CN108579722A - One kind is for light-catalysed semiconductor nano material and preparation method thereof - Google Patents

One kind is for light-catalysed semiconductor nano material and preparation method thereof Download PDF

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CN108579722A
CN108579722A CN201810618584.7A CN201810618584A CN108579722A CN 108579722 A CN108579722 A CN 108579722A CN 201810618584 A CN201810618584 A CN 201810618584A CN 108579722 A CN108579722 A CN 108579722A
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parts
solution
nano material
light
semiconductor nano
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姬晓旭
赵庆怀
王爱华
程艺苑
盛至铭
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Nanyang Normal University
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Nanyang Normal University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/18Arsenic, antimony or bismuth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/20Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
    • B01J35/23Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/391Physical properties of the active metal ingredient
    • B01J35/393Metal or metal oxide crystallite size
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • B01J37/10Heat treatment in the presence of water, e.g. steam
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/344Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
    • B01J37/346Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy

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Abstract

The invention discloses one kind being used for light-catalysed semiconductor nano material, including following raw material:Stannous chloride methanol solution, acid solution, bismuth chloride solution, aqueous dimethylethanolamine, sodium hydrate aqueous solution;Wherein, it according to weight ratio is 2 that the acid solution, which is oxalic acid, deionized water and absolute ethyl alcohol,:3:10 ratio mixes.The invention also discloses the preparation methods for light-catalysed semiconductor nano material.Prepared by the present invention has good photocatalytic activity for light-catalysed semiconductor nano material, it is prepared by ultrasonic microwave synergistic combination effect most short up to 30 nanometers for light-catalysed semiconductor nano material length, catalytic activity simultaneously in photocatalytic activity evaluation is good, it can be used for photocatalysis Decomposition inorganic matter and organic matter generate nontoxic, tasteless carbon dioxide, water etc., problem of environmental pollution is advantageously accounted for, foreground is had a vast market.

Description

One kind is for light-catalysed semiconductor nano material and preparation method thereof
Technical field
The present invention relates to functional material preparing technical field, it is specifically a kind of for light-catalysed semiconductor nano material and Preparation method.
Background technology
Nanotechnology need not be set as a kind of emerging science and technology of most market application potential, potential importance Doubt, nano material refer in three dimensions it is at least one-dimensional in nano-scale (0.1-100 nm) or by them as basic The material that unit is constituted.By the way that nano material is made in the semi-conducting materials such as silicon, GaAs, there can be many excellent properties. For example, the quantum tunneling effect in Nano semiconductor makes electron transport abnormality, the conductivity of certain semi-conducting materials reduce, conductance Hot coefficient also declines with the reduction of particle size, or even negative value occurs, these characteristics are in LSI devices, photoelectricity The fields such as device play an important role.
Current mankind is faced with problem of environmental pollution, and a large amount of organic and inorganic refuse brings people’s lives and environment Adverse effect, therefore, the electrons and holes generated when being irradiated using Nano semiconductor particles light have stronger reduction and oxygen Change ability designs a kind of semiconductor nano material, and nontoxic, tasteless dioxy is generated for photocatalysis Decomposition inorganic matter and organic matter The problem of changing carbon, water etc., becoming urgent need to resolve.
Invention content
The purpose of the present invention is to provide one kind for light-catalysed semiconductor nano material and preparation method thereof, to solve The problems mentioned above in the background art.
To achieve the above object, the present invention provides the following technical solutions:
One kind being used for light-catalysed semiconductor nano material, including below according to the raw material of parts by weight:Stannous chloride methanol solution 5- 12 parts, 22-35 parts of acid solution, 1-5 parts of bismuth chloride solution, 0.5-1.5 parts of aqueous dimethylethanolamine, sodium hydroxide it is water-soluble 70-85 parts of liquid;Wherein, it according to weight ratio is 2 that the acid solution, which is oxalic acid, deionized water and absolute ethyl alcohol,:3:10 ratio It mixes.
As a further solution of the present invention:Including below according to the raw material of parts by weight:6-10 parts of stannous chloride methanol solution, 25-32 parts of acid solution, 2-4 parts of bismuth chloride solution, 0.7-1.2 parts of aqueous dimethylethanolamine, sodium hydrate aqueous solution 75- 82 parts.
