CN105271363A - Preparation method of superfine zinc oxide powder - Google Patents
Preparation method of superfine zinc oxide powder Download PDFInfo
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- CN105271363A CN105271363A CN201510738118.9A CN201510738118A CN105271363A CN 105271363 A CN105271363 A CN 105271363A CN 201510738118 A CN201510738118 A CN 201510738118A CN 105271363 A CN105271363 A CN 105271363A
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Abstract
The invention discloses a preparation method of superfine zinc oxide powder. According to the method, crude particle zinc oxide or metal zinc is used as raw materials; an organic zinc salt solution is generated through organic dissolution; oxalic acid is added to generate zinc oxalate sediments; filtering is performed to obtain zinc oxalate solids and organic acid; organic acid is used as a raw material for dissolving the crude particle zinc oxide or metal zinc in the next batch; the zinc oxalate is calcined to obtain uniform-particle zinc oxide powder. The method has the advantages that no waste liquid or waste solids are discharged in the preparation process; the average grain diameter of particles of the obtained zinc oxide powder is in a range being 30 to 200nm and can be regulated through the raw material proportion.
Description
Technical field
The invention belongs to superfine powdery material preparation field, relate to a kind of preparation method of eco-friendly super fine zinc oxide powder.
Background technology
Zinc oxide powder is a kind of white powder, and have high refractive index, excellent thermal conductivity, antibacterial and uvioresistant character, purposes is very extensive.In fields such as plastics, synthetic rubber, coating, papermaking, zinc oxide is widely used as covering agent, tinting material, is commonly called as zinc white; In the sunscreen of makeup, zinc oxide, as sun-screening agent, plays and intercepts ultraviolet effect.The normal temperature luminescent properties of zinc oxide excellence, is also used widely at semiconductor applications, as all having application in the products such as liquid-crystal display, thin film transistor, photodiode.At food and field of medicaments, zinc oxide uses as nutrition-fortifying agent, antiseptic-germicide, astringent matter.On chemical industry also useful zinc oxide as the composition of sweetening agent.
The application of zinc oxide in above-mentioned different field is distributed with certain requirement often to particle diameter and particle diameter.The such as application of zinc oxide in coating, general employing micron order zinc oxide; And as antibacterial use, in general the less antibacterial effect of particle diameter is better; And as sun-screening agent, general requirement particle diameter is more suitable at about 100nm.The general narrow ditribution of size distribution of zinc oxide product needs more, because narrow ditribution gives particle comparatively unified performance.
The production method of common zinc oxide has direct method, indirect method and wet method.
Method that direct method also claims " Webster stove ", because first appearing at the U.S., also known as " U.S. law ".Direct method produces zinc oxide, and advantage is that cost is lower, and thermo-efficiency is high.Containing the raw material of zinc at 1000 ~ 1200 DEG C, be that main carbonaceous material reduces by coal.They are imported oxidation furnaces, oxidizing reaction are carried out completely by the zinc fume contained in burning gas and CO, then through over-heat-exchanger, enter cloth bag separator and collect finished product after cooling.The zinc oxide that direct method is produced is acicular structure, is micron industrial level zinc oxide.American process zinc oxide preparation process impurity is not separated completely, and whiteness is bad, and the price that market is sold is also lower.
Indirect method originates from France, also referred to as " method national law ".Industrial, indirect method is produced ZnO and first spelter at high temperature melting is flashed to zinc fume, and then oxidation generates ZnO.The purity of product is relevant with spelter purity used.
In above-mentioned two kinds of methods, direct method does not have dedoping step, and the purity zinc oxide of production is not very high, and particle size and distribution do not have conservative control yet; Indirect method adopts high-purity zinc ingot metal to be that raw material can obtain highly purified zinc oxide, but particle diameter is generally about micron order, and size distribution is also very wide.
In order to improve the quality of zinc oxide, people have employed a lot of method and improve.Wet production zinc oxide is a kind of common method.The zinc oxide specific surface area that these class methods are produced is large, so be also called active ZnO.
