of condition;
3. step 2 gained concentrate is after drying put into calciner, at the roasting temperature 2-5 hour of 400-700 DEG C;
4. take out from calciner after the concentrate cooling after roasting, through grinding, obtain catalytic wet oxidation catalyst.
Further technical scheme is that above-mentioned steps 2 replaces with following step:
A. be immersed among the aqueous solution by the concentrate of step 1 gained, dip time is between 10-48 hour;
B. step a gained is passed through filtration, washing step through the concentrate of impregnation process, concentrate is in without maceration extract Restzustand, put into drying box dry under 50-100 DEG C of condition.
Further technical scheme to be natural crystal be in ilmenite, vanadium titano-magnetite, pyrolusite, cuprite one or more.
Further technical scheme is drying box is thermostatic drying chamber.
The further technical scheme one that to be the aqueous solution be in acid, alkali, saline solution.
Further technical scheme is acid, alkali, salt comprises: hydrochloric acid, nitric acid, sulfuric acid; Ammoniacal liquor, NaOH; One in ammonium chloride, ammonium sulfate.
Further technical scheme is the aqueous solution when being ammonia spirit, and described ammonia spirit concentration is 22%-25%; The described aqueous solution is that except ammonia spirit during other acid-base salt solution, concentration is 0.5-5%.
Further technical scheme grinds the graininess that the powdered or diameter of concentrate is 0.01 millimeter to 1.5 millimeters in preparation method in step 4; In above-mentioned preparation method, grind into powder there is no very little particle requirement, only requires generally Powdered; Catalyst can directly be applied among catalytic wet oxidation process with Powdered, applies after also can carrying out forming processes to powder again.
Further technical scheme is the catalytic wet oxidation catalyst application organic matter in catalytic wet oxidation Treatment Solution prepared.
Further technical scheme is that the catalytic wet oxidation catalyst application for preparing is in catalytic wet oxidation process organic pollutant waste water.
Compared with prior art, one of beneficial effect of the present invention is: the present invention directly adopts natural crystal separation and concentration gained concentrate gained catalyst after simple process, compared to the catalytic wet oxidation catalyst preparation mode of carrier+active component in the past, start a kind of new thoughtcast.The preparation method of catalyst is convenient and simple, with the obvious advantage economically.When gained solid catalyst is applied to heterogeneous Fenton system, obvious to the organic treatment effect in water.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment 1
The preparation of catalyst
(1) by the separation and concentration after ore dressing of one or more in natural ilmenite, vanadium titano-magnetite, pyrolusite, cuprite, in the present embodiment, selected natural ore is just enumerated, be not exhaustive, as long as there is the natural crystal of catalytic wet oxidation catalyst activity component namely within the scope of this, what exemplify in concrete the present embodiment is select vanadium titano-magnetite, the ilmenite concentrate that separation and concentration obtains after ore dressing;
(2), among concentrated ammonia liquor gained ilmenite concentrate being immersed in 22%, dip time was at 24 hours;
(3) step (2) gained is passed through filtration through the ilmenite concentrate of impregnation process, the steps such as washing make it to be in without ammoniacal liquor Restzustand, put into thermostatic drying chamber with 60 DEG C of dryings;
(4) step (3) gained ilmenite concentrate is after drying divided into 3 parts, is labeled as catalyst A, catalyst B, catalyst C put into different roaster respectively at the roasting temperature 3 hours of 300 DEG C, 450 DEG C, 600 DEG C.
(5) take out from roaster after the ilmenite concentrate cooling after roasting, grind into powder, obtains catalyst A, catalyst B, catalyst C.
The application of catalyst
The initial concentration of organic wastewater is the phenol solution of 10mg/L, and the initial concentration of hydrogen peroxide is commercially available hydrogen peroxide concentration, atmospheric operation, pH=5, after process 90min.Catalyst A use amount is 30g/l, and treatment temperature is 30 DEG C, and the clearance of Pyrogentisinic Acid can reach more than 90%; Catalyst B use amount is 30g/l, and treatment temperature is 20 DEG C, and the clearance of Pyrogentisinic Acid can reach more than 96%; Catalyst C use amount is 40g/l, and treatment temperature is 30 DEG C, and the clearance of Pyrogentisinic Acid can reach more than 88%.
Embodiment 2
The preparation of catalyst
(1) natural vanadium titano-magnetite separation and concentration after ore dressing is obtained ilmenite concentrate;
(2), among sodium hydroxide solution gained ilmenite concentrate being immersed in concentration 12g/l, dip time was at 20 hours;
(3) step (2) gained is passed through filtration through the ilmenite concentrate of impregnation process, the steps such as washing make it to be in without maceration extract Restzustand, put into thermostatic drying chamber with 50 DEG C of dryings;
(4) step (3) gained ilmenite concentrate is after drying put into roaster at the roasting temperature 3 hours of 450 DEG C.
(5) take out from roaster after the ilmenite concentrate cooling after roasting, grind into powder, obtains catalyst D.