As further scheme of the invention:Including below according to the raw material of parts by weight:8 parts of stannous chloride methanol solution, 30 parts of acid solution, 3 parts of bismuth chloride solution, 1 part of aqueous dimethylethanolamine, 80 parts of sodium hydrate aqueous solution.
As further scheme of the invention:A concentration of 0.1-3mol/L of the sodium hydrate aqueous solution;Described two A concentration of 0.001-0.01mol/L of methyl ethanol amine aqueous solution.
As further scheme of the invention:A concentration of 3mol/L of the oxalic acid;The concentration of the bismuth chloride solution For 0.02mol/L;A concentration of 0.4mol/L of the stannous chloride methanol solution.
As further scheme of the invention:The preparation method of the bismuth chloride solution is to be fitted what bismuth chloride was added to In the polyethylene glycol of amount, ultrasonic disperse 10-30min is carried out to get the bismuth chloride solution with the supersonic frequency of 20-45kHz.
The preparation method for light-catalysed semiconductor nano material, steps are as follows:
1)Stannous chloride methanol solution is weighed according to parts by weight, bismuth chloride solution is added while stirring under the conditions of 15-25 DEG C, is sent into In ultrasonic microwave composite reaction instrument, processing 2-10min is carried out at normal temperatures, obtains mixed liquor A;
2)Acid solution is weighed according to parts by weight, a dropping step 1 while stirring under the conditions of 15-25 DEG C)In obtained mixed liquor A continues to stir 30-50min, obtains mixed liquid B;
3)By step 2)In obtained mixed liquid B ageing 4-10h, ethyl alcohol and ionized water are spent after filtering and is alternately cleaned, is then put Enter in vacuum drying chamber and be dried at 65 DEG C 4 hours, obtains mixture C;
4)By step 3)In in obtained mixture C merging Muffle furnace, 500 DEG C of progress are warming up to 6 DEG C/min of heating rate It is calcined 4-6h, sample D must be calcined;
5)By step 4)In obtained calcining sample D be uniformly mixed with aqueous dimethylethanolamine, be placed in inner liner polytetrafluoroethylene In the stainless steel cauldron of material, addition sodium hydrate aqueous solution, reaction time 18-20 hour under the conditions of 110-130 DEG C, instead It is cooled to room temperature after answering, filters taking precipitate, washed with the diluted nitric acid aqueous solution of 0.1mol/L, then be washed with deionized water Wash, be subsequently placed in vacuum drying chamber dry, crush to get.
As further scheme of the invention:Step 1)In, the processing item of the ultrasonic microwave composite reaction instrument Part is:Ultrasonic frequency is 30kHz, ultrasonic power 20-80W, microwave frequency 2000MHz, microwave power 20-80W.
As further scheme of the invention:Step 2)In, the stir speed (S.S.) of the stirring is 200-400r/min;Institute The rate for stating dropwise addition is 60 drops/minute.
Described is used for purposes of the light-catalysed semiconductor nano material in preparing nano material.
Compared with prior art, the beneficial effects of the invention are as follows:
Prepared by the present invention has good photocatalytic activity for light-catalysed semiconductor nano material, passes through ultrasonic microwave Synergistic combination effect is prepared most short up to 30 nanometers for light-catalysed semiconductor nano material length, while being lived in photocatalysis Property evaluation in catalytic activity it is good, can be used for photocatalysis Decomposition inorganic matter and organic matter generate nontoxic, tasteless titanium dioxide Carbon, water etc., advantageously account for problem of environmental pollution, have a vast market foreground.
Specific implementation mode
Technical scheme of the present invention is described in more detail With reference to embodiment.
