CN105271363B - A kind of preparation method of super fine zinc oxide powder - Google Patents
A kind of preparation method of super fine zinc oxide powder Download PDFInfo
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- CN105271363B CN105271363B CN201510738118.9A CN201510738118A CN105271363B CN 105271363 B CN105271363 B CN 105271363B CN 201510738118 A CN201510738118 A CN 201510738118A CN 105271363 B CN105271363 B CN 105271363B
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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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- 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
Abstract
The invention discloses a kind of preparation method of super fine zinc oxide powder, using coarse granule zinc oxide or metallic zinc as raw material, dissolves generation organic acid zinc salting liquid by organic acid, adds oxalic acid generation zinc oxalate precipitation.Zinc oxalate solid and organic acid are filtrated to get, organic acid set is used as lower batch dissolving coarse granule zinc oxide or the raw material of metallic zinc, zinc oxalate obtain evengranular Zinc oxide powder through calcining.Without waste liquid, useless solid discharge, obtained Zinc oxide powder average particle size can be adjusted the inventive method preparation process in the range of 30 200nm by raw material proportioning.
Description
Technical field
The invention belongs to superfine powdery material preparation field, is related to a kind of preparation of environment-friendly super fine zinc oxide powder
Method.
Background technology
Zinc oxide powder is a kind of white powder, has high index of refraction, excellent thermal conductivity, antibacterial and uviolresistance
Matter, purposes are quite varied.In fields such as plastics, synthetic rubber, coating, papermaking, zinc oxide is widely used as covering agent, coloring
Agent, it is commonly called as zinc white；In the suncream of cosmetics, zinc oxide plays a part of obstructing ultraviolet as sun-screening agent.Zinc oxide is excellent
Different normal temperature luminescent properties, are also used widely in semiconductor applications, such as liquid crystal display, thin film transistor (TFT), light-emitting diodes
There is application in the products such as pipe.In food and field of medicaments, zinc oxide uses as nutrition fortifier, antiseptic, astringent.Change
Learn industrial composition of the also useful zinc oxide as desulfurizing agent.
Often certain requirement is distributed with to particle diameter and particle diameter in application of the zinc oxide in above-mentioned different field.Such as oxygen
Change application of the zinc in coating, typically use micron order zinc oxide；And used as antibacterial, in general the smaller antibacterial of particle diameter is imitated
Fruit is better；And be used as sun-screening agent, typically require that particle diameter is more suitable in 100nm or so.The particle diameter distribution one of zinc oxide product
As narrow ditribution more need because narrow ditribution assigns particle more unified performance.
The production method of common zinc oxide has direct method, indirect method and wet method.
Direct method is also referred to as " Webster stove " method, because primarily occur inning the U.S., also known as " U.S. law ".Direct method produces zinc oxide,
Advantage is that cost is relatively low, and the thermal efficiency is high.Raw material containing zinc is reduced at 1000~1200 DEG C by the carbonaceous material based on coal.
The zinc fume and CO contained in combustion gas, is introduced into oxidation furnaces, oxidation reaction is carried out completely, then by heat exchange
Device, cloth bag separator is entered after cooling and collects finished product.The zinc oxide of direct method production is acicular texture, is micron industrial level oxygen
Change zinc.American process zinc oxide preparation process impurity is not separated completely, and whiteness is bad, price on the market also compared with
It is low.
Indirect method is also referred to as " method national law " originating from France.Industrially, indirect method production ZnO is first by spelter in high temperature
It is lower melting and flash to zinc fume, and then aoxidize generation ZnO.The purity of product is relevant with spelter purity used.
In above two method, direct method does not have a dedoping step, the purity zinc oxide of production be not it is very high, particle size and
Distribution does not also control rationally；Indirect method uses high-purity zinc ingot metal that the zinc oxide of high-purity, but particle diameter one can be made for raw material
As it is also very wide in micron order or so, particle diameter distribution.
In order to improve the quality of zinc oxide, people employ many methods and are improved.Wet production zinc oxide is common
A kind of method.The zinc oxide specific surface area of this kind of method production is big, so also referred to as active ZnO.