The application of catalyst
The initial concentration of organic wastewater is the phenol solution of 10mg/L, and catalyst D consumption is 30g/l, and the initial concentration of hydrogen peroxide is commercially available hydrogen peroxide concentration, and treatment temperature is 30 DEG C, atmospheric operation, pH=5, and after process 90min, the clearance of phenol can reach more than 96%.
Embodiment 3
The preparation of catalyst
(1) natural vanadium titano-magnetite separation and concentration after ore dressing is obtained ilmenite concentrate;
(2), among hydrochloric acid solution gained ilmenite concentrate being immersed in concentration 0.4mol/l, dip time was at 20 hours;
(3) step (2) gained is passed through filtration through the ilmenite concentrate of impregnation process, the steps such as washing make it to be in without maceration extract Restzustand, put into thermostatic drying chamber with 50 DEG C of dryings;
(4) step (3) gained ilmenite concentrate is after drying put into roaster at the roasting temperature 3 hours of 450 DEG C.
(5) take out from roaster after the ilmenite concentrate cooling after roasting, grind into powder, obtains catalyst E.The application of catalyst
The initial concentration of organic wastewater is the phenol solution of 10mg/L, and catalyst E consumption is 10g/l, and the initial concentration of hydrogen peroxide is commercially available hydrogen peroxide concentration, and treatment temperature is 30 DEG C, atmospheric operation, pH=5, and after process 90min, the clearance of phenol can reach more than 90%.
Embodiment 4
The preparation of catalyst
(1) natural vanadium titano-magnetite separation and concentration after ore dressing is obtained ilmenite concentrate;
(2), among ammonium sulfate gained ilmenite concentrate being immersed in concentration 20g/l, dip time was at 20 hours;
(3) step (2) gained is passed through filtration through the ilmenite concentrate of impregnation process, the steps such as washing make it to be in without maceration extract Restzustand, put into thermostatic drying chamber with 50 DEG C of dryings;
(4) step (3) gained ilmenite concentrate is after drying put into roaster at the roasting temperature 3 hours of 450 DEG C.
(5) take out from roaster after the ilmenite concentrate cooling after roasting, grind into powder, obtains catalyst F.
The application of catalyst
The initial concentration of organic wastewater is the phenol solution of 10mg/L, and catalyst F consumption is 10g/l, and the initial concentration of hydrogen peroxide is commercially available hydrogen peroxide concentration, and treatment temperature is 10 DEG C, atmospheric operation, pH=5, and after process 90min, the clearance of phenol can reach more than 92%.
Embodiment 5
The preparation of catalyst
(1) natural vanadium titano-magnetite separation and concentration after ore dressing is obtained ilmenite concentrate;
(2), among ammonium chloride solution gained ilmenite concentrate being immersed in concentration 20g/l, dip time was at 20 hours;
(3) step (2) gained is passed through filtration through the ilmenite concentrate of impregnation process, the steps such as washing make it to be in without maceration extract Restzustand, put into thermostatic drying chamber with 50 DEG C of dryings;
(4) step (3) gained ilmenite concentrate is after drying put into roaster at the roasting temperature 3 hours of 450 DEG C.
(5) take out from roaster after the ilmenite concentrate cooling after roasting, grind into powder, obtains catalyst G.The application of catalyst
The initial concentration of organic wastewater is the phenol solution of 10mg/L, and catalyst G consumption is 10g/l, and the initial concentration of hydrogen peroxide is commercially available hydrogen peroxide concentration, and treatment temperature is 10 DEG C, atmospheric operation, pH=5, and after process 90min, the clearance of phenol can reach more than 92%.
Embodiment 6
The preparation of catalyst
(1) natural vanadium titano-magnetite is obtained ilmenite concentrate after beneficiation enrichment is separated;
(2) step (1) gained ilmenite concentrate is passed through washing, after the steps such as filtration make it, put into thermostatic drying chamber with 80 DEG C of dryings;
(3) step (2) gained ilmenite concentrate is after drying put into roaster with the temperature calcination 3 hours of 450 DEG C.
(4) take out from roaster after the ilmenite concentrate cooling after roasting, grind into powder, obtains catalyst H.Without the need to soaking the concentrate of natural minerals in the present embodiment, simpler in operation, cost is lower.
The application of catalyst
The initial concentration of organic wastewater is the phenol solution of 10mg/L, and catalyst H consumption is 5g/l, and the initial concentration of hydrogen peroxide is commercially available hydrogen peroxide concentration, and treatment temperature is 10 DEG C, atmospheric operation, pH=5, and after process 80min, the clearance of phenol can reach more than 98%.Catalytic wet oxidation mineral catalysis agent process organic wastewater Be very effective prepared by the present embodiment.Above-described embodiment takes the lead in introducing a kind of a whole new mind pattern, carrier and active component are organically combined, natural minerals is adopted to carry out Kaolinite Preparation of Catalyst through processing process, without the need to manually combining carrier and active component, carrier fills in conjunction with effect with active component, be used for processing organic polluting water, above-mentioned have processed organic pollutants only to enumerate, and non exhaustive.