Embodiment 1
One kind being used for light-catalysed semiconductor nano material, including below according to the raw material of parts by weight:Stannous chloride methanol solution 5 Part, 22 parts of acid solution, 1 part of bismuth chloride solution, 0.5 part of aqueous dimethylethanolamine, 70 parts of sodium hydrate aqueous solution.Its In, a concentration of 1mol/L of the sodium hydrate aqueous solution;A concentration of 0.005mol/L of the aqueous dimethylethanolamine; A concentration of 3mol/L of the oxalic acid;A concentration of 0.02mol/L of the bismuth chloride solution;The stannous chloride methanol solution it is dense Degree is 0.4mol/L;It according to weight ratio is 2 that the acid solution, which is oxalic acid, deionized water and absolute ethyl alcohol,:3:10 ratio is mixed It closes;The preparation method of the bismuth chloride solution is ultrasonic disperse in the suitable polyethylene glycol for being added to bismuth chloride 20min, the supersonic frequency of the ultrasonic disperse are 35kHz to get the bismuth chloride solution.
In the present embodiment, the preparation method for light-catalysed semiconductor nano material, steps are as follows:
1)Stannous chloride methanol solution is weighed according to parts by weight, bismuth chloride solution is added while stirring under the conditions of 20 DEG C, is sent into super Sound wave microwave combination reacts in instrument, carries out processing 6min, the processing item of the ultrasonic microwave composite reaction instrument at normal temperatures Part is:Ultrasonic frequency is 30kHz, ultrasonic power 40W, microwave frequency 2000MHz, and microwave power 40W obtains mixed liquor A;
2)Acid solution is weighed according to parts by weight, a dropping step 1 while stirring under the conditions of 20 DEG C)In obtained mixed liquor A, institute The rate for stating dropwise addition is 60 drops/minute, then continues to stir 40min with the stir speed (S.S.) of 300r/min, obtains mixed liquid B;
3)By step 2)In obtained mixed liquid B ageing 6h, ethyl alcohol and ionized water are spent after filtering and is alternately cleaned, is then placed in true It is dried in empty drying box, the drying time is 4 hours, and the drying temperature is 65 DEG C, obtains mixture C;
4)By step 3)In be calcined in obtained mixture C merging Muffle furnace, the calcination temperature is 500 DEG C, the forging The burning time is 5h, and heating rate is 6 DEG C/min, must calcine sample D;
5)By step 4)In obtained calcining sample D be uniformly mixed with aqueous dimethylethanolamine, be placed in inner liner polytetrafluoroethylene In the stainless steel cauldron of material, sodium hydrate aqueous solution is added, in 18 hours reaction time under the conditions of 120 DEG C, reaction terminates Postcooling filters taking precipitate, is washed with the diluted nitric acid aqueous solution of 0.1mol/L, then be washed with deionized, then to room temperature Be placed in vacuum drying chamber dry, crush to get.
Embodiment 2
One kind being used for light-catalysed semiconductor nano material, including below according to the raw material of parts by weight:Stannous chloride methanol solution 12 Part, 35 parts of acid solution, 5 parts of bismuth chloride solution, 1.5 parts of aqueous dimethylethanolamine, 85 parts of sodium hydrate aqueous solution.Its In, a concentration of 1mol/L of the sodium hydrate aqueous solution;A concentration of 0.005mol/L of the aqueous dimethylethanolamine; A concentration of 3mol/L of the oxalic acid;A concentration of 0.02mol/L of the bismuth chloride solution;The stannous chloride methanol solution it is dense Degree is 0.4mol/L;It according to weight ratio is 2 that the acid solution, which is oxalic acid, deionized water and absolute ethyl alcohol,:3:10 ratio is mixed It closes;The preparation method of the bismuth chloride solution is ultrasonic disperse in the suitable polyethylene glycol for being added to bismuth chloride 20min, the supersonic frequency of the ultrasonic disperse are 35kHz to get the bismuth chloride solution.
