CN104646020A - Ozone catalyst and preparation method - Google Patents
Ozone catalyst and preparation method Download PDFInfo
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- CN104646020A CN104646020A CN201310576895.9A CN201310576895A CN104646020A CN 104646020 A CN104646020 A CN 104646020A CN 201310576895 A CN201310576895 A CN 201310576895A CN 104646020 A CN104646020 A CN 104646020A
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Abstract
The invention discloses an ozone catalyst and a preparation method. The catalyst comprises the following components by weight: 70 to 80% of a modified active carbon carrier and active components, namely, 10 to 20% of Fe2O3 and 10 to 20% of MnO2. The modified active carbon carrier is prepared by cleaning active carbon with a sodium hydroxide solution, then dipping the cleaned active carbon with dilute nitric acid, cleaning the dipped active carbon with deionized water and carrying out drying. The preparation method comprises the following steps: loading the active components on the modified active carbon carrier according to the above-mentioned amounts; and carrying out drying and roasting so as to prepare the ozone catalyst. The catalyst provided by the invention has good stability, overcomes the problems of dissolution and loss of metal oxide active components and exerts good effect on COD removal, decolorization, deodorization, degradation of toxic pollutants and improvement of biodegradability of wastewater.
Description
Technical field
The present invention relates to catalytic ozonation technical field, furtherly, relate to a kind of ozone catalyst and preparation method.
Background technology
Catalytic ozonation technology be that developed recently gets up a kind of novel, those are difficult to be oxidized separately with ozone or the method for oxidation operation of difficult degradation at normal temperatures and pressures, the same with other high-level oxidation technology, catalytic ozonation technology utilizes ozone under the effect of catalyst, produce a large amount of strong oxidizing property hydroxyl radical free radical oxidation Decomposition organic matters, thus reach the object of purification of water quality.
Catalytic ozonation technology can be divided into two classes according to used catalyst difference: a class take metal ion as the homogeneous catalyst of catalyst; Another kind of is use solid metallic or metal oxide supported heterogeneous catalysis on carrier.In homogeneous catalysis ozonation technique, catalyst distribution is even and catalytic activity is high, and the mechanism of action is clear, is easy to research and holds.But also clearly, catalyst mixes water-soluble its shortcoming, cause it easily to run off, not easily reclaim and produce secondary pollution, operating cost is higher, adds cost of water treatment.Compared with homogeneous catalysis ozonisation, heterogeneous ozone catalyst, accelerates the oxidation reaction of liquid phase at ambient pressure, and catalyst is with solid-state existence, and be easy to be separated with water, secondary pollution is few, simplifies handling process, thus more and more causes the extensive attention of people.
At present, heterogeneous ozone catalyst mainly contains noble metal series, manganese series and the serial three major types of transition metal.Wherein manganese catalyst series is most widely used, but it is active and the life-span is all not ideal enough; Noble metal catalyst series is then due to reasons such as the life-span are short and expensive, and its application is restricted.Main flow is become gradually based on the research of low-valent metal and metal oxide thereof.
Summary of the invention
For solving in prior art short, the easy stripping of active component in heterogeneous ozonisation catalyst service life, and causing the problem of secondary pollution, the invention provides a kind of ozone catalyst and preparation method.Catalyst of the present invention has good stability, solves the problem that the stripping of metal oxide active component is run off, and has good effect to the removal of COD, decolouring, de-stench, degraded toxic pollutant and the biodegradability that improves waste water.
An object of the present invention is to provide a kind of ozone catalyst.
Comprise following component by weight percentage:
Modified active high-area carbon: 70% ~ 80%;
Described active component is Fe
2o
3and MnO
2, wherein: Fe
2o
3: 10% ~ 20%; MnO
2: 10% ~ 20%;
Described modified active high-area carbon is cleaned by active carbon sodium hydroxide solution, afterwards with dust technology dipping, cleans, obtained after drying.
The specific area of described modified active high-area carbon is 1500 ~ 2000m
2/ g.
