CN108620086A - The preparation method of novel flakes Zn-Cu-W photochemical catalysts - Google Patents
The preparation method of novel flakes Zn-Cu-W photochemical catalysts Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004202 carbamide Substances 0.000 claims abstract description 11
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 11
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 11
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000004090 dissolution Methods 0.000 claims abstract description 7
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008236 heating water Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000011701 zinc Substances 0.000 abstract 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/342—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electric, magnetic or electromagnetic fields, e.g. for magnetic separation
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Optics & Photonics (AREA)
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- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a kind of preparation methods of novel flakes Zn Cu W photochemical catalysts, include the following steps：It is made into microemulsion after methanol, isopropanol, water are mixed, zinc sulfate, copper chloride, sodium tungstate are added after mixed system is heated up, 10 30min of ultrasonic dissolution, ultrasonic power is 20 800W, and urea liquid is added dropwise after sample all dissolving, stirs evenly, the solution of preparation is put into stable state magnetostatic field environment, 2 30h are reacted, is filtered, washed, dries after reaction, obtain the Zn Cu W photochemical catalysts of flakes.Ternary photochemical catalyst prepared by the present invention has flakes pattern, it is seen that photocatalytic activity is high, excellent catalytic effect.
Description
Technical field
The invention belongs to photocatalysis technology fields, and in particular to a kind of preparation of novel flakes Zn-Cu-W photochemical catalysts
Method.
Background technology
With the continuous consumption of economic fast development and fossil fuel, the environment and energy problem thus caused is increasingly convex
It is aobvious.Photocatalysis technology is expected to administer using solar energy as one gets dirty environment and prepares the green of fossil fuel alternative energy source on the way
Diameter has obtained more and more concerns.Japanese Scientists Fujishima in 1972 etc. has found TiO2Light may be implemented in monocrystalline electricity grade
Water is catalytically decomposed（Fujishima A., 1972）, find nano-TiO again later2Ability with photocatalytic degradation organic matter,
TiO2As the research hotspot of Material Field.But it there are sun light utilization efficiency is low, photo-generate electron-hole is to recombination rate height etc.
The shortcomings that being not easily overcome.Therefore, carry out the research of novel non-traditional high activity, high energy efficiency catalysis material, it has also become photocatalysis
One important directions in field.
Invention content
To make up the deficiencies in the prior art, the present invention provides a kind of preparation side of novel flakes Zn-Cu-W photochemical catalysts
Method, the photocatalytic activity with stability and high efficiency, has broad application prospects to the degradation of heavy metal ions in wastewater.
The present invention is achieved through the following technical solutions：
A kind of preparation method of novel flakes Zn-Cu-W photochemical catalysts, is characterized in that：Include the following steps：
（1）It is made into microemulsion after methanol, isopropanol, water are mixed；
（2）Zinc sulfate, copper chloride, sodium tungstate, ultrasonic dissolution 10-30min, ultrasonic power are added after above-mentioned mixed system is heated up
For 20-800W, urea liquid is added dropwise after sample all dissolving, stirs evenly；
（3）By step（2）The solution of preparation is put into stable state magnetostatic field environment, reacts 2-30h；
（4）It is filtered, washed, dries after reaction, obtain the Zn-Cu-W photochemical catalysts of flakes.
Step（1）Middle methanol, isopropanol, water volume ratio be 1:1:2.
Step（2）The middle mass ratio that zinc sulfate, copper chloride, sodium tungstate and microemulsion mixed system is added is 1：（1.5-2）：
（2-2.5）：（15-18）.
Further, step（2）The middle urea liquid volume and the volume ratio of microemulsion mixed system of being added is 1：（30-
50）, the mass concentration of urea liquid is 2%.
Further, step（2）In, first mixed system is put into beaker, beaker, which is transferred to 25 DEG C of waters bath with thermostatic control, to be stirred
It mixes in device, then zinc sulfate, copper chloride, sodium tungstate is added to 45 DEG C in warming while stirring.
Step（3）The magnetic density of middle stable state magnetostatic field is 0.5-10 teslas.
Further, step（3）Middle reaction temperature is 30 DEG C, using heating water bath.
The beneficial effects of the invention are as follows：Zn-Cu-W ternary photochemical catalysts prepared by the present invention have flakes pattern, it is seen that
Photocatalytic activity is high, excellent catalytic effect, has excellent effect, the degradation rate in 60min to the degradation of heavy metal ions in wastewater
Up to 97% or more.
