CN102909037A - Preparation method of porous cobalt selenide photocatalyst - Google Patents
Preparation method of porous cobalt selenide photocatalyst Download PDFInfo
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- CN102909037A CN102909037A CN2012104108849A CN201210410884A CN102909037A CN 102909037 A CN102909037 A CN 102909037A CN 2012104108849 A CN2012104108849 A CN 2012104108849A CN 201210410884 A CN201210410884 A CN 201210410884A CN 102909037 A CN102909037 A CN 102909037A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- QVYIMIJFGKEJDW-UHFFFAOYSA-N cobalt(ii) selenide Chemical compound [Se]=[Co] QVYIMIJFGKEJDW-UHFFFAOYSA-N 0.000 title abstract description 5
- 239000011941 photocatalyst Substances 0.000 title abstract 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims abstract description 15
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 7
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229960001471 sodium selenite Drugs 0.000 claims abstract description 7
- 239000011781 sodium selenite Substances 0.000 claims abstract description 7
- 235000015921 sodium selenite Nutrition 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 25
- -1 cobaltous selenide Chemical class 0.000 claims description 18
- 239000002244 precipitate Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000012423 maintenance Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000005406 washing Methods 0.000 abstract description 10
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 239000003344 environmental pollutant Substances 0.000 abstract description 5
- 231100000719 pollutant Toxicity 0.000 abstract description 5
- 239000002351 wastewater Substances 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 abstract 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000000593 degrading effect Effects 0.000 abstract 1
- 239000013049 sediment Substances 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000002242 deionisation method Methods 0.000 description 4
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 4
- 229960001545 hydrotalcite Drugs 0.000 description 4
- 229910001701 hydrotalcite Inorganic materials 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical group O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 241000446313 Lamella Species 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 238000007146 photocatalysis Methods 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
- 230000009467 reduction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910020639 Co-Al Inorganic materials 0.000 description 1
- 229910020675 Co—Al Inorganic materials 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- CQPFMGBJSMSXLP-UHFFFAOYSA-M acid orange 7 Chemical compound [Na+].OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 CQPFMGBJSMSXLP-UHFFFAOYSA-M 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 150000001449 anionic compounds Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910001412 inorganic anion Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002891 organic anions Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a porous cobalt selenide photocatalyst for catalyzing and degrading waste water or waste pollutants, comprising the following steps of: dissolving Cl2 and AlCl3 in water respectively and preparing two solutions with the concentration of 1-2mol/L, mixing the two solutions and keeping the mole ratio of Co to Al at 2-4, dropping NaOH into a water bath at the constant temperature of 70-80 DEG C, keeping the pH value at 12-13, reacting for 2-3h, aging, separating sediments and washing by using deionized water; adding the obtained solid into a sodium selenite solution with the concentration of 1-2mol/L according to a solid-to-liquid ratio of 1:20-1:50, washing the obtained solid and calcining at 400-500 DEG C; and adding the product obtained by calcining per one gramme of the solid into 20-40mL of hydrazine hydrate solution with the concentration of 20-40% to obtain the porous cobalt selenide photocatalyst, wherein the porous cobalt selenide photocatalyst has a good aperture structure and greater specific surface area and is beneficial to absorption and catalysis.
Description
Technical field
The present invention relates to the development field of environmental pollution control new material, relate in particular to the preparation method of the porous type cobaltous selenide photochemical catalyst of a kind of catalytic degradation waste water or waste pollutant.
Background technology
1972, Fujishma and Honda wait found to carry out UV Light with nano titanium oxide as the light anode can decomposing H
2O is H
2And O
2, this indicates that multiphase photocatalysis is from basic research to the application study New Times.Since then, be accompanied by the appearance of the outburst of energy crisis in the world wide and ecological deterioration problem etc., multiphase photocatalysis research causes people's concern day by day.Its target be utilize nature the abundantest the energy---solar energy is applied to energy conversion and utilization.
But because TiO
2Forbidden band wide (Eg=3.2 eV) cause it can not effectively utilize visible light part in the sunshine and TiO
2The right probability of recombination in light induced electron-hole is higher, has reduced its quantum efficiency, to such an extent as to there is not so far large-scale industrial application.