Wherein,
The concentration of described sodium hydroxide solution is 5% ~ 15%;
The concentration of described dust technology is 5% ~ 15%, and the dip time of dust technology is 1 ~ 2h.
Two of object of the present invention is to provide a kind of preparation method of ozone catalyst.
Comprise:
Described active component loads on modified active high-area carbon by described consumption, obtained described ozone catalyst after drying, roasting.
Dipping method of the present invention can adopt common dipping method in prior art, and the time of oven dry, roasting is also process conditions conventional in this area, in the present invention, and can be preferred:
Adopt the nitrate solution dipping of active component, dipping temperature is 50 ~ 80 DEG C, and dip time is 3 ~ 5h.
Bake out temperature is 100 ~ 120 DEG C, and drying time is 2 ~ 3h.
Sintering temperature is 300 ~ 500 DEG C, and roasting time is 2 ~ 3h.
The present invention can by the following technical solutions:
Catalyst of the present invention is the method adopting order dipping, drying, roasting, reduction and obtaining, and concrete operation step is as follows:
(1) with 20 ~ 60 order cocoanut active charcoals for raw material, take absorbent charcoal carrier by above-mentioned mass percent, with 5% ~ 15% NaOH solution cleaning, afterwards with 5% ~ 15% dust technology dipping 1 ~ 2h, distilled water clean, oven dry;
(2) infusion process introduces active component: take the active component existed with nitrate salts by above-mentioned mass percent, be made into active component salt solution;
(3) modified activated carbon that step (1) is dried being impregnated in step (2) makes in active component salt solution, dipping 3 ~ 5h, and dipping temperature is 50 ~ 80 DEG C, and period stirs for several times;
(4) product of step (3) is placed in water-bath to dry, bake out temperature is 100 ~ 120 DEG C, and drying time is 2 ~ 3h;
(5) by the product repeated impregnations of step (4), oven dry 2 steps 2 time.
(6) by product roasting in Muffle furnace of step (5), heating rate is 2 DEG C/min, and temperature is 300 ~ 500 DEG C, keeps 2 ~ 3h.
Catalyst of the present invention be with through chemically treated modified activated carbon for carrier, active carbon after chemical modification has abundant oxy radical, utilize oxy radical to fix transition metal ions, thus form stable metal complex, be i.e. catalytic active center.Catalyst has absorption, catalysis dual property.In catalytic oxidation process, first this catalyst utilizes high adsorption by Adsorption of Organic at filling surface, and then active component O3 catalytic oxidation reaction produces a large amount of strong oxidizing property hydroxyl radical free radicals, is decomposed by the oxidation operation being adsorbed on surface.Avoid the accumulation of intermediate product at catalyst surface in adsoption catalysis process, thus well ensure Catalyst Adsorption and reusing.This catalyst does not affect by PH simultaneously, solves the problem that the stripping of metal oxide active component is run off, has good stability.
Carrier of the present invention is preferably through modified cocoanut active charcoal: particle diameter 20 ~ 60 order, specific area 1500 ~ 2000m
2/ g, efficiently solves the defect that small-bore catalyst makes some large molecules its duct active sites inaccessibility, greatly improves the activity of catalyst.Catalyst of the present invention for active component, improves the capacity of decomposition to hardly degraded organic substance with the ferrimanganic composite metal oxide of proper proportion when catalytic ozonation reacts, be eager to excel than simple metal or metal oxide oxidation catalyst performance.
