CN115818698A - Preparation method of nano zinc oxide - Google Patents
Preparation method of nano zinc oxide Download PDFInfo
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- CN115818698A CN115818698A CN202211679589.3A CN202211679589A CN115818698A CN 115818698 A CN115818698 A CN 115818698A CN 202211679589 A CN202211679589 A CN 202211679589A CN 115818698 A CN115818698 A CN 115818698A
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- 239000000243 solution Substances 0.000 claims abstract description 39
- 150000003751 zinc Chemical class 0.000 claims abstract description 23
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 19
- 239000012266 salt solution Substances 0.000 claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 15
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 13
- 239000004246 zinc acetate Substances 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 6
- 229960001763 zinc sulfate Drugs 0.000 claims description 6
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 239000001099 ammonium carbonate Substances 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- VQBIMXHWYSRDLF-UHFFFAOYSA-M sodium;azane;hydrogen carbonate Chemical compound [NH4+].[Na+].[O-]C([O-])=O VQBIMXHWYSRDLF-UHFFFAOYSA-M 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- CYJRNFFLTBEQSQ-UHFFFAOYSA-N 8-(3-methyl-1-benzothiophen-5-yl)-N-(4-methylsulfonylpyridin-3-yl)quinoxalin-6-amine Chemical compound CS(=O)(=O)C1=C(C=NC=C1)NC=1C=C2N=CC=NC2=C(C=1)C=1C=CC2=C(C(=CS2)C)C=1 CYJRNFFLTBEQSQ-UHFFFAOYSA-N 0.000 claims 1
- 125000003827 glycol group Chemical group 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000011701 zinc Substances 0.000 abstract description 9
- 229910052725 zinc Inorganic materials 0.000 abstract description 9
- 238000010924 continuous production Methods 0.000 abstract description 3
- 239000002351 wastewater Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 8
- 239000012798 spherical particle Substances 0.000 description 8
- 238000005406 washing Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000001788 irregular Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- -1 and has high purity Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of nano zinc oxide, which comprises the following steps: introducing the reaction liquid into a microchannel reactor for reaction to obtain reaction liquid A, and calcining the reaction liquid A to obtain the nano zinc oxide; wherein the reaction solution comprises a zinc salt solution; the flow rate of the reaction liquid is 150-300mL/min; the structure of the microchannel reactor is a concentric circle structure. The invention takes zinc salt solution with low price as zinc source, and leads the zinc source into a microchannel reactor with a concentric circle structure at a certain flow rate, and can prepare the nano zinc oxide with controllable grain diameter. The preparation method of the invention does not introduce other components, does not generate new waste water, is environment-friendly, has safe, efficient, green and continuous process route, and can obtain the nano zinc oxide particles with smaller size and better monodispersity in a short time.
Description
Technical Field
The invention relates to a preparation method of nano zinc oxide.
Background
The production method of zinc oxide mainly includes three methods of direct method, indirect method and liquid phase synthesis method. The direct and indirect methods are also known as dry methods. The direct method uses zinc ore as raw material, and makes it react with coke under heating to make zinc salt reduce into zinc vapour at high temp., then make it oxidate with air, and after cooling, the zinc oxide is collected. The product obtained by the method has thick and irregular particles and low purity. The indirect method uses metal zinc as raw material, heats it to produce zinc vapor, then combines it with oxygen to form zinc oxide, and has high purity, fine particles and round shape. The products produced by the two methods can not reach the nanometer level and have agglomeration. In the synthesis of the micro-nano zinc oxide material, a liquid phase method such as a precipitation method, a hydrothermal method, a solvothermal method, a sol-gel method, a microemulsion method and the like is frequently used. However, these liquid phase synthesis methods are generally carried out in a batch stirred tank reactor, and some methods require preparation of a precursor, some methods require a special surfactant, some methods require a high-temperature and high-pressure apparatus, and most methods require subsequent heat treatment, and these limitations are more or less inconvenient for industrial production.
