CN105233838A - Preparation method of O3/H2O2 catalyst using activated bentonite as carrier, catalyst and application thereof - Google Patents

Preparation method of O3/H2O2 catalyst using activated bentonite as carrier, catalyst and application thereof Download PDF

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Publication number
CN105233838A
CN105233838A CN201510760538.7A CN201510760538A CN105233838A CN 105233838 A CN105233838 A CN 105233838A CN 201510760538 A CN201510760538 A CN 201510760538A CN 105233838 A CN105233838 A CN 105233838A
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catalyst
activated bentonite
carrier
metal ion
bentonite
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CN105233838B (en
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杨佘维
黄志华
汪永红
李朝晖
叶向东
王开演
黄振雄
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Environmental Science and Technology Co., Ltd. of Guangdong Academy of Environmental Sciences
Guangdong Provincial Academy of Environmental Science
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GUANGDONG PROVINCIAL ACADEMY OF ENVIRONMENTAL SCIENCE
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Abstract

The invention provides a preparation method of an O3/H2O2 catalyst using activated bentonite as a carrier, the catalyst prepared by means of the preparation method and application thereof. The activated bentonite is used as the carrier, and a part of the carrier is impregnated in a metal salt solution and then is loaded on the other unimpregnated part of the carrier to obtain the catalyst through drying and calcination. The catalyst obtained by means of the method is suitable for catalytic O3/H2O2 oxidation water treatment and is suitable for large-scale production, and the manufacturing cost and operation cost are somewhat reduced.