It is wider that cobalt class catalyst is used, and particularly aspect the pollutant of some difficult degradations of catalytic oxidation, preferably application prospect arranged, such as: the organic matter such as catalyze oxidation of formaldehyde, catalytic oxidation of cyclohexane at room temperature.Utilize liquid-phase synthesis process to obtain a kind of non-integer than cobaltous selenide (Co0.85Se) nanometer sheet, preparation process need not to use organic formwork and surfactant, and the thickness of sheet is less than 10 nanometers; Studies show that, the synthetic product that obtains can effectively adsorb the organic dyestuff methylene blue, can be used for adsorbing the organic dyestuff (" Chinese Chemical Society the 28th Annual Conference the 4th sub-venue summary collection " 2012) in the sewage.But this material granule is too little, and the Separation of Solid and Liquid difficulty need to load on the carrier and just can give full play to its catalytic effect; By a step low-temperature hydro-thermal synthesis, on electro-conductive glass growth in situ cobaltous selenide and nickelous selenide nanocrystalline, need not any post processing, directly apply to dye-sensitized solar cells, obtained good battery performance, particularly cobaltous selenide has the electrocatalysis characteristic (JACS, DOI:10.1021/ja303034w) higher than metal platinum.The catalyst of cobaltous selenide class is owing to needing carrier just larger specific area can be arranged at present, and therefore exploitation has the catalyst than bigger serface from pore-forming, and applying of such catalyst had positive effect.
Hydrotalcite-based compound (LDHs) is to pile up the compound that forms by interlayer anion and positively charged laminate.The hydrotalcite chemical structure of general formula is: [M
2+ 1-xM
3+X (OH)
2]
X+[(A
N-)
X/nMH
2O], M wherein
2+And M
3+Be respectively the divalence and the trivalent metal cation that are positioned on the main body laminate, such as Mg
2+, Ni
2+, Zn
2+, Mn
2+, Cu
2+, Co
2+, Pd
2+, Fe
2+Deng bivalent cation and Al
3+, Cr
3+, Co
3+, Fe
3+All can form hydrotalcite Deng Tricationic; A
N –Be interlayer anion, can comprise inorganic anion, organic anion, complex anion, same many and heteropolyanion; X is M
3+/ (M
2++ M
3+) molar ratio, approximately be that 4:1 is to 2:1; M is the number of intermediary water molecule.Its structure is similar to shepardite Mg (OH)
2, share seamed edge and form the main body laminate by octahedron.Be positioned at the divalent metal M on the laminate
2+Can be by the close trivalent metal cation M of ion half price in certain proportion
3+The isomorphous replaces so that laminate is positively charged, interlayer exist can exchange anion and the positive charge balance on the laminate so that the overall structure of LDHs is electroneutral.The anion of interlayer can be exchanged, and through a series of modifications, hydrotalcite material can obtain the many kinds of materials that performance is different.
Summary of the invention
The objective of the invention is provides a kind of preparation method of porous type cobaltous selenide photochemical catalyst for overcoming the deficiency that the carrier price is high in the prior art, load process is responsible for.
The technical solution used in the present invention is in turn include the following steps: 1) with CoCl
2And AlCl
3Be dissolved into respectively in the water, be configured to concentration and be two kinds of solution of 1 ~ 2 mol/L, two kinds of solution are mixed, Co in the maintenance mixed solution and the mol ratio of Al are 2 ~ 4, splash into NaOH in 70 ~ 80 ℃ of water-baths of constant temperature, and keeping the pH value is 12 ~ 13, reaction 2 ~ 3 h, aging 12 ~ 24 h, precipitate and separate is washed 2 ~ 3 times with deionized water; 2) solid that step 1) is obtained joins in the sodium selenite solution that concentration is 1 ~ 2 mol/L, and solid-to-liquid ratio is 1:20 ~ 1:50, stirs 4 ~ 5 h, and precipitate and separate is after the solid of acquisition washs 2 ~ 3 times with deionized water, at 400 ~ 500 ℃ temperature lower calcination; 3) it is in 20% ~ 40% the hydrazine hydrate solution, to obtain porous type cobaltous selenide catalyst that the product that per 1 g calcining is obtained joins 20 ~ 40 mL concentration.
