CN109499563A - A kind of preparation method of zinc oxide-active carbon composite catalyst - Google Patents
A kind of preparation method of zinc oxide-active carbon composite catalyst Download PDFInfo
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- CN109499563A CN109499563A CN201710833989.8A CN201710833989A CN109499563A CN 109499563 A CN109499563 A CN 109499563A CN 201710833989 A CN201710833989 A CN 201710833989A CN 109499563 A CN109499563 A CN 109499563A
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- active carbon
- solution
- zinc oxide
- composite catalyst
- carbon composite
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- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 84
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000003054 catalyst Substances 0.000 title claims abstract description 41
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000011701 zinc Substances 0.000 title claims abstract description 37
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 37
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 7
- -1 carbon inorganic acid Chemical class 0.000 claims abstract description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 48
- 239000011787 zinc oxide Substances 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 150000007522 mineralic acids Chemical class 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 2
- 229910052760 oxygen Inorganic materials 0.000 claims 2
- 239000001301 oxygen Substances 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 239000010842 industrial wastewater Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 10
- 239000003610 charcoal Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- 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
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0207—Pretreatment of the support
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0211—Impregnation using a colloidal suspension
Abstract
The invention discloses a kind of zinc oxide-active carbon composite catalyst preparation methods, include: the pretreatment of (1) active carbon: by active carbon inorganic acid solution impregnate 12~for 24 hours, filtering, deionized water is washed till neutrality, again with inorganic alkali solution impregnate 12~for 24 hours, filtering, be washed with deionized water to neutrality, it is dry, obtain pretreated active carbon；(2) above-mentioned pretreated active carbon is added in deionized water, 6~8h of ultrasonic disperse obtains active carbon suspension；(3) carbonate solution is added in Xiang Shangshu active carbon suspension, stirs 15~30min, adds zinc solution, stirs 3~5h, filters, it is dry, in 280~400 DEG C of 1~2h of temperature lower calcination, obtain zinc oxide-active carbon composite catalyst.Zinc oxide-active carbon composite catalyst in the present invention has good photocatalysis effect, industrial wastewater, exhaust gas processing in terms of have a good application prospect.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of zinc oxide-active carbon composite catalyst preparation side
Method.
Background technique
Organic wastewater is a kind of waste water difficult to degrade.By taking dyeing waste water as an example, discharge amount is big, organic pollutant content
Height, type are complicated.Since organic chemical contaminant stable structure, toxicity are big, processing difficulty is high, traditional processing technique by
Serious challenge.It is applied to Technology development, such as the method for physico-chemical process, chemical method and bioanalysis and combinations thereof, is extremely difficult to
Satisfied treatment effect.
The hot spot that various organic matters difficult to degrade in waste water have become current people's research is handled using photocatalysis technology
Project.Currently, common photochemical catalyst is mostly nano semiconductor material, but since the size of nanoparticle is small, is easy to produce
Agglomeration, while being easy to run off in use, therefore, in recent years, people have carried out research work to loaded photocatalyst
Make.
The materials such as active carbon, carbon fiber have the characteristics that light, porous, large specific surface area, adsorption capacity are strong, and become good
Good catalyst carrier material.But in the prior art, the catalyst based on active carbon and oxide-based nanomaterial obtains not yet
To being widely applied, the photocatalysis effect of obtained composite catalyst is unsatisfactory.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of zinc oxide-active carbon composite catalyst,
It is able to solve problems of the prior art.
Summary of the invention
It is existing to overcome the purpose of the present invention is to provide a kind of zinc oxide-active carbon composite catalyst preparation method
Deficiency in technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of zinc oxide-active carbon composite catalyst, comprising:
(1) pretreatment of active carbon: active carbon inorganic acid solution is impregnated 12~for 24 hours, filtering, during deionized water is washed till
Property, then impregnate 12 with inorganic alkali solution~for 24 hours, filtering is washed with deionized water to neutrality, and it is dry, obtain pretreated activity
Charcoal；
(2) above-mentioned pretreated active carbon is added in deionized water, 6~8h of ultrasonic disperse, obtains active carbon suspension
Liquid；
(3) carbonate solution is added in Xiang Shangshu active carbon suspension, stirs 15~30min, adds zinc solution, stir
3~5h is mixed, is filtered, it is dry, in 280~400 DEG C of 1~2h of temperature lower calcination, obtain zinc oxide-active carbon composite catalyst.
Preferably, in the zinc oxide-active carbon composite catalyst, the mass ratio of zinc oxide and active carbon is 1:2~10.
Preferably, in the zinc oxide-active carbon composite catalyst, the mass ratio of zinc oxide and active carbon is 1:2~6.
Preferably, in step (3), the volume ratio of the carbonate solution and the zinc solution is 1:1~5.
Preferably, in step (3), the zinc solution is in liquor zinci chloridi, zinc nitrate solution, solution of zinc sulfate
It is a kind of.
