CN108435149A - A kind of nano cuprous oxide radical dye sorbing material and preparation method thereof - Google Patents
A kind of nano cuprous oxide radical dye sorbing material and preparation method thereof Download PDFInfo
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- CN108435149A CN108435149A CN201810054831.5A CN201810054831A CN108435149A CN 108435149 A CN108435149 A CN 108435149A CN 201810054831 A CN201810054831 A CN 201810054831A CN 108435149 A CN108435149 A CN 108435149A
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- cuprous oxide
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- oxide radical
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- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 56
- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 56
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 49
- 238000001179 sorption measurement Methods 0.000 claims abstract description 26
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 22
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 22
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 22
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000010949 copper Substances 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052802 copper Inorganic materials 0.000 claims abstract description 17
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000002244 precipitate Substances 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 15
- 238000001556 precipitation Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000001103 potassium chloride Substances 0.000 claims abstract description 8
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 5
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims description 28
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 16
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 16
- 235000011150 stannous chloride Nutrition 0.000 claims description 16
- 239000001119 stannous chloride Substances 0.000 claims description 16
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 18
- 238000000034 method Methods 0.000 abstract description 9
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 230000035484 reaction time Effects 0.000 abstract description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 abstract 2
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000000975 dye Substances 0.000 description 37
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 18
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 16
- 229920006395 saturated elastomer Polymers 0.000 description 10
- 239000003643 water by type Substances 0.000 description 10
- 230000003647 oxidation Effects 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 9
- 238000011282 treatment Methods 0.000 description 7
- 239000002351 wastewater Substances 0.000 description 7
- 229940045803 cuprous chloride Drugs 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000013049 sediment Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 2
- 229930003268 Vitamin C Natural products 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 235000019154 vitamin C Nutrition 0.000 description 2
- 239000011718 vitamin C Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 238000009303 advanced oxidation process reaction Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000003851 biochemical process Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
-
- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
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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
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- 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
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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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- 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
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- 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
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- 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
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Abstract
The cuprous oxide based composites and preparation method thereof that the present invention relates to a kind of for Dye Adsorption.The preparation method of the material is：(1) copper chloride solution is prepared；(2) ammonium hydroxide will be added in the copper chloride solution, stirs, form copper ammon solution；(3) in the mixed solution, ascorbic acid solution is added, stirring generates white precipitate；(4) white precipitate that step (3) obtains is centrifuged and is cleaned with deionized water, obtain presoma；(5) potassium chloride is dissolved in deionized water, a certain amount of CTAB and ascorbic acid is added later to form mixed solution；(6) presoma made from step (4) is added in mixed solution made from step (5), a small amount of ammonium hydroxide is added, stirred, generate precipitation；(7) the precipitation separation that obtains step (6), is dried in vacuo to get to cuprous oxide radical dye adsorption composite material cleaning.This method preparation process is simple, at low cost, reaction time is short, other than it can be used for Dye Adsorption, applies also for the fields such as photocatalysis, air-sensitive.
Description
Technical field
The invention belongs to Dye Adsorption technical field, more particularly to a kind of cuprous oxide base composite wood for Dye Adsorption
The preparation method of material.
Background technology
Dyeing, as the key link of textile deep processing and raising added value, the dyeing in China is sent out very much
It reaches, especially in Jiangsu and Zhejiang Provinces area.According to statistics, China often produces 150000 tons of amount of dye per year, is directly arranged with waste water without dealing carefully with
Being put into the marine dyestuff of rivers, there are about 10% -15%.Due to dyeing waste water complicated component, concentration is high, coloration is big and discharge capacity
Greatly, and in many dyestuffs certain carcinogens are rich in, have the characteristics that complicated, resistance to photodissociation, resistance to oxidation are brought to environment
Serious pollution, further, since the anti-light solution of complicated components, dyestuff, inoxidizability brought to waste water from dyestuff improvement by force it is prodigious
It is difficult.How effectively to solve pollution problem caused by waste water from dyestuff becomes the task of top priority.
Include at present biochemical process, absorption method, ion-exchange, chemical precipitation for the treatment technology of waste water from dyestuff
Method, electrochemical process etc., but these technologies still have certain defect so that and they can not completely remove pollutant, or even can
Can there is also introduce secondary pollution the problem of.High-level oxidation technology (Advance oxidation processed, AOPs) is in recent years
It has begun to substitute traditional treatment technology, for handling many toxic organic compounds, conductor photocatalysis in waste water
Degradation technique is to apply most one of high-level oxidation technologies at present.Wherein, titanium dioxide (TiO2) due to its good photocatalysis
Effect becomes research emphasis.However, titanium dioxide can only respond ultraviolet light (wavelength is less than 380nm), but receive on earth
To sunlight in, ultraviolet light content only accounts for 4%, and visible light accounts for 43%.
