CN108855111A - A kind of preparation method of stannic oxide-copper oxide composite catalyst - Google Patents
A kind of preparation method of stannic oxide-copper oxide composite catalyst Download PDFInfo
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- CN108855111A CN108855111A CN201810728897.8A CN201810728897A CN108855111A CN 108855111 A CN108855111 A CN 108855111A CN 201810728897 A CN201810728897 A CN 201810728897A CN 108855111 A CN108855111 A CN 108855111A
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- copper oxide
- composite catalyst
- stannic
- tin tetrachloride
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- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/835—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with germanium, tin or lead
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Abstract
The invention discloses a kind of stannic oxide-copper oxide composite catalyst preparation methods, including：(1) a certain amount of nano oxidized copper powders are added in deionized water, 1~3h of ultrasonic disperse obtains copper oxide suspension, wherein the concentration of the copper oxide suspension is 2~10g/L；(2) Tin tetrachloride pentahydrate is dissolved in deionized water, gained tin tetrachloride solution is added in above-mentioned copper oxide suspension, a certain amount of urea is added while stirring in 80~90 DEG C of water bath conditions, continue magnetic agitation after adding and reacts 30~40min, the pH value for adjusting reaction solution simultaneously is 2~3, it stands, it is cooling, obtain mixed sediment；(3) above-mentioned mixed sediment is centrifugated, taking precipitate is washed with dehydrated alcohol and deionized water respectively, and drying calcines 1~2h under the conditions of being placed on 450~600 DEG C, obtains stannic oxide-copper oxide composite catalyst.In stannic oxide-copper oxide composite catalyst in the present invention, stannic oxide particle is uniformly dispersed, and thermal stability is good, and catalytic performance is high.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of preparation of stannic oxide-copper oxide composite catalyst
Method.
Background technique
Stannic oxide (SnO2) be a kind of broad stopband, direct band gap n-type semiconductor, band gap width is 3.6~
3.8eV has excellent flame-retardant conductive performance, also has infrared radiation reflecting and shading, absorption, stable chemical performance, have
Highlight catalytic active etc..Due to the greater band gap of stannic oxide, responding to visible light spectrum is few, so directly being urged using stannic oxide light
The correlative study for changing degradation of contaminant is seldom.But the thermal stability of pure stannic oxide nano powder is poor, catalytic activity and
Gas-sensitive property is also undesirable.
In order to improve the catalytic performance of stannic oxide, selection is very effective with the lesser semiconductors coupling of other band gap
One of method.Since stannic oxide is n-type semiconductor, so selecting itself and the lesser p-type semiconductor copper oxide of band gap
(0.96eV) is compound, prepares novel p-n heterojunction composite semiconductor stannic oxide-copper oxide nano material, becomes photocatalysis neck
The primary study content in domain.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of preparation method of stannic oxide-copper oxide composite catalyst,
It is able to solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of stannic oxide-copper oxide composite catalyst preparation methods, existing to overcome
There is the deficiency in technology.
To achieve the above object, the present invention provides the following technical solutions：
A kind of preparation method of stannic oxide-copper oxide composite catalyst, including：
(1) a certain amount of nano oxidized copper powders are added in deionized water, it is outstanding to obtain copper oxide by 1~3h of ultrasonic disperse
Supernatant liquid, wherein the concentration of the copper oxide suspension is 2~10g/L；
(2) Tin tetrachloride pentahydrate is dissolved in deionized water, gained tin tetrachloride solution is added above-mentioned copper oxide and suspends
In liquid, a certain amount of urea is added while stirring in 80~90 DEG C of water bath conditions, add after continue magnetic agitation reaction 30~
40min, while the pH value for adjusting reaction solution is 2~3, is stood, it is cooling, obtain mixed sediment；
(3) above-mentioned mixed sediment is centrifugated, taking precipitate is washed with dehydrated alcohol and deionized water respectively, dry
1~2h is calcined under the conditions of being placed on 450~600 DEG C, obtains stannic oxide-copper oxide composite catalyst.
Preferably, in step (1), the concentration of the copper oxide suspension is 5g/L.
Preferably, in step (2), the concentration of the tin tetrachloride solution is 0.01~0.05mol/L.
