CN105565367A - Preparation method of nanometer zinc oxide powder material - Google Patents
Preparation method of nanometer zinc oxide powder material Download PDFInfo
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- CN105565367A CN105565367A CN201610066167.7A CN201610066167A CN105565367A CN 105565367 A CN105565367 A CN 105565367A CN 201610066167 A CN201610066167 A CN 201610066167A CN 105565367 A CN105565367 A CN 105565367A
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- C—CHEMISTRY; METALLURGY
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a preparation method of a nanometer zinc oxide powder material. The method includes the following steps of preparing a zinc acetate solution and a hexamethylenetetramine aqueous solution which have the same mole ratios, conducting ultrasonic mixing, regulating PH through acetic acid or sodium hydroxide, adding a surface active agent and a chemical-resistant modifying agent, evenly stirring the mixture, putting the mixture in a reaction kettle, conducting constant-temperature reaction for 3-6 hours, putting obtained zinc oxide sediment in a sintering furnace of 160-510 DEG C to be annealed for 1-4 hours after washing and drying the zinc oxide sediment, and modifying obtained nanometer zinc oxide powder. The obtained nanometer zinc oxide powder material grows on a central face; a high specific area is achieved; meanwhile, the transmission route is greatly shortened when electrons are transmitted on a plane, the electron hole recombination rate is easily decreased, and the utilization rate of photoproduction electrons is increased; and the obtained nanometer zinc oxide powder material has good dispersity and stability.
Description
Technical field
The present invention relates to technical field of nano material, be specifically related to a kind of preparation method of nanometer Zinc oxide powder material.
Background technology
Nano zine oxide is a kind of inorganic UV shield agent of excellent performance, is widely used in the fields such as sun care preparations, nano-function textile, functional plastics and coating.But nano zine oxide is a kind of inorganic oxide, its size is little, surface energy is high, be difficult to compatible with organic composition, very easily produces serious agglomeration.
Although simultaneously the particulate state nano zine oxide of general pattern has larger specific surface area, electronics is longer to the process path of electrode from pellet transportation, causes electronics not arrive electrode just and hole-recombination.In energy storage material, as in lithium ion battery, oarse-grained zinc oxide is unfavorable for the embedding deintercalation of lithium ion, particle often in charge and discharge cycles because volume change causes efflorescence etc., be unfavorable for improving the charge-discharge magnification of zinc oxide and electrode stability.
Summary of the invention
For solving the problem, the invention provides a kind of preparation method of nanometer Zinc oxide powder material, the nanometer Zinc oxide powder material of gained has dispersed and stability preferably.
For achieving the above object, the technical scheme that the present invention takes is:
A preparation method for nanometer Zinc oxide powder material, comprises the steps:
The zinc acetate solution of S1, preparation equimolar ratio and the hexamethylenetetramine aqueous solution;
S2, the zinc acetate solution that step S1 is prepared and the hexamethylenetetramine aqueous solution ultrasonic mixing 30-40min, after regulating PH to be 5.9-6.9 with acetic acid or sodium hydroxide, add tensio-active agent at 3: 1-1: 6 in molar ratio, and add chemicals-resistant properties-correcting agent stir at 10: 1-3: 1 in molar ratio;
S3, to be placed in by the solution of step S2 gained and to be provided with in teflon-lined reactor, 90-110 DEG C, 3-6 hour is carried out in isothermal reaction, obtains zinc oxide precipitate;
S4, by after the zinc oxide precipitate cleaning-drying of gained, be placed in the sintering oven anneal 1-4 hour of 160-510 DEG C, obtain nanometer Zinc oxide powder;
S5, the nanometer Zinc oxide powder of gained be impregnated in the normal hexane solvent of methyl-silicone oil, after stirring, evaporate to dryness, and be put in baking oven and carry out drying, obtain modified nano zinc oxide;
S6, the modified nano zinc oxide of gained is placed in retort furnace, under excess oxygen, with the ramp of 5-10 DEG C/min to 400-500 DEG C, keeps 3-6h, obtain nano zinc oxide material.