Common wet oxidation zinc preparation process is with zinc sulfate ZnSO
4or zinc chloride ZnCl
2for raw material, through removing impurity, add sodium carbonate Na
2cO
3solution, generates zinc subcarbonate Zn
2(OH)
2cO
3precipitation, again through rinsing repeatedly, filtration, removing foreign ion, mainly remove sulfate ion or chlorion, sodium ion etc., water lotion ionic strength constantly declines along with water washing process, be reduced to a certain degree, then drying, high-temperature roasting obtain ZnO, this method also claims sodium carbonate method.The Zinc oxide powder purity that wet method obtains not only depends on zinc sulfate ZnSO
4or zinc chloride ZnCl
2raw material, also depends on the degree of washing.If wash insufficient, will residual sulphate or chlorion, sodium ion, finally affect the quality of zinc oxide product.In wet method except adopting sodium carbonate precipitation agent, adopt sodium bicarbonate, ammonium oxalate, urea etc. in addition, adopt the object of these precipitation agents mainly to control precipitin reaction, and then control size and the distribution of final zinc oxide particle diameter.But no matter adopt what precipitation agent, the washing in process keeps away unavoidable.Water washing process water loss is very large, water loss be the 10-100 of product weight doubly, need recycling utilization or process discharge, the ionogen washed out concentrates, crystallization, process be all very large consumption and a difficult problem, water washing process brings a lot of trouble to wet chemistry method.Such technique produces a large amount of refuses, and power consumption is large, does not meet the theory of green low-carbon.
Austrian patent (AuspitzerOtto.Zinkoxyd:AT, 176207 [P] .1953-09-25) report a kind of method, the coarse particles zinc oxide high by purity prepares zinc subcarbonate with carbon dioxide reaction under hydrothermal conditions, and then obtains Zinc oxide particles through calcining.Namely in the autoclave pressure containing water and high-purity tutty particle, pass into carbon dioxide, keep certain temperature and pressure, when reaction proceeds to certain zinc carbonate content, isolate zinc subcarbonate, then drying, calcining obtain particle diameter about 0.05 μm, narrow diameter distribution, active zinc flower powder that purity is high.All clearly, to the advantages and disadvantages of this method advantage to introduce foreign ion, and product purity is high, the prior environmental stress being that of avoiding water washing process and bringing; Shortcoming needs to carry out at elevated pressures, and facility investment is large, operation inconvenience, then to have be adopt carbon dioxide to be raw material, and high-purity carbon dioxide gas is not only originated inconvenience, and needs to compress charging.
The zinc oxide preparation method of research report also has a lot, as adopted solid-phase grinding, microwave field radiant heating, induction heating method, plasma heating method, electron beam heating and LASER HEATING method, sputtering method, gravity Method, microemulsion method etc., these method general operation inconvenience, be not suitable for large-scale industrial production, only rest on the experimental phase.
Summary of the invention
The object of the present invention is to provide a kind of method preparing super fine zinc oxide powder, described method is applicable to large-scale production, does not need water washing process, and do not have liquid debris and solid waste discharge, product cut size is evenly distributed, size controllable.
For achieving the above object, the present invention adopts following technical scheme: add in organic acid soln by coarse particles Zinc oxide powder or metallic zinc, transparent liquid is dissolved completely to Zinc oxide particles or metallic zinc, add oxalic acid again, generate precipitation, filter and be precipitated thing and filtrate, throw out is zinc oxalate, by throw out at 80-300 DEG C of dry white powder, wherein the dry gas phase portion condensation produced is reclaimed and is merged with filtrate; Dried powder, at 400-600 DEG C of temperature lower calcination 1-4 hour, obtains zinc oxide ultra-fine powder, and the filtrate of merging is organic acid soln, reuses, and is directly used in lower batch and dissolves tutty particle or metallic zinc.
It is that organic acid can select acetic acid, formic acid, phenylformic acid, lactic acid etc., or their mixture in order to dissolve tutty or metallic zinc that organic acid of the present invention adds.Organic acid add-on is to be converted into the aqueous solution of organic zinc salt completely for benchmark by metallic zinc or zinc oxide, excessive organic acid can accelerate dissolution process, but excessively there is no need equally too much, therefore suitable ratio is ZnO or Zn: organic acid (mol ratio)=1:2-1:3.