Preferably, in step (2), the ratio between volume of the tin tetrachloride solution and the copper oxide suspension is 1:1~
4。
Preferably, in step (2), the amount of the substance of the urea is 0.5~1.5mol.
Preferably, in step (2), the preparation method of the Tin tetrachloride pentahydrate includes：It is measured by reaction, with metallic tin
Flower, the hydrochloric acid of 25~32wt% concentration and 20~30wt% concentration hydrogen peroxide be raw material, one-step synthesis tin tetrachloride aqueous solution,
Using filter, concentration, crystallization operation, colorless and transparent stannic chloride pentahydrate is obtained.
Compared with the prior art, the advantages of the present invention are as follows：Stannic oxide-copper oxide composite catalyst in the present invention
In, stannic oxide particle is uniformly dispersed, and thermal stability is good, and catalytic performance is high.
Specific embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used
In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of stannic oxide-copper oxide composite catalyst, including：
(1) a certain amount of nano oxidized copper powders are added in deionized water, it is outstanding to obtain copper oxide by 1~3h of ultrasonic disperse
Supernatant liquid, wherein the concentration of the copper oxide suspension is 2~10g/L；
(2) Tin tetrachloride pentahydrate is dissolved in deionized water, gained tin tetrachloride solution is added above-mentioned copper oxide and suspends
In liquid, a certain amount of urea is added while stirring in 80~90 DEG C of water bath conditions, add after continue magnetic agitation reaction 30~
40min, while the pH value for adjusting reaction solution is 2~3, is stood, it is cooling, obtain mixed sediment；
(3) above-mentioned mixed sediment is centrifugated, taking precipitate is washed with dehydrated alcohol and deionized water respectively, dry
1~2h is calcined under the conditions of being placed on 450~600 DEG C, obtains stannic oxide-copper oxide composite catalyst.
Wherein, the concentration of the copper oxide suspension is 5g/L.
Wherein, the concentration of the tin tetrachloride solution is 0.01~0.05mol/L, it is preferred that the tin tetrachloride solution
Concentration be 0.02mol/L.
Wherein, the ratio between volume of the tin tetrachloride solution and the copper oxide suspension is 1:1~4, it is preferred that described
The ratio between volume of tin tetrachloride solution and the copper oxide suspension is 1:3.
Wherein, the amount of the substance of the urea is 0.5~1.5mol, it is preferred that the amount of the substance of the urea is
1.2mol。
In one embodiment, the preparation method of the Tin tetrachloride pentahydrate includes：
It is measured by reaction, the hydrogen peroxide with metallic tin flower, the hydrochloric acid of 25~32wt% concentration and 20~30wt% concentration is
Raw material, one-step synthesis tin tetrachloride aqueous solution obtain colorless and transparent stannic chloride pentahydrate using filter, concentration, crystallization operation.
It is following that stannic oxide in the present invention-copper oxide composite catalyst preparation side is illustrated with specifically embodiment
Method.
Embodiment 1
(1) a certain amount of nano oxidized copper powders are added in deionized water, ultrasonic disperse 1h, obtain copper oxide suspension
Liquid, wherein the concentration of the copper oxide suspension is 2g/L；
(2) Tin tetrachloride pentahydrate is dissolved in deionized water, obtains the tin tetrachloride solution that concentration is 0.01mol/L,
It is 1 by the ratio between volume:1 tin tetrachloride solution is uniformly mixed with above-mentioned copper oxide suspension, is stirred in 80 DEG C of water bath condition sides
The urea that the amount of substance is 0.5mol is added in side, continues magnetic agitation reaction 30min after adding, while adjusting the pH of reaction solution
Value is 2, is stood, cooling, obtains mixed sediment；
(3) above-mentioned mixed sediment is centrifugated, taking precipitate is washed with dehydrated alcohol and deionized water respectively, dry
1h is calcined under the conditions of being placed on 450 DEG C, obtains stannic oxide-copper oxide composite catalyst.