Description

A kind of take activated bentonite as the O of carrier 3/ H 2o 2the preparation method of catalyst, catalyst and application thereof
Technical field
The present invention relates to treatment catalyst field, being specifically related to a kind of take activated bentonite as the O of carrier 3/ H 2o 2the preparation method of catalyst, the catalyst prepared by the method and application thereof.
Background technology
Fenton process (Fenton method) and Ozonation are the most ripe advanced oxidation processes of current industrialization, but Fenton method requires strict to pH, and effluent color dilution increases and can produce a large amount of chemical sludges; In Ozonation, the oxidability of ozone is not as hydroxyl radical free radical, and oxidation product is generally monoaldehyde, dialdehyde, aldehydic acid, monocarboxylic acid, dicarboxylic acids organic molecule, is difficult to thorough mineralising, although by adding Fe 3+, Mn 2+strengthening ozone oxidation, but also existence is similar to the same problem of Fenton method.In order to the oxidability improving ozone mainly contains two kinds of approach, the first is introduced 3d transition metal ions and maybe will be had the 3d transition metal ions load of catalytic performance on carrier, produces oxidability stronger free radical O, OH by the catalysis of 3d transition metal ions; It two is by introducing physical field radiation, mainly containing light, sound, electricity, magnetic etc.
O 3/ H 2o 2be change simple ozonidation into advanced oxidation processes most economical and the most feasible approach, it has and is better than the feature of traditional single oxidizing process as ozone or hydrogen peroxide oxidation process.O 3/ H 2o 2can produce the OH free radical that oxidability is very strong, its oxidizing potential is 2.80V, compares O 3(oxidizing potential 2.07V) and H 2o 2(oxidizing potential 1.76V) difference more than high 35% and 59%, oxidability is only second to fluorine.OH radical pair organic matter does not have selective, can be carbon dioxide, water or mineral salt by its direct oxidation, can not cause new environmental problem.
O 3/ H 2o 2though technique is reality easily, O 3with H 2o 2the collaborative OH amount that produces affects comparatively large by waste water quality, reaction environment, introduces catalyst, physical field to O in system 3/ H 2o 2carrying out catalysis, improve the productive rate of OH, and introduce interfacial reaction, add the approach of reaction, improve and make its oxidability, thus reduce Sewage advanced treatment cost, is current O 3/ H 2o 2the focus of application study.
The O of current reported in literature 3/ H 2o 2catalyst is with metal ion, i.e. catalyst wiring solution-forming, adds in waste water, then adds O 3with H 2o 2carry out catalytic reaction, catalyst exists with the form of ionic state.Although this liquid catalyst can improve O 3/ H 2o 2the oxidability of system, but there is catalyst and cannot reuse, easily cause secondary pollution, increase the shortcomings such as the difficulty of subsequent treatment.If a kind of catalyst of solid can be prepared, make it to O 3/ H 2o 2system has good catalytic action, and in the process of water treatment, these solid catalysts are retained in ozone catalytic reactor always and play catalysed oxidn, do not need follow-up separating measure, will have its actual application value.
Summary of the invention
The object of the invention is to propose a kind of take activated bentonite as the O of carrier 3/ H 2o 2catalysts and its preparation method.
For achieving the above object, the present invention by the following technical solutions.
A kind of take activated bentonite as the O of carrier 3/ H 2o 2the preparation method of catalyst, comprises the following steps:
(1) Bentonite Activation: acid solution is mixed with bentonite, under the condition of 50 ~ 80 DEG C after stirring reaction 6 ~ 8h, standing 4 ~ 5h, then filters, and washing, to neutral, is dried, roasting, grinds 200 ~ 250 orders that sieve, obtains activated bentonite; Described acid solution is hydrochloric acid, sulfuric acid or salpeter solution, and acid solution and bentonitic mass ratio are 1:500 ~ 1:200; The activated bentonite prepared is for subsequent use, uses respectively in step (2) thereafter and step (3);
(2) raw material core preparation: get activated bentonite, prepare spherical raw material core by sugar-coat draft machine;
(3) alta-mud load metal ion: separately get activated bentonite, add in metal ion solution and mix, under the condition of 50 ~ 80 DEG C, stir 6 ~ 8h, leave standstill 10 ~ 12h, dry solution or after solution all volatilizees, obtain the activated bentonite of loaded metal ion; Described metal ion solution is Mn 2+, Fe 3+, Al 3+, Cu 2+nitrate or sulfate;
