CN109012576A - A kind of preparation method and application loading cuprous oxide particle active carbon - Google Patents
A kind of preparation method and application loading cuprous oxide particle active carbon Download PDFInfo
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- CN109012576A CN109012576A CN201810704313.3A CN201810704313A CN109012576A CN 109012576 A CN109012576 A CN 109012576A CN 201810704313 A CN201810704313 A CN 201810704313A CN 109012576 A CN109012576 A CN 109012576A
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- Prior art keywords
- active carbon
- cuprous oxide
- oxide particle
- discarded
- obtains
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 71
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 42
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 42
- 239000002245 particle Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000011068 loading method Methods 0.000 title claims abstract description 5
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000007788 liquid Substances 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000012545 processing Methods 0.000 claims abstract description 16
- 239000000706 filtrate Substances 0.000 claims abstract description 14
- 239000012153 distilled water Substances 0.000 claims abstract description 13
- 235000019441 ethanol Nutrition 0.000 claims abstract description 11
- 238000009833 condensation Methods 0.000 claims abstract description 9
- 230000005494 condensation Effects 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000010992 reflux Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- UGWKCNDTYUOTQZ-UHFFFAOYSA-N copper;sulfuric acid Chemical compound [Cu].OS(O)(=O)=O UGWKCNDTYUOTQZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000004448 titration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 18
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 12
- 229910052740 iodine Inorganic materials 0.000 claims description 12
- 239000011630 iodine Substances 0.000 claims description 12
- 238000001179 sorption measurement Methods 0.000 claims description 12
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 6
- 239000003610 charcoal Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000003756 stirring Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 21
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 9
- 229940012189 methyl orange Drugs 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 239000001048 orange dye Substances 0.000 description 5
- 239000000987 azo dye Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021386 carbon form Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- ZONODCCBXBRQEZ-UHFFFAOYSA-N platinum tungsten Chemical compound [W].[Pt] ZONODCCBXBRQEZ-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000001507 sample dispersion Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 230000000280 vitalizing effect Effects 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01J23/72—Copper
-
- 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
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of preparation method and application for loading cuprous oxide particle active carbon, belong to photocatalysis field and technical field of resource comprehensive utilization.Discarded active carbon is placed in the HNO that concentration is the mol/L of 2 mol/L ~ 6 first33 ~ 5h of processing under room temperature in solution obtains pretreated discarded active carbon L after filtering, distillation water washing, drying after the completion of processing；Distilled water is added to discarded active carbon L, ethyl alcohol and diethylene glycol solution is then added, 6 ~ 12 h of stirring obtain mixed liquor A；Configuration concentration is 0.2g/mL copper-bath, and the titrated sulfuric acid copper solution into mixed liquor A obtains mixed liquid B after the completion of titration；Mixed liquid B is placed in the device with reflux condensation mode and handles 6h, then filters and is dried to obtain filtrate；Obtained filtrate is roasted into 20min under the conditions of microwave power is 200 ~ 800W, heating temperature is 300 ~ 500 DEG C, obtains the active carbon of load cuprous oxide particle.The present invention using reflux condensation mode to activated carbon supported, can very fully will be on Metal Supported to active carbon.
Description
Technical field
The present invention relates to it is a kind of load cuprous oxide particle active carbon preparation method and application, belong to photocatalysis field and
Technical field of resource comprehensive utilization.
Background technique
Photocatalysis oxidation technique is to generate light induced electron and hole to deoxidation using reproducible solar energy vitalizing semiconductor
Change or reduction organic matter generates H2O、CO2, inorganic ions, achieve the purpose that permineralization, while having that low energy consumption, easy to operate,
The characteristics of can reacting under normal temperature and pressure and avoiding secondary pollution, is concerned in photocatalysis technology field.
