CN107128965A - A kind of preparation method of the nano zine oxide with barrier ultraviolet light and blue light - Google Patents
A kind of preparation method of the nano zine oxide with barrier ultraviolet light and blue light Download PDFInfo
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- CN107128965A CN107128965A CN201710397071.3A CN201710397071A CN107128965A CN 107128965 A CN107128965 A CN 107128965A CN 201710397071 A CN201710397071 A CN 201710397071A CN 107128965 A CN107128965 A CN 107128965A
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- nano zine
- blue light
- zine oxide
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- ultraviolet light
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C01—INORGANIC CHEMISTRY
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
- C01P2002/54—Solid solutions containing elements as dopants one element only
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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Abstract
The present invention relates to a kind of preparation method for the nano zine oxide for having and obstructing ultraviolet light and blue light, comprise the following steps：(1) gallium oxide is added in sodium hydroxide solution, heating response under stirring condition, transparent precursor liquid is made；(2) precursor liquid is slowly added in acetic acid zinc solution while stirring, muddy mixed liquor is made；(3) sodium hydroxide solution is slowly added in mixed liquor while stirring generate latax, then heating stirring, then latax is put into reactor carries out hydro-thermal reaction；(4) sediment is generated after hydro-thermal reaction, after sediment is washed, dried, crush, then by high-temperature calcination is to obtain the nano zine oxide with barrier ultraviolet light and blue light.Compared with prior art, present invention synthesis cost is low, pollution-free, and the suitable obtained nano zine oxide product purity of production in enormous quantities is high, rate of absorbing UV>99%, the 480nm absorptivities of blue light 400>90%, it is seen that light transmission rate>85%.
Description
Technical field
The present invention relates to a kind of nano zine oxide preparation method, more particularly, to a kind of efficient barrier ultraviolet light and blue light
The preparation method of doped gallium nano zinc oxide material.
Background technology
Nano zine oxide is a kind of new high function fine inorganic chemical products of Twenty-First Century, due to size
Small, specific surface area is big, imitated with skin effect, bulk effect, quantum size effect, macro quanta tunnel effect and dielectric confinement
It should wait, with many special properties, such as nontoxic and non-migratory, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability,
Had a wide range of applications in industries such as rubber, coating, ceramics, weaving, cosmetics, as new functional.
Wherein the small-size effect of zinc oxide nano-particle, significantly improves its ultraviolet absorption ability opposite bank material.By
There is shielding action to long wave ultraviolet and ultraviolet B radiation in nano zine oxide, can be as ultraviolet light screener, applied to change
The sun-screening agent of cosmetic and fibrous material field.
And in nano-zinc oxide composite material research, be using the material for improving nano zine oxide performance as main purpose
It is main, mainly study the properties such as spectral emissions, conductance, light transmission rate, photoelectricity transmission, gas sensing property.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of product purity is high, close
It is low, pollution-free into cost, it is adapted to the preparation method of the nano zine oxide with barrier ultraviolet light and blue light produced in enormous quantities.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of the nano zine oxide with barrier ultraviolet light and blue light, comprises the following steps：
(1) gallium oxide is added in sodium hydroxide solution, heating response under stirring condition, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.01~0.1:1, precursor liquid is slowly added in acetic acid zinc solution while stirring,
Muddy mixed liquor is made；
(3) sodium hydroxide solution is slowly added in mixed liquor while stirring generate latax, controls the latax of generation
PH be 8~9, then heating stirring, then latax is put into reactor carries out hydro-thermal reaction；
(4) sediment is generated after hydro-thermal reaction, after sediment is washed, dried, crush, then by high-temperature calcination is to obtain
Nano zine oxide with barrier ultraviolet light and blue light.
The condition of heating response in step (1) is：1~5h of stirring reaction at a temperature of 40~100 DEG C.
Sodium hydroxide solution described in step (1) is the concentrated solution of sodium hydroxide, the sodium hydroxide described in step (3)
Solution is the weak solution of sodium hydroxide.