Specific implementation mode
The present invention will be further described in detail with reference to the specific embodiments, to help those skilled in the art
There is more complete, accurate and deep understanding to the inventive concept of the present invention, technical solution, protection scope of the present invention includes but not
It is limited to following embodiment, any details to technical scheme of the present invention under the premise of without departing from spirit and scope
It is each fallen in protection scope of the present invention with the modification that form is made.
Embodiment 1
A kind of preparation method of novel flakes Zn-Cu-W photochemical catalysts, includes the following steps：
It is made into microemulsion after 10ml methanol, 10ml isopropanols, 20ml water are mixed；Above-mentioned mixed system is put into beaker, and
Beaker is transferred in 25 DEG C of water bath with thermostatic control blenders, 45 DEG C is warming up to and 2g zinc sulfate, 3.5g copper chlorides, 4.3g wolframic acids is added
1ml 2% is added dropwise after sample all dissolving in 20 min of ultrasonic dissolution in sodium ultrasonic cleaner, 500 W of ultrasonic power
Urea liquid, continue stir 30 min；The solution of preparation is added in the stable state magnetostatic field environment of 2 teslas, is continued anti-
It answers 12 hours, temperature uses heating water bath, controlled at 30 DEG C；It is filtered, washed, dries after reaction, obtain flakes
Zn-Cu-W photochemical catalysts.
Embodiment 2
A kind of preparation method of novel flakes Zn-Cu-W photochemical catalysts, includes the following steps：
It is made into microemulsion after 10ml methanol, 10ml isopropanols, 20ml water are mixed；Above-mentioned mixed system is put into beaker, and
Beaker is transferred in 25 DEG C of water bath with thermostatic control blenders, 45 DEG C is warming up to and 2g zinc sulfate, 3.5g copper chlorides, 4.3g wolframic acids is added
1ml 2% is added dropwise after sample all dissolving in 20 min of ultrasonic dissolution in sodium ultrasonic cleaner, 100 W of ultrasonic power
Urea liquid, continue stir 30 min；The solution of preparation is added in the stable state magnetostatic field environment of 6 teslas, is continued anti-
It answers 10 hours, temperature uses heating water bath, controlled at 30 DEG C；It is filtered, washed, dries after reaction, obtain flakes
Zn-Cu-W photochemical catalysts.
Embodiment 3
A kind of preparation method of novel flakes Zn-Cu-W photochemical catalysts, includes the following steps：
It is made into microemulsion after 10ml methanol, 10ml isopropanols, 20ml water are mixed；Above-mentioned mixed system is put into beaker, and
Beaker is transferred in 25 DEG C of water bath with thermostatic control blenders, 45 DEG C is warming up to and 2g zinc sulfate, 3.5g copper chlorides, 4.3g wolframic acids is added
1ml 2% is added dropwise after sample all dissolving in 20 min of ultrasonic dissolution in sodium ultrasonic cleaner, 700 W of ultrasonic power
Urea liquid, continue stir 30 min；The solution of preparation is added in the stable state magnetostatic field environment of 10 teslas, is continued anti-
It answers 25 hours, temperature uses heating water bath, controlled at 30 DEG C；It is filtered, washed, dries after reaction, obtain flakes
Zn-Cu-W photochemical catalysts.
Embodiment 4
A kind of preparation method of novel flakes Zn-Cu-W photochemical catalysts, includes the following steps：
It is made into microemulsion after 10ml methanol, 10ml isopropanols, 20ml water are mixed；Above-mentioned mixed system is put into beaker, and
Beaker is transferred in 25 DEG C of water bath with thermostatic control blenders, 45 DEG C is warming up to and 2g zinc sulfate, 3.5g copper chlorides, 4.3g wolframic acids is added
1ml 2% is added dropwise after sample all dissolving in 20 min of ultrasonic dissolution in sodium ultrasonic cleaner, 800 W of ultrasonic power
Urea liquid, continue stir 30 min；The solution of preparation is added in the stable state magnetostatic field environment of 1 tesla, is continued anti-
It answers 30 hours, temperature uses heating water bath, controlled at 30 DEG C；It is filtered, washed, dries after reaction, obtain flakes
Zn-Cu-W photochemical catalysts.
