CN111437808A - Density-controllable catalyst material for catalyzing ozone oxidation - Google Patents
Density-controllable catalyst material for catalyzing ozone oxidation Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
- B01J23/68—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/688—Silver or gold with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with manganese, technetium or rhenium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
Abstract
The invention provides a density-controllable catalyst material for catalyzing ozone oxidation, which is characterized by comprising active catalytic component salt: adhesive: hollow microspheres: the surfactant is used in a mass ratio of 0.5-40: 0-35: 0.5-80: 0 to 5. The hollow glass beads (spheres) are used as main components for regulating and controlling the density of the catalyst, and have the effect similar to that of swimming bladders, so that the effect of suspending or floating the catalyst in a water phase is achieved, and the blocking effect of solid relative to bubbles is reduced. When small bubbles are attached to catalyst particles, the buoyancy of the catalyst is increased, and the catalyst is easy to float or turn over due to the fact that the density of the catalyst is close to that of water, so that further mixing of the catalyst and gas is generated. The small bubbles newly entering the water body and the migrated catalytic site surface have adsorption effect, so that the blending effect of the catalyst and the gas is greatly increased, and the ozone solubility and the three-phase reaction interface site are increased.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to a density-controllable catalyst material for catalyzing ozone oxidation.
Background
Catalytic ozonation as an advanced oxidation technology becomes a research hotspot in the field of advanced wastewater treatment in recent years. The catalytic ozonation technology is further divided into homogeneous catalytic ozonation and heterogeneous catalytic ozonation. The homogeneous catalytic ozonation technology is a catalytic ozonation technology that reactants and a catalyst are in the same phase in water and are not separated; however, the method has the disadvantages of secondary pollution of metal ions and difficult recovery and separation.
At present, heterogeneous catalysts are a kind of catalysts which are used more in environmental engineering, gas-liquid-solid three phases are involved in the heterogeneous ozone catalytic oxidation process, and the form of the catalyst has direct influence on the performance of the ozone catalytic oxidation performance. It mainly includes supported catalysts and unsupported catalysts, and usually consists of stable components such as metal oxides or inorganic non-metallic ceramics, although the types are various. Such substances have high density, and are often formed into a stacked form after being filled into a reaction cavity in the use process, and even if a catalyst in a powder form is adopted, thick mud-like deposition is still formed at the bottom. The structure can lead small bubble gas introduced in the reaction to be extruded and converged at the bottom layer of the catalyst, and combined to form large bubbles to flow upwards (see figure 1), finally lead the diffusion distance of the ozone gas to be increased, reduce the gas-liquid contact area and reduce the dissolution efficiency of the ozone; secondly, the utilization rate of the catalyst at the bottom is high, but the utilization rate at the middle part and above is reduced, part of the catalyst can not contact with ozone, and the efficiency of the whole catalytic reaction device is greatly inhibited.
In the prior art, a two-component composite metal catalyst and application thereof, as well as a carrier Al2O3The active substances of copper oxide and ruthenium are loaded on the catalyst. The catalytic oxidation efficiency of the catalyst is improved by utilizing the characteristic of high catalytic activity of the noble metal. In addition, there has been provided a three-component composite metal catalyst V2O5-TiO2-AlF3/Al2O3And an aluminum oxide carrier is used for loading active components of vanadium pentoxide, titanium dioxide and aluminum fluoride. Because the metal oxide is used as the catalyst component, the density of the catalyst is higher than that of water, and the catalyst is deposited at the bottom, so that the mass transfer efficiency of ozone is reduced. Much research is currently focused on the formulation of catalyst components, but few solutions are available to adjust the catalyst density and thus improve the ozone mass transfer process.
Disclosure of Invention
The invention provides a density-controllable catalyst material for catalyzing ozone oxidation, which adjusts the mixing effect of gas and catalyst particles in catalytic reaction by adjusting the density.
A catalyst material for catalytic ozonation with controllable density, comprising an active catalytic component salt: adhesive: hollow microspheres: the surfactant is used in a mass ratio of 0.5-40: 0-35: 0.5-80: 0 to 5.
Further, the hollow microspheres are one or a combination of hollow glass microspheres, hollow ceramic microspheres and fly ash hollow microspheres.
Further, the density of the hollow microspheres is 0.1-1.0g/cm3Preferably 0.3 to 0.6g/cm 3; the particle size ranges from 1um to 1mm, preferably from 10um to 120 um.
Further, the density of the hollow microspheres is 0.3-0.6g/cm 3; the particle size ranges from 10um to 120 um.