In the present embodiment, the preparation method for light-catalysed semiconductor nano material, steps are as follows:
1)Stannous chloride methanol solution is weighed according to parts by weight, bismuth chloride solution is added while stirring under the conditions of 20 DEG C, is sent into super Sound wave microwave combination reacts in instrument, carries out processing 6min, the processing item of the ultrasonic microwave composite reaction instrument at normal temperatures Part is:Ultrasonic frequency is 30kHz, ultrasonic power 40W, microwave frequency 2000MHz, and microwave power 40W obtains mixed liquor A;
2)Acid solution is weighed according to parts by weight, a dropping step 1 while stirring under the conditions of 20 DEG C)In obtained mixed liquor A, institute The rate for stating dropwise addition is 60 drops/minute, then continues to stir 40min with the stir speed (S.S.) of 300r/min, obtains mixed liquid B;
3)By step 2)In obtained mixed liquid B ageing 6h, ethyl alcohol and ionized water are spent after filtering and is alternately cleaned, is then placed in true It is dried in empty drying box, the drying time is 4 hours, and the drying temperature is 65 DEG C, obtains mixture C;
4)By step 3)In be calcined in obtained mixture C merging Muffle furnace, the calcination temperature is 500 DEG C, the forging The burning time is 5h, and heating rate is 6 DEG C/min, must calcine sample D;
5)By step 4)In obtained calcining sample D be uniformly mixed with aqueous dimethylethanolamine, be placed in inner liner polytetrafluoroethylene In the stainless steel cauldron of material, sodium hydrate aqueous solution is added, in 18 hours reaction time under the conditions of 120 DEG C, reaction terminates Postcooling filters taking precipitate, is washed with the diluted nitric acid aqueous solution of 0.1mol/L, then be washed with deionized, then to room temperature Be placed in vacuum drying chamber dry, crush to get.
Embodiment 3
One kind being used for light-catalysed semiconductor nano material, including below according to the raw material of parts by weight:Stannous chloride methanol solution 8.5 Part, 28.5 parts of acid solution, 3 parts of bismuth chloride solution, 1 part of aqueous dimethylethanolamine, 77.5 parts of sodium hydrate aqueous solution.Its In, a concentration of 1mol/L of the sodium hydrate aqueous solution;A concentration of 0.005mol/L of the aqueous dimethylethanolamine; A concentration of 3mol/L of the oxalic acid;A concentration of 0.02mol/L of the bismuth chloride solution;The stannous chloride methanol solution it is dense Degree is 0.4mol/L;It according to weight ratio is 2 that the acid solution, which is oxalic acid, deionized water and absolute ethyl alcohol,:3:10 ratio is mixed It closes;The preparation method of the bismuth chloride solution is ultrasonic disperse in the suitable polyethylene glycol for being added to bismuth chloride 20min, the supersonic frequency of the ultrasonic disperse are 35kHz to get the bismuth chloride solution.
In the present embodiment, the preparation method for light-catalysed semiconductor nano material, steps are as follows:
1)Stannous chloride methanol solution is weighed according to parts by weight, bismuth chloride solution is added while stirring under the conditions of 20 DEG C, is sent into super Sound wave microwave combination reacts in instrument, carries out processing 6min, the processing item of the ultrasonic microwave composite reaction instrument at normal temperatures Part is:Ultrasonic frequency is 30kHz, ultrasonic power 40W, microwave frequency 2000MHz, and microwave power 40W obtains mixed liquor A;
2)Acid solution is weighed according to parts by weight, a dropping step 1 while stirring under the conditions of 20 DEG C)In obtained mixed liquor A, institute The rate for stating dropwise addition is 60 drops/minute, then continues to stir 40min with the stir speed (S.S.) of 300r/min, obtains mixed liquid B;
3)By step 2)In obtained mixed liquid B ageing 6h, ethyl alcohol and ionized water are spent after filtering and is alternately cleaned, is then placed in true It is dried in empty drying box, the drying time is 4 hours, and the drying temperature is 65 DEG C, obtains mixture C;
4)By step 3)In be calcined in obtained mixture C merging Muffle furnace, the calcination temperature is 500 DEG C, the forging The burning time is 5h, and heating rate is 6 DEG C/min, must calcine sample D;
5)By step 4)In obtained calcining sample D be uniformly mixed with aqueous dimethylethanolamine, be placed in inner liner polytetrafluoroethylene In the stainless steel cauldron of material, sodium hydrate aqueous solution is added, in 18 hours reaction time under the conditions of 120 DEG C, reaction terminates Postcooling filters taking precipitate, is washed with the diluted nitric acid aqueous solution of 0.1mol/L, then be washed with deionized, then to room temperature Be placed in vacuum drying chamber dry, crush to get.