For cuprous oxide as a kind of important p-type semiconductor material, band-gap energy is suctions of the 2.0-2.2eV in visible region
Receive coefficient it is higher, energy transformation ratio theoretically up to 12%, but they there is a problem of it is low to Dye Adsorption efficiency.In photocatalysis
In reaction process, absorption is that a critically important step is only adsorbed to research shows that absorption is the precondition of light-catalyzed reaction
Contaminant molecule on photochemical catalyst could further divide degradation.
2015, Yang Renchun was prepared for Cu using hydro-thermal method2O-CuCl composite materials (Renchun Yang, Xiaojia
Lu,Xiang Huang,Applied Catalysis B:Environmental,2015,170-171,225).Research shows that with
Pure Cu2O is compared, Cu2O-CuCl composite materials have the photocatalytic activity of narrower band gap and enhancing.However this method pair is set
It is standby it is more demanding, preparation process is complicated, of high cost.
Therefore, how using simple method, lower cost, the strong Cu of adsorption capacity is prepared2O based composites have
It is significant.
Invention content
The purpose of the present invention is to solve existing cuprous oxide sorbing material there are preparation methods skills such as complicated, of high cost
Art problem, provide a kind of having engine dyeing to organic dyestuff excellent adsorption and its light-catalysed absorption region in visible light region
Adsorbent and preparation method thereof is expected, so as to the processing applied to high-chromaticity dye wastewater.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of nano cuprous oxide radical dye sorbing material includes oxygen in the nano cuprous oxide radical dye sorbing material
Change cuprous and stannous chloride, the mass ratio of the cuprous oxide and stannous chloride is (67.4~84):(16~32.6).
A kind of preparation method of nano cuprous oxide radical dye sorbing material, includes the following steps：
(1) copper chloride dihydrate is dissolved in deionized water, is stirred, form copper chloride solution；
(2) ammonium hydroxide is added into copper chloride solution, forms copper ammon solution；
(3) ascorbic acid solution is added into copper ammon solution, stirs, generates white precipitate；
(4) white precipitate is centrifuged and is cleaned with deionized water, obtain presoma；
(5) potassium chloride is dissolved in deionized water, and be added cetyl trimethylammonium bromide and ascorbic acid formed it is mixed
Close solution；
(6) presoma made from step (4) is added in mixed solution made from step (5), adds ammonium hydroxide, stirs
It mixes, generates precipitation；
(7) it is cleaned precipitation and centrifugal separation that step (6) obtains and with deionized water, vacuum drying is to get to nano oxygen
Change cuprous radical dye sorbing material.
Further, a concentration of 0.1~0.6mol/L of copper chloride solution in the step (1).
Further, in the step (2) in the addition Yu step (1) of ammonium hydroxide the substance of the addition of copper chloride amount ratio
It is 4.5:1, to ensure to be fully converted to copper ammon solution.
Further, a concentration of 0.3~1.2mol/L for the ascorbic acid solution being added in the step (3), Vitamin C
The amount ratio of the addition of acid and the substance of the addition of copper chloride in step (2) is 0.9:1.
Further, the mixing time of the step (3) is 10~25 minutes, which is 20~35 DEG C,
The Period Process is short, and reaction temperature is close to room temperature.
Further, a concentration of 0.3~0.9mol/L for the ascorbic acid solution being added in the step (5), Vitamin C
The amount ratio of the addition of acid and the substance of the addition of copper chloride in step (2) is 1:(2~4.2).
Further, the mixing time of the step (6) is 30~120 minutes, which is 15~20 DEG C,
The temperature of slightly below room temperature is conducive to conversion of the stannous chloride to cuprous oxide.
Further, in the step (6) by before the precipitation and centrifugal separation of acquisition, need to by solution cooled to room temperature,
It is centrifuged, is washed again, is dried.
The preparation method of the cuprous oxide based composites of the present invention is not necessarily to valuable instrument and equipment.Pass through rational technique
The preparation of cuprous oxide based composites is realized in control, and the cuprous oxide based composites are uniform in size, well dispersed, have
Preferable porosity, and preparation process is simple, at low cost, reaction time is short, other than it can be used for Dye Adsorption, applies also for
The fields such as photocatalysis, air-sensitive.