Further, the active catalytic component is one or more water-soluble salts of Mg, Cu, Co, Ni, Mn, Fe, Zn, Ti, Ce, Al, V, Sc, Y, L a, Ag, Au, Pd and Pt.
Further, the active catalytic component is a carbon source such as glucose, chitosan, graphene oxide, etc. to form a carbon material.
Further, the binder includes clay, silicate, titanium oxide, aluminum oxide, etc.,
further, the surfactant comprises one or more of sodium dodecyl benzene sulfonate anionic surfactant, quaternary ammonium salt cationic surfactant and polyoxyethylene nonionic surfactant.
By adopting the technical scheme of the invention, the invention has the following technical effects:
the hollow glass beads (spheres) are used as main components for regulating and controlling the density of the catalyst, and have the effect similar to that of swimming bladders, so that the effect of suspending or floating the catalyst in a water phase is achieved, and the blocking effect of solid relative to bubbles is reduced. When small bubbles are attached to catalyst particles, the buoyancy of the catalyst is increased, and the catalyst is easy to float or turn over due to the fact that the density of the catalyst is close to that of water, so that further mixing of the catalyst and gas is generated. The small bubbles newly entering the water body and the migrated catalytic site surface have adsorption effect, so that the blending effect of the catalyst and the gas is greatly increased, and the ozone solubility and the three-phase reaction interface site are increased.
Drawings
FIG. 1 is a reaction diagram of a conventional alumina-supported catalyst.
FIG. 2 is a reaction diagram of a supported catalyst according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
soaking 100 g of glass microspheres (the density of hollow glass microspheres is 0.6, and the particle size D50 is 45um) in a sodium hydroxide solution, washing with pure water, adding into 500ml of water, adding 1 g of sodium dodecyl benzene sulfonate, uniformly mixing the solution by using a magnetic constant-temperature stirrer, controlling the temperature, and slowly dropwise adding 600ml of Ti (SO)4)2/Ce(NO3)3Mixing the solution with Ti (SO)4)2At a concentration of 0.21 mole/L, Ce (NO)3)3The concentration is 0.02 mole/L, ammonia water is dripped at the same time to always maintain the pH value of the system to be nearly neutral, the reaction lasts for 2 hours, the pH value is 7 after suction filtration and water washing, the powder cake is transferred to an oven with the temperature of 80 ℃ to be dried into powder, the powder is heated to the temperature of 600 ℃ to be calcined for 1 hour, and the activity is obtainedThe component-coated glass bead carrier catalyst has a true density of 0.90g/cm as measured by a gas displacement method3。
Example 2:
soaking 100 g of glass microspheres (the density of the hollow glass microspheres is 0.5, the particle size D50 is 58um) in a sodium hydroxide solution, washing with pure water, adding 300ml of 0.3 wt.% SDBS aqueous solution for soaking, uniformly mixing under mechanical stirring, and dropwise adding 100ml of Cu (Ac)2/Co(Ac)2/Ni (Ac)2Glucose mixed solution of Cu (Ac)2Concentration of 0.6 mole/L, Co (Ac)2Concentration of 0.3 mole/L, Ni (Ac)2The concentration is 0.3 mole/L, the glucose concentration is 0.3 mole/L, the temperature is raised to be about 100 ℃, the liquid is evaporated to dryness under the condition of stirring, the powder is obtained by kneading after cooling, the powder is heated to 580 ℃ and calcined for 2 hours under the protective atmosphere to obtain the glass bead carrier catalyst coated with the active component, and the real density of the glass bead carrier catalyst is 0.98g/cm by a gas replacement method3。
Example 3:
1000 g of glass microspheres (the density of the hollow glass microspheres is 0.3, and the particle size D50 is 72um) are soaked in a sodium hydroxide solution, washed by pure water and dried for later use.