The micro chemical technology is the technology frontier field of multidisciplinary intersection which is started in the early 90 s of the 20 th century. The technology is mainly characterized in that various unit operations and reaction processes are realized by adopting microchannels with characteristic sizes of tens to hundreds of microns. Because the size of the channel is obviously reduced, the heat and mass transfer process is obviously strengthened, the utilization efficiency of energy in the reaction process and the production capacity of unit volume can be greatly improved, and the strengthening, the miniaturization and the greening of the chemical process are realized. In recent years, the preparation of nanomaterials by using the micro-chemical technology has attracted extensive attention in academia and industry. However, there have been few reports of the development of nano-oxide production in microchannel reactors.
Disclosure of Invention
The invention aims to overcome the defects that the zinc oxide prepared by the preparation method of the zinc oxide in the prior art has low purity, cannot reach the nano level, has agglomeration, is complex in preparation method and the like, and provides the preparation method of the nano zinc oxide. The invention takes zinc salt solution with low price as zinc source, and leads the zinc source into a microchannel reactor with a concentric circle structure at a certain flow rate, and can prepare the nano zinc oxide with controllable grain diameter. The preparation method of the invention does not introduce other components, does not generate new waste water, is environment-friendly, has safe, efficient, green and continuous process route, and can obtain the nano zinc oxide particles with smaller size and better monodispersity in a short time.
The technical scheme of the invention is as follows:
the invention provides a preparation method of nano zinc oxide, which comprises the following steps:
introducing the reaction liquid into a microchannel reactor for reaction to obtain reaction liquid A, and calcining the reaction liquid A to obtain the nano zinc oxide;
wherein the reaction solution comprises a zinc salt solution; the flow rate of the reaction liquid is 150-300mL/min; the structure of the microchannel reactor is a concentric circle structure.
In the present invention, the reaction solution is preferably a zinc salt solution, or the reaction solution does not contain an alkaline substance.
In the present invention, the preparation method of the zinc salt solution preferably comprises the following steps: and mixing the zinc salt and the solvent, and stirring to obtain the zinc salt solution. The stirring time is preferably 10-120min, for example 60min.
Wherein, the zinc salt can comprise one or more of zinc sulfate, zinc chloride, zinc acetate and zinc nitrate, preferably zinc sulfate or zinc acetate.
Wherein the solvent may be a solvent capable of dissolving the zinc salt, such as ethylene glycol or water, which is conventional in the art.
In the present invention, the concentration of the zinc salt solution may be 0.2 to 2mol/L, for example 0.5mol/L, 1mol/L or 2mol/L.
In the present invention, the reaction solution is preferably introduced at a flow rate of 180 to 250mL/min, for example, 200mL/min.
In the present invention, the inner diameter of the pipe of the microchannel reactor may be 2 to 5mm, for example, 4mm. The inner diameter of the pipe represents the inner diameter of the pipe for the reaction liquid to enter the microchannel reactor.
In the present invention, the material of the microchannel reactor is preferably 625 nickel.
In the invention, the difference between the inner diameter and the outer diameter of the concentric circle structure of the microchannel reactor is consistent with the inner diameter of the pipeline of the microchannel reactor. The difference between the inner and outer diameters of the concentric circular structures of the microchannel reactor may be 2-5mm, for example 4mm.
In the invention, in the concentric circle structure of the microchannel reactor, the number of the concentric circles can be determined according to the flow rate of the reaction liquid. The number of concentric circles may be 6-10, for example 8.
In the present invention, the temperature of the reaction is preferably 100 to 120 ℃ such as 110 ℃.
In the present invention, the reaction time is preferably 10 to 30min, for example 20min.
In the present invention, the temperature of the calcination is preferably 200 to 400 ℃, for example, 300 ℃.
In the present invention, the calcination time is preferably 1 to 3 hours, for example, 2 hours.
In the present invention, the reaction solution may further include an alkaline substance. The reaction solution can be obtained by mixing a zinc salt solution and an alkali solution.
Among them, the method for preparing the alkali solution preferably includes the steps of: mixing alkaline substance and solvent, stirring to obtain the alkaline solution. The stirring time is preferably 10-120min, for example 60min.