The inventive method, organic acid soln is quantitative recovery substantially, and whole preparation process does not produce waste water and solid waste.
The precipitation agent that the present invention uses is band crystal water or the oxalic acid not with crystal water.
The even particle size distribution of the super fine zinc oxide powder obtained by the inventive method, and size is controlled.Applicant finds, the median size of super fine zinc oxide product regulates by the mol ratio adjusting metallic zinc or zinc oxide and the oxalic acid added, and can obtain average particle size is 30-200nm super fine zinc oxide, and preferable particle size is at 50-150nm.Adjustment ZnO or Zn and oxalic acid proportioning (mol ratio) are 0.5-1.5:1, preferably 0.8 ~ 1.2:1, can obtain the zinc oxide requiring particle diameter, table 1 lists zinc oxide particles Average Particle Diameters under different ZnO or Zn and oxalic acid proportioning (mol ratio).
Table 1
| ZnO or Zn: oxalic acid (mol ratio) | Median size (unit: nm; Deviation ± 5) |
| 0.8 | 50 |
| 0.9 | 85 |
| 1.0 | 100 |
| 1.1 | 120 |
| 1.2 | 140 |
Beneficial effect: the preparation method of super fine zinc oxide powder of the present invention, without waste liquid, the useless solid discharge of nothing in the process preparing super fine zinc oxide, zinc oxide product size tunable, even particle size distribution.The present invention is suitable for large-scale industrial production, solve traditional precipitator method and prepare a large amount of useless water problem of generation in super fine zinc oxide process, do not produce other solid waste simultaneously yet, environmentally friendly, institute's product cut size that obtains is controlled, because not adding other auxiliary agents, impurity is few, can meet the application in the fields such as daily use chemicals, coating, rubber, electronics, absorbing material.
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not limited with embodiment, but is limited by claim.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
The Zinc oxide particles electromicroscopic photograph that Fig. 2 embodiment 1 is obtained.
In Fig. 3 embodiment 1, filtrate applies mechanically rear obtained Zinc oxide particles electromicroscopic photograph.
The Zinc oxide particles electromicroscopic photograph that Fig. 4 embodiment 2 is obtained.
In Fig. 5 embodiment 2, filtrate applies mechanically rear obtained Zinc oxide particles electromicroscopic photograph.
The Zinc oxide particles electromicroscopic photograph that Fig. 6 embodiment 3 is obtained.
In Fig. 7 embodiment 3, filtrate applies mechanically rear obtained Zinc oxide particles electromicroscopic photograph.
The Zinc oxide particles electromicroscopic photograph that Fig. 8 embodiment 4 is obtained.
In Fig. 9 embodiment 4, filtrate applies mechanically rear obtained Zinc oxide particles electromicroscopic photograph.
The Zinc oxide particles electromicroscopic photograph that Figure 10 embodiment 5 is obtained.
In Figure 11 embodiment 5, filtrate applies mechanically rear obtained Zinc oxide particles electromicroscopic photograph.
The Zinc oxide particles electromicroscopic photograph that Figure 12 embodiment 6 is obtained.
In Figure 13 embodiment 6, filtrate applies mechanically rear obtained Zinc oxide particles electromicroscopic photograph.
The Zinc oxide particles electromicroscopic photograph that Figure 14 embodiment 7 is obtained.
In Figure 15 embodiment 7, filtrate applies mechanically rear obtained Zinc oxide particles electromicroscopic photograph.
Embodiment
Below by specific embodiment, technical solutions according to the invention are further described in detail, but are necessary to point out that following examples are only for the description to summary of the invention, do not form limiting the scope of the invention.
Embodiment 1
27.67 kilograms of (340 moles) coarse particles Zinc oxide powders slowly add 242.86 liters, concentration is (containing acetic acid 680 moles) in 2.8mol/L acetum, stir lower Zinc oxide particles and dissolve transparent liquid gradually completely, add two oxalic acid hydrates (340 moles) of 42.86 kilograms again, adularescent precipitation generates, and filters and is precipitated cake and filtrate.