Dissolving 250 g of 3000-mesh industrial yellow clay powder, 80 g of tetrahydrate manganese acetate, 4.5 g of silver nitrate and 15g of sodium dodecyl benzene sulfonate in 1L pure water under mechanical stirring to obtain a dispersion liquid, then carrying out spray dispersion on the dispersion liquid in a disc granulator, granulating the hollow glass bead powder to obtain particles with the size of 1-4mm, transferring the particles to a 50 ℃ oven for drying, heating to 500 ℃ after drying for calcining for 2h, heating to 620 ℃ again for calcining for 30 min to obtain catalyst particles with the active component blended with the glass beads, and testing the actual density of the catalyst particles to be 1.02g/cm by using a gas displacement method3。
Example 4:
soaking 100 g of glass microspheres (the density of hollow glass microspheres is 0.3, and the particle size D50 is 72um) in a sodium hydroxide solution, washing with pure water, adding into 500ml of water, uniformly mixing the solution by using a magnetic constant-temperature stirrer, controlling the temperature, and slowly dropwise adding 600ml of Al2(SO4)3/Mn(NO3)2Mixed solution of Al2(SO4)3Mn (NO) at a concentration of 0.16 mole/L3)3The concentration is 0.31 mole/L, ammonia water is dripped to always maintain the pH value of the system to be nearly neutral, the reaction lasts for 2 hours, the reaction is carried out after the reaction is carried out for washing until the pH value is 7, the pressed powder is transferred to an oven with the temperature of 80 ℃ to be dried into powder, the temperature of the powder is raised to 600 ℃ to be calcined for 1 hour, the glass bead carrier catalyst coated with the active component is obtained, and the actual density of the glass bead carrier catalyst is 1.3。
Example 5:
1000 g of glass microspheres (the density of the hollow glass microspheres is 0.3, and the particle size D50 is 72um) are soaked in a sodium hydroxide solution, washed by pure water and dried for later use.
588 g of 3000-mesh industrial yellow clay powder, 8.4 g of manganese acetate and 84 g of sodium dodecyl sulfate are dissolved in 1.3L pure water under the condition of mechanical stirring to obtain a dispersion liquid, then the dispersion liquid is sprayed and dispersed in a disc granulator to granulate the hollow glass bead powder to obtain particles with the size of 1-4mm, the particles are transferred to a 50 ℃ oven for drying, the temperature is raised to 500 ℃ after drying and calcined for 2 hours, the temperature is raised to 620 ℃ again and calcined for 30 minutes to obtain catalyst particles with the active component, the binder and the glass beads blended, and the actual density of the catalyst particles is tested to be 1.05g/cm by a gas displacement method3The catalytic ozonation performance of the ozone oxidation catalyst in the invention is further explained by taking phenol solution as model organic wastewater and carrying out ozone catalytic oxidation treatment, wherein 300m L100 ppm phenol solution is filled into 5 completely identical 500m L glass column type reaction vessels, the pH of the initial solution is 5-7, one of the reaction vessels is not added with catalyst to be used as a blank control test, 40g of alumina control group catalyst and the ozone oxidation catalyst prepared in the embodiments 1, 2, 3, 4 and 5 of the invention are respectively added into the other three reaction vessels, then ozone mixed gas with effective ozone concentration of 50mg/min is continuously introduced, the sampling is carried out after 20min of reaction, the concentration of TOC in water is analyzed, and the gas is naturally mixed without mechanical stirring in the whole experimental process.
Alumina control group:
adding 100 g of 325-mesh alumina powder into 500ml of water, and adding 1 g of dodecylSodium benzenesulfonate, mixing the solution with magnetic constant temperature stirrer, controlling the temperature, and slowly adding 60ml of Ti (SO)4)2/Ce(NO3)3Mixing the solution with Ti (SO)4)2At a concentration of 0.21 mole/L, Ce (NO)3)3The concentration is 0.02 mole/L, ammonia water is dripped at the same time to always maintain the pH value of the system to be nearly neutral, the reaction lasts for 2 hours, the reaction is carried out by pumping filtration and washing until the pH value is 7, the pressed powder is transferred to an oven with the temperature of 80 ℃ to be dried into powder, the temperature is raised to 600 ℃ after the drying, and the powder alumina carrier catalyst is obtained after the calcination for 1 hour.
The experimental data of the examples and the control group are as follows:
| name of catalyst | TOC concentration of influent water | TOC concentration of effluent | TOC removal Rate |
| Catalyst free blank | 76.5mg/L | 45.5mg/L | 40.5％ |
| Alumina control group | 76.5mg/L | 30.4mg/L | 60.2％ |
| Example 1 | 76.5mg/L | 22.6mg/L | 70.4％ |
| Example 2 | 76.5mg/L | 20.4mg/L | 73.3％ |
| Example 3 | 76.5mg/L | 17.2mg/L | 77.5％ |
| Example 4 | 76.5mg/L | 16.7mg/L | 78.2％ |
| Example 5 | 76.5mg/L | 23.0mg/L | 70.0％ |
In the invention, hollow glass beads (spheres) are used as main components for regulating and controlling the density of the catalyst, and the effect similar to that of swimming bladder is achieved, so that the effect of suspending or floating the catalyst in a water phase is achieved, and the blocking effect of solid relative to bubbles is reduced. When small bubbles are attached to catalyst particles, the buoyancy of the catalyst is increased, and the catalyst is easy to float or turn over due to the fact that the density of the catalyst is close to that of water, so that further mixing of the catalyst and gas is generated. The small bubbles newly entering the water body and the migrated catalytic site surface have adsorption effect, so that the blending effect of the catalyst and the gas is greatly increased, and the ozone solubility and the three-phase reaction interface site are increased.