Common wet oxidation zinc preparation process is with zinc sulfate ZnSO4Or zinc chloride ZnCl2For raw material, through going the removal of impurity,
Add sodium carbonate Na2CO3Solution, generation basic zinc carbonate Zn2(OH)2CO3Precipitation, then by rinsing, filtering repeatedly, remove impurity
Ion, mainly removes sulfate ion or chlorion, sodium ion etc., and water lotion ionic strength is carried out constantly with water-washing process
Decline, after reducing to a certain extent, then through drying, high-temperature roasting obtain ZnO, this method is also referred to as sodium carbonate method.What wet method obtained
Zinc oxide powder purity depends not only on zinc sulfate ZnSO4Or zinc chloride ZnCl2Raw material, additionally depend on the degree of washing.If water
Wash it is insufficient, will residual sulphate or chlorion, sodium ion, the final quality for influenceing zinc oxide product.Except adopting in wet method
With outside sodium carbonate precipitating reagent, also using sodium acid carbonate, ammonium oxalate, urea etc., mainly controlled using the purpose of these precipitating reagents
Precipitation reaction processed, and then control size and the distribution of final zinc oxide particle diameter.But no matter what precipitating reagent used, during water
It is unavoidable to wash.Water-washing process water consumption is very big, and water consumption is 10-100 times of product weight, it is necessary to recycling utilization
Or processing discharge, electrolyte concentration, crystallization, the processing of wash-off are all very big consumption and problem, and water-washing process is to wet chemistry method
Bring many troubles.Such technique produces substantial amounts of waste, and it is big to consume energy, and does not meet the theory of green low-carbon.
Austrian patent (Ausp itzerOtto.Zinkoxyd:AT, 176207 [P] .1953-09-25) report one kind
Method, basic zinc carbonate, Ran Houzai are prepared with carbon dioxide reaction by the high coarse granule zinc oxide of purity under hydrothermal conditions
Zinc oxide particles are obtained through calcining.I.e. in the autoclave pressure containing water and high-purity tutty particle, carbon dioxide is passed through,
Keep certain temperature and pressure, when reaction proceeds to certain carbonic acid Zn content, isolate basic zinc carbonate, then through drying,
Calcining obtains 0.05 μm or so of particle diameter, the activated zinc oxide powder that particle diameter distribution is narrow, purity is high.The advantages of this method and deficiency
All it is obvious that advantage is will not to introduce foreign ion, product purity is high, it is often more important that avoids ring caused by water-washing process
Border pressure；Shortcoming is to need to carry out at elevated pressures, and equipment investment is big, operation inconvenience, then it is to use carbon dioxide to have
For raw material, the not only source inconvenience of high-purity carbon dioxide gas, and needs compression charging.
It is also many to study the zinc oxide preparation method of report, such as using solid-phase grinding, microwave field radiant heating, high frequency
Induction heating, plasma heating method, electron beam heating and laser heating, sputtering method, gravity Method, microemulsion method etc.
Deng, these method general operations inconvenience, be not suitable for large-scale industrial production, only rest on the experimental stage.
The content of the invention
It is an object of the invention to provide a kind of method for preparing super fine zinc oxide powder, described method is adapted to scale
Production, it is not necessary to which water-washing process, without liquid debris and solid waste discharge, product cut size is evenly distributed, particle size
It is controllable.
For achieving the above object, the present invention adopts the following technical scheme that：By coarse granule Zinc oxide powder or metallic zinc
Adding in organic acid soln, transparent liquid is completely dissolved to Zinc oxide particles or metallic zinc, add oxalic acid, generation precipitates,
Sediment and filtrate are filtrated to get, sediment is zinc oxalate, by sediment in 80-300 DEG C of dry white powder, wherein drying
Caused gas phase portion condensation recovery merges with filtrate；Dried powder was obtained in 400-600 DEG C of temperature lower calcination 1-4 hour
To zinc oxide ultra-fine powder, the filtrate of merging is organic acid soln, is reused, and is directly used in lower batch dissolving tutty
Grain or metallic zinc.
Acetic acid, formic acid, benzene can be selected in be added to dissolve tutty or metallic zinc, the organic acid of organic acid of the present invention
Formic acid, lactic acid etc., or their mixture.The addition of organic acid by metallic zinc or zinc oxide to be fully converted to organic zinc salt
The aqueous solution on the basis of, excessive organic acid can accelerate course of dissolution, but excessive too much also without necessity, therefore suitably
Ratio is ZnO or Zn:Organic acid (mol ratio)=1:2-1:3.
The inventive method, organic acid soln substantially quantitative recovery, whole preparation process do not produce waste water and solid waste.
The precipitating reagent that the present invention uses is the oxalic acid with the crystallization water or without the crystallization water.