Description of the drawings
Fig. 1 and Fig. 2 is the scanning electron of cuprous oxide based composites particle prepared by second of embodiment of the invention
Microscope (SEM) photo；
Fig. 3 is the x-ray diffraction collection of illustrative plates of cuprous oxide based composites particle prepared by second of embodiment of the invention.
Specific implementation mode
With reference to specific embodiment, the invention will be further described.
Embodiment 1
A kind of nano cuprous oxide radical dye sorbing material in the present embodiment includes cuprous oxide and stannous chloride, oxidation
Cuprous and stannous chloride mass ratio is 84:16.
The preparation method of above-mentioned nano cuprous oxide radical dye sorbing material, includes the following steps：
(1) 0.699g copper chloride dihydrates are dissolved in 10ml deionized waters, stir 10min, forms a concentration of 0.5mol/L
Copper chloride solution；
(2) 25% ammonium hydroxide 1.5mL is added into copper chloride solution, forms copper ammon solution；
(3) ascorbic acid solution of a concentration of 1.2mol/L of 3mL is added into copper ammon solution, is stirred at a temperature of 25 DEG C
15 minutes, generate white precipitate；
(4) white precipitate is centrifuged and is cleaned with deionized water, obtain presoma, as CuCl presomas；
(5) 0.0456g potassium chloride is dissolved in 20ml deionized waters, and a concentration of 0.0025molL of 30ml is added-1's
The ascorbic acid of cetyl trimethylammonium bromide and a concentration of 0.6mol/L of 2.0mL form mixed solution；
(6) CuCl presomas made from step (4) are added in mixed solution made from step (5), add 210 μ L
Ammonium hydroxide, stirred 90 minutes at a temperature of 18 DEG C, generate precipitation；
(7) the solution cooled to room temperature for obtaining step (6), sediment are centrifuged and are cleaned with deionized water,
In 40 DEG C of vacuum drying treatments to get to nano cuprous oxide radical dye sorbing material.
The cuprous oxide radical dye adsorption composite material is 55mgg to the saturated extent of adsorption of methyl orange-1, to methylenum careuleum
Saturated extent of adsorption is 60mgg-1。
Embodiment 2
A kind of nano cuprous oxide radical dye sorbing material in the present embodiment includes cuprous oxide and stannous chloride, oxidation
Cuprous and stannous chloride mass ratio is 67.4:32.6.
The preparation method of above-mentioned nano cuprous oxide radical dye sorbing material, includes the following steps：
(1) 0.341g copper chloride dihydrates are dissolved in 10ml deionized waters, stir 10min, forms a concentration of 0.2mol/L
Copper chloride solution；
(2) 25% ammonium hydroxide 0.6mL is added into copper chloride solution, forms copper ammon solution；
(3) ascorbic acid solution of a concentration of 0.6mol/L of 3mL is added into copper ammon solution, is stirred at a temperature of 20 DEG C
10 minutes, generate white precipitate；
(4) white precipitate is centrifuged and is cleaned with deionized water, obtain presoma, as CuCl presomas；
(5) 0.0256g potassium chloride is dissolved in 20ml deionized waters, and a concentration of 0.0025molL of 30ml is added-1's
The ascorbic acid of cetyl trimethylammonium bromide and a concentration of 0.5mol/L of 2.0mL form mixed solution；
(6) CuCl presomas made from step (4) are added in mixed solution made from step (5), add 310 μ L
Ammonium hydroxide, stirred 60 minutes at a temperature of 20 DEG C, generate precipitation；
(7) the solution cooled to room temperature for obtaining step (6), sediment are centrifuged and are cleaned with deionized water,
In 40 DEG C of vacuum drying treatments to get to nano cuprous oxide radical dye sorbing material.
The cuprous oxide radical dye adsorption composite material is 48mgg to the saturated extent of adsorption of methyl orange-1, to methylenum careuleum
Saturated extent of adsorption is 56mgg-1。
The cuprous oxide based composites particle prepared in example 2 as can be seen from Figure 1 by well dispersed diameter 250~
The irregular particle of 450nm forms.Observe individual particle by nano level laminar structured group from the higher Fig. 2 of amplification factor
At.Fig. 3 shows the x-ray diffraction collection of illustrative plates of material, should be the result shows that the composite material is made of cuprous oxide and stannous chloride.
Embodiment 3
A kind of nano cuprous oxide radical dye sorbing material in the present embodiment includes cuprous oxide and stannous chloride, oxidation
Cuprous and stannous chloride mass ratio is 72:28.