In the reaction process, a catalyst adopting the traditional alumina as a carrier can form a deposit layer at the bottom of the reaction column, and ozone bubbles become large, as shown in figure 1; the catalyst adopting the hollow glass microspheres for regulating and controlling the catalyst density can be uniformly dispersed in a liquid phase system and is driven to mix by airflow; the introduced ozone bubbles were uniformly distributed without aggregation, as shown in fig. 2. When 20min sampling point, the efficiency is improved by about 10-15% on the whole.
It will be appreciated that the parameters of examples 1 to 5 should not be construed as limiting the invention, i.e. the ratio of the active catalytic component salt to the hollow microspheres is not limited to the above examples, generally the mass ratio of the components is: 0.5-40 parts of active catalytic component salt, 0-35 parts of binder, 0.5-80 parts of hollow microspheres and 0-5 parts of surfactant; wherein, the binder and the surfactant can be selected and added according to the design requirement of the material.
The hollow glass microspheres, or hollow ceramic microspheres, fly ash hollow microspheres and the like adopted in the invention are used as density adjusting components, and the real density range is 0.1-1.0g/cm3, preferably 0.3-0.6g/cm 3; the particle size ranges from 1um to 1mm, preferably from 10um to 120 um.
The active catalytic component, the binder and the surfactant of the present invention can be reasonably expanded, and should fall within the protection scope of the present invention as long as the object of the present invention can be achieved, for example:
in the invention, the active catalytic component is water-soluble salt of one or more of metals such as Mg, Cu, Co, Ni, Mn, Fe, Zn, Ti, Ce, Al, V, Sc, Y, L a, Ag, Au, Pd, Pt and the like, and carbon sources such as glucose, chitosan, graphene oxide and the like can be introduced to form the carbon material.
The binder introduced in the invention comprises clay, silicate, titanium oxide, aluminum oxide and other components, and can be used or not additionally introduced according to specific process requirements.
The surfactant adopted in the invention comprises anionic surfactants such as sodium dodecyl benzene sulfonate and the like, cationic surfactants such as quaternary ammonium salt and the like, or polyoxyethylene nonionic surfactants, and one or more of the above.
In the invention, in order to prepare the core-shell structure catalyst coated with the glass microspheres, solid powder can be obtained by adopting a sol-gel method, and large particles can also be obtained by adopting a disc granulation technology.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A density-controlled catalytic ozonation catalyst material comprising an active catalytic component salt: adhesive: hollow microspheres: the surfactant is used in a mass ratio of 0.5-40: 0-35: 0.5-80: 0 to 5.
2. The catalyst material for catalyzing ozonation according to claim 1, wherein the hollow microspheres are one or a combination of hollow glass microspheres, hollow ceramic microspheres and fly ash hollow microspheres.
3. A catalyst material for catalytic ozonation according to claim 1, wherein the density of the hollow microspheres is 0.1 to 1.0g/cm3, preferably 0.3 to 0.6g/cm 3; the particle size ranges from 1um to 1mm, preferably from 10um to 120 um.
4. The controlled density catalytic ozonation catalyst material of claim 3, wherein the hollow microspheres have a density of 0.3 to 0.6g/cm 3; the particle size ranges from 10um to 120 um.
5. The catalyst material for catalytic ozonation with controlled density according to claim 1, wherein the active catalytic component is a water-soluble salt of one or more of Mg, Cu, Co, Ni, Mn, Fe, Zn, Ti, Ce, Al, V, Sc, Y, L a, Ag, Au, Pd, and Pt.
6. The catalyst material for catalytic ozonation according to claim 1, wherein the active catalytic component is a carbon source such as glucose, chitosan, graphene oxide, etc. to form the carbon material.
7. The catalyst material for catalytic ozonation according to claim 1, wherein the binder comprises one or more of clay, silicate, titanium oxide, and aluminum oxide.
8. The catalyst material for catalyzing ozone oxidation with controllable density as claimed in claim 1, wherein the surfactant comprises one or more of sodium dodecyl benzene sulfonate anion active agent, quaternary ammonium salt cation active agent and polyoxyethylene nonionic surfactant.
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