CN106881130A - A kind of silver carbonate loads the preparation method of cobalt carbonate/silver chlorate photochemical catalyst - Google Patents
A kind of silver carbonate loads the preparation method of cobalt carbonate/silver chlorate photochemical catalyst Download PDFInfo
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- CN106881130A CN106881130A CN201710201055.2A CN201710201055A CN106881130A CN 106881130 A CN106881130 A CN 106881130A CN 201710201055 A CN201710201055 A CN 201710201055A CN 106881130 A CN106881130 A CN 106881130A
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- Prior art keywords
- silver
- carbonate
- cobalt
- carbonic acid
- colloid
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- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910021446 cobalt carbonate Inorganic materials 0.000 title claims abstract description 23
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 title claims abstract description 23
- 229910001958 silver carbonate Inorganic materials 0.000 title claims abstract description 23
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 title claims abstract description 23
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 title claims abstract description 23
- 239000003054 catalyst Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 32
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000084 colloidal system Substances 0.000 claims abstract description 24
- LKZMBDSASOBTPN-UHFFFAOYSA-N carbonic acid;silver Chemical compound [Ag].OC(O)=O LKZMBDSASOBTPN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 17
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 7
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 150000002500 ions Chemical class 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 238000004821 distillation Methods 0.000 claims abstract description 5
- ZJRWDIJRKKXMNW-UHFFFAOYSA-N carbonic acid;cobalt Chemical compound [Co].OC(O)=O ZJRWDIJRKKXMNW-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 3
- 238000004042 decolorization Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- 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 1
- 241000220317 Rosa Species 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The present invention discloses the preparation method that a kind of silver carbonate loads cobalt carbonate/silver chlorate photochemical catalyst, comprises the following steps that:Silver nitrate solution and sodium carbonate liquor are mixed, colloid substance is formed, 3~4h is persistently stirred, sodium carbonate and silver nitrate react in whipping process, generate carbonic acid silver colloid;Carbonic acid silver colloid is placed in pellicle bag, with distillation water washing 3~4 times, dissociated ion is got rid of, then the carbonic acid silver colloid is added in the cobalt chloride solution that 60~80mL concentration is 1~2mol/L, soaked 1~5 day, carbonic acid cobalt nano-particle is formed in silver carbonate particle surface, there are a small amount of silver chlorate and the Particles dispersed, separation of solid and liquid, deionized water washing solid 2~3 times simultaneously, 75~105 DEG C of drying, are obtained a kind of silver carbonate load cobalt carbonate/silver chlorate photochemical catalyst.Silver carbonate and cobalt carbonate/silver chlorate are compound, and synergy can make cobalt carbonate also to play catalytic action in the presence of visible ray and can obtain good catalytic effect.
Description
Technical field
The present invention relates to the preparation method that a kind of silver carbonate loads cobalt carbonate/silver chlorate photochemical catalyst, belong to environmental protection
Middle technical field of sewage.
Background technology
Traditional method for treating water efficiency is low, high cost, there are secondary pollution problems, and waste water control always cannot be well
Solution.The development and application of nanometer technology are likely to thoroughly solve this problem.Start within 1972 to find TiO2Oxidation activity
Higher, chemical stability is good, harmless to the human body, and low cost is pollution-free, has a wide range of application, thus is most paid attention to, but TiO2
Larger (such as anatase TiO of energy gap2Energy gap Eg=3.2eV), be only capable of absorb ultraviolet region (wavelength is less than
Light 387nm), the utilization ratio to solar energy is relatively low.
In contaminant degradation and production of energy field, conductor photocatalysis are one of most promising methods.Work as energy
Amount will produce dividing for electron-hole pair when being more than or equal to the photon irradiation of semiconductor energy gap in photocatalyst surface
From this is the initial basic step of light-catalyzed reaction.In order to find efficient photochemical catalyst, numerous studies work is all concentrated on
Study in the influence factor of photocatalytic activity.Not only there is catalysis activity Yuan due to silver but also lewis acidic property can have been shown,
Meanwhile, silver is compared with other metals, such as gold, platinum, and price is more cheap, therefore with stronger industrial applicability.But carbonic acid
Due to the limitation of itself characteristic, in terms of photocatalytic degradation, performance need to be improved silver.