Precipitated filter cakes is at 105 DEG C of dry white powders.The white powder that drying obtains was 500-600 DEG C of temperature lower calcination 1.5 hours, and obtaining median size is 100 nanometer Zinc oxide powder 27 kilograms.Powder electromicroscopic photograph is shown in Fig. 2.
Filtrate test acidity, adds the Glacial acetic acid of metering and water and forms 242.86 liters of 2.8mol/L concentration acetums and apply mechanically, and repeating said process, to obtain median size be 101 nano zine oxide superfine powder 27 kilograms.Powder electromicroscopic photograph is shown in Fig. 3.
Embodiment 2
27.67 kilograms of (340 moles) coarse particles Zinc oxide powders slowly add 242.86 liters, concentration is (containing 728.6 moles, phenylformic acid) in 3.0mol/L benzoic acid solution, stir lower Zinc oxide particles and dissolve transparent liquid gradually completely, add two oxalic acid hydrates (340 moles) of 42.86 kilograms again, adularescent precipitation generates, and filters and is precipitated thing and filtrate.
Precipitated filter cakes is at 105 DEG C of dry white powders.The white powder that drying obtains was 500-600 DEG C of temperature lower calcination 2 hours, and obtaining median size is 103 nano zine oxide superfine powder 27.67 kilograms.Powder electromicroscopic photograph is shown in Fig. 4.
Filtrate test acidity, adds the phenylformic acid of metering and water and forms 242.86 liters of 3.0mol/L concentration benzoic acid solutions and apply mechanically, and repeating said process, to obtain median size be 98nm zinc oxide ultra-fine powder 27.67 kilograms.Powder electromicroscopic photograph is shown in Fig. 5.
Embodiment 3
27.67 kilograms of (340 moles) coarse particles Zinc oxide powders slowly add 242.86 liters, concentration is (containing acetic acid 816 moles) in 3.36mol/L acetum, stir lower Zinc oxide particles and dissolve transparent liquid gradually completely, add two oxalic acid hydrates (306 moles) of 38.57 kilograms again, adularescent precipitation generates, and filters and is precipitated thing and filtrate.
Precipitated filter cakes is at 105 DEG C of dry white powders.The white powder that drying obtains was 500-600 DEG C of temperature lower calcination 4 hours, and obtaining median size is 85 nano zine oxide superfine powder 27 kilograms.Powder electromicroscopic photograph is shown in Fig. 6.
Filtrate test acidity, adds the acetic acid of metering and water and forms 242.86 liters of 2.8mol/L concentration acetums and apply mechanically, and repeating said process, to obtain median size be 87 nano zine oxide superfine powder 27 kilograms.Powder electromicroscopic photograph is shown in Fig. 7.
Embodiment 4
27.67 kilograms of (340 moles) coarse particles Zinc oxide powders slowly add 242.86 liters, concentration is (containing 748 moles, formic acid) in 3.08mol/L formic acid solution, stir lower Zinc oxide particles and dissolve transparent liquid gradually completely, add two oxalic acid hydrates (374 moles) of 47.15 kilograms again, adularescent precipitation generates, and filters and is precipitated thing and filtrate.
Precipitated filter cakes part is at 105 DEG C of dry white powders.The white powder that drying obtains was 500-600 DEG C of temperature lower calcination 2 hours, and obtaining median size is 121 nano zine oxide superfine powder 27 kilograms.Powder electromicroscopic photograph is shown in Fig. 8.
Filtrate test acidity, adds the formic acid of metering and water and forms 242.86 liters of 2.8mol/L concentration formic acid solutions and apply mechanically, and repeating said process, to obtain median size be 123 nano zine oxide superfine powder 27 kilograms.Powder electromicroscopic photograph is shown in Fig. 9.
Embodiment 5
27.67 kilograms of (340 moles) coarse particles Zinc oxide powders slowly add 242.86 liters, concentration is (containing lactic acid 680 moles) in 2.8mol/L lactic acid solution, stir lower Zinc oxide particles and dissolve transparent liquid gradually completely, add two oxalic acid hydrates (374 moles) of 47.15 kilograms again, adularescent precipitation generates, and filters and is precipitated thing and filtrate.