Preferably, described tensio-active agent is positively charged ion and nonionic surface active agent 1: 2 composite gained in molar ratio.
Preferably, described cationic surfactant is quaternary.
Preferably, described nonionic surface active agent is arlacels.
Preferably, described chemicals-resistant properties-correcting agent is fluorinated additive, and molecular weight is 1000-10000, can exist for liquid or solid form.
Preferably, described fluorinated additive is the acrylic acid series additive containing perfluoroalkyl.
Preferably, the volume ratio of described methyl-silicone oil and normal hexane solvent is 1: 3, and described nanometer Zinc oxide powder and the mass volume ratio of methyl-silicone oil are 2g: 7mL.
The present invention has following beneficial effect:
The nanometer Zinc oxide powder Material growth of gained is on a centerplane, and while having high-specific surface area, electronics transmission on the whole substantially reduces transmission route, is conducive to reducing electron-hole recombination rate, improves the utilization ratio of light induced electron; Carry out siliceous deposits modification on the surface of nano zine oxide, inhibit the stripping of nano zine oxide, improve the dispersiveness of nano zine oxide; Introduce the acrylic acid series additive of perfluoroalkyl as chemicals-resistant properties-correcting agent, the transport efficiency of this additive is high, can move to surface completely and form a kind of protective membrane, thus improve the stability of nano zine oxide in the process of preparation.
Embodiment
In order to make objects and advantages of the present invention clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
In following examples, the tensio-active agent used is positively charged ion and nonionic surface active agent 1: 2 composite gained in molar ratio.The cationic surfactant used is quaternary, and the nonionic surface active agent used is arlacels.The volume ratio of methyl-silicone oil and normal hexane solvent is 1: 3, and the mass volume ratio of nanometer Zinc oxide powder and methyl-silicone oil is 2g: 7mL.
Embodiment 1
The zinc acetate solution of S1, preparation equimolar ratio and the hexamethylenetetramine aqueous solution;
S2, the zinc acetate solution that step S1 is prepared and the hexamethylenetetramine aqueous solution ultrasonic mixing 30min, PH is regulated to be after 5.9 with acetic acid or sodium hydroxide, add tensio-active agent at 3: 1 in molar ratio, and add chemicals-resistant properties-correcting agent stir at 10: 1 in molar ratio; Described chemicals-resistant properties-correcting agent is the acrylic acid series additive containing perfluoroalkyl, and molecular weight is 1000, can exist for liquid or solid form.
S3, to be placed in by the solution of step S2 gained and to be provided with in teflon-lined reactor, 90 DEG C, isothermal reaction carries out 3 hours, obtains zinc oxide precipitate;
S4, by after the zinc oxide precipitate cleaning-drying of gained, be placed in the sintering oven anneal 1-4 hour of 160 DEG C, obtain nanometer Zinc oxide powder;
S5, the nanometer Zinc oxide powder of gained be impregnated in the normal hexane solvent of methyl-silicone oil, after stirring, evaporate to dryness, and be put in baking oven and carry out drying, obtain modified nano zinc oxide;
S6, the modified nano zinc oxide of gained is placed in retort furnace, under excess oxygen, with the ramp to 400 DEG C of 5 DEG C/min, keeps 3h, obtain nano zinc oxide material.
Embodiment 2
The zinc acetate solution of S1, preparation equimolar ratio and the hexamethylenetetramine aqueous solution;
S2, the zinc acetate solution that step S1 is prepared and the hexamethylenetetramine aqueous solution ultrasonic mixing 40min, be after 6.9 with acetic acid or sodium hydroxide adjustment PH, add tensio-active agent at 1: 6 in molar ratio, and add chemicals-resistant properties-correcting agent stir at 3: 1 in molar ratio; Described chemicals-resistant properties-correcting agent is the acrylic acid series additive containing perfluoroalkyl, and molecular weight is 10000, can exist for liquid or solid form.