(4) after being mixed with the activated bentonite of loaded metal ion by spherical raw material core, by sugar-coat draft machine, make the activated bentonite of loaded metal ion be attached to spherical raw material core surface, make particle diameter continue to increase, obtain catalyst idiosome; Catalyst idiosome is first dried rear high-temperature roasting, is the O of carrier with activated bentonite described in obtaining 3/ H 2o 2catalyst.
Further, in above-mentioned steps (1), the concentration of acid solution is preferably 5 ~ 10mol/L.
Further, in above-mentioned steps (2), the particle diameter of the spherical raw material core prepared is 1 ~ 2.5mm.
Further, in above-mentioned steps (3), the mass fraction of described metal ion solution is 5 ~ 30%; The mass ratio of activated bentonite and metal ion solution is 10:1 ~ 20:1.
Further, in above-mentioned steps (4), the particle diameter of the catalyst idiosome prepared is 3 ~ 8mm.
Further, in above-mentioned steps (1), the temperature of described oven dry is 150 ~ 160 DEG C, the time is 1 ~ 2h, and the temperature of described roasting is 800 ~ 1000 DEG C, the time is 4 ~ 5h; In step (4), the temperature of described oven dry is 150 ~ 160 DEG C, the time is 1 ~ 2h, and the temperature of described roasting is 1000 ~ 1200 DEG C, the time is 4 ~ 5h.
The present invention also provides by the above-mentioned catalyst prepared, and this catalyst is at catalysis O 3/ H 2o 2application in oxidizing process water treatment.
Compared with prior art, the present invention has following characteristics:
The present invention's preparation take activated bentonite as the catalyst of carrier, is difficult to effective catalysis O in view of being carried on inner active component (metal ion) 3, H 2o 2, the catalyst that therefore prepared by the present invention is after Component Vectors impregnating metal salting liquid, then load is on the non-impregnated carrier of another part, while can ensureing catalytic performance like this, saves the use amount of slaine.In addition, the active component due to catalyst is that because its material is close, therefore its adhesive strength is high, can reduce catalyst loss rate, effectively prevent secondary pollution with the aqueous solution and activated bentonite mixing back loading on original raw material core; And the ceramsite catalyst of preparation can be reused, reduce O 3/ H 2o 2system running cost, more easily realizes large-scale industrial production.
Catalyst by once sintered shaping, the key of technology be manganese sulfate, aluminum sulfate, ferrous sulfate, ferric sulfate when high temperature more than 800 DEG C, all resolve into metal oxide and sulfur dioxide gas, gas discharges after treatment with the tail gas of heating furnace.And the metal oxide be decomposed to form, particle is tiny, is evenly distributed, and improves the utilization rate of metal oxide active component, also reduces production cost.
This invention can process water separately, also can with additive method coupling.O 3/ H 2o 2after catalyst prepared by the present invention, define solid, liquid, gas three-phase oxidation system, add interfacial reaction, improve the output of OH, more effectively can remove organic pollutants, its oxidability is significantly improved, condition of compatibility is more broad, reduces O 3, H 2o 2dosage, from another angle save operating cost.
Detailed description of the invention
According to the method that content of the present invention provides, in described catalyst, active component is MnO 2, Al 2o 3, Fe 2o 3, Fe 3o 4, one or more compounds in CuO, the carrier of catalyst is activated bentonite.
Manganese sulfate, cobaltous sulfate, copper sulphate and ferric sulfate aqueous solution mixing bentonite material, under the high temperature action more than 800 DEG C, form fine MnO 2, Al 2o 3, Fe 2o 3, Fe 3o 4, the particle such as CuO, be evenly distributed in the surface of haydite.During actual production, it is 1000 ~ 1200 DEG C that haydite dries the condition of burning, and prepares O 3/ H 2o 2catalyst.This catalyst, when carrying out catalytic reaction, can play simultaneously improve O 3, H 2o 2the effect of oxidability, not easily runs off again and cause secondary pollution to waste water.
O 3/ H 2o 2catalyst carries out catalytic oxidation organic pollutants by joining in catalyst reaction device.In water inlet pipe, waste water is mixed into H through pipe-line mixer 2o 2, add O by bottom aerator simultaneously 3, enter catalytic reactor in the lump.Catalytic reactor can be divided into downflow type (water flows from the bottom up) and reverse-flow (water flows from top to bottom) two kinds according to water (flow) direction, can adjust according to Practical Project.Waste water enters bentonite catalytic filler layer, and have the catalytic action of metal oxide catalyst in load under, emerging pollutant is oxidized further.Outlet system loads filter screen and makes to be with the carrier of catalyst not taken out of, and the ozone that tail gas absorber is residual after collecting reaction if ozone is not recycled, is then processed ozone by ozone tail gas destructor, and overflowing to prevent ozone pollutes.