Embodiment 4
One kind being used for light-catalysed semiconductor nano material, including below according to the raw material of parts by weight:Stannous chloride methanol solution 6 Part, 25 parts of acid solution, 2 parts of bismuth chloride solution, 0.7 part of aqueous dimethylethanolamine, 75 parts of sodium hydrate aqueous solution.Its In, a concentration of 1mol/L of the sodium hydrate aqueous solution;A concentration of 0.005mol/L of the aqueous dimethylethanolamine; A concentration of 3mol/L of the oxalic acid;A concentration of 0.02mol/L of the bismuth chloride solution;The stannous chloride methanol solution it is dense Degree is 0.4mol/L;It according to weight ratio is 2 that the acid solution, which is oxalic acid, deionized water and absolute ethyl alcohol,:3:10 ratio is mixed It closes;The preparation method of the bismuth chloride solution is ultrasonic disperse in the suitable polyethylene glycol for being added to bismuth chloride 20min, the supersonic frequency of the ultrasonic disperse are 35kHz to get the bismuth chloride solution.
In the present embodiment, the preparation method for light-catalysed semiconductor nano material, steps are as follows:
1)Stannous chloride methanol solution is weighed according to parts by weight, bismuth chloride solution is added while stirring under the conditions of 20 DEG C, is sent into super Sound wave microwave combination reacts in instrument, carries out processing 6min, the processing item of the ultrasonic microwave composite reaction instrument at normal temperatures Part is:Ultrasonic frequency is 30kHz, ultrasonic power 40W, microwave frequency 2000MHz, and microwave power 40W obtains mixed liquor A;
2)Acid solution is weighed according to parts by weight, a dropping step 1 while stirring under the conditions of 20 DEG C)In obtained mixed liquor A, institute The rate for stating dropwise addition is 60 drops/minute, then continues to stir 40min with the stir speed (S.S.) of 300r/min, obtains mixed liquid B;
3)By step 2)In obtained mixed liquid B ageing 6h, ethyl alcohol and ionized water are spent after filtering and is alternately cleaned, is then placed in true It is dried in empty drying box, the drying time is 4 hours, and the drying temperature is 65 DEG C, obtains mixture C;
4)By step 3)In be calcined in obtained mixture C merging Muffle furnace, the calcination temperature is 500 DEG C, the forging The burning time is 5h, and heating rate is 6 DEG C/min, must calcine sample D;
5)By step 4)In obtained calcining sample D be uniformly mixed with aqueous dimethylethanolamine, be placed in inner liner polytetrafluoroethylene In the stainless steel cauldron of material, sodium hydrate aqueous solution is added, in 18 hours reaction time under the conditions of 120 DEG C, reaction terminates Postcooling filters taking precipitate, is washed with the diluted nitric acid aqueous solution of 0.1mol/L, then be washed with deionized, then to room temperature Be placed in vacuum drying chamber dry, crush to get.
Embodiment 5
One kind being used for light-catalysed semiconductor nano material, including below according to the raw material of parts by weight:Stannous chloride methanol solution 10 Part, 32 parts of acid solution, 4 parts of bismuth chloride solution, 1.2 parts of aqueous dimethylethanolamine, 82 parts of sodium hydrate aqueous solution.Its In, a concentration of 1mol/L of the sodium hydrate aqueous solution;A concentration of 0.005mol/L of the aqueous dimethylethanolamine; A concentration of 3mol/L of the oxalic acid;A concentration of 0.02mol/L of the bismuth chloride solution;The stannous chloride methanol solution it is dense Degree is 0.4mol/L;It according to weight ratio is 2 that the acid solution, which is oxalic acid, deionized water and absolute ethyl alcohol,:3:10 ratio is mixed It closes;The preparation method of the bismuth chloride solution is ultrasonic disperse in the suitable polyethylene glycol for being added to bismuth chloride 20min, the supersonic frequency of the ultrasonic disperse are 35kHz to get the bismuth chloride solution.