The particle diameter distribution of super fine zinc oxide powder obtained by the inventive method is uniform, and particle size is controllable.Applicant
It was found that the average grain diameter of super fine zinc oxide product can be adjusted by adjusting the metallic zinc added or the mol ratio of zinc oxide and oxalic acid
Section, it is 30-200nm super fine zinc oxides that can obtain average particle size, and preferable particle size is in 50-150nm.Adjust ZnO or Zn with
Oxalic acid proportioning (mol ratio) is 0.5-1.5:1, preferably 0.8~1.2：1, it can obtain requiring the zinc oxide of particle diameter, table 1 lists
Different ZnO or Zn and zinc oxide particles Average Particle Diameters under oxalic acid proportioning (mol ratio).
Table 1
| ZnO or Zn:Oxalic acid (mol ratio) | Average grain diameter (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 the super fine zinc oxide powder of the present invention, the nothing during super fine zinc oxide is prepared
The useless solid discharge of waste liquid, nothing, zinc oxide product size tunable, particle diameter distribution are uniform.The present invention is suitable for large-scale industrial production,
Solve the problems, such as that traditional precipitation method produce a large amount of waste water during preparing super fine zinc oxide, while also do not produce other solids and give up
Gurry, environmentally friendly, resulting product cut size is controllable, and because not adding other auxiliary agents, impurity is few, can meet daily use chemicals, coating, rubber
The application in the fields such as glue, electronics, absorbing material.
With reference to specific embodiment, the present invention will be described in detail.Protection scope of the present invention is not with specific implementation
Mode is limited, but is defined in the claims.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Zinc oxide particles electromicroscopic photograph made from Fig. 2 embodiments 1.
Obtained Zinc oxide particles electromicroscopic photograph after filtrate is applied mechanically in Fig. 3 embodiments 1.
Zinc oxide particles electromicroscopic photograph made from Fig. 4 embodiments 2.
Obtained Zinc oxide particles electromicroscopic photograph after filtrate is applied mechanically in Fig. 5 embodiments 2.
Zinc oxide particles electromicroscopic photograph made from Fig. 6 embodiments 3.
Obtained Zinc oxide particles electromicroscopic photograph after filtrate is applied mechanically in Fig. 7 embodiments 3.
Zinc oxide particles electromicroscopic photograph made from Fig. 8 embodiments 4.
Obtained Zinc oxide particles electromicroscopic photograph after filtrate is applied mechanically in Fig. 9 embodiments 4.
Zinc oxide particles electromicroscopic photograph made from Figure 10 embodiments 5.
Obtained Zinc oxide particles electromicroscopic photograph after filtrate is applied mechanically in Figure 11 embodiments 5.
Zinc oxide particles electromicroscopic photograph made from Figure 12 embodiments 6.
Obtained Zinc oxide particles electromicroscopic photograph after filtrate is applied mechanically in Figure 13 embodiments 6.
Zinc oxide particles electromicroscopic photograph made from Figure 14 embodiments 7.
Obtained Zinc oxide particles electromicroscopic photograph after filtrate is applied mechanically in Figure 15 embodiments 7.
Embodiment
Technical solutions according to the invention are further described in detail below by specific embodiment, but are necessary
Point out that following examples are served only for the description to the content of the invention, do not form limiting the scope of the invention.
Embodiment 1
27.67 kilograms of (340 moles) coarse granule Zinc oxide powders are slowly added to 242.86 liters, and concentration is 2.8mol/L acetic acid
(contain 680 moles of acetic acid) in solution, stir lower Zinc oxide particles and be gradually completely dissolved transparent liquid, add 42.86 kilograms
Two oxalic acid hydrates (340 moles), have white precipitate generation, be filtrated to get precipitation cake and filtrate.
Precipitated filter cakes are in 105 DEG C of dry white powders.The white powder being dried to obtain is in 500-600 DEG C of temperature lower calcination
1.5 hours, it was 27 kilograms of 100 nanometer Zinc oxide powder to obtain average grain diameter.Powder electromicroscopic photograph is shown in Fig. 2.
Filtrate tests acidity, and the glacial acetic acid and water for adding metering form 242.86 liters of 2.8mol/L concentration acetum sets
With it is 27 kilograms of 101 nano zine oxide superfine powder to repeat said process and obtain average grain diameter.Powder electromicroscopic photograph is shown in Fig. 3.