Precipitated filter cakes part is at 105 DEG C of dry white powders.The white powder that drying obtains was 500-600 DEG C of temperature lower calcination 2 hours, and obtaining median size is 141 nano zine oxide superfine powder 27.67 kilograms.Powder electromicroscopic photograph is shown in Figure 10.
Filtrate test acidity, adds the lactic acid of metering and water and forms 242.86 liters of 2.8mol/L concentration lactic acid solutions and apply mechanically, and repeating said process, to obtain median size be 138 nano zine oxide superfine powder 27.67 kilograms.Powder electromicroscopic photograph is shown in Figure 11.
Embodiment 6
27.67 kilograms of (340 moles) coarse particles Zinc oxide powders slowly add 242.86 liters, concentration is (containing acetic acid 741.2 moles) in 3.052mol/L acetum, stir lower Zinc oxide particles and dissolve transparent liquid gradually completely, add two oxalic acid hydrates (272 moles) of 34.29 kilograms again, adularescent precipitation generates, and filters and is precipitated thing and filtrate.
Precipitated filter cakes part is at 105 DEG C of dry white powders.The white powder that drying obtains was 500-600 DEG C of temperature lower calcination 1 hour, and obtaining median size is 55 nano zine oxide superfine powder 27.67 kilograms.Powder electromicroscopic photograph is shown in Figure 12.
Filtrate test acidity, adds the Glacial acetic acid of metering and water and forms 242.86 liters of 2.8mol/L concentration acetums and apply mechanically, and repeating said process, to obtain median size be 54 nano zine oxide superfine powder 27.67 kilograms.Powder electromicroscopic photograph is shown in Figure 13.
Embodiment 7
22.23 kilograms of (340 moles) zinc powders slowly add 242.86 liters, concentration is (containing 510 moles, formic acid, 510 moles, phenylformic acid) in 4.2mol/L formic acid and phenylformic acid mixing solutions, stir lower Zinc oxide particles and dissolve transparent liquid gradually completely, add two oxalic acid hydrates (374 moles) of 47.15 kilograms again, adularescent precipitation generates, and filters and is precipitated thing and filtrate.
Precipitated filter cakes is at 105 DEG C of dry white powders.The white powder that drying obtains was 500-600 DEG C of temperature lower calcination 4 hours, and obtaining median size is 116 nano zine oxide superfine powder 27 kilograms.Powder electromicroscopic photograph is shown in Figure 14.
Filtrate test acidity, adds the formic acid of metering and water and forms 242.86 liters of 2.8mol/L concentration formic acid solutions and apply mechanically, and repeating said process, to obtain median size be 117 nano zine oxide superfine powder 27 kilograms.Powder electromicroscopic photograph is shown in Figure 15.
Claims (8)
1. a preparation method for super fine zinc oxide powder, is characterized in that, adds in organic acid soln by coarse particles Zinc oxide powder or metallic zinc, forms organic zinc salt solution, then adds oxalic acid generation white precipitate, filters and is precipitated thing and filtrate; Throw out is zinc oxalate, throw out is carried out drying, calcining obtains super fine zinc oxide powder; Filtrate is organic acid soln, reuses.
2. the preparation method of super fine zinc oxide powder according to claim 1, is characterized in that, the temperature of described drying is 80-300 DEG C, and the dry condensable gases produced reclaims through condensation and is merged in organic acid soln.
3. the preparation method of super fine zinc oxide powder according to claim 1, is characterized in that, the temperature of described calcining is 400-600 DEG C, time 1-4 hour.
4. the preparation method of super fine zinc oxide powder according to claim 1, is characterized in that, described organic acid is selected from one or more in acetic acid, formic acid, phenylformic acid or lactic acid.
5. the preparation method of super fine zinc oxide powder according to claim 1, is characterized in that, described organic acid consumption is, coarse particles zinc oxide or zinc and organic acid mole ratio are 1:2 ~ 1:3.