In the present embodiment, the preparation method for light-catalysed semiconductor nano material, steps are as follows:
1)Stannous chloride methanol solution is weighed according to parts by weight, bismuth chloride solution is added while stirring under the conditions of 20 DEG C, is sent into super Sound wave microwave combination reacts in instrument, carries out processing 6min, the processing item of the ultrasonic microwave composite reaction instrument at normal temperatures Part is:Ultrasonic frequency is 30kHz, ultrasonic power 40W, microwave frequency 2000MHz, and microwave power 40W obtains mixed liquor A;
2)Acid solution is weighed according to parts by weight, a dropping step 1 while stirring under the conditions of 20 DEG C)In obtained mixed liquor A, institute The rate for stating dropwise addition is 60 drops/minute, then continues to stir 40min with the stir speed (S.S.) of 300r/min, obtains mixed liquid B;
3)By step 2)In obtained mixed liquid B ageing 6h, ethyl alcohol and ionized water are spent after filtering and is alternately cleaned, is then placed in true It is dried in empty drying box, the drying time is 4 hours, and the drying temperature is 65 DEG C, obtains mixture C;
4)By step 3)In be calcined in obtained mixture C merging Muffle furnace, the calcination temperature is 500 DEG C, the forging The burning time is 5h, and heating rate is 6 DEG C/min, must calcine sample D;
5)By step 4)In obtained calcining sample D be uniformly mixed with aqueous dimethylethanolamine, be placed in inner liner polytetrafluoroethylene In the stainless steel cauldron of material, sodium hydrate aqueous solution is added, in 18 hours reaction time under the conditions of 120 DEG C, reaction terminates Postcooling filters taking precipitate, is washed with the diluted nitric acid aqueous solution of 0.1mol/L, then be washed with deionized, then to room temperature Be placed in vacuum drying chamber dry, crush to get.
Embodiment 6
One kind being used for light-catalysed semiconductor nano material, including below according to the raw material of parts by weight:Stannous chloride methanol solution 8 Part, 28.5 parts of acid solution, 3 parts of bismuth chloride solution, 0.95 part of aqueous dimethylethanolamine, sodium hydrate aqueous solution 78.5 Part.Wherein, a concentration of 1mol/L of the sodium hydrate aqueous solution;The aqueous dimethylethanolamine it is a concentration of 0.005mol/L;A concentration of 3mol/L of the oxalic acid;A concentration of 0.02mol/L of the bismuth chloride solution;The protochloride A concentration of 0.4mol/L of tin methanol solution;It according to weight ratio is 2 that the acid solution, which is oxalic acid, deionized water and absolute ethyl alcohol,: 3:10 ratio mixes;The preparation method of the bismuth chloride solution is the suitable polyethylene glycol for being added to bismuth chloride In, ultrasonic disperse 20min, the supersonic frequency of the ultrasonic disperse is 35kHz to get the bismuth chloride solution.
In the present embodiment, the preparation method for light-catalysed semiconductor nano material, steps are as follows:
1)Stannous chloride methanol solution is weighed according to parts by weight, bismuth chloride solution is added while stirring under the conditions of 20 DEG C, is sent into super Sound wave microwave combination reacts in instrument, carries out processing 6min, the processing item of the ultrasonic microwave composite reaction instrument at normal temperatures Part is:Ultrasonic frequency is 30kHz, ultrasonic power 40W, microwave frequency 2000MHz, and microwave power 40W obtains mixed liquor A;
2)Acid solution is weighed according to parts by weight, a dropping step 1 while stirring under the conditions of 20 DEG C)In obtained mixed liquor A, institute The rate for stating dropwise addition is 60 drops/minute, then continues to stir 40min with the stir speed (S.S.) of 300r/min, obtains mixed liquid B;
3)By step 2)In obtained mixed liquid B ageing 6h, ethyl alcohol and ionized water are spent after filtering and is alternately cleaned, is then placed in true It is dried in empty drying box, the drying time is 4 hours, and the drying temperature is 65 DEG C, obtains mixture C;
4)By step 3)In be calcined in obtained mixture C merging Muffle furnace, the calcination temperature is 500 DEG C, the forging The burning time is 5h, and heating rate is 6 DEG C/min, must calcine sample D;
5)By step 4)In obtained calcining sample D be uniformly mixed with aqueous dimethylethanolamine, be placed in inner liner polytetrafluoroethylene In the stainless steel cauldron of material, sodium hydrate aqueous solution is added, in 18 hours reaction time under the conditions of 120 DEG C, reaction terminates Postcooling filters taking precipitate, is washed with the diluted nitric acid aqueous solution of 0.1mol/L, then be washed with deionized, then to room temperature Be placed in vacuum drying chamber dry, crush to get.