Embodiment 2
27.67 kilograms of (340 moles) coarse granule Zinc oxide powders are slowly added to 242.86 liters, and concentration is 3.0mol/L benzene first
(contain 728.6 moles of benzoic acid) in acid solution, stir lower Zinc oxide particles and be gradually completely dissolved transparent liquid, add
42.86 kilograms of two oxalic acid hydrates (340 moles), have white precipitate generation, are filtrated to get sediment and filtrate.
Precipitated filter cakes are in 105 DEG C of dry white powders.The white powder being dried to obtain is in 500-600 DEG C of temperature lower calcination
2 hours, it was 27.67 kilograms of 103 nano zine oxide superfine powder to obtain average grain diameter.Powder electromicroscopic photograph is shown in Fig. 4.
Filtrate tests acidity, and the benzoic acid and water for adding metering form 242.86 liters of 3.0mol/L concentration benzoic acid solution sets
With it is 27.67 kilograms of 98nm zinc oxide ultra-fines powder to repeat said process and obtain average grain diameter.Powder electromicroscopic photograph is shown in Fig. 5.
Embodiment 3
27.67 kilograms of (340 moles) coarse granule Zinc oxide powders are slowly added to 242.86 liters, and concentration is 3.36mol/L vinegar
(contain 816 moles of acetic acid) in acid solution, stir lower Zinc oxide particles and be gradually completely dissolved transparent liquid, it is public to add 38.57
Two oxalic acid hydrates (306 moles) of jin, have white precipitate generation, are filtrated to get sediment and filtrate.
Precipitated filter cakes are in 105 DEG C of dry white powders.The white powder being dried to obtain is in 500-600 DEG C of temperature lower calcination
4 hours, it was 27 kilograms of 85 nano zine oxide superfine powder to obtain average grain diameter.Powder electromicroscopic photograph is shown in Fig. 6.
Filtrate tests acidity, adds the acetic acid of metering and water forms 242.86 liters of 2.8mol/L concentration acetums and applied mechanically,
It is 27 kilograms of 87 nano zine oxide superfine powder to repeat said process and obtain average grain diameter.Powder electromicroscopic photograph is shown in Fig. 7.
Embodiment 4
27.67 kilograms of (340 moles) coarse granule Zinc oxide powders are slowly added to 242.86 liters, and concentration is 3.08mol/L first
(contain 748 moles of formic acid) in acid solution, stir lower Zinc oxide particles and be gradually completely dissolved transparent liquid, it is public to add 47.15
Two oxalic acid hydrates (374 moles) of jin, have white precipitate generation, are filtrated to get sediment and filtrate.
Precipitated filter cakes part is in 105 DEG C of dry white powders.The white powder being dried to obtain is at a temperature of 500-600 DEG C
Calcining 2 hours, it is 27 kilograms of 121 nano zine oxide superfine powder to obtain average grain diameter.Powder electromicroscopic photograph is shown in Fig. 8.
Filtrate tests acidity, adds the formic acid of metering and water forms 242.86 liters of 2.8mol/L concentration formic acid solutions and applied mechanically,
It is 27 kilograms of 123 nano zine oxide superfine powder to repeat said process and obtain average grain diameter.Powder electromicroscopic photograph is shown in Fig. 9.
Embodiment 5
27.67 kilograms of (340 moles) coarse granule Zinc oxide powders are slowly added to 242.86 liters, and concentration is 2.8mol/L lactic acid
(contain 680 moles of lactic acid) in solution, stir lower Zinc oxide particles and be gradually completely dissolved transparent liquid, add 47.15 kilograms
Two oxalic acid hydrates (374 moles), have white precipitate generation, be filtrated to get sediment and filtrate.
Precipitated filter cakes part is in 105 DEG C of dry white powders.The white powder being dried to obtain is at a temperature of 500-600 DEG C
Calcining 2 hours, it is 27.67 kilograms of 141 nano zine oxide superfine powder to obtain average grain diameter.Powder electromicroscopic photograph is shown in Figure 10.
Filtrate tests acidity, adds the lactic acid of metering and water forms 242.86 liters of 2.8mol/L concentration lactic acid solutions and applied mechanically,
It is 27.67 kilograms of 138 nano zine oxide superfine powder to repeat said process and obtain average grain diameter.Powder electromicroscopic photograph is shown in Figure 11.
Embodiment 6
27.67 kilograms of (340 moles) coarse granule Zinc oxide powders are slowly added to 242.86 liters, and concentration is 3.052mol/L vinegar
(contain 741.2 moles of acetic acid) in acid solution, stir lower Zinc oxide particles and be gradually completely dissolved transparent liquid, add 34.29
Kilogram two oxalic acid hydrates (272 moles), have white precipitate generation, be filtrated to get sediment and filtrate.