The concentration of the concentrated solution of sodium hydroxide described in step (1) is more than 15mol/L, the hydroxide described in step (3)
Sodium solution is less than 2mol/L for the concentration of the weak solution of sodium hydroxide.
The concentrated solution of sodium hydroxide in step (1) is being met on the premise of sodium hydroxide can dissolve, and concentration is as far as possible
It is big.
In step (1), sodium hydroxide is excessive relative to gallium oxide.
Preferably, the solubility of the weak solution of the sodium hydroxide in step (3) is less than 1mol/L, more than 0.1mol/L.
The condition of heating stirring in step (3) is：0.5~3h is stirred at a temperature of 80~95 DEG C.
The condition of hydro-thermal reaction in step (3) is：5~16h is reacted at a temperature of 120~200 DEG C.
The condition of high-temperature calcination in step (4) is：350~700 DEG C of 5~10h of calcining.
Speed of agitator in step (1) and the rotating speed of the heating stirring in step (3) control respectively 300~500 turns/
min；Crushing in step (4) uses pulverizer, and pulverization conditions are：Under 2000~15000 turns/min rotating speed crush 5~
30min。
Preferably, the addition speed of precursor liquid is controlled in step (2), the addition of precursor liquid is completed in 0.5~6h；Step
(3) speed that sodium hydroxide solution is added, completes the addition of precursor liquid in 0.5~6h.
The concentration of described acetic acid zinc solution is 0.01~1mol/L.
Preferably, the concentration of described acetic acid zinc solution is 0.02~0.1mol/L.
The present invention uses hydrothermal deposition method, and adulterate gallium element, crosses the selection of technological parameter, finds best process flow, changes
Become the doping concentration of gallium element, the experiment parameter such as reaction time, reaction temperature, calcining heat, finally of the present invention each
In process parameters range, rate of absorbing UV is made>99%, blue light 400~480nm absorptivities>90%, it is seen that light transmission rate>
85% zinc oxide nano-powder, not only perfect ultraviolet screener effect, and the further radiation for having obstructed blue light, are widened
The application of nanometer Zinc oxide powder.
Compared with prior art, the invention has the advantages that：
The present invention is swift in response, product purity high, synthesis cost is low, pollution-free, is adapted to produce in enormous quantities, obtained gallium is mixed
Zinc oxide powder particle diameter is small, narrowly distributing, is difficult to reunite, stability is good.Target product rate of absorbing UV>99%, blue light 400~
480nm absorptivities>90%, it is seen that light transmission rate>85%, excellent performance.
Embodiment
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
(1) gallium oxide is mixed in the strong caustic that concentration is more than 15mol/L, controls 300 turns/min of mixing speed,
In 80 DEG C of water-bath 2h, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.08:1, precursor liquid is stirred while be slowly added in acetic acid zinc solution,
Muddiness mixed liquor is made；
(3) sodium hydroxide solution that the concentration after dilution is less than 2mol/L is stirred while be slowly added to mixed liquor,
The latax PH for controlling generation is 8；At 80 DEG C, latax stirring in water bath is reacted 2h by 300 turns/min, places into reactor water
Thermal response, 120 DEG C of reaction 16h, naturally cools to room temperature；
(4) after reaction precipitate washing is dried, crushed, 12000 turns/min, crush 10min；Again through 500 DEG C of calcinings
5h produces target product.
Embodiment 2
(1) gallium oxide is mixed in the strong caustic that concentration is more than 15mol/L, controls 400 turns/min of mixing speed,
In 40 DEG C of water-bath 5h, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.05:1, precursor liquid is stirred while be slowly added in acetic acid zinc solution,
Muddiness mixed liquor is made；
(3) sodium hydroxide solution that the concentration after dilution is less than 2mol/L is stirred while be slowly added to mixed liquor,
The latax PH for controlling generation is 9；At 90 DEG C, latax stirring in water bath is reacted 2h by 300 turns/min, places into reactor water
Thermal response, 150 DEG C of reaction 10h, naturally cools to room temperature；
(4) after reaction precipitate washing is dried, crushed, 5000 turns/min, crush 15min；Again through 700 DEG C of calcining 3h
Produce target product.