Embodiment 7
One kind being used for light-catalysed semiconductor nano material, including below according to the raw material of parts by weight:Stannous chloride methanol solution 8 Part, 30 parts of acid solution, 3 parts of bismuth chloride solution, 1 part of aqueous dimethylethanolamine, 80 parts of sodium hydrate aqueous solution.Wherein, A concentration of 1mol/L of the sodium hydrate aqueous solution;A concentration of 0.005mol/L of the aqueous dimethylethanolamine;Institute State a concentration of 3mol/L of oxalic acid;A concentration of 0.02mol/L of the bismuth chloride solution;The concentration of the stannous chloride methanol solution For 0.4mol/L;It according to weight ratio is 2 that the acid solution, which is oxalic acid, deionized water and absolute ethyl alcohol,:3:10 ratio mixing It forms;The preparation method of the bismuth chloride solution is ultrasonic disperse in the suitable polyethylene glycol for being added to bismuth chloride 20min, the supersonic frequency of the ultrasonic disperse are 35kHz to get the bismuth chloride solution.
In the present embodiment, the preparation method for light-catalysed semiconductor nano material, steps are as follows:
1)Stannous chloride methanol solution is weighed according to parts by weight, bismuth chloride solution is added while stirring under the conditions of 20 DEG C, is sent into super Sound wave microwave combination reacts in instrument, carries out processing 6min, the processing item of the ultrasonic microwave composite reaction instrument at normal temperatures Part is:Ultrasonic frequency is 30kHz, ultrasonic power 40W, microwave frequency 2000MHz, and microwave power 40W obtains mixed liquor A;
2)Acid solution is weighed according to parts by weight, a dropping step 1 while stirring under the conditions of 20 DEG C)In obtained mixed liquor A, institute The rate for stating dropwise addition is 60 drops/minute, then continues to stir 40min with the stir speed (S.S.) of 300r/min, obtains mixed liquid B;
3)By step 2)In obtained mixed liquid B ageing 6h, ethyl alcohol and ionized water are spent after filtering and is alternately cleaned, is then placed in true It is dried in empty drying box, the drying time is 4 hours, and the drying temperature is 65 DEG C, obtains mixture C;
4)By step 3)In be calcined in obtained mixture C merging Muffle furnace, the calcination temperature is 500 DEG C, the forging The burning time is 5h, and heating rate is 6 DEG C/min, must calcine sample D;
5)By step 4)In obtained calcining sample D be uniformly mixed with aqueous dimethylethanolamine, be placed in inner liner polytetrafluoroethylene In the stainless steel cauldron of material, sodium hydrate aqueous solution is added, in 18 hours reaction time under the conditions of 120 DEG C, reaction terminates Postcooling filters taking precipitate, is washed with the diluted nitric acid aqueous solution of 0.1mol/L, then be washed with deionized, then to room temperature Be placed in vacuum drying chamber dry, crush to get.
Prepared by the present invention has good photocatalytic activity for light-catalysed semiconductor nano material, passes through ultrasonic wave Microwave cooperating combined effect is prepared most short up to 30 nanometers for light-catalysed semiconductor nano material length, while being urged in light Change in activity rating, 60 minutes degradation rates can reach 96.0%, and catalytic activity is good, can be used for photocatalysis Decomposition inorganic matter Nontoxic, tasteless carbon dioxide, water etc. are generated with organic matter, problem of environmental pollution is advantageously accounted for, before having a vast market Scape.
The better embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party Formula, one skilled in the relevant art within the scope of knowledge, can also be without departing from the purpose of the present invention Various changes can be made.There is no necessity and possibility to exhaust all the enbodiments.And it thus amplifies out apparent Variation or variation be still in the protection scope of this invention.

Claims (10)

1. one kind being used for light-catalysed semiconductor nano material, which is characterized in that including below according to the raw material of parts by weight:Chlorination 5-12 parts of stannous methanol solution, 22-35 parts of acid solution, 1-5 parts of bismuth chloride solution, 0.5-1.5 parts of aqueous dimethylethanolamine, 70-85 parts of sodium hydrate aqueous solution;Wherein, the acid solution is oxalic acid solution, deionized water and absolute ethyl alcohol according to weight Than being 2:3:10 ratio mixes.