Advantage of the present invention is:
(1) passes through coprecipitation reaction, form the larger lamellar structure of specific area that cobalt is being mingled with aluminium, enter the selenous acid ion at Inter layer exchange again, form supporting construction by high-temperature calcination again, make and separate between lamella and the lamella and fixing, can not separate or closure, make this material have good pore space structure and larger specific area, be conducive to absorption and catalysis.
(2) after calcining, form oxide, at last this oxide is utilized hydrazine hydrate reduction, obtain being doped with the cobaltous selenide that aluminium supports.
(3) be doped with part aluminium in this catalyst, in catalyst, form skeleton function, and between catalyst and skeleton, stronger active force is arranged, can prevent that catalyst from coming off or reunite and reduce the catalysis area and affect catalytic action.
The specific embodiment
With CoCl
2And AlCl
3Be dissolved into respectively in the water, be configured to concentration and be the solution of 1 ~ 2 mol/L, two kinds of solution are mixed, keeping the mol ratio of Co and Al is 2 ~ 4, in 70 ~ 80 ℃ of water-baths of constant temperature, splash into a certain amount of NaOH, keeping the pH value is 12 ~ 13, reaction 2 ~ 3 h, aging 12 ~ 24 h, in this process, form the precipitation with layer structure, precipitate and separate, deionization washing 2 ~ 3 times prepares Co-Al type houghite in this process.This houghite is joined in the sodium selenite solution that concentration is 1 ~ 2 mol/L, and solid-to-liquid ratio is 1:20 ~ 1:50, stirs 4 ~ 5 h, precipitate and separate, and the solid of acquisition is after with deionized water washing 2 ~ 3 times, at 400 ~ 500 ℃ temperature lower calcination; It is in 20% ~ 40% the hydrazine hydrate solution that the product that per 1 g calcining is obtained joins 20 ~ 40 mL concentration, utilizes the reduction of hydrazine hydrate, and the selenium cobalt/cobalt oxide is reduced into cobaltous selenide, obtains porous type cobaltous selenide catalyst.
3 embodiment of the present invention below further are provided:
Embodiment 1
With CoCl
2And AlCl
3Be dissolved into respectively in the water, be configured to the solution that concentration is 1 mol/L, two kinds of solution are mixed, and keeping the mol ratio of Co and Al is 2, splashes into a certain amount of NaOH in 70 ℃ of water-baths of constant temperature, keeping the pH value is 12, react 2 h, aging 12 h form the precipitation with layer structure in this process, precipitate and separate, deionization washing 2 times; The solid that precipitation is obtained joins in the sodium selenite solution that concentration is 1 mol/L, and solid-to-liquid ratio is 1:50, stirs 4h, precipitate and separate, and the solid of acquisition is after with deionized water washing 2 times, at 400 ℃ temperature lower calcination; It is in 40% the hydrazine hydrate solution, to obtain porous type cobaltous selenide catalyst that the product that 1 g calcining is obtained joins 20 mL concentration.
Adopt L shaped pipe (internal diameter 10 mm) continuous-flow reaction evaluating device, in the synthetic catalyst disposed tubes that obtains of weighing 100 mg, the coaxial quartz ampoule that is provided with in the vertical part glass jar of L shaped pipe, it is the uviol lamp of 6W that power is arranged in the pipe, the flow velocity of regulating air is 40 mL/min, Air Flow drives formaldehyde gas and enters in the U-shaped pipe reactor, and the gas volume (being air speed) that per hour flows through every liter of catalyst is 55000 h
-1Under 25 ℃ of conditions, it is that the formaldehyde gas complete oxidation of 100 ppm is carbon dioxide and water that this catalyst can make 85% concentration.
Embodiment 2
With CoCl
2And AlCl
3Be dissolved into respectively in the water, be configured to the solution that concentration is 2 mol/L, two kinds of solution are mixed, and keeping the mol ratio of Co and Al is 4, splashes into a certain amount of NaOH in 80 ℃ of water-baths of constant temperature, keeping the pH value is 13, react 3 h, aging 24 h form the precipitation with layer structure in this process, precipitate and separate, deionization washing 3 times; The solid that precipitation is obtained joins in the sodium selenite solution that concentration is 2 mol/L, and solid-to-liquid ratio is 1:20, stirs 5 h, precipitate and separate, and the solid of acquisition is after with deionized water washing 3 times, at 500 ℃ temperature lower calcination; It is in 20% the hydrazine hydrate solution, to obtain porous type cobaltous selenide catalyst that the product that 1 g calcining is obtained joins 40 mL concentration.