In order to improve the absorption property of active carbon, improving has targetedly selective power to pollutant, it is necessary to work
Property charcoal it is modified using certain technology.Currently, loaded modified is that metal or compound are attached on activated carbon surface.Oxygen
Change cuprous (Cu2O) as a kind of p-type narrow gap semiconductor typically with unique light, magnetism characteristic, convert in solar energy,
Electronics, secondary storage device, bio-sensing and catalysis aspect have potential application, have excellent photocatalysis performance, by
The extensive concern of domestic and international scientific research circle.The band gap width of cuprous oxide is 2.1eV, and exciton can be transmitted continuously in single crystal,
Make its absorptivity with higher, becomes the important materials of production photovoltaic converter.Currently, for the common side of Metal Supported
Method has impregnation-calcination method, baking mixed method, admixture activation method, chemical vapor infiltration, sol-gal process etc..However, these are negative
The sample dispersion that support method prepares is poor, has great importance so preparing a kind of good material of physical and chemical performance.This
Invention is turned waste into wealth using discarded active carbon as catalyst carrier, recycles waste.
Applicant is in the patent application of 107051569 A of CN in patent publication No., discloses a kind of " support type spherical shape
The preparation method of active carbon photochemical catalyst ", this method are that spherical activated charcoal is impregnated in the presoma dissolution saturation containing carbon nitrogen source
Solvent solution in, obtain roasting raw material, be subsequently placed in tubular type kiln roasting to get to spherical activated charcoal photochemical catalyst.On
Invention is stated compared with the present invention, only with simple dipping and roasting in above method preparation process, metal can not be well
It is attached on activated carbon surface, and bad dispersibility.
Applicant is in the patent application of 107737596 A of CN in patent publication No., is disclosed " a kind of activated carbon supported
Platinum-tungsten catalyst preparation method and application that Cu, Al are modified altogether ", this method are that metatungstic acid is added in active carbon dispersion liquid
Ammonium salt solution adds a certain amount of chloroplatinic acid aqueous solution, by a certain percentage addition nitric acid presoma, reacting drying calcining reduction,
Obtain catalyst.The higher cost of the platinum and tungsten metal that are used in above-mentioned preparation.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides a kind of load cuprous oxide particle active carbon
Preparation method and application.The present invention using reflux condensation mode to activated carbon supported, can be very fully by Metal Supported to active
On charcoal；The present invention reduces preparation cost by supported copper, and is conducive to restore the hole of discarded active carbon by microwave calcining
Structure makes active carbon form the load that certain hole defect is conducive to cuprous oxide.The present invention passes through using discarded active carbon as raw material
Regeneration duties make active carbon restore absorption property, have reached recycled for multiple times；And photocatalytic degradation, which is utilized, takes it
Light source not to the utmost reduces energy output.The invention is realized by the following technical scheme.
A kind of preparation method loading cuprous oxide particle active carbon, the specific steps of which are as follows:
Step 1, first by discarded active carbon according to solid-to-liquid ratio be 1:5 ~ 1:10g/mL be placed in concentration be the mol/L of 2 mol/L ~ 6
HNO33 ~ 5h of processing under room temperature in solution obtains pretreated discarded activity after filtering, distillation water washing, drying after the completion of processing
Charcoal；
Step 2, the discarded active carbon for obtaining step 1 are that distilled water is added in 50:500g/mL according to solid-to-liquid ratio, and second is then added
Pure and mild diethylene glycol solution, wherein distilled water, ethyl alcohol, diethylene glycol solution volume ratio are 500:300:50, are 160 ~ 280r/ in revolving speed
6 ~ 12h is stirred under the conditions of min, obtains mixed liquor A；
Step 3, configuration concentration are 0.2g/mL copper-bath, are 2 according to mixed liquor A volume ratio in copper-bath and step 2
~ 8:30 ~ 80 titrated sulfuric acid copper solution into mixed liquor A obtains mixed liquid B after the completion of titration；
Mixed liquid B is placed in the device with reflux condensation mode by step 4, and being heated to temperature is 20 ~ 60 DEG C of processing 6h, is then filtered
And it is dried to obtain filtrate；
Step 5 roasts the filtrate that step 4 obtains under the conditions of microwave power is 200 ~ 800W, heating temperature is 300 ~ 500 DEG C
20min is burnt, the active carbon of load cuprous oxide particle is obtained.
It is 120 ~ 200 mesh that active carbon is discarded in the step 1, and iodine sorption value is 354 ~ 573mg/g, and specific surface area is
256m2/g~431m2/g。
A kind of load cuprous oxide particle active carbon, can apply in azo dyes Photocatalytic Degradation Process.