Spoken of in this manual " embodiment ", " another embodiment ", " embodiment ", etc., refer to the specific features, structure or the feature that describe in conjunction with this embodiment and be included at least one embodiment of the application's generality description.Multiple place occurs that statement of the same race is not necessarily refer to same embodiment in the description.Furthermore, when describing specific features, structure or a feature in conjunction with any one embodiment, what advocate is also fall within the scope of the invention to realize this feature, structure or feature in conjunction with other embodiments.
Although with reference to the multiple explanatory embodiment of inventing, invention has been described here, but, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.More particularly, in the scope of the open claim of the application, multiple modification and improvement can be carried out to the building block of subject combination layout and/or layout.Except the modification of carrying out building block and/or layout is with except improvement, to those skilled in the art, other purposes also will be obvious.
Claims (8)
1. a catalytic wet oxidation method for preparing catalyst, is characterized in that: described preparation method comprises the following steps:
1), the natural crystal with catalytic wet oxidation catalyst activity component is obtained natural minerals concentrate after Mineral separation enrichment; Described natural crystal is one or more in ilmenite, vanadium titano-magnetite, pyrolusite, cuprite;
2), by step 1) concentrate of gained through washing, filtration step, put into drying box dry;
3), by step 2) gained concentrate after drying puts into calciner, at the roasting temperature 2-5 hour of 400-700 DEG C;
4) take out from calciner after the concentrate cooling, after roasting, through grinding, obtain catalytic wet oxidation catalyst;
The described catalytic wet oxidation catalyst application prepared organic matter in catalytic wet oxidation Treatment Solution.
2. catalytic wet oxidation method for preparing catalyst according to claim 1, is characterized in that described step 2) replace with following step:
A. by step 1) concentrate of gained is immersed among the aqueous solution, and dip time is between 10-48 hour;
B. step a gained is passed through filtration, washing step through the concentrate of impregnation process, concentrate is in without maceration extract Restzustand, put into drying box dry under 50-100 DEG C of condition.
3. catalytic wet oxidation method for preparing catalyst according to claim 1 and 2, is characterized in that described drying box is thermostatic drying chamber.
4. catalytic wet oxidation method for preparing catalyst according to claim 2, is characterized in that the described aqueous solution is the one in acid, alkali, saline solution.
5. catalytic wet oxidation method for preparing catalyst according to claim 4, is characterized in that described acid, alkali, salt comprise: hydrochloric acid, nitric acid, sulfuric acid; Ammoniacal liquor, NaOH; One in ammonium chloride, ammonium sulfate.
6. the catalytic wet oxidation method for preparing catalyst according to claim 2 or 4, when it is characterized in that the described aqueous solution is ammonia spirit, described ammonia spirit concentration is 22%-25%; The described aqueous solution is that except ammonia spirit during other acid-base salt solution, concentration is 0.5-5%.
7. catalytic wet oxidation method for preparing catalyst according to claim 1 and 2, is characterized in that described step 4) in the powdered or diameter of grinding concentrate be the graininess of 0.01 millimeter to 1.5 millimeters.
8. catalytic wet oxidation method for preparing catalyst according to claim 1, is characterized in that the described catalytic wet oxidation catalyst application prepared is in catalytic wet oxidation process organic pollutant wastewater.
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| CN1857768A (en) * | 2006-06-06 | 2006-11-08 | 北京科技大学 | Process of preparing photocatalyst material with concentrated ilmenite |
| CN101259413A (en) * | 2008-04-03 | 2008-09-10 | 北京科技大学 | Method for preparing photocatalytic material by titanic iron ore ore concentrate wet chemical method |
| CN101422721A (en) * | 2008-11-06 | 2009-05-06 | 浙江工业大学 | Novel absorption material and preparation method and use thereof |
| CN102502944A (en) * | 2011-11-21 | 2012-06-20 | 北京林业大学 | Zone heterogeneous catalytic oxidation technology for removing pollutants by red-mud catalyst |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1857768A (en) * | 2006-06-06 | 2006-11-08 | 北京科技大学 | Process of preparing photocatalyst material with concentrated ilmenite |
| CN101259413A (en) * | 2008-04-03 | 2008-09-10 | 北京科技大学 | Method for preparing photocatalytic material by titanic iron ore ore concentrate wet chemical method |
| CN101422721A (en) * | 2008-11-06 | 2009-05-06 | 浙江工业大学 | Novel absorption material and preparation method and use thereof |
| CN102502944A (en) * | 2011-11-21 | 2012-06-20 | 北京林业大学 | Zone heterogeneous catalytic oxidation technology for removing pollutants by red-mud catalyst |
Non-Patent Citations (1)
| Title |
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| 膨润土改性与印染废水脱色研究;林蔚 等;《齐齐哈尔大学学报》;20100531;第26卷(第3期);参见第1.1、1.3.1.1、1.3.1.2、1.3.1.3、1.3.1.4节、第3节 * |
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