Precipitated filter cakes part is in 105 DEG C of dry white powders.The white powder being dried to obtain is at a temperature of 500-600 DEG C
Calcining 1 hour, it is 27.67 kilograms of 55 nano zine oxide superfine powder to obtain average grain diameter.Powder electromicroscopic photograph is shown in Figure 12.
Filtrate tests acidity, and the glacial acetic acid and water for adding metering form 242.86 liters of 2.8mol/L concentration acetum sets
With it is 27.67 kilograms of 54 nano zine oxide superfine powder to repeat said process and obtain average grain diameter.Powder electromicroscopic photograph is shown in Figure 13.
Embodiment 7
22.23 kilograms of (340 moles) zinc powders are slowly added to 242.86 liters, and concentration is that 4.2mol/L formic acid mixes with benzoic acid
(containing 510 moles of formic acid, 510 moles of benzoic acid) in solution, stir lower Zinc oxide particles and be gradually completely dissolved transparent liquid, then
47.15 kilograms of two oxalic acid hydrates (374 moles) are added, has white precipitate generation, is filtrated to get sediment and filtrate.
Precipitated filter cakes are in 105 DEG C of dry white powders.The white powder being dried to obtain is in 500-600 DEG C of temperature lower calcination
4 hours, it was 27 kilograms of 116 nano zine oxide superfine powder to obtain average grain diameter.Powder electromicroscopic photograph is shown in Figure 14.
Filtrate tests acidity, adds the formic acid of metering and water forms 242.86 liters of 2.8mol/L concentration formic acid solutions and applied mechanically,
It is 27 kilograms of 117 nano zine oxide superfine powder to repeat said process and obtain average grain diameter.Powder electromicroscopic photograph is shown in Figure 15.
Claims (6)
1. a kind of preparation method of super fine zinc oxide powder, it is characterised in that add coarse granule Zinc oxide powder or metallic zinc
In organic acid soln, organic zinc salt solution, the one kind of described organic acid in acetic acid, formic acid, benzoic acid or lactic acid are formed
It is or several；Oxalic acid generation white precipitate is added, coarse granule zinc oxide or the mol ratio of zinc and oxalic acid are 0.5~1.5: 1, filtering
Obtain sediment and filtrate；Sediment is zinc oxalate, and sediment is dried, calcines and obtains super fine zinc oxide powder；Filtrate
For organic acid soln, reuse.
2. the preparation method of super fine zinc oxide powder according to claim 1, it is characterised in that the temperature of the drying is
80-300 DEG C, the condensed recovery of condensable gas caused by drying is merged into organic acid soln.
3. the preparation method of super fine zinc oxide powder according to claim 1, it is characterised in that the temperature of the calcining is
400-600 DEG C, hour time 1-4.
4. the preparation method of super fine zinc oxide powder according to claim 1, it is characterised in that the use of described organic acid
Measure and be, coarse granule zinc oxide or the mole ratio of zinc and organic acid are 1: 2~1: 3.
5. the preparation method of super fine zinc oxide powder according to claim 1, it is characterised in that described coarse granule oxidation
The mol ratio of zinc or zinc and oxalic acid is 0.8~1.2: 1.
6. the preparation method of super fine zinc oxide powder according to claim 1, it is characterised in that prepared by described method
The average particle size range of super fine zinc oxide powder particle is at 30 nanometers 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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| 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 |
| 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 |
| 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 |
| CN114906871B (en) * | 2022-06-08 | 2023-05-26 | 桂林理工大学 | Method for preparing nano zinc oxide by using secondary zinc oxide |
| CN114956158A (en) * | 2022-06-13 | 2022-08-30 | 河北戴桥医药科技有限公司 | Preparation method of calamine powder |
| 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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| JPH0350119A (en) * | 1989-07-19 | 1991-03-04 | Mitsubishi Materials Corp | Production of fine zinc oxide particles |
| 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 |
| 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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| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: No. 299 Changfeng River Road, Nanjing Chemical Industrial Park, Jiangsu, Jiangsu Patentee after: Nanjing Huashi New Material Co., Ltd. Address before: 210047, -66, No. 90, Tai Fang Road, Nanjing chemical industry park, Jiangsu, Nanjing Patentee before: Nanjing Huashi Chemical Co., Ltd. |