Preferably, in step (3), the carbonate solution is in sodium carbonate liquor, solution of potassium carbonate, sal volatile
One kind.
Preferably, in step (1), inorganic acid solution is in hydrochloric acid solution, sulfuric acid solution, nitric acid solution, phosphoric acid solution
One kind.
Preferably, in step (1), inorganic alkali solution is in sodium hydroxide solution, potassium hydroxide solution, ammonia spirit
It is a kind of.
Compared with the prior art, the advantages of the present invention are as follows: zinc oxide-active carbon composite catalyst in the present invention has
Good photocatalysis effect, industrial wastewater, exhaust gas processing in terms of have a good application prospect.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of zinc oxide-active carbon composite catalyst, comprising:
(1) pretreatment of active carbon: active carbon inorganic acid solution is impregnated 12~for 24 hours, filtering, during deionized water is washed till
Property, then impregnate 12 with inorganic alkali solution~for 24 hours, filtering is washed with deionized water to neutrality, and it is dry, obtain pretreated activity
Charcoal；
(2) above-mentioned pretreated active carbon is added in deionized water, 6~8h of ultrasonic disperse, obtains active carbon suspension
Liquid；
(3) carbonate solution is added in Xiang Shangshu active carbon suspension, stirs 15~30min, adds zinc solution, stir
3~5h is mixed, is filtered, it is dry, in 280~400 DEG C of 1~2h of temperature lower calcination, obtain zinc oxide-active carbon composite catalyst.
In above-mentioned steps (1), inorganic acid solution in hydrochloric acid solution, sulfuric acid solution, nitric acid solution, phosphoric acid solution one
Kind；Inorganic alkali solution is selected from one of sodium hydroxide solution, potassium hydroxide solution, ammonia spirit.
In above-mentioned steps (3), the zinc solution in liquor zinci chloridi, zinc nitrate solution, solution of zinc sulfate one
Kind, it is preferred that the zinc solution is zinc nitrate solution；The carbonate solution is selected from sodium carbonate liquor, solution of potassium carbonate, carbon
One of acid ammonium solution, it is preferred that the carbonate solution is sodium carbonate.
Wherein, the volume ratio of the carbonate solution and the zinc solution is 1:1~5, it is preferred that the carbonate is molten
The volume ratio of liquid and the zinc solution is 1:1~2, it is further preferred that the carbonate solution and the zinc solution
Volume ratio is 1:1.5.
In the present invention, in the zinc oxide according to obtained by the above method-active carbon composite catalyst, zinc oxide and active carbon
Mass ratio be 1:2~10, it is preferred that the mass ratio of zinc oxide and active carbon be 1:2~6, it is further preferred that zinc oxide and
The mass ratio of active carbon is 1:5.
Embodiment 1
Active carbon inorganic acid solution is impregnated into 12h, filtering, deionized water is washed till neutrality, then is impregnated with inorganic alkali solution
12h, filtering are washed with deionized water to neutrality, dry, obtain pretreated active carbon；
Above-mentioned pretreated active carbon is added in deionized water, ultrasonic disperse 6h obtains active carbon suspension；
Carbonate solution is added into above-mentioned active carbon suspension, stirs 15~30min, adds zinc solution, stirs
3h is filtered, dry, in 280 DEG C of temperature lower calcination 1h, obtains zinc oxide-active carbon composite catalyst.
In the present embodiment, in the zinc oxide according to obtained by the above method-active carbon composite catalyst, zinc oxide and activity
The mass ratio of charcoal is 1:10, and the photocatalysis efficiency of the catalyst is 80%.
Embodiment 2
Active carbon inorganic acid solution is impregnated into 18h, filtering, deionized water is washed till neutrality, then is impregnated with inorganic alkali solution
18h, filtering are washed with deionized water to neutrality, dry, obtain pretreated active carbon；
Above-mentioned pretreated active carbon is added in deionized water, ultrasonic disperse 7h obtains active carbon suspension；
Carbonate solution is added into above-mentioned active carbon suspension, stirs 15~30min, adds zinc solution, stirs
4h is filtered, dry, in 300 DEG C of temperature lower calcination 1.5h, obtains zinc oxide-active carbon composite catalyst.
In the present embodiment, in the zinc oxide according to obtained by the above method-active carbon composite catalyst, zinc oxide and activity
The mass ratio of charcoal is 1:5, and the photocatalysis efficiency of the catalyst is 95%.
Embodiment 3
Active carbon inorganic acid solution is impregnated for 24 hours, filtering, deionized water is washed till neutrality, then is impregnated with inorganic alkali solution
For 24 hours, it filters, is washed with deionized water to neutrality, it is dry, obtain pretreated active carbon；
Above-mentioned pretreated active carbon is added in deionized water, ultrasound divides 8h, obtains active carbon suspension；
Carbonate solution is added into above-mentioned active carbon suspension, stirs 15~30min, adds zinc solution, stirs
5h is filtered, dry, in 400 DEG C of temperature lower calcination 2h, obtains zinc oxide-active carbon composite catalyst.