Wherein the alkaline substance may include one or more of sodium hydroxide, potassium hydroxide, sodium carbonate and ammonium carbonate. The solvent may be a solvent capable of dissolving the alkali source, such as water.
Wherein the concentration of the alkali solution may be 0.2 to 2mol/L, such as 0.5mol/L, 1mol/L or 2mol/L.
Wherein the introduction flow rate of the alkali solution can be 150-300mL/min.
In the present invention, the reaction preferably further comprises the steps of separating, washing and drying in this order after the reaction and before the calcination.
Wherein the separation may be conventional in the art, such as centrifugation.
Wherein the drying operations and conditions may be conventional in the art. The temperature of the drying may be 80 ℃.
In the present invention, the shape of the nano zinc oxide is preferably spherical.
In the present invention, the particle size of the nano zinc oxide is preferably 25 to 50nm.
In the preparation process of the nano zinc oxide, the reaction liquid can be collided for multiple times in the microchannel reactor, so that the continuous production of the nano zinc oxide can be realized.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
according to the invention, a zinc salt solution with low price is taken as a zinc source, a microchannel reactor with a concentric circle structure is introduced at a flow rate of 150-300mL/min, and multiple high-speed collisions of a reaction solution are realized in a limited space by utilizing the microscale in the microchannel reactor to improve the mixing performance of the reaction solution, so that the rapid consumption of the reaction solution is effectively promoted, the explosive nucleation of the zinc salt solution is further promoted, and the controllable preparation of nano zinc oxide particles with the particle size of 25-50nm is realized. The preparation method of the invention does not introduce other components, does not generate new waste water, is environment-friendly and is beneficial to popularization and application; and the process route is simple, and the nano zinc oxide particles with controllable size and good monodispersity can be obtained in a short time.
Drawings
Fig. 1 is an SEM image of nano zinc oxide prepared in example 1.
Fig. 2 is an SEM image of nano zinc oxide prepared in comparative example 1.
FIG. 3 is a schematic diagram of microchannel reactors used in examples 1-7 and comparative examples 2-3.
FIG. 4 is a graph showing the difference of the inner and outer diameters of concentric circles in the microchannel reactors used in examples 1-7 and comparative examples 2-3.
FIG. 5 is a schematic diagram showing the inner diameters of the reaction liquid inlet tubes of the microchannel reactors used in examples 1 to 7 and comparative examples 2 to 3.
Description of reference numerals:
a reaction liquid inlet 1; a reaction liquid inlet 2; difference 3 between inner and outer diameters of concentric circles; the reaction solution inlet pipe has an inner diameter 4.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
Examples 1 to 7 and comparative examples 2 to 3 described below were each prepared using a microchannel reactor as shown in fig. 3. The microchannel reactor is made of 625 nickel, the difference between the inner diameter and the outer diameter of the concentric circles is 4mm (the direction parallel to the flow direction of the reactant liquid is taken as the cross-sectional direction of the concentric circles, and fig. 4 is a schematic diagram showing the difference between the inner diameter and the outer diameter of the concentric circles), the inner diameter of the pipeline is 4mm (the direction perpendicular to the flow direction of the reactant liquid is taken as the cross-sectional direction of the inner diameter of the pipeline, and fig. 5 is a schematic diagram showing the inner diameter of the reactant liquid inlet pipeline), and the number of the concentric circles is 8.
Example 1
(1) Mixing zinc acetate with ethylene glycol, and stirring for 60min to obtain 0.5mol/L zinc acetate solution.
(2) Mixing sodium hydroxide with water, and stirring for 60min to obtain 0.5mol/L sodium hydroxide solution.
(3) And (3) respectively introducing the zinc acetate solution and the alkali solution into the microchannel reactor from the reactor inlet 1 and the reactor inlet 2 at the flow rate of 150mL/min, and carrying out contact, mixing and reaction at the reaction temperature of 110 ℃ for 20min. And centrifugally separating and washing the reacted solution, drying at 80 ℃, and calcining at 300 ℃ for 2 hours. The SEM characterization results are shown in FIG. 1. The shape of the particles is spherical particles, the distribution is uniform, and the diameter is about 40nm.