Embodiment 3
(1) gallium oxide is mixed in the strong caustic that concentration is more than 15mol/L, controls 500 turns/min of mixing speed,
In 60 DEG C of water-bath 3h, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.02:1, precursor liquid is stirred while be slowly added in acetic acid zinc solution,
Muddiness mixed liquor is made；
(3) sodium hydroxide solution that the concentration after dilution is less than 2mol/L is stirred while be slowly added to mixed liquor,
The latax PH for controlling generation is 9；At 95 DEG C, latax stirring in water bath is reacted 1.5h by 400 turns/min, places into reactor
Hydro-thermal reaction, 150 DEG C of reaction 12h, naturally cools to room temperature；
(4) after reaction precipitate washing is dried, crushed, 15000 turns/min, crush 5min；Again through 350 DEG C of calcinings
10h produces target product.
Embodiment 4
(1) gallium oxide is mixed in the strong caustic that concentration is more than 15mol/L, controls 300 turns/min of mixing speed,
In 70 DEG C of water-bath 3h, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.01:1, precursor liquid is stirred while be slowly added in acetic acid zinc solution,
Muddiness mixed liquor is made；
(3) sodium hydroxide solution that the concentration after dilution is less than 2mol/L is stirred while be slowly added to mixed liquor,
The latax PH for controlling generation is 8.5；At 90 DEG C, latax stirring in water bath is reacted 2h by 350 turns/min, places into reactor
Hydro-thermal reaction, 200 DEG C of reaction 5h, naturally cools to room temperature；
(4) after reaction precipitate washing is dried, crushed, 10000 turns/min, crush 15min；Again through 600 DEG C of calcinings
4.5h produces target product.
Embodiment 5
(1) gallium oxide is mixed in the strong caustic that concentration is more than 15mol/L, controls 400 turns/min of mixing speed,
In 50 DEG C of water-bath 4h, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.07:1, precursor liquid is stirred while be slowly added in acetic acid zinc solution,
Muddiness mixed liquor is made；
(3) sodium hydroxide solution that the concentration after dilution is less than 2mol/L is stirred while be slowly added to mixed liquor,
The latax PH for controlling generation is 8；At 80 DEG C, latax stirring in water bath is reacted 2h by 300 turns/min, places into reactor water
Thermal response, 200 DEG C of reaction 6h, naturally cools to room temperature；
(4) after reaction precipitate washing is dried, crushed, 12000 turns/min, crush 20min；Again through 700 DEG C of calcinings
5h produces target product.
Embodiment 6
(1) gallium oxide is mixed in the strong caustic that concentration is more than 15mol/L, controls 300 turns/min of mixing speed,
In 95 DEG C of water-bath 1h, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.08:1, precursor liquid is stirred while be slowly added in acetic acid zinc solution,
Muddiness mixed liquor is made；
(3) sodium hydroxide solution that the concentration after dilution is less than 2mol/L is stirred while be slowly added to mixed liquor,
The latax PH for controlling generation is 9；At 90 DEG C, latax stirring in water bath is reacted 0.5h by 500 turns/min, places into reactor
Hydro-thermal reaction, 180 DEG C of reaction 8h, naturally cools to room temperature；
(4) after reaction precipitate washing is dried, crushed, 2000 turns/min, crush 30min；Again through 600 DEG C of calcining 7h
Produce target product.
Embodiment 7
(1) gallium oxide is mixed in the strong caustic that concentration is more than 15mol/L, controls 300 turns/min of mixing speed,
In 80 DEG C of water-bath 3h, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.06:1, precursor liquid is stirred while be slowly added in acetic acid zinc solution,
Muddiness mixed liquor is made；
(3) sodium hydroxide solution that the concentration after dilution is less than 2mol/L is stirred while be slowly added to mixed liquor,
The latax PH for controlling generation is 8.5；At 95 DEG C, latax stirring in water bath is reacted 1h by 500 turns/min, places into reactor
Hydro-thermal reaction, 120 DEG C of reaction 16h, naturally cools to room temperature；
(4) after reaction precipitate washing is dried, crushed, 4000 turns/min, crush 20min；Again through 350 DEG C of calcinings
10h produces target product.