2. according to claim 1 be used for light-catalysed semiconductor nano material, which is characterized in that including below according to weight Measure the raw material of part:6-10 parts of stannous chloride methanol solution, 25-32 parts of acid solution, 2-4 parts of bismuth chloride solution, dimethylethanolamine 0.7-1.2 parts of aqueous solution, 75-82 parts of sodium hydrate aqueous solution.
3. according to claim 2 be used for light-catalysed semiconductor nano material, which is characterized in that including below according to weight Measure the raw material of part:8 parts of stannous chloride methanol solution, 30 parts of acid solution, 3 parts of bismuth chloride solution, aqueous dimethylethanolamine 1 Part, 80 parts of sodium hydrate aqueous solution.
4. according to claim 1 or 2 or 3 be used for light-catalysed semiconductor nano material, which is characterized in that the hydrogen-oxygen Change a concentration of 0.1-3mol/L of sodium water solution;A concentration of 0.001-0.01mol/L of the aqueous dimethylethanolamine.
5. according to claim 3 be used for light-catalysed semiconductor nano material, which is characterized in that the concentration of the oxalic acid For 3mol/L;A concentration of 0.02mol/L of the bismuth chloride solution;A concentration of 0.4mol/L of the stannous chloride methanol solution.
6. according to claim 5 be used for light-catalysed semiconductor nano material, which is characterized in that the bismuth chloride solution Preparation method be that ultrasonic disperse is carried out with the supersonic frequency of 20-45kHz in the suitable polyethylene glycol for being added to bismuth chloride 10-30min is to get the bismuth chloride solution.
7. a kind of preparation method for light-catalysed semiconductor nano material as described in claim 1-6 is any, feature It is, steps are as follows:
1) stannous chloride methanol solution is weighed according to parts by weight, bismuth chloride solution is added while stirring under the conditions of 15-25 DEG C, be sent into In ultrasonic microwave composite reaction instrument, processing 2-10min is carried out at normal temperatures, obtains mixed liquor A;
2) weigh acid solution according to parts by weight, a dropping step 1 while stirring under the conditions of 15-25 DEG C) in obtained mixed liquor A continues to stir 30-50min, obtains mixed liquid B;
3) mixed liquid B obtained in step 2) is aged 4-10h, ethyl alcohol is spent after filtering and ionized water alternately cleans, is then put Enter in vacuum drying chamber and be dried at 65 DEG C 4 hours, obtains mixture C;
4) by the mixture C merging Muffle furnaces obtained in step 3), 500 DEG C of progress are warming up to 6 DEG C/min of heating rate It is calcined 4-6h, sample D must be calcined;
5) the calcining sample D obtained in step 4) is uniformly mixed with aqueous dimethylethanolamine, is placed in inner liner polytetrafluoroethylene In the stainless steel cauldron of material, addition sodium hydrate aqueous solution, reaction time 18-20 hour under the conditions of 110-130 DEG C, instead It is cooled to room temperature after answering, filters taking precipitate, washed with the diluted nitric acid aqueous solution of 0.1mol/L, then be washed with deionized water Wash, be subsequently placed in vacuum drying chamber dry, crush to get.
8. the preparation method according to claim 7 for light-catalysed semiconductor nano material, which is characterized in that step 1) in, the treatment conditions of the ultrasonic microwave composite reaction instrument are:Ultrasonic frequency is 30kHz, ultrasonic power 20- 80W, microwave frequency 2000MHz, microwave power 20-80W.
9. the preparation method according to claim 8 for light-catalysed semiconductor nano material, which is characterized in that step 2) in, the stir speed (S.S.) of the stirring is 200-400r/min;The rate of the dropwise addition is 60 drops/minute.
10. a kind of being used for light-catalysed semiconductor nano material in preparing nano material as described in claim 1-6 is any Purposes.
CN201810618584.7A 2018-06-15 2018-06-15 One kind is for light-catalysed semiconductor nano material and preparation method thereof Pending CN108579722A (en)

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