The content of the invention
The purpose of the present invention is to solve the shortcomings of the prior art, propose a kind of silver carbonate load cobalt carbonate/silver chlorate light
The preparation method of catalyst, the method is to form catalyst in carrier surface, and catalyst and carrier are combined closely.
The technical solution adopted by the present invention is to use following steps:
1) 12~16mmol silver nitrates are weighed, the silver nitrate solution of 15mmol/L is configured to, 6.6~8mmol carbonic acid is weighed
Sodium, is configured to the sodium carbonate liquor of 20mmol/L;
2) both the above solution is mixed under 350~400 revs/min of rotating speed, forms colloid substance, persistently stir 3
~4h, sodium carbonate and silver nitrate react in whipping process, generate carbonic acid silver colloid;
3) carbonic acid silver colloid is placed in pellicle bag, with water washing is distilled 3~4 times, gets rid of dissociated ion, then should
Carbonic acid silver colloid is added in the cobalt chloride solution that 60~80mL concentration is 1~2mol/L, is soaked 1~5 day, in carbonic acid Argent grain
Surface forms carbonic acid cobalt nano-particle, while have a small amount of silver chlorate and the Particles dispersed, separation of solid and liquid, deionized water washing solid
2~3 times, 75~105 DEG C of drying are obtained a kind of silver carbonate load cobalt carbonate/silver chlorate photochemical catalyst.
The beneficial effects of the invention are as follows:(1) this method forms solubility using the difference of solubility product constant in carbonic acid silver surface
The smaller cobalt carbonate crystal of product constant, the silver ion for cementing out and chlorion form silver chloride particle.
(2) silver carbonate and cobalt carbonate/silver chlorate are compound, synergy, can make cobalt carbonate in the presence of visible ray
Catalytic action can be played and good catalytic effect can be obtained.
Specific embodiment
Embodiment 1
16mmol silver nitrates are weighed, the silver nitrate solution of 15mmol/L is configured to, 8mmol sodium carbonate is weighed, is configured to
The sodium carbonate liquor of 20mmol/L;Both the above solution is mixed under 400 revs/min of rotating speed, colloid substance is formed, continued
Stirring 4h, sodium carbonate and silver nitrate react in whipping process, generate carbonic acid silver colloid.
Carbonic acid silver colloid is placed in pellicle bag, with distillation water washing 4 times, dissociated ion is got rid of, then by the carbonic acid
Silver colloid is added in the cobalt chloride solution that 80mL concentration is 2mol/L, is soaked 5 days, and cobalt carbonate is formed in silver carbonate particle surface
Nano particle, while have a small amount of silver chlorate and the Particles dispersed, separation of solid and liquid, deionized water washing solid 3 times, 105 DEG C of drying,
A kind of silver carbonate load cobalt carbonate/silver chlorate photochemical catalyst is obtained.
It is 40mg/L's that the silver carbonate load cobalt carbonate/silver chlorate photochemical catalyst 0.5g that will be obtained is added to 200mL concentration
In acid red waste water, under the irradiation of 300w Metal halogen lamps, 30min is reacted, percent of decolourization is 97.5%, catalyst can be repeated after separating
Utilize.
Embodiment 2
12mmol silver nitrates are weighed, the silver nitrate solution of 15mmol/L is configured to, 6.6mmol sodium carbonate is weighed, is configured to
The sodium carbonate liquor of 20mmol/L;Both the above solution is mixed under 350 revs/min of rotating speed, colloid substance is formed, continued
Stirring 3h, sodium carbonate and silver nitrate react in whipping process, generate carbonic acid silver colloid.