6. the preparation method of super fine zinc oxide powder according to claim 1, is characterized in that, described oxalic acid add-on is, the mol ratio of coarse particles zinc oxide or zinc and oxalic acid is 0.5 ~ 1.5:1.
7. the preparation method of super fine zinc oxide powder according to claim 6, is characterized in that, described coarse particles zinc oxide or the mol ratio of zinc and oxalic acid are 0.8 ~ 1.2:1.
8. the preparation method of super fine zinc oxide powder according to claim 1, is characterized in that, the average particle size range of super fine zinc oxide powder particle prepared by described method is in 30 nanometer to 200 nanometers.
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| CN201510738118.9A CN105271363B (en) | 2015-08-14 | 2015-11-03 | A kind of preparation method of super fine zinc oxide powder |
| PCT/CN2016/084924 WO2017075990A1 (en) | 2015-08-14 | 2016-06-06 | Method for preparing superfine zinc oxide powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105819492A (en) * | 2016-03-17 | 2016-08-03 | 安徽颖达锌业发展有限公司 | Preparation method of ultrafine zinc oxide powder |
| WO2017075990A1 (en) * | 2015-08-14 | 2017-05-11 | 南京华狮新材料有限公司 | Method for preparing superfine zinc oxide powder |
| CN107624788A (en) * | 2017-09-20 | 2018-01-26 | 山东星美新材料股份有限公司 | A kind of Nano composite granules, its preparation method and the application of antibacterial and mouldproof smelly eliminating |
| CN115820117A (en) * | 2023-01-10 | 2023-03-21 | 福州大学 | Antibacterial super-hydrophobic composite coating and preparation method thereof |
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| CN113716600A (en) * | 2021-09-24 | 2021-11-30 | 石家庄志亿锌业有限公司 | Preparation method of nano zinc oxide |
| CN114479184A (en) * | 2022-02-28 | 2022-05-13 | 江苏爱特恩高分子材料有限公司 | Preparation method of high-dispersion zinc oxide |
| CN115120613B (en) * | 2022-05-18 | 2023-09-29 | 山东鲁西药业有限公司 | Preparation method and application of calamine powder |
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| RU2206508C1 (en) * | 2002-01-23 | 2003-06-20 | Мельникова Нина Борисовна | Zinc oxide production process |
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| JPH0350119A (en) * | 1989-07-19 | 1991-03-04 | Mitsubishi Materials Corp | Production of fine zinc oxide particles |
| CN102070182B (en) * | 2009-11-21 | 2012-08-22 | 中国科学院合肥物质科学研究院 | Porous zinc oxide micro powder and preparation method and application thereof |
| CN102161501B (en) * | 2011-02-24 | 2012-11-07 | 北京科技大学 | Method for preparing zinc oxalate with pearl luster and zinc oxide powder with pearl luster |
| CN105271363B (en) * | 2015-08-14 | 2017-12-22 | 南京华狮化工有限公司 | A kind of preparation method of super fine zinc oxide powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2206508C1 (en) * | 2002-01-23 | 2003-06-20 | Мельникова Нина Борисовна | Zinc oxide production process |
| CN1418818A (en) * | 2002-12-23 | 2003-05-21 | 崔春芳 | Tech. for prepn. of nano zinc oxide powder |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017075990A1 (en) * | 2015-08-14 | 2017-05-11 | 南京华狮新材料有限公司 | Method for preparing superfine zinc oxide powder |
| CN105819492A (en) * | 2016-03-17 | 2016-08-03 | 安徽颖达锌业发展有限公司 | Preparation method of ultrafine zinc oxide powder |
| CN107624788A (en) * | 2017-09-20 | 2018-01-26 | 山东星美新材料股份有限公司 | A kind of Nano composite granules, its preparation method and the application of antibacterial and mouldproof smelly eliminating |
| CN115820117A (en) * | 2023-01-10 | 2023-03-21 | 福州大学 | Antibacterial super-hydrophobic composite coating and preparation method thereof |
| CN115820117B (en) * | 2023-01-10 | 2023-08-01 | 福州大学 | Antibacterial super-hydrophobic composite coating and preparation method thereof |
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| CN105271363B (en) | 2017-12-22 |
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