Compared with prior art, tool has the following advantages the heterogeneous catalyst of catalytic ozonation of the present invention:
(1) loaded catalyst of the present invention be with the active carbon through chemical modification for carrier, to utilize on carrier abundant oxy radical to fix transition metal ions, thus form stable metal complex, i.e. catalytic active center.Catalyst has high stability, high efficiency and longer service life, and metal ion can not depart from carrier, can not cause secondary pollution to environment.Be conducive to the application of this catalyst in ozone heterogeneous catalysis system;
(2) catalyst of the present invention uses Mn, Fe bimetallic active component, and hardly degraded organic substance clearance is all higher than corresponding single-metal reforming catalyst performance;
(3) catalyst of the present invention uses Fe as the second active component, and effectively reduce the use amount of Mn, and do not introduce noble metal as active component, catalyst cost significantly reduces;
(4) catalyst of the present invention can reclaim and recycle, and more meets environmental requirement compared with homogeneous oxidation catalyst, and can reduce costs;
(5) catalyst application of the present invention is in extensive range, can be used for the oxidative degradation process of multiple pollutant in water body, and general treatment technology can only be used for processing the pollutant of relatively less kind in waste water, such as, waste water hydrogen peroxide oxidation method, waste water by ozone oxidizing process, wastewater biochemical method etc.
Detailed description of the invention
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment 1:
(1) activated carbon modified: to get 20 ~ 60 order cocoanut active charcoal (commercially available) 80g, with the NaOH solution cleaning of 5%, flood 1h with the dust technology of 5% afterwards, temperature remains on 50 DEG C; Distilled water is cleaned, and in 105 DEG C of dry 24h, the active carbon of obtained modification, specific area is 1500 ㎡/g.
(2) preparation of maceration extract: accurately take Fe(NO
3)
39H
2o solid (analyzing pure, commercially available) 50.5g, Mn(NO
3)
24H
2o solid (analyzing pure, commercially available) 28.85g, is placed in beaker, adds suitable quantity of water, be under agitation heated to 50 DEG C, after solid dissolves completely, place cooling.Cooled liquid rotating is moved in 500ml volumetric flask, shake up with distilled water constant volume, stand for standby use.
(3) preparation of catalyst: Fe(NO in measuring bottle of trying to please
3)
3, Mn(NO
3)
2solution 500ml is in beaker, stir, add obtained modified active high-area carbon 80g again, 3h is flooded keep the condition of 60 DEG C in temperature under, maceration extract is filtered, the carrier being adsorbed with maceration extract is put and drips NaOH after 100 DEG C of dry 1h in an oven and make hydrated ferric oxide and hydrated manganese oxide be deposited in activated carbon surface, wash by deionized water; Again at 100 DEG C of dry 1h.
(4) by the product repeated impregnations of step (3), oven dry 2 steps 2 time.
(5) by product roasting in Muffle furnace of step (4), heating rate is 2 DEG C/min, and temperature is 300 DEG C, keeps 2h naturally cool and obtain Fe
2o
3~ MnO
2/ activated carbon catalysis ozonisation catalyst.In this catalyst, each constituent mass percentage is: cocoanut active charcoal: 80%; Fe
2o
3: 10%; MnO
2: 10%.
Take ozone as oxidant, adopt heterogeneous catalytic oxidation method process manufactured coal gas plant and coke-oven plant containing wastewater containing phenol and cyanide, to the Fe obtained by embodiment 1
2o
3~ MnO
2/ activated carbon catalysis ozonisation catalyst performance is evaluated.At ozone gas phase mass concentration 1.0mg/L, under the condition of gas phase flow velocity 2.0L/min, process 60min can make phenol in phenol cyanogen mixed liquor and CN
-clearance reach more than 85%, COD
crclearance reaches 78.56%.
Embodiment 2:
(1) activated carbon modified: to get 20 ~ 60 order cocoanut active charcoal (commercially available) 70g, with the NaOH solution cleaning of 10%, flood 2h with the dust technology of 10% afterwards, temperature remains on 50 DEG C; Distilled water is cleaned, and in 105 DEG C of dry 24h, the active carbon of obtained modification, specific area is 2000 ㎡/g.
(2) preparation of maceration extract: accurately take Fe(NO
3)
39H
2o solid (analyzing pure, commercially available) 101g, Mn(NO
3)
24H
2o solid (analyzing pure, commercially available) 28.85g, is placed in beaker, adds suitable quantity of water, be under agitation heated to 50 DEG C, after solid dissolves completely, place cooling.Cooled liquid rotating is moved in 500ml volumetric flask, shake up with distilled water constant volume, stand for standby use.