Example 2
The difference from example 1 is that: zinc sulfate is adopted in the step (1); in the step (3), the reaction temperature is 100 ℃, and the reaction time is 30min.
The obtained nano zinc oxide is spherical particles, is uniformly distributed and has the diameter of about 38nm.
Example 3
The difference from example 1 is that: mixing zinc acetate with water in the step (1); in the step (3), the reaction temperature is 120 ℃, and the reaction time is 10min.
The obtained nano zinc oxide is spherical particles, is uniformly distributed and has the diameter of about 45nm.
Example 4
The difference from example 1 is that: the step (2) is cancelled; the step (3) is as follows: and (3) introducing the zinc acetate solution into the microchannel reactor from the inlet 1 of the reactor at the flow rate of 150mL/min, and carrying out contact, mixing and reaction at the reaction temperature of 110 ℃ for 20min. And centrifugally separating and washing the reacted solution, drying at 80 ℃, and calcining at 300 ℃ for 2 hours.
The obtained nano zinc oxide is spherical particles, is uniformly distributed and has the diameter of about 40nm.
Example 5
The difference from example 2 is that: step (2) is eliminated. The step (3) is as follows: and (3) introducing the zinc sulfate solution into the microchannel reactor from the inlet 1 of the reactor at the flow rate of 150mL/min, and carrying out contact, mixing and reaction at the reaction temperature of 100 ℃ for 30min. And centrifugally separating and washing the reacted solution, drying at 80 ℃, and calcining at 300 ℃ for 2 hours.
The obtained nano zinc oxide is spherical particles, is uniformly distributed and has the diameter of about 41nm.
Example 6
The difference from example 3 is that: the concentration of the zinc acetate solution in the step (1) is 2mol/L; the step (2) is cancelled; the step (3) is as follows: and (3) introducing the zinc acetate solution into the microchannel reactor from the inlet 1 of the reactor at the flow rate of 300mL/min, and carrying out contact, mixing and reaction at the reaction temperature of 120 ℃ for 10min. And centrifugally separating and washing the reacted solution, drying at 80 ℃, and calcining at 300 ℃ for 2 hours.
The obtained nano zinc oxide is spherical particles, is uniformly distributed and has the diameter of about 26nm.
Example 7
The difference from example 1 is that: the concentration of the zinc acetate solution in the step (1) is 1mol/L; the step (2) is cancelled; the step (3) is as follows: and (3) introducing the zinc acetate solution into the microchannel reactor from the inlet 1 of the reactor at the flow rate of 200mL/min, and carrying out contact, mixing and reaction at the reaction temperature of 110 ℃ for 20min. And (3) performing centrifugal separation and cleaning on the solution after reaction, drying at 80 ℃, and calcining at 300 ℃ for 2 hours.
The obtained nano zinc oxide is spherical particles, is uniformly distributed and has the diameter of about 32nm.
Comparative example 1
The difference from example 1 is that: the step (3) adopts a kettle type reactor.
The SEM characterization result of the obtained nano zinc oxide is shown in figure 2. The morphology is uneven spherical particles with a diameter of about 150nm.
Comparative example 2
The differences from example 4 are: the flow rate in the step (3) is 500mL/min, the reaction temperature is 150 ℃, and the reaction time is 5min.
The obtained nano zinc oxide has irregular shape and diameter of about 100-500nm.
Comparative example 3
The difference from example 4 is that: the flow rate in the step (3) is 100mL/min, the reaction temperature is 80 ℃, and the reaction time is 40min.
The obtained nano zinc oxide has irregular shape and diameter of about 100-500nm.
The above description is only a preferred embodiment of the present patent, and it should be noted that, for those skilled in the art, several modifications and decorations can be made without departing from the inventive concept, and these modifications and decorations should also be regarded as the protection scope of the present patent.