Embodiment 8
(1) gallium oxide is mixed in the strong caustic that concentration is more than 15mol/L, controls 500 turns/min of mixing speed,
In 100 DEG C of water-bath 1h, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.01:1, precursor liquid is stirred while be slowly added in acetic acid zinc solution,
Muddiness mixed liquor is made；
(3) sodium hydroxide solution that the concentration after dilution is less than 2mol/L is stirred while be slowly added to mixed liquor,
The latax PH for controlling generation is 8；At 95 DEG C, latax stirring in water bath is reacted 1h by 300 turns/min, places into reactor water
Thermal response, 250 DEG C of reaction 5h, naturally cools to room temperature；
(4) after reaction precipitate washing is dried, crushed, 6000 turns/min, crush 15min；Again through 600 DEG C of calcining 5h
Produce target product.
Embodiment 9
(1) gallium oxide is mixed in the strong caustic that concentration is more than 15mol/L, controls 300 turns/min of mixing speed,
In 80 DEG C of water-bath 2h, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.1:1, precursor liquid is stirred while being slowly added in acetic acid zinc solution, control
System adds speed, completes to add in 0.5~6h, and muddiness mixed liquor is made；
(3) sodium hydroxide solution that the concentration after dilution is less than 2mol/L is stirred while be slowly added to mixed liquor,
Control adds speed, completes to add in 0.5~6h, and the latax PH for controlling generation is 8；At 80 DEG C, 300 turns/min is by breast
Glue stirring in water bath reacts 2h, places into reactor hydro-thermal reaction, and 120 DEG C of reaction 16h naturally cool to room temperature；
(4) after reaction precipitate washing is dried, crushed, 12000 turns/min, crush 10min；Again through 500 DEG C of calcinings
5h produces target product.
Embodiment 10
At (1) 100 DEG C, gallium oxide is mixed in saturation strong caustic, sodium hydroxide is excessive relative to gallium oxide,
500 turns/min of mixing speed is controlled, in 100 DEG C of water-bath 1h, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.03:1, precursor liquid is stirred while be slowly added in acetic acid zinc solution,
Control adds speed, and 1h completes to add, and muddiness mixed liquor is made；
(3) concentration after dilution is stirred while be slowly added to mixed liquor for 0.2mol/L sodium hydroxide solution,
Control adds speed, and 1h completes to add, and the latax PH for controlling generation is 8；At 95 DEG C, 300 turns/min is by latax water-bath
Stirring reaction 1h, places into reactor hydro-thermal reaction, and 220 DEG C of reaction 6h naturally cool to room temperature；
(4) after reaction precipitate washing is dried, crushed, 12000 turns/min, crush 20min；Again through 600 DEG C of calcinings
7h produces target product.
Target product rate of absorbing UV 99.6% made from the present embodiment, 400~480nm of blue light absorptivities 95%, it is seen that
Light transmission rate>90%, particle diameter is small, narrowly distributing, is difficult to reunite, stability is good, places more than 2 years without substantially reunion, performance is without bright
Aobvious decay.
Claims (10)
1. a kind of preparation method of the nano zine oxide with barrier ultraviolet light and blue light, it is characterised in that comprise the following steps：
(1) gallium oxide is added in sodium hydroxide solution, heating response under stirring condition, transparent precursor liquid is made；
(2) Ga is pressed3+With Zn2+Mol ratio 0.01~0.1:1, precursor liquid is slowly added in acetic acid zinc solution while stirring, is made
Muddy mixed liquor；
(3) sodium hydroxide solution is slowly added in mixed liquor while stirring generate latax, controls the pH of the latax of generation
For 8~9, then heating stirring, then latax is put into reactor carries out hydro-thermal reaction；
(4) sediment is generated after hydro-thermal reaction, after sediment is washed, dried, crush, then by high-temperature calcination is to be had
Obstruct the nano zine oxide of ultraviolet light and blue light.