(3) preparation of catalyst: Fe(NO in measuring bottle of trying to please
3)
3, Mn(NO
3)
2solution 500ml is in beaker, stir, add obtained modified active high-area carbon 70g again, 5h is flooded keep the condition of 60 DEG C in temperature under, maceration extract is filtered, the carrier being adsorbed with maceration extract is put and drips NaOH after 120 DEG C of dry 1h in an oven and make hydrated ferric oxide and hydrated manganese oxide be deposited in activated carbon surface, wash by deionized water; Again at 120 DEG C of dry 1h.
(4) by the product repeated impregnations of step (3), oven dry 2 steps 2 time.
(5) by product roasting in Muffle furnace of step (4), heating rate is 2 DEG C/min, and temperature is 500 DEG C, keeps 3h naturally cool and obtain Fe
2o
3~ MnO
2/ activated carbon catalysis ozonisation catalyst.In this catalyst, each constituent mass percentage is: cocoanut active charcoal: 70%; Fe
2o
3: 20%; MnO
2: 10%.
Take ozone as oxidant, adopt heterogeneous catalytic oxidation method process manufactured coal gas plant and coke-oven plant containing wastewater containing phenol and cyanide, to the Fe obtained by embodiment 2
2o
3~ MnO
2/ activated carbon catalysis ozonisation catalyst performance is evaluated.At ozone gas phase mass concentration 1.5mg/L, under the condition of gas phase flow velocity 2.0L/min, process 60min can make phenol in phenol cyanogen mixed liquor and CN
-clearance reach more than 90%, COD
crclearance reaches 82.59%.
Embodiment 3:
(1) activated carbon modified: to get 20 ~ 60 order cocoanut active charcoal (commercially available) 70g, with the NaOH solution cleaning of 10%, flood 1.5h with the dust technology of 10% afterwards, temperature remains on 50 DEG C; Distilled water is cleaned, and in 105 DEG C of dry 24h, the active carbon of obtained modification, specific area is 1700 ㎡/g.
(2) preparation of maceration extract: accurately take Fe(NO
3)
39H
2o solid (analyzing pure, commercially available) 50.5g, Mn(NO
3)
24H
2o solid (analyzing pure, commercially available) 57.7g, is placed in beaker, adds suitable quantity of water, be under agitation heated to 50 DEG C, after solid dissolves completely, place cooling.Cooled liquid rotating is moved in 500ml volumetric flask, shake up with distilled water constant volume, stand for standby use.
(3) preparation of catalyst: Fe(NO in measuring bottle of trying to please
3)
3, Mn(NO
3)
2solution 500ml is in beaker, stir, add obtained modified active high-area carbon 70g again, 5h is flooded keep the condition of 60 DEG C in temperature under, maceration extract is filtered, the carrier being adsorbed with maceration extract is put and drips NaOH after 120 DEG C of dry 1h in an oven and make hydrated ferric oxide and hydrated manganese oxide be deposited in activated carbon surface, wash by deionized water; Again at 120 DEG C of dry 1h.
(4) by the product repeated impregnations of step (3), oven dry 2 steps 2 time.
(5) by product roasting in Muffle furnace of step (4), heating rate is 2 DEG C/min, and temperature is 500 DEG C, keeps 3h naturally cool and obtain Fe
2o
3~ MnO
2/ activated carbon catalysis ozonisation catalyst.In this catalyst, each constituent mass percentage is: cocoanut active charcoal: 70%; Fe
2o
3: 10%; MnO
2: 20%.
Take ozone as oxidant, adopt heterogeneous catalytic oxidation method process manufactured coal gas plant and coke-oven plant containing wastewater containing phenol and cyanide, to the Fe obtained by embodiment 3
2o
3~ MnO
2/ activated carbon catalysis ozonisation catalyst performance is evaluated.At ozone gas phase mass concentration 1.5mg/L, under the condition of gas phase flow velocity 2.0L/min, process 60min can make phenol in phenol cyanogen mixed liquor and CN
-clearance reach more than 90%, COD
crclearance reaches 81.33%.