Embodiment 2
(1) a certain amount of nano oxidized copper powders are added in deionized water, ultrasonic disperse 2h, obtain copper oxide suspension
Liquid, wherein the concentration of the copper oxide suspension is 5g/L；
(2) Tin tetrachloride pentahydrate is dissolved in deionized water, obtains the tin tetrachloride solution that concentration is 0.02mol/L,
It is 1 by the ratio between volume:3 tin tetrachloride solution is uniformly mixed with above-mentioned copper oxide suspension, is stirred in 85 DEG C of water bath condition sides
The urea that the amount of substance is 1.2mol is added in side, continues magnetic agitation reaction 35min after adding, while adjusting the pH of reaction solution
Value is 2.6, is stood, cooling, obtains mixed sediment；
(3) above-mentioned mixed sediment is centrifugated, taking precipitate is washed with dehydrated alcohol and deionized water respectively, dry
1.5h is calcined under the conditions of being placed on 520 DEG C, obtains stannic oxide-copper oxide composite catalyst.
Embodiment 3
(1) a certain amount of nano oxidized copper powders are added in deionized water, ultrasonic disperse 3h, obtain copper oxide suspension
Liquid, wherein the concentration of the copper oxide suspension is 10g/L；
(2) Tin tetrachloride pentahydrate is dissolved in deionized water, obtains the tin tetrachloride solution that concentration is 0.05mol/L,
It is 1 by the ratio between volume:4 tin tetrachloride solution is uniformly mixed with above-mentioned copper oxide suspension, is stirred in 90 DEG C of water bath condition sides
The urea that the amount of substance is 1.5mol is added in side, continues magnetic agitation reaction 40min after adding, while adjusting the pH of reaction solution
Value is 3, is stood, cooling, obtains mixed sediment；
(3) above-mentioned mixed sediment is centrifugated, taking precipitate is washed with dehydrated alcohol and deionized water respectively, dry
2h is calcined under the conditions of being placed on 600 DEG C, obtains stannic oxide-copper oxide composite catalyst.
Stannic oxide made from method in the present invention-copper oxide composite catalyst, tin dioxide nano-particle can be equal
It is dispersed in the surface of copper oxide evenly, there is preferable stability, and the preparation method is simple, it is environmentally protective, have preferable
Application prospect.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Claims (6)
1. a kind of stannic oxide-copper oxide composite catalyst preparation method, which is characterized in that including：
(1) a certain amount of nano oxidized copper powders being added in deionized water, 1~3h of ultrasonic disperse obtains copper oxide suspension,
Wherein, the concentration of the copper oxide suspension is 2~10g/L；
(2) Tin tetrachloride pentahydrate being dissolved in deionized water, gained tin tetrachloride solution is added in above-mentioned copper oxide suspension,
A certain amount of urea is added while stirring in 80~90 DEG C of water bath conditions, continues magnetic agitation after adding and reacts 30~40min,
The pH value for adjusting reaction solution simultaneously is 2~3, is stood, cooling, obtains mixed sediment；
(3) above-mentioned mixed sediment is centrifugated, taking precipitate is washed with dehydrated alcohol and deionized water respectively, dry postposition
1~2h is calcined under the conditions of 450~600 DEG C, obtains stannic oxide-copper oxide composite catalyst.
2. stannic oxide according to claim 1-copper oxide composite catalyst preparation method, which is characterized in that step
(1) in, the concentration of the copper oxide suspension is 5g/L.
3. stannic oxide according to claim 1-copper oxide composite catalyst preparation method, which is characterized in that step
(2) in, the concentration of the tin tetrachloride solution is 0.01~0.05mol/L.
4. stannic oxide according to claim 1-copper oxide composite catalyst preparation method, which is characterized in that step
(2) in, the ratio between volume of the tin tetrachloride solution and the copper oxide suspension is 1:1~4.
5. stannic oxide according to claim 1-copper oxide composite catalyst preparation method, which is characterized in that step
(2) in, the amount of the substance of the urea is 0.5~1.5mol.
6. stannic oxide according to claim 1-copper oxide composite catalyst preparation method, which is characterized in that step
(2) in, the preparation method of the Tin tetrachloride pentahydrate includes：It is measured by reaction, it is colored, 25~32wt% concentration with metallic tin
Hydrochloric acid and the hydrogen peroxide of 20~30wt% concentration are raw material, one-step synthesis tin tetrachloride aqueous solution, using filter, concentration, crystallization
Operation, obtains colorless and transparent stannic chloride pentahydrate.
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