S3, to be placed in by the solution of step S2 gained and to be provided with in teflon-lined reactor, 110 DEG C, isothermal reaction carries out 6 hours, obtains zinc oxide precipitate;
S4, by after the zinc oxide precipitate cleaning-drying of gained, be placed in the sintering oven anneal 4 hours of 510 DEG C, obtain nanometer Zinc oxide powder;
S5, the nanometer Zinc oxide powder of gained be impregnated in the normal hexane solvent of methyl-silicone oil, after stirring, evaporate to dryness, and be put in baking oven and carry out drying, obtain modified nano zinc oxide;
S6, the modified nano zinc oxide of gained is placed in retort furnace, under excess oxygen, with the ramp to 500 DEG C of 10 DEG C/min, keeps 6h, obtain nano zinc oxide material.
Embodiment 3
The zinc acetate solution of S1, preparation equimolar ratio and the hexamethylenetetramine aqueous solution;
S2, the zinc acetate solution that step S1 is prepared and the hexamethylenetetramine aqueous solution ultrasonic mixing 30-40min, PH is regulated to be after 6 with acetic acid or sodium hydroxide, add tensio-active agent at 19: 12 in molar ratio, and add chemicals-resistant properties-correcting agent stir at 7: 1 in molar ratio; Described chemicals-resistant properties-correcting agent is the acrylic acid series additive containing perfluoroalkyl, and molecular weight is 5500, can exist for liquid or solid form.
S3, to be placed in by the solution of step S2 gained and to be provided with in teflon-lined reactor, 100 DEG C, isothermal reaction carries out 4.5 hours, obtains zinc oxide precipitate;
S4, by after the zinc oxide precipitate cleaning-drying of gained, be placed in the sintering oven anneal 2.5 hours of 335 DEG C, obtain nanometer Zinc oxide powder;
S5, the nanometer Zinc oxide powder of gained be impregnated in the normal hexane solvent of methyl-silicone oil, after stirring, evaporate to dryness, and be put in baking oven and carry out drying, obtain modified nano zinc oxide;
S6, the modified nano zinc oxide of gained is placed in retort furnace, under excess oxygen, with the ramp to 450 DEG C of 7.5 DEG C/min, keeps 4.5h, obtain nano zinc oxide material
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. a preparation method for nanometer Zinc oxide powder material, is characterized in that, comprises the steps:
The zinc acetate solution of S1, preparation equimolar ratio and the hexamethylenetetramine aqueous solution;
S2, the zinc acetate solution that step S1 is prepared and the hexamethylenetetramine aqueous solution ultrasonic mixing 30-40min, after regulating PH to be 5.9-6.9 with acetic acid or sodium hydroxide, add tensio-active agent at 3: 1-1: 6 in molar ratio, and add chemicals-resistant properties-correcting agent stir at 10: 1-3: 1 in molar ratio;
S3, to be placed in by the solution of step S2 gained and to be provided with in teflon-lined reactor, 90-110 DEG C, 3-6 hour is carried out in isothermal reaction, obtains zinc oxide precipitate;
S4, by after the zinc oxide precipitate cleaning-drying of gained, be placed in the sintering oven anneal 1-4 hour of 160-510 DEG C, obtain nanometer Zinc oxide powder;
S5, the nanometer Zinc oxide powder of gained be impregnated in the normal hexane solvent of methyl-silicone oil, after stirring, evaporate to dryness, and be put in baking oven and carry out drying, obtain modified nano zinc oxide;
S6, the modified nano zinc oxide of gained is placed in retort furnace, under excess oxygen, with the ramp of 5-10 DEG C/min to 400-500 DEG C, keeps 3-6h, obtain nano zinc oxide material.
2. the preparation method of a kind of nanometer Zinc oxide powder material according to claim 1, is characterized in that, described tensio-active agent is positively charged ion and nonionic surface active agent 1: 2 composite gained in molar ratio.