Embodiment 1
Add in bentonite by 5mol/L salpeter solution, salpeter solution and bentonitic mass ratio control at 1:200; Under the condition of 80 DEG C after stirring reaction 6h, leave standstill 4h, then filter, washing is to neutral, and 150 DEG C of dry 2h, 800 DEG C of roasting 5h, grind 200 orders that sieve, obtain activated bentonite; Get partial activation bentonite, prepare by sugar-coat draft machine the spherical raw material core that particle diameter is 2.5mm; Separately get partial activation bentonite, add quantitative Mn (NO 3) 2, Fe (NO 3) 3, Al 2(SO 4) 3, Cu (NO 3) 2metal ion solution in mix, the mass ratio of four kinds of salt is 2:5:2:1, and the mass fraction of metal ion solution is 30%, and the mass ratio of activated bentonite and metal ion solution is 20:1.Under the condition of 80 DEG C, stir 6h, leave standstill 10h, obtain the activated bentonite of loaded metal ion; After spherical raw material core is mixed with the activated bentonite of loaded metal ion, by sugar-coat draft machine, the activated bentonite of loaded metal ion is made to be attached to spherical raw material core surface, prepare the catalyst idiosome that particle diameter is 8mm, after catalyst idiosome is dried 1h at 160 DEG C, at 1000 DEG C of high-temperature roasting 5h, make the O that activated bentonite is carrier 3/ H 2o 2catalyst.Utilize this catalyst O 3/ H 2o 2the tail water of oxidation depth process municipal sewage plant after secondary biochemical treatment, H 2o 2, O 3dosage and COD crmass ratio be H 2o 2: O 3: COD cr=1:2:4, does not add catalyst and the COD adding catalyst in technique crremoval situation as shown in Table 1.
Table one embodiment 1 sewage treatment plant tail water process data
Number of times 1 2 3 4
Influent COD (not adding catalyst) 45 52 43 55
Water outlet COD (not adding catalyst) 34 37 34 39
COD clearance (not adding catalyst) 24.44% 28.85% 20.93% 29.09%
Influent COD (adding catalyst) 42 48 56 58
Water outlet COD (adding catalyst) 26 28 27 26
COD clearance (adding catalyst) 38.10% 41.67% 51.79% 55.17%
Independent H 2o 2/ O 3oxidation technology is to the COD of municipal wastewater tail water craverage removal rate is 25.83%, the heterogeneous catalysis H built after adding bentonite catalyst 2o 2/ O 3oxidation technology, COD craverage removal rate is 46.68%, than independent H 2o 2/ O 3technique improves 20.85%.Except investigating this catalyst to except ozone oxidation degradation of organic substances, also this catalyst surface active component being run off in catalytic oxidation process and analyzing, the results are shown in Table two.This catalyst in catalytic oxidation process only copper have very little loss.
Loss of active component data in table two embodiment 1 catalyst
Embodiment 2
Add in bentonite by 10mol/L sulfuric acid solution, sulfuric acid solution and bentonitic mass ratio control at 1:500; Under the condition of 50 DEG C after stirring reaction 8h, leave standstill 5h, then filter, washing is to neutral, and 160 DEG C of dry 1h, 1000 DEG C of roasting 4h, grind 250 orders that sieve, obtain activated bentonite; Get partial activation bentonite, prepare by sugar-coat draft machine the spherical raw material core that particle diameter is 1mm; Separately get partial activation bentonite, add quantitative MnSO 4, Fe 2(SO 4) 3, Al 2(SO 4) 3, CuSO 4metal ion solution in mix, the mass ratio of four kinds of salt is 2:5:2:1, and the mass fraction of metal ion solution is 5%, and the mass ratio of activated bentonite and metal ion solution is 10:1.Under the condition of 50 DEG C, stir 8h, leave standstill 12h, obtain the activated bentonite of loaded metal ion; After spherical raw material core is mixed with the activated bentonite of loaded metal ion, by sugar-coat draft machine, the activated bentonite of loaded metal ion is made to be attached to spherical raw material core surface, prepare the catalyst idiosome that particle diameter is 3mm, after catalyst idiosome is dried 2h at 150 DEG C, at 1200 DEG C of high-temperature roasting 4h, make the O that activated bentonite is carrier 3/ H 2o 2catalyst.Utilize this catalyst O 3/ H 2o 2the waste water of oxidation depth process pharmacy waste water after secondary biochemical treatment, H 2o 2, O 3the mass ratio of dosage and COD is H 2o 2: O 3: COD=2:4:5, typical organic matter Diclofenac, carbamazepine, ROX, erythromycin degradation rate are respectively 64%, 78%, 73%, 69%, add catalyst, under same oxidant dosage, the degradation rate of four kinds of typical organic matters is 87%, 100%, 92%, 86%, improves 23%, 22%, 19%, 17% respectively.
Except investigating this catalyst to except ozone oxidation degradation of organic substances, also this catalyst surface active component being run off in catalytic oxidation process and analyzing, the results are shown in Table three.This catalyst in catalytic oxidation process only iron have very little loss.
Loss of active component data in table three embodiment 2 catalyst