The catalyst 0.5g that obtains is joined in the Orange II waste water that 500 mL concentration are 50mg/L, under the irradiation of 500w Metal halogen lamp, react 3 h, percent of decolourization is 95%, illustrates that this catalyst also can catalytic reaction oxidation removal pollutant under visible light.
Embodiment 3
With CoCl
2And AlCl
3Be dissolved into respectively in the water, be configured to the solution that concentration is 2 mol/L, two kinds of solution are mixed, and keeping the mol ratio of Co and Al is 3, splashes into a certain amount of NaOH in 75 ℃ of water-baths of constant temperature, keeping the pH value is 13, react 3 h, aging 18 h form the precipitation with layer structure in this process, precipitate and separate, deionization washing 3 times; The solid that precipitation is obtained joins in the sodium selenite solution that concentration is 1.5 mol/L, and solid-to-liquid ratio is 1:30, stirs 4 h, precipitate and separate, and the solid of acquisition is after with deionized water washing 3 times, at 450 ℃ temperature lower calcination; It is in 30% the hydrazine hydrate solution, to obtain porous type cobaltous selenide catalyst that the product that 1 g calcining is obtained joins 30 mL concentration.
The catalyst 0.5g that obtains is joined in the methylene blue waste water that 500 mL concentration are 50mg/L, under the irradiation of 500w Metal halogen lamp, react 3 h, percent of decolourization is 90%, illustrates that this catalyst can catalytic reaction oxidation removal pollutant under visible light.
Claims (1)
1. the preparation method of a porous type cobaltous selenide photochemical catalyst is characterized in that in turn including the following steps:
1) with CoCl
2And AlCl
3Be dissolved into respectively in the water, be configured to two kinds of solution that concentration is 1 ~ 2 mol/L, two kinds of solution are mixed, Co in the maintenance mixed solution and the mol ratio of Al are 2 ~ 4, splash into NaOH in 70 ~ 80 ℃ of water-baths of constant temperature, and keeping the pH value is 12 ~ 13, reaction 2 ~ 3 h, aging 12 ~ 24 h, precipitate and separate is washed 2 ~ 3 times with deionized water;
2) solid that step 1) is obtained joins in the sodium selenite solution that concentration is 1 ~ 2 mol/L, and solid-to-liquid ratio is 1:20 ~ 1:50, stirs 4 ~ 5 h, and precipitate and separate is after the solid of acquisition washs 2 ~ 3 times with deionized water, at 400 ~ 500 ℃ temperature lower calcination;
3) it is in 20% ~ 40% the hydrazine hydrate solution, to obtain porous type cobaltous selenide catalyst that the product that per 1 g calcining is obtained joins 20 ~ 40 mL concentration.
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Cited By (3)
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|---|---|---|---|---|
| CN103466566A (en) * | 2013-08-30 | 2013-12-25 | 天津大学 | Method for synthesizing cobalt diselenide nanocrystal in polyalcohol-base solution |
| CN104383943A (en) * | 2014-09-16 | 2015-03-04 | 安徽大学 | Preparation method for catalyst efficiently catalyzing hydrogenation reduction of 4-nitrophenol |
| CN115069301A (en) * | 2022-05-27 | 2022-09-20 | 恒天嘉华非织造有限公司 | Composite material for printing and dyeing textile wastewater treatment and preparation method thereof |
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Cited By (4)
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| CN103466566A (en) * | 2013-08-30 | 2013-12-25 | 天津大学 | Method for synthesizing cobalt diselenide nanocrystal in polyalcohol-base solution |
| CN104383943A (en) * | 2014-09-16 | 2015-03-04 | 安徽大学 | Preparation method for catalyst efficiently catalyzing hydrogenation reduction of 4-nitrophenol |
| CN104383943B (en) * | 2014-09-16 | 2017-03-15 | 安徽大学 | A kind of preparation method of efficient catalytic p-nitrophenol hydro-reduction catalyst |
| CN115069301A (en) * | 2022-05-27 | 2022-09-20 | 恒天嘉华非织造有限公司 | Composite material for printing and dyeing textile wastewater treatment and preparation method thereof |
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