Claims (10)
1. The preparation method of the nano zinc oxide is characterized by comprising the following steps: introducing the reaction liquid into a microchannel reactor for reaction to obtain reaction liquid A, and calcining the reaction liquid A to obtain the nano zinc oxide;
wherein the reaction solution comprises a zinc salt solution; the flow rate of the reaction liquid is 150-300mL/min; the structure of the microchannel reactor is a concentric circle structure.
2. The method for preparing nano zinc oxide according to claim 1, wherein the inner diameter of the pipeline of the microchannel reactor is 2-5mm, such as 4mm;
and/or the difference between the inner diameter and the outer diameter of the concentric circle structures of the microchannel reactor is 2-5mm, such as 4mm;
and/or the number of the concentric circles in the concentric circle structure of the microchannel reactor is 6-10, such as 8.
3. The method for preparing nano zinc oxide according to claim 1, wherein the reaction solution is a zinc salt solution;
alternatively, the reaction solution does not contain an alkaline substance.
4. The method for preparing nano zinc oxide according to claim 1, wherein the method for preparing the zinc salt solution comprises the following steps: mixing zinc salt with a solvent, and stirring to obtain a zinc salt solution; the stirring time is preferably 10-120min, such as 60min;
wherein, the zinc salt preferably comprises one or more of zinc sulfate, zinc chloride, zinc acetate and zinc nitrate, and more preferably zinc sulfate or zinc acetate;
wherein, the solvent is preferably glycol or water.
5. The method for preparing nano zinc oxide according to claim 1, wherein the concentration of the zinc salt solution is 0.2-2mol/L, such as 0.5mol/L, 1mol/L or 2mol/L;
and/or the flow rate of the reaction liquid is 180-250mL/min, such as 200mL/min;
and/or the temperature of the reaction is between 100 and 120 ℃, for example 110 ℃;
and/or the reaction time is 10-30min, such as 20min;
and/or the temperature of the calcination is 200-400 ℃, e.g., 300 ℃;
and/or the calcination time is 1 to 3 hours, for example 2 hours.
6. The method for preparing nano zinc oxide according to claim 1, wherein the reaction solution further comprises an alkaline substance; the reaction solution is preferably obtained by mixing a zinc salt solution and an alkali solution.
7. The method for preparing nano zinc oxide according to claim 6, wherein the method for preparing the alkali solution comprises the following steps: mixing an alkaline substance with a solvent, and stirring to obtain the alkaline solution; the stirring time is preferably 10-120min, such as 60min;
wherein, the alkaline substance preferably comprises one or more of sodium hydroxide, potassium hydroxide, sodium carbonate and ammonium carbonate;
wherein the solvent is preferably water.
8. The method for preparing nano zinc oxide according to claim 6, wherein the concentration of the alkali solution is 0.2 to 2mol/L, such as 0.5mol/L, 1mol/L or 2mol/L;
and/or the introduction flow rate of the alkali solution is 150-300mL/min.
9. The method for preparing nano zinc oxide according to claim 1, characterized in that the method further comprises the steps of separating, cleaning and drying in sequence after the reaction and before the calcination;
wherein the separation is preferably a centrifugal separation;
wherein the temperature of the drying is preferably 80 ℃.
10. The method for preparing nano zinc oxide according to claim 1, wherein the shape of the nano zinc oxide is spherical;
and/or the particle size of the nano zinc oxide is 25-50nm.
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| CN207237948U (en) * | 2017-08-03 | 2018-04-17 | 山东豪迈化工技术有限公司 | A kind of micro- reaction channel, substrate and microreactor |
| CN112777627A (en) * | 2021-01-13 | 2021-05-11 | 北京化工大学 | Preparation method of nano zinc oxide and nano zinc oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN207237948U (en) * | 2017-08-03 | 2018-04-17 | 山东豪迈化工技术有限公司 | A kind of micro- reaction channel, substrate and microreactor |
| CN112777627A (en) * | 2021-01-13 | 2021-05-11 | 北京化工大学 | Preparation method of nano zinc oxide and nano zinc oxide |
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