In the present embodiment, in the zinc oxide according to obtained by the above method-active carbon composite catalyst, zinc oxide and activity
The mass ratio of charcoal is 1:2, and the photocatalysis efficiency of the catalyst is 74%.
It is compound by carrying out zinc oxide and active carbon in the present invention, since the specific surface area of active carbon is larger, adsorption energy
Power is strong, the zinc oxide of generation-activity Carbon composites can be securely adsorbed on its surface, therefore, when zinc oxide-active carbon is compound
When the mass ratio of zinc oxide and active carbon in catalyst is 1:5, catalytic effect is best, therefore, in industrial wastewater, exhaust gas
Processing aspect has a good application prospect.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (8)
1. a kind of zinc oxide-active carbon composite catalyst preparation method characterized by comprising
(1) pretreatment of active carbon: active carbon inorganic acid solution is impregnated 12~for 24 hours, filtering, deionized water is washed till neutrality,
12 are impregnated with inorganic alkali solution again~for 24 hours, filtering is washed with deionized water to neutrality, and it is dry, obtain pretreated active carbon；
(2) above-mentioned pretreated active carbon is added in deionized water, 6~8h of ultrasonic disperse obtains active carbon suspension；
(3) carbonate solution is added in Xiang Shangshu active carbon suspension, stirs 15~30min, adds zinc solution, stirring 3
~5h is filtered, dry, in 280~400 DEG C of 1~2h of temperature lower calcination, obtains zinc oxide-active carbon composite catalyst.
2. zinc oxide according to claim 1-active carbon composite catalyst preparation method, which is characterized in that the oxygen
Change in zinc-active carbon composite catalyst, the mass ratio of zinc oxide and active carbon is 1:2~10.
3. zinc oxide according to claim 2-active carbon composite catalyst preparation method, which is characterized in that the oxygen
Change in zinc-active carbon composite catalyst, the mass ratio of zinc oxide and active carbon is 1:2~6.
4. zinc oxide according to claim 1-active carbon composite catalyst preparation method, which is characterized in that step (3)
In, the volume ratio of the carbonate solution and the zinc solution is 1:1~5.
5. zinc oxide according to claim 1-active carbon composite catalyst preparation method, which is characterized in that step (3)
In, the zinc solution is selected from one of liquor zinci chloridi, zinc nitrate solution, solution of zinc sulfate.
6. zinc oxide according to claim 1-active carbon composite catalyst preparation method, which is characterized in that step (3)
In, the carbonate solution is selected from one of sodium carbonate liquor, solution of potassium carbonate, sal volatile.
7. zinc oxide according to claim 1-active carbon composite catalyst preparation method, which is characterized in that step (1)
In, inorganic acid solution is selected from one of hydrochloric acid solution, sulfuric acid solution, nitric acid solution, phosphoric acid solution.
8. zinc oxide according to claim 1-active carbon composite catalyst preparation method, which is characterized in that step (1)
In, inorganic alkali solution is selected from one of sodium hydroxide solution, potassium hydroxide solution, ammonia spirit.
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| CN201710833989.8A CN109499563A (en) | 2017-09-15 | 2017-09-15 | A kind of preparation method of zinc oxide-active carbon composite catalyst |
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| CN201710833989.8A CN109499563A (en) | 2017-09-15 | 2017-09-15 | A kind of preparation method of zinc oxide-active carbon composite catalyst |
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Family
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110201660A (en) * | 2019-06-19 | 2019-09-06 | 塔里木大学 | A kind of zinc oxide/cotton stalk biomass carbon composite material and preparation method and application |
| CN111036189A (en) * | 2019-11-29 | 2020-04-21 | 昆明理工大学 | ZnO/CuO or ZnO/CuO/Cu loaded on activated carbon2Preparation method of O photocatalytic composite powder |
| CN111589415A (en) * | 2020-05-14 | 2020-08-28 | 内蒙古浦瑞芬环保科技有限公司 | Preparation method of active carbon loaded with zinc oxide in situ |
| CN111974374A (en) * | 2020-08-20 | 2020-11-24 | 昆明理工大学 | Preparation method of biochar modified nano ZnO composite powder |
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| CN111036189B (en) * | 2019-11-29 | 2021-11-30 | 昆明理工大学 | ZnO/CuO or ZnO/CuO/Cu loaded on activated carbon2Preparation method of O photocatalytic composite powder |
| CN111589415A (en) * | 2020-05-14 | 2020-08-28 | 内蒙古浦瑞芬环保科技有限公司 | Preparation method of active carbon loaded with zinc oxide in situ |
| CN111974374A (en) * | 2020-08-20 | 2020-11-24 | 昆明理工大学 | Preparation method of biochar modified nano ZnO composite powder |
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Application publication date: 20190322 |