Claims (8)

1. one kind take activated bentonite as the O of carrier 3/ H 2o 2the preparation method of catalyst, is characterized in that, comprises the following steps:
(1) Bentonite Activation: acid solution is mixed with bentonite, under the condition of 50 ~ 80 DEG C after stirring reaction 6 ~ 8h, standing 4 ~ 5h, then filters, and washing, to neutral, is dried, roasting, grinds 200 ~ 250 orders that sieve, obtains activated bentonite; Described acid solution is hydrochloric acid, sulfuric acid or salpeter solution, and acid solution and bentonitic mass ratio are 1:500 ~ 1:200;
(2) raw material core preparation: get activated bentonite, prepare spherical raw material core by sugar-coat draft machine;
(3) alta-mud load metal ion: separately get activated bentonite, add in metal ion solution and mix, stirs 6 ~ 8h under the condition of 50 ~ 80 DEG C, leaves standstill 10 ~ 12h, obtains the activated bentonite of loaded metal ion; Described metal ion solution is Mn 2+, Fe 3+, Al 3+, Cu 2+nitrate or sulfate;
(4) after spherical raw material core being mixed with the activated bentonite of loaded metal ion, by sugar-coat draft machine, make the activated bentonite of loaded metal ion be attached to spherical raw material core surface, obtain catalyst idiosome; Catalyst idiosome is first dried rear high-temperature roasting, is the O of carrier with activated bentonite described in obtaining 3/ H 2o 2catalyst.
2. be the O of carrier as claimed in claim 1 with activated bentonite 3/ H 2o 2the preparation method of catalyst, is characterized in that, in step (1), the concentration of described acid solution is 5 ~ 10mol/L.
3. be the O of carrier as claimed in claim 1 with activated bentonite 3/ H 2o 2the preparation method of catalyst, is characterized in that, in step (2), the particle diameter of the spherical raw material core prepared is 1 ~ 2.5mm.
4. be the O of carrier as claimed in claim 1 with activated bentonite 3/ H 2o 2the preparation method of catalyst, is characterized in that, in step (3), the mass fraction of described metal ion solution is 5 ~ 30%; The mass ratio of activated bentonite and metal ion solution is 10:1 ~ 20:1.
5. be the O of carrier as claimed in claim 1 with activated bentonite 3/ H 2o 2the preparation method of catalyst, is characterized in that, in step (4), the particle diameter of the catalyst idiosome prepared is 3 ~ 8mm.
6. as described in as arbitrary in Claims 1 to 5 take activated bentonite as the O of carrier 3/ H 2o 2the preparation method of catalyst, is characterized in that, in step (1), the temperature of described oven dry is 150 ~ 160 DEG C, the time is 1 ~ 2h, and the temperature of described roasting is 800 ~ 1000 DEG C, the time is 4 ~ 5h; In step (4), the temperature of described oven dry is 150 ~ 160 DEG C, the time is 1 ~ 2h, and the temperature of described roasting is 1000 ~ 1200 DEG C, the time is 4 ~ 5h.
7. the catalyst that the preparation method as described in as arbitrary in claim 1 ~ 6 prepares.
8. catalyst as claimed in claim 7 is at catalysis O 3/ H 2o 2application in oxidizing process water treatment.
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CN108497221A (en) * 2018-04-27 2018-09-07 宿松县龙源水产养殖专业合作社 A kind of promotion growth loach nutrition and health care feed

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN107235571A (en) * 2016-03-28 2017-10-10 宝山钢铁股份有限公司 A kind of efficient method and apparatus for removing SCOD in coking reverse osmosis concentrated water
CN107235571B (en) * 2016-03-28 2021-02-19 宝山钢铁股份有限公司 Method and device for efficiently removing SCOD (selective catalytic oxidation) in coking reverse osmosis concentrated water
CN105772021A (en) * 2016-04-08 2016-07-20 北京今大禹环境技术股份有限公司 Preparation method of supported metal oxide catalyst for reinforcing ozonolysis and ozone catalytic ozonation catalyst prepared through preparation method
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CN108497221A (en) * 2018-04-27 2018-09-07 宿松县龙源水产养殖专业合作社 A kind of promotion growth loach nutrition and health care feed

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