The beneficial effects of the present invention are:
(1) present invention reduces discharge and the environmental pollution of waste, realizes waste using discarded active carbon as raw material
Comprehensive utilization of resources.
(2) the method for the present invention is low in cost, pollution-free, and metal can be attached on activated carbon surface well excessively.
(3) present invention uses microwave heating, is heated using the selectivity of microwave, and low energy consumption, and heating speed is fast, and also utilizing can
Light-exposed degradation methyl orange dye is conducive to improve industrialized production efficiency and energy output.
Detailed description of the invention
Fig. 1 is the SEM figure for the load cuprous oxide particle active carbon that the embodiment of the present invention 3 is prepared.
Fig. 2 is the EDS figure for the load cuprous oxide particle active carbon that the embodiment of the present invention 3 is prepared.
Fig. 3 is the Raman figure for the load cuprous oxide particle active carbon that the embodiment of the present invention 3 is prepared.
Fig. 4 is that the wavelength for the load cuprous oxide particle active carbon degradation methyl orange that the embodiment of the present invention 3 is prepared becomes
Change curve graph.
Fig. 5 is load cuprous oxide active carbon energy photo-catalytic degradation of methyl-orange dyestuff mechanism figure.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
The active carbon of load cuprous oxide particle in following example is according to GB/T 12496.8-2015 " wooden activity
The measurement of charcoal test method iodine sorption value " measurement iodine sorption value, methyl orange azo dyes is chosen as photocatalytic degradation object.
Embodiment 1
The preparation method of the load cuprous oxide particle active carbon, the specific steps of which are as follows:
Step 1, by discarded active carbon, (discarded active carbon is 120 mesh, iodine sorption value 354mg/g, and specific surface area is first
256m2/ g) it according to solid-to-liquid ratio is that be placed in concentration be 2 mol/LHNO to 1:5g/mL33h is handled under room temperature in solution, after the completion of processing
Pretreated discarded active carbon is obtained after filtering, distillation water washing, drying；
It is that distilled water is added in 50:500g/mL that step 2, the 50g for obtaining step 1, which discard active carbon according to solid-to-liquid ratio, is then added
Ethyl alcohol and diethylene glycol solution, wherein distilled water, ethyl alcohol, diethylene glycol solution volume ratio are 500:300:50, are 160r/ in revolving speed
6h is stirred under the conditions of min, obtains mixed liquor A；
Step 3, configuration concentration are 0.2g/mL copper-bath, are according to copper-bath and mixed liquor A volume ratio in step 2
2:30 titrated sulfuric acid copper solution into mixed liquor A obtains mixed liquid B after the completion of titration；
Mixed liquid B is placed in the device with reflux condensation mode by step 4, and being heated to temperature is 20 DEG C of processing 6h, is then filtered and is done
It is dry to obtain filtrate；
The filtrate that step 4 obtains is roasted 20min under the conditions of microwave power is 200W, heating temperature is 500 DEG C by step 5,
Obtain the active carbon of load cuprous oxide particle.
The iodine sorption value for the load cuprous oxide active carbon being prepared through above-mentioned steps is 894mg/g, and specific surface area is
692m2/ g has reached 73% to the degradation rate for the methyl orange dye that initial concentration is 100mg/L.
Embodiment 2
The preparation method of the load cuprous oxide particle active carbon, the specific steps of which are as follows:
Step 1, by discarded active carbon, (discarded active carbon is 180 mesh, iodine sorption value 452mg/g, and specific surface area is first
345m2/ g) it according to solid-to-liquid ratio is that be placed in concentration be 6 mol/LHNO to 1:5g/mL34h is handled under room temperature in solution, after the completion of processing
Pretreated discarded active carbon is obtained after filtering, distillation water washing, drying；
It is that distilled water is added in 50:500g/mL that step 2, the 50g for obtaining step 1, which discard active carbon according to solid-to-liquid ratio, is then added
Ethyl alcohol and diethylene glycol solution, wherein distilled water, ethyl alcohol, diethylene glycol solution volume ratio are 500:300:50, are 200r/ in revolving speed
8h is stirred under the conditions of min, obtains mixed liquor A；
Step 3, configuration concentration are 0.2g/mL copper-bath, are according to copper-bath and mixed liquor A volume ratio in step 2
8:80 titrated sulfuric acid copper solution into mixed liquor A obtains mixed liquid B after the completion of titration；
Mixed liquid B is placed in the device with reflux condensation mode by step 4, and being heated to temperature is 60 DEG C of processing 6h, is then filtered and is done
It is dry to obtain filtrate；
The filtrate that step 4 obtains is roasted 20min under the conditions of microwave power is 200W, heating temperature is 400 DEG C by step 5,
Obtain the active carbon of load cuprous oxide particle.