2. a kind of preparation method of nano zine oxide with barrier ultraviolet light and blue light according to claim 1, it is special
Levy and be, the condition of the heating response in step (1) is：1~5h of stirring reaction at a temperature of 40~100 DEG C.
3. a kind of preparation method of nano zine oxide with barrier ultraviolet light and blue light according to claim 1, it is special
Levy and be, the sodium hydroxide solution described in step (1) is the concentrated solution of sodium hydroxide, the sodium hydroxide described in step (3)
Solution is the weak solution of sodium hydroxide.
4. a kind of preparation method of nano zine oxide with barrier ultraviolet light and blue light according to claim 3, it is special
Levy and be, the concentration of the concentrated solution of the sodium hydroxide described in step (1) is more than 15mol/L, the sodium hydroxide described in step (3)
Solution is less than 2mol/L for the concentration of the weak solution of sodium hydroxide.
5. a kind of preparation method of nano zine oxide with barrier ultraviolet light and blue light according to claim 1, it is special
Levy and be, the condition of the heating stirring in step (3) is：0.5~3h is stirred at a temperature of 80~95 DEG C.
6. a kind of preparation method of nano zine oxide with barrier ultraviolet light and blue light according to claim 1, it is special
Levy and be, the condition of the hydro-thermal reaction in step (3) is：5~16h is reacted at a temperature of 120~250 DEG C.
7. a kind of preparation method of nano zine oxide with barrier ultraviolet light and blue light according to claim 1, it is special
Levy and be, the condition of the high-temperature calcination in step (4) is：350~700 DEG C of 3~10h of calcining.
8. a kind of preparation method of nano zine oxide with barrier ultraviolet light and blue light according to claim 1, it is special
Levy and be, the rotating speed of the speed of agitator in step (1) and the heating stirring in step (3) control respectively 300~500 turns/
min；Crushing in step (4) uses pulverizer, and pulverization conditions are：Under 2000~15000 turns/min rotating speed crush 5~
30min。
9. a kind of preparation method of nano zine oxide with barrier ultraviolet light and blue light according to claim 1, it is special
Levy and be, the concentration of described acetic acid zinc solution is 0.01~1mol/L.
10. a kind of preparation method of nano zine oxide with barrier ultraviolet light and blue light according to claim 9, it is special
Levy and be, the concentration of described acetic acid zinc solution is 0.02~0.1mol/L.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102723120A (en) * | 2012-06-14 | 2012-10-10 | 天津大学 | Doped zinc oxide nanometer conductive powder material and preparation method thereof |
| CN104495928A (en) * | 2015-01-09 | 2015-04-08 | 中国科学院上海硅酸盐研究所 | Preparation method of vanadium dioxide/zinc oxide nano composite powder |
| CN105540640A (en) * | 2016-01-26 | 2016-05-04 | 东北林业大学 | Preparation method of flower-shaped nanometer zinc oxide |
-
2017
- 2017-05-31 CN CN201710397071.3A patent/CN107128965A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102723120A (en) * | 2012-06-14 | 2012-10-10 | 天津大学 | Doped zinc oxide nanometer conductive powder material and preparation method thereof |
| CN104495928A (en) * | 2015-01-09 | 2015-04-08 | 中国科学院上海硅酸盐研究所 | Preparation method of vanadium dioxide/zinc oxide nano composite powder |
| CN105540640A (en) * | 2016-01-26 | 2016-05-04 | 东北林业大学 | Preparation method of flower-shaped nanometer zinc oxide |
Non-Patent Citations (1)
| Title |
|---|
| 董永春主编: "《纺织助剂化学》", 31 January 2010 * |
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