Carbonic acid silver colloid is placed in pellicle bag, with distillation water washing 3 times, dissociated ion is got rid of, then by the carbonic acid
Silver colloid is added in the cobalt chloride solution that 60mL concentration is 1mol/L, is soaked 1 day, and cobalt carbonate is formed in silver carbonate particle surface
Nano particle, while have a small amount of silver chlorate and the Particles dispersed, separation of solid and liquid, deionized water washing solid 2 times, 75 DEG C of drying,
A kind of silver carbonate load cobalt carbonate/silver chlorate photochemical catalyst is obtained.
It is 40mg/L's that the silver carbonate load cobalt carbonate/silver chlorate photochemical catalyst 0.5g that will be obtained is added to 200mL concentration
In the waste water of gold orange 7, under the irradiation of 300w Metal halogen lamps, 30min is reacted, percent of decolourization is 96.5%, catalyst can be repeated after separating
Utilize.For identical waste water at identical conditions, the degradation efficiency of pure silver carbonate is 81.2%.
Embodiment 3
16mmol silver nitrates are weighed, the silver nitrate solution of 15mmol/L is configured to, 8mmol sodium carbonate is weighed, is configured to
The sodium carbonate liquor of 20mmol/L;Both the above solution is mixed under 400 revs/min of rotating speed, colloid substance is formed, continued
3~4h of stirring, sodium carbonate and silver nitrate react in whipping process, generate carbonic acid silver colloid.
Carbonic acid silver colloid is placed in pellicle bag, with distillation water washing 4 times, dissociated ion is got rid of, then by the carbonic acid
Silver colloid is added in the cobalt chloride solution that 60mL concentration is 2mol/L, is soaked 3 days, and cobalt carbonate is formed in silver carbonate particle surface
Nano particle, while have a small amount of silver chlorate and the Particles dispersed, separation of solid and liquid, deionized water washing solid 3 times, 95 DEG C of drying,
A kind of silver carbonate load cobalt carbonate/silver chlorate photochemical catalyst is obtained.
It is 40mg/L's that the silver carbonate load cobalt carbonate/silver chlorate photochemical catalyst 0.5g that will be obtained is added to 200mL concentration
In rose red b waste water, under the irradiation of 300w Metal halogen lamps, 30min is reacted, percent of decolourization is 97.2%, catalyst can be after separating again
It is multiple to utilize.
Claims (1)
1. a kind of silver carbonate loads the preparation method of cobalt carbonate/silver chlorate photochemical catalyst, it is characterized in that in turn including the following steps:
1) 12~16mmol silver nitrates are weighed, the silver nitrate solution of 15mmol/L is configured to, 6.6~8mmol sodium carbonate is weighed, is matched somebody with somebody
It is set to the sodium carbonate liquor of 20mmol/L;
2) both the above solution is mixed under 350~400 revs/min of rotating speed, forms colloid substance, persistently stir 3~4h,
Sodium carbonate and silver nitrate react in whipping process, generate carbonic acid silver colloid;
3) carbonic acid silver colloid is placed in pellicle bag, with distillation water washing 3~4 times, gets rid of dissociated ion, then by the carbonic acid
Silver colloid is added in the cobalt chloride solution that 60~80mL concentration is 1~2mol/L, is soaked 1~5 day, in silver carbonate particle surface
Carbonic acid cobalt nano-particle is formed, while have a small amount of silver chlorate and the Particles dispersed, separation of solid and liquid, deionized water washing solid 2~3
Secondary, 75~105 DEG C of drying are obtained a kind of silver carbonate load cobalt carbonate/silver chlorate photochemical catalyst.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113546642A (en) * | 2020-04-24 | 2021-10-26 | 南京大学 | Nano Ag modified sea urchin-shaped porous basic cobalt carbonate composite material and preparation method thereof |
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2017
- 2017-03-30 CN CN201710201055.2A patent/CN106881130A/en active Pending
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