The iodine sorption value for the load cuprous oxide active carbon being prepared through above-mentioned steps is 964mg/g, and specific surface area is
784m2/ g has reached 76% to the degradation rate for the methyl orange dye that initial concentration is 100mg/L.
Embodiment 3
The preparation method of the load cuprous oxide particle active carbon, the specific steps of which are as follows:
Step 1, by discarded active carbon, (discarded active carbon is 200 mesh, iodine sorption value 573mg/g, and specific surface area is first
431m2/ g) it according to solid-to-liquid ratio is that be placed in concentration be 4 mol/LHNO to 1:8g/mL35h is handled under room temperature in solution, after the completion of processing
Pretreated discarded active carbon is obtained after filtering, distillation water washing, drying；
It is that distilled water is added in 50:500g/mL that step 2, the 50g for obtaining step 1, which discard active carbon according to solid-to-liquid ratio, is then added
Ethyl alcohol and diethylene glycol solution, wherein distilled water, ethyl alcohol, diethylene glycol solution volume ratio are 500:300:50, are 250r/ in revolving speed
10h is stirred under the conditions of min, obtains mixed liquor A；
Step 3, configuration concentration are 0.2g/mL copper-bath, are according to copper-bath and mixed liquor A volume ratio in step 2
6:50 titrated sulfuric acid copper solution into mixed liquor A obtains mixed liquid B after the completion of titration；
Mixed liquid B is placed in the device with reflux condensation mode by step 4, and being heated to temperature is 40 DEG C of processing 6h, is then filtered and is done
It is dry to obtain filtrate；
The filtrate that step 4 obtains is roasted 20min under the conditions of microwave power is 600W, heating temperature is 500 DEG C by step 5,
Obtain the active carbon of load cuprous oxide particle.
The SEM for the load cuprous oxide particle active carbon that the present embodiment is prepared schemes as shown in Figure 1, can from Fig. 1
The active carbon pore structure for the load cuprous oxide particle being prepared out using the method is more obvious, and can be clear on its surface
It is seen that there is the cuprous oxide particle of spheroidal clearly, illustrates that regeneration duties effect is good.Fig. 2 is the load cuprous oxide being prepared
The EDS of particulate activated carbon schemes, it can be seen that contains Cu element in Activated Carbon with Cu, illustrates that such method successfully loads to copper
On active carbon.Fig. 3 is the Raman figure for the load cuprous oxide particle active carbon being prepared, it can be found that about in 1340cm-1
With 1600 cm-1Occur the peak D and the peak G respectively, this is two main peaks of apparent active carbon, and loads the process of cuprous oxide
Graphite microcrystalline structure can slightly be destroyed.
The iodine sorption value for the load cuprous oxide active carbon being prepared through above-mentioned steps is 1121 mg/g, specific surface area
For 913m2/ g has reached 81% to the degradation rate for the methyl orange dye that initial concentration is 100mg/L.