Claims (7)
1. a kind of preparation method of novel flakes Zn-Cu-W photochemical catalysts, it is characterised in that：Include the following steps：
（1）It is made into microemulsion after methanol, isopropanol, water are mixed；
（2）Zinc sulfate, copper chloride, sodium tungstate, ultrasonic dissolution 10-30min, ultrasonic power are added after above-mentioned mixed system is heated up
For 20-800W, urea liquid is added dropwise after sample all dissolving, stirs evenly；
（3）By step（2）The solution of preparation is put into stable state magnetostatic field environment, reacts 2-30h；
（4）It is filtered, washed, dries after reaction, obtain the Zn-Cu-W photochemical catalysts of flakes.
2. the preparation method of novel flakes Zn-Cu-W photochemical catalysts according to claim 1, it is characterised in that：Step
（1）Middle methanol, isopropanol, water volume ratio be 1:1:2.
3. the preparation method of novel flakes Zn-Cu-W photochemical catalysts according to claim 2, it is characterised in that：Step
（2）The middle mass ratio that zinc sulfate, copper chloride, sodium tungstate and microemulsion mixed system is added is 1：（1.5-2）：（2-2.5）：（15-
18）.
4. the preparation method of novel flakes Zn-Cu-W photochemical catalysts according to claim 1 or 3, it is characterised in that：Step
Suddenly（2）The middle urea liquid volume and the volume ratio of microemulsion mixed system of being added is 1：（30-50）, the mass concentration of urea liquid
It is 2%.
5. the preparation method of novel flakes Zn-Cu-W photochemical catalysts according to claim 4, it is characterised in that：Step
（2）In, first mixed system is put into beaker, beaker is transferred in 25 DEG C of water bath with thermostatic control blenders, warming while stirring is extremely
45 DEG C, zinc sulfate, copper chloride, sodium tungstate is then added.
6. the preparation method of novel flakes Zn-Cu-W photochemical catalysts according to claim 1, it is characterised in that：Step
（3）The magnetic density of middle stable state magnetostatic field is 0.5-10 teslas.
7. the preparation method of novel flakes Zn-Cu-W photochemical catalysts according to claim 1 or 6, it is characterised in that：Step
Suddenly（3）Middle reaction temperature is 30 DEG C, using heating water bath.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810295629.1A CN108620086B (en) | 2018-04-04 | 2018-04-04 | The preparation method of flakes Zn-Cu-W photochemical catalyst |
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| CN108620086A true CN108620086A (en) | 2018-10-09 |
| CN108620086B CN108620086B (en) | 2019-03-19 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102872918A (en) * | 2012-11-02 | 2013-01-16 | 北京化工大学 | ZnTi hydrotalcite nanosheet catalyst and application of catalyst in hydrogen preparation by photoactivating and decomposing water |
| CN104276606A (en) * | 2014-07-30 | 2015-01-14 | 安顺学院 | Preparation method, application and regenerating method of silicon magnetic hollow sphere ZnSixFe2-xO4 |
| CN105435796A (en) * | 2014-08-18 | 2016-03-30 | 中国科学院理化技术研究所 | Monovalent-zinc-doped hydrotalcite nano photocatalyst and preparation method and application thereof |
| CN105727963A (en) * | 2016-04-18 | 2016-07-06 | 盐城工学院 | Fe and Cu co-doped nano-sized ZnO photocatalyst and preparation method thereof |
-
2018
- 2018-04-04 CN CN201810295629.1A patent/CN108620086B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102872918A (en) * | 2012-11-02 | 2013-01-16 | 北京化工大学 | ZnTi hydrotalcite nanosheet catalyst and application of catalyst in hydrogen preparation by photoactivating and decomposing water |
| CN104276606A (en) * | 2014-07-30 | 2015-01-14 | 安顺学院 | Preparation method, application and regenerating method of silicon magnetic hollow sphere ZnSixFe2-xO4 |
| CN105435796A (en) * | 2014-08-18 | 2016-03-30 | 中国科学院理化技术研究所 | Monovalent-zinc-doped hydrotalcite nano photocatalyst and preparation method and application thereof |
| CN105727963A (en) * | 2016-04-18 | 2016-07-06 | 盐城工学院 | Fe and Cu co-doped nano-sized ZnO photocatalyst and preparation method thereof |
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