3. the preparation method of a kind of nanometer Zinc oxide powder material according to claim 2, is characterized in that, described cationic surfactant is quaternary.
4. the preparation method of a kind of nanometer Zinc oxide powder material according to claim 2, is characterized in that, described nonionic surface active agent is arlacels.
5. the preparation method of a kind of nanometer Zinc oxide powder material according to claim 1, is characterized in that, described chemicals-resistant properties-correcting agent is fluorinated additive, and molecular weight is 1000-10000, can exist for liquid or solid form.
6. the preparation method of a kind of nanometer Zinc oxide powder material according to claim 5, is characterized in that, described fluorinated additive is the acrylic acid series additive containing perfluoroalkyl.
7. the preparation method of a kind of nanometer Zinc oxide powder material according to claim 1, is characterized in that, the volume ratio of described methyl-silicone oil and normal hexane solvent is 1: 3, and described nanometer Zinc oxide powder and the mass volume ratio of methyl-silicone oil are 2g: 7mL.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109825112A (en) * | 2019-03-22 | 2019-05-31 | 河南大学 | A kind of perfluorocarboxylic acid modification zinc oxide nanoparticle and its preparation method and application |
| CN111261400A (en) * | 2020-03-31 | 2020-06-09 | 哈尔滨学院 | Preparation method of magnetic nano material |
| CN111573713A (en) * | 2020-06-29 | 2020-08-25 | 陕西延长石油（集团）有限责任公司 | Synthesis method and application of controllable growth of crystal face of nano zinc oxide |
| CN112777629A (en) * | 2021-03-24 | 2021-05-11 | 洛阳理工学院 | Nano zinc oxide modification method by using double carboxylate anionic surfactant |
| CN114656824A (en) * | 2022-04-15 | 2022-06-24 | 肇庆市盛浩新材料科技有限公司 | Modified nano zinc oxide powder and preparation method and application thereof |
| CN115028191A (en) * | 2022-07-26 | 2022-09-09 | 宣城晶瑞新材料有限公司 | Preparation method of composite nano zinc oxide |
| CN118652734A (en) * | 2024-05-28 | 2024-09-17 | 嘉善江南纺织材料股份有限公司 | A water-repellent automobile cleaning agent and preparation method thereof |
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| CN109825112A (en) * | 2019-03-22 | 2019-05-31 | 河南大学 | A kind of perfluorocarboxylic acid modification zinc oxide nanoparticle and its preparation method and application |
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| CN111261400A (en) * | 2020-03-31 | 2020-06-09 | 哈尔滨学院 | Preparation method of magnetic nano material |
| CN111573713A (en) * | 2020-06-29 | 2020-08-25 | 陕西延长石油（集团）有限责任公司 | Synthesis method and application of controllable growth of crystal face of nano zinc oxide |
| CN112777629A (en) * | 2021-03-24 | 2021-05-11 | 洛阳理工学院 | Nano zinc oxide modification method by using double carboxylate anionic surfactant |
| CN114656824A (en) * | 2022-04-15 | 2022-06-24 | 肇庆市盛浩新材料科技有限公司 | Modified nano zinc oxide powder and preparation method and application thereof |
| CN114656824B (en) * | 2022-04-15 | 2023-08-11 | 肇庆市盛浩新材料科技有限公司 | Modified nano zinc oxide powder and preparation method and application thereof |
| CN115028191A (en) * | 2022-07-26 | 2022-09-09 | 宣城晶瑞新材料有限公司 | Preparation method of composite nano zinc oxide |
| CN115028191B (en) * | 2022-07-26 | 2024-03-01 | 宣城晶瑞新材料有限公司 | Preparation method of composite nano zinc oxide |
| CN118652734A (en) * | 2024-05-28 | 2024-09-17 | 嘉善江南纺织材料股份有限公司 | A water-repellent automobile cleaning agent and preparation method thereof |
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