Fig. 4 is the wavelength change figure for the load cuprous oxide active carbon photo-catalytic degradation of methyl-orange being prepared, from figure
As can be seen that preceding 80min wavelength curve variation range is smaller under dark condition, and under the radiation of visible light it is 100min-
It when 140min, is considerably reduced much in the absorbance of maximum absorption wave strong point, this explanation is prepared negative with such method
Carrying cuprous oxide active carbon can degrade azo dyes.Fig. 5 is the mechanism figure of cuprous oxide photocatalysis azo dyes.It is main anti-
Answer equation as follows:
Embodiment 4
The preparation method of the load cuprous oxide particle active carbon, the specific steps of which are as follows:
Step 1, by discarded active carbon, (discarded active carbon is 200 mesh, iodine sorption value 573mg/g, and specific surface area is first
431m2/ g) it according to solid-to-liquid ratio is that be placed in concentration be 4 mol/LHNO to 1:10g/mL35h is handled under room temperature in solution, after the completion of processing
Pretreated discarded active carbon is obtained after filtering, distillation water washing, drying；
It is that distilled water is added in 50:500g/mL that step 2, the 50g for obtaining step 1, which discard active carbon according to solid-to-liquid ratio, is then added
Ethyl alcohol and diethylene glycol solution, wherein distilled water, ethyl alcohol, diethylene glycol solution volume ratio are 500:300:50, are 280r/ in revolving speed
12h is stirred under the conditions of min, obtains mixed liquor A；
Step 3, configuration concentration are 0.2g/mL copper-bath, are according to copper-bath and mixed liquor A volume ratio in step 2
8:80 titrated sulfuric acid copper solution into mixed liquor A obtains mixed liquid B after the completion of titration；
Mixed liquid B is placed in the device with reflux condensation mode by step 4, and being heated to temperature is 30 DEG C of processing 6h, is then filtered and is done
It is dry to obtain filtrate；
The filtrate that step 4 obtains is roasted 20min under the conditions of microwave power is 800W, heating temperature is 300 DEG C by step 5,
Obtain the active carbon of load cuprous oxide particle.
The iodine sorption value for the load cuprous oxide active carbon being prepared through above-mentioned steps is 1038mg/g, and specific surface area is
849 m2/ g has reached 78% to the degradation rate for the methyl orange dye that initial concentration is 100mg/L.
In conjunction with attached drawing, the embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned
Embodiment within the knowledge of a person skilled in the art can also be before not departing from present inventive concept
Put that various changes can be made.
Claims (3)
1. a kind of preparation method for loading cuprous oxide particle active carbon, it is characterised in that specific step is as follows:
Step 1, first by discarded active carbon according to solid-to-liquid ratio be 1:5 ~ 1:10g/mL be placed in concentration be the mol/L of 2 mol/L ~ 6
HNO33 ~ 5h of processing under room temperature in solution obtains pretreated discarded work after filtering, distillation water washing, drying after the completion of processing
Property charcoal；
Step 2, the discarded active carbon for obtaining step 1 are that distilled water is added in 50:500g/mL according to solid-to-liquid ratio, and second is then added
Pure and mild diethylene glycol solution, wherein distilled water, ethyl alcohol, diethylene glycol solution volume ratio are 500:300:50, are 160 ~ 280r/ in revolving speed
6 ~ 12h is stirred under the conditions of min, obtains mixed liquor A；
Step 3, configuration concentration are 0.2g/mL copper-bath, are 2 according to mixed liquor A volume ratio in copper-bath and step 2
~ 8:30 ~ 80 titrated sulfuric acid copper solution into mixed liquor A obtains mixed liquid B after the completion of titration；
Mixed liquid B is placed in the device with reflux condensation mode by step 4, and being heated to temperature is 20 ~ 60 DEG C of processing 6h, is then filtered
And it is dried to obtain filtrate；
Step 5 roasts the filtrate that step 4 obtains under the conditions of microwave power is 200 ~ 800W, heating temperature is 300 ~ 500 DEG C
20min is burnt, the active carbon of load cuprous oxide particle is obtained.
2. the preparation method of load cuprous oxide particle active carbon according to claim 1, it is characterised in that: the step
It is 120 ~ 200 mesh that active carbon is discarded in 1, and iodine sorption value is 354 ~ 573mg/g, specific surface area 256m2/g~431m2/g。
3. it is a kind of according to claim 1 or the 2 load cuprous oxide particle active carbons that are prepared, can apply and be contaminated in azo
Expect Photocatalytic Degradation Process.
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| CN113209973A (en) * | 2021-04-22 | 2021-08-06 | 昆明理工大学 | ZnO-Cu2Preparation method and application of O-AC photocatalyst |
| CN114904483A (en) * | 2022-04-18 | 2022-08-16 | 东北林业大学 | Wood-based carbon/Cu capable of efficiently adsorbing anionic dye 2 Preparation method of O adsorbent |
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Application publication date: 20181218 |