The preparation method of above-mentioned nano cuprous oxide radical dye sorbing material, includes the following steps：
(1) 0.171g copper chloride dihydrates are dissolved in 10ml deionized waters, stir 10min, forms a concentration of 0.1mol/L
Copper chloride solution；
(2) 25% ammonium hydroxide 0.3mL is added into copper chloride solution, forms copper ammon solution；
(3) ascorbic acid solution of a concentration of 0.3mol/L of 3mL is added into copper ammon solution, is stirred at a temperature of 30 DEG C
20 minutes, generate white precipitate；
(4) white precipitate is centrifuged and is cleaned with deionized water, obtain presoma, as CuCl presomas；
(5) 0.0556g potassium chloride is dissolved in 20ml deionized waters, and a concentration of 0.0025molL of 30ml is added-1's
The ascorbic acid of cetyl trimethylammonium bromide and a concentration of 0.3mol/L of 2.0mL form mixed solution；
(6) CuCl presomas made from step (4) are added in mixed solution made from step (5), add 450 μ L
Ammonium hydroxide, stirred 30 minutes at a temperature of 15 DEG C, generate precipitation；
(7) the solution cooled to room temperature for obtaining step (6), sediment are centrifuged and are cleaned with deionized water,
In 40 DEG C of vacuum drying treatments to get to nano cuprous oxide radical dye sorbing material.
The cuprous oxide radical dye adsorption composite material is 58mgg to the saturated extent of adsorption of methyl orange-1, to methylenum careuleum
Saturated extent of adsorption is 63mgg-1。
Embodiment 4
A kind of nano cuprous oxide radical dye sorbing material in the present embodiment includes cuprous oxide and stannous chloride, oxidation
Cuprous and stannous chloride mass ratio is 81:19.
The preparation method of above-mentioned nano cuprous oxide radical dye sorbing material, includes the following steps：
(1) 2.046g copper chloride dihydrates are dissolved in 10ml deionized waters, stir 10min, forms a concentration of 0.6mol/L
Copper chloride solution；
(2) 25% ammonium hydroxide 1.8mL is added into copper chloride solution, forms copper ammon solution；
(3) ascorbic acid solution of a concentration of 0.9mol/L of 3mL is added into copper ammon solution, is stirred at a temperature of 35 DEG C
25 minutes, generate white precipitate；
(4) white precipitate is centrifuged and is cleaned with deionized water, obtain presoma, as CuCl presomas；
(5) 0.0756g potassium chloride is dissolved in 20ml deionized waters, and a concentration of 0.0025molL of 30ml is added-1's
The ascorbic acid of cetyl trimethylammonium bromide and a concentration of 1.2mol/L of 2.0mL form mixed solution；
(6) CuCl presomas made from step (4) are added in mixed solution made from step (5), add 560 μ L
Ammonium hydroxide, stirred 120 minutes at a temperature of 18 DEG C, generate precipitation；
(7) the solution cooled to room temperature for obtaining step (6), sediment are centrifuged and are cleaned with deionized water,
In 40 DEG C of vacuum drying treatments to get to nano cuprous oxide radical dye sorbing material.
The cuprous oxide radical dye adsorption composite material is 52mgg to the saturated extent of adsorption of methyl orange-1, to methylenum careuleum
Saturated extent of adsorption is 69mgg-1。
Embodiment 5
A kind of nano cuprous oxide radical dye sorbing material in the present embodiment includes cuprous oxide and stannous chloride, oxidation
Cuprous and stannous chloride mass ratio is 74:26.
The preparation method of above-mentioned nano cuprous oxide radical dye sorbing material, includes the following steps：
(1) 0.341g copper chloride dihydrates are dissolved in 10ml deionized waters, stir, forms the chlorination of a concentration of 0.2mol/L
Copper solution；
(2) 25% ammonium hydroxide 0.6mL is added into copper chloride solution, forms copper ammon solution；
(3) ascorbic acid solution of a concentration of 0.6mol/L of 3mL is added into copper ammon solution, is stirred at a temperature of 35 DEG C
25 minutes, generate white precipitate；
(4) white precipitate is centrifuged and is cleaned with deionized water, obtain presoma, as CuCl presomas；
(5) 0.0256g potassium chloride is dissolved in 20ml deionized waters, and a concentration of 0.0025molL of 30ml is added-1's
The ascorbic acid of cetyl trimethylammonium bromide and a concentration of 0.3mol/L of 2.0mL form mixed solution；
(6) CuCl presomas made from step (4) are added in mixed solution made from step (5), add 660 μ L
Ammonium hydroxide, stirred 120 minutes at a temperature of 18 DEG C, generate precipitation；
(7) the solution cooled to room temperature for obtaining step (6), sediment are centrifuged and are cleaned with deionized water,
In 40 DEG C of vacuum drying treatments to get to nano cuprous oxide radical dye sorbing material.