Embodiment 4:
(1) activated carbon modified: to get 20 ~ 60 order cocoanut active charcoal (commercially available) 70g, with the NaOH solution cleaning of 15%, flood 2h with the dust technology of 15% afterwards, temperature remains on 50 DEG C; Distilled water is cleaned, and in 105 DEG C of dry 24h, the active carbon of obtained modification, specific area is 1900 ㎡/g.
(2) preparation of maceration extract: accurately take Fe(NO
3)
39H
2o solid (analyzing pure, commercially available) 75.75g, Mn(NO
3)
24H
2o solid (analyzing pure, commercially available) 43.28g, is placed in beaker, adds suitable quantity of water, be under agitation heated to 50 DEG C, after solid dissolves completely, place cooling.Cooled liquid rotating is moved in 500ml volumetric flask, shake up with distilled water constant volume, stand for standby use.
(3) preparation of catalyst: Fe(NO in measuring bottle of trying to please
3)
3, Mn(NO
3)
2solution 500ml is in beaker, stir, add obtained modified active high-area carbon 70g again, 5h is flooded keep the condition of 60 DEG C in temperature under, maceration extract is filtered, the carrier being adsorbed with maceration extract is put and drips NaOH after 120 DEG C of dry 1h in an oven and make hydrated ferric oxide and hydrated manganese oxide be deposited in activated carbon surface, wash by deionized water; Again at 120 DEG C of dry 1h.
(4) by the product repeated impregnations of step (3), oven dry 2 steps 2 time.
(5) by product roasting in Muffle furnace of step (4), heating rate is 2 DEG C/min, and temperature is 500 DEG C, keeps 3h naturally cool and obtain Fe
2o
3~ MnO
2/ activated carbon catalysis ozonisation catalyst.In this catalyst, each constituent mass percentage is: cocoanut active charcoal: 70%; Fe
2o
3: 15%; MnO
2: 15%.
Take ozone as oxidant, adopt heterogeneous catalytic oxidation method process manufactured coal gas plant and coke-oven plant containing wastewater containing phenol and cyanide, to the Fe obtained by embodiment 4
2o
3~ MnO
2/ activated carbon catalysis ozonisation catalyst performance is evaluated.At ozone gas phase mass concentration 1.5mg/L, under the condition of gas phase flow velocity 2.0L/min, process 60min can make phenol in phenol cyanogen mixed liquor and CN
-clearance reach more than 90%, COD
crclearance reaches 81.89%.
Claims (6)
1. an ozone catalyst, is characterized in that:
Described catalyst comprises following component by weight percentage:
Modified active high-area carbon: 70% ~ 80%;
Described active component is Fe
2o
3and MnO
2;
Wherein: Fe
2o
3: 10% ~ 20%; MnO
2: 10% ~ 20%;
Described modified active high-area carbon is cleaned by active carbon sodium hydroxide solution, and afterwards with dust technology dipping, deionized water is cleaned, obtained after drying.
2. ozone catalyst as claimed in claim 1, is characterized in that:
The specific area of described modified active high-area carbon is 1500 ~ 2000m
2/ g.
3. ozone catalyst as claimed in claim 1, is characterized in that:
The concentration of described sodium hydroxide solution is 5% ~ 15%;
The concentration of described dust technology is 5% ~ 15%, and the dip time of dust technology is 1 ~ 2h.
4. a preparation method for the ozone catalyst as described in claims 1 to 3, is characterized in that described method comprises:
Described active component loads on described modified active high-area carbon by described consumption, obtained described ozone catalyst after drying, roasting.
5. preparation method as claimed in claim 4, is characterized in that:
Adopt the nitrate solution dipping of active component, dipping temperature is 50 ~ 80 DEG C, and dip time is 3 ~ 5h.
6. preparation method as claimed in claim 4, is characterized in that:
Bake out temperature is 100 ~ 120 DEG C, and drying time is 2 ~ 3h;
Sintering temperature is 300 ~ 500 DEG C, and roasting time is 2 ~ 3h.
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