The cuprous oxide radical dye adsorption composite material is 52mgg to the saturated extent of adsorption of methyl orange-1, to methylenum careuleum
Saturated extent of adsorption is 69mgg-1。
The invention is not limited in above-described embodiment, the variation of many details is possible, but therefore this does not violate this
The scope and spirit of invention.
The embodiment of the present invention is explained in detail above, but the present invention is not limited to above-described embodiments, in ability
Domain those of ordinary skill within the scope of knowledge, can also make various changes without departing from the purpose of the present invention
Change.
Claims (9)
1. a kind of nano cuprous oxide radical dye sorbing material, it is characterised in that：The nano cuprous oxide radical dye adsorption material
Include cuprous oxide and stannous chloride in material, the mass ratio of the cuprous oxide and stannous chloride is (67.4~84):(16~
32.6)。
2. a kind of preparation method of nano cuprous oxide radical dye sorbing material, it is characterised in that：Include the following steps：
(1) copper chloride dihydrate is dissolved in deionized water, is stirred, form copper chloride solution；
(2) ammonium hydroxide is added into copper chloride solution, forms copper ammon solution；
(3) ascorbic acid solution is added into copper ammon solution, stirs, generates white precipitate；
(4) white precipitate is centrifuged and is cleaned with deionized water, obtain presoma；
(5) potassium chloride is dissolved in deionized water, and cetyl trimethylammonium bromide and ascorbic acid is added to form mixing molten
Liquid；
(6) presoma made from step (4) is added in mixed solution made from step (5), adds ammonium hydroxide, stirred, production
Raw precipitation；
(7) it is cleaned precipitation and centrifugal separation that step (6) obtains and with deionized water, vacuum drying is to get to nano oxidized Asia
Copper-based Dye Adsorption material.
3. a kind of preparation method of nano cuprous oxide radical dye sorbing material according to claim 2, it is characterised in that：
A concentration of 0.1~0.6mol/L of copper chloride solution in the step (1).
4. a kind of preparation method of nano cuprous oxide radical dye sorbing material according to claim 3, it is characterised in that：
The amount ratio of the substance of the addition of copper chloride is 4.5 in the addition Yu step (1) of ammonium hydroxide in the step (2):1.
5. a kind of preparation method of nano cuprous oxide radical dye sorbing material according to claim 4, it is characterised in that：
A concentration of 0.3~the 1.2mol/L for the ascorbic acid solution being added in the step (3), ascorbic acid addition and step (2)
The amount ratio of the substance of the addition of middle copper chloride is 0.9:1.
6. a kind of preparation method of nano cuprous oxide radical dye sorbing material according to claim 5, it is characterised in that：
The mixing time of the step (3) is 10~25 minutes, which is 20~35 DEG C.
7. a kind of preparation method of nano cuprous oxide radical dye sorbing material according to claim 6, it is characterised in that：
A concentration of 0.3~the 0.9mol/L for the ascorbic acid solution being added in the step (5), the addition and step of ascorbic acid
(2) the amount ratio of the substance of the addition of copper chloride is 1 in:(2~4.2).
8. a kind of preparation method of nano cuprous oxide radical dye sorbing material according to claim 7, it is characterised in that：
The mixing time of the step (6) is 30~120 minutes, which is 15~20 DEG C.
9. special according to a kind of preparation method of nano cuprous oxide radical dye sorbing material of claim 2-8 any one of them
Sign is：, need to be by solution cooled to room temperature by before the precipitation and centrifugal separation of acquisition in the step (6), then centrifuged,
Washing is dried.
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| CN114682226A (en) * | 2022-03-24 | 2022-07-01 | 西北大学 | Novel cuprous oxide and phenylacetylene copper compounded organic wastewater adsorbent |
| CN115041126A (en) * | 2022-06-13 | 2022-09-13 | 五邑大学 | Adsorbent and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109926047A (en) * | 2019-03-21 | 2019-06-25 | 华南师范大学 | A kind of copper oxide-cuprous oxide photocatalyst and preparation method thereof |
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| CN114682226A (en) * | 2022-03-24 | 2022-07-01 | 西北大学 | Novel cuprous oxide and phenylacetylene copper compounded organic wastewater adsorbent |
| CN115041126A (en) * | 2022-06-13 | 2022-09-13 | 五邑大学 | Adsorbent and preparation method and application thereof |
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