JPH0350119A - Production of fine zinc oxide particles - Google Patents
Production of fine zinc oxide particlesInfo
- Publication number
- JPH0350119A JPH0350119A JP18459789A JP18459789A JPH0350119A JP H0350119 A JPH0350119 A JP H0350119A JP 18459789 A JP18459789 A JP 18459789A JP 18459789 A JP18459789 A JP 18459789A JP H0350119 A JPH0350119 A JP H0350119A
- Authority
- JP
- Japan
- Prior art keywords
- zinc oxide
- particles
- zinc
- wet
- oxalate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000002245 particle Substances 0.000 title abstract description 14
- ZPEJZWGMHAKWNL-UHFFFAOYSA-L zinc;oxalate Chemical compound [Zn+2].[O-]C(=O)C([O-])=O ZPEJZWGMHAKWNL-UHFFFAOYSA-L 0.000 claims abstract description 13
- 238000010304 firing Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 abstract description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 abstract description 8
- 238000010298 pulverizing process Methods 0.000 abstract description 8
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 abstract description 4
- 239000011701 zinc Substances 0.000 abstract description 3
- 235000006408 oxalic acid Nutrition 0.000 abstract description 2
- 235000005074 zinc chloride Nutrition 0.000 abstract description 2
- 239000011592 zinc chloride Substances 0.000 abstract description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 229910052725 zinc Inorganic materials 0.000 abstract 1
- 235000014692 zinc oxide Nutrition 0.000 description 15
- 238000000034 method Methods 0.000 description 9
- 239000010419 fine particle Substances 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000010908 decantation Methods 0.000 description 4
- 239000002537 cosmetic Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000003937 drug carrier Substances 0.000 description 2
- 239000012776 electronic material Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000002529 flux (metallurgy) Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 150000003752 zinc compounds Chemical class 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は電子材料、触媒、化粧料、医薬品基材等に用い
られる高純度の微粒子酸化亜鉛（亜鉛華）の製造方法に
関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing high-purity particulate zinc oxide (zinc white) used for electronic materials, catalysts, cosmetics, pharmaceutical base materials, etc.
微細な酸化亜鉛粉末の製造方法の一つに塩基性炭酸亜鉛
もしくはシュウ酸亜鉛の熱分解法がある。One of the methods for producing fine zinc oxide powder is the thermal decomposition method of basic zinc carbonate or zinc oxalate.
しかしこの方法は、中間化合物である炭酸亜鉛とシュウ
酸亜鉛は湿式法により合成されるため水溶液中しこ共在
する不純物イオンが中間化合物に吸着、吸蔵され混入す
る問題がある。また、塩基性炭酸塩から得られた酸化亜
鉛粉末はｐｉが８以上の塩基性を示し化粧料原料として
使用した場合には雑菌の繁殖の点から好ましくない。However, in this method, since the intermediate compounds, zinc carbonate and zinc oxalate, are synthesized by a wet method, there is a problem that impurity ions, which coexist in the aqueous solution, are adsorbed and occluded by the intermediate compounds. Further, zinc oxide powder obtained from basic carbonate has a basicity with a pi of 8 or more, and is not preferred from the viewpoint of bacterial growth when used as a raw material for cosmetics.
［本発明の知見］
シュウ酸亜鉛を熱分解して得られた粉末はｐＨが７以下
の酸性を示すことが知られている。そこで本発明者らは
シュウ酸塩を湿式合成する際に随伴する不純物を除去し
た高純度微粒子酸化亜鉛の製造法を検討した。[Findings of the present invention] It is known that the powder obtained by thermally decomposing zinc oxalate exhibits acidity with a pH of 7 or less. Therefore, the present inventors investigated a method for producing high-purity particulate zinc oxide by removing impurities accompanying the wet synthesis of oxalate.
シュウ酸亜鉛の不純物は出発原料である亜鉛化合物から
くる硫酸イオン、塩素イオン等で、これらが物理的に吸
着・吸蔵されて含まれるため、水洗のみでは除去するこ
とができない。Impurities in zinc oxalate include sulfate ions and chloride ions that come from the zinc compound that is the starting material, and because these are physically adsorbed and occluded, they cannot be removed by washing with water alone.
また、シュウ酸亜鉛の焼成を６００℃以上の高い温度で
行なうため粒子が粗大となり（１０ｒｒｒ／ｇ以下）、
微粒子状の酸化亜鉛粉末は得られない。本発明者等の研
究の結果、水または有機酸を含む水溶液を用いてシュウ
酸亜鉛を湿式粉砕することにより吸着・吸蔵されている
前記不純物を除去することができ、さらに粒子が微細化
されるためにより低い温度で焼成することができ、微粒
子酸化亜鉛が得られることを見出した。In addition, since zinc oxalate is fired at a high temperature of 600°C or higher, the particles become coarse (10rrr/g or less).
Fine particulate zinc oxide powder cannot be obtained. As a result of the research conducted by the present inventors, the adsorbed and occluded impurities can be removed by wet-pulverizing zinc oxalate using water or an aqueous solution containing an organic acid, and the particles can be further refined. Therefore, it has been found that firing can be performed at a lower temperature and fine particle zinc oxide can be obtained.
すなわち本発明の目的は、従来の方法では得ることので
きない比表面積が２５ｒｒｒ／ｇ以上でかつ高純度の微
粒子酸化亜鉛を製造することを目的とする。That is, an object of the present invention is to produce highly pure particulate zinc oxide having a specific surface area of 25 rrr/g or more, which cannot be obtained by conventional methods.
本発明は、シュウ酸亜鉛を焼成して酸化亜鉛粉末を製造
する方法において、予めシュウ酸亜鉛を湿式粉砕し、そ
の後３５０〜４５０℃で焼成することを特徴とする微粒
子酸化亜鉛の製造方法を提供する。The present invention provides a method for producing zinc oxide powder by firing zinc oxalate, which is characterized in that zinc oxalate is wet-pulverized in advance and then fired at 350 to 450°C. do.
本発明の原料とするシュウ酸亜鉛（ＺｎＣ２０，）は公
知の方法によって製造されたものでもよく、特に限定さ
れない。たとえば硫酸亜鉛（ＺｎＳＯ４・７Ｈ，Ｏ）あ
るいは塩化亜鉛（ＺｎＣΩ２）等の水溶液とシュウ酸（
ＣｚＯＪａ）水溶液とを混合、反応させて製造される。Zinc oxalate (ZnC20,) used as a raw material in the present invention may be produced by a known method and is not particularly limited. For example, an aqueous solution of zinc sulfate (ZnSO4.7H,O) or zinc chloride (ZnCΩ2) and oxalic acid (
CzOJa) and an aqueous solution and react with each other.
反応の結果析出したＺｎＣ，０４はデカンテーションに
より未反応物および副生物を十分洗浄して除去された後
、湿式粉砕にかけられる。 ＺｎＣ２Ｏ４の湿式粉砕は
公知の粉砕機たとえばボールミル、ハンマーミル、ビー
ズミル等湿式粉砕のできる装置を使用することができ特
に限定されるものではない。湿式粉砕時の媒体は水が好
適で、温度は常温で行なわれる。ZnC,04 precipitated as a result of the reaction is thoroughly washed and removed by decantation to remove unreacted substances and by-products, and then subjected to wet pulverization. Wet pulverization of ZnC2O4 can be carried out using any known pulverizer, such as a ball mill, a hammer mill, a bead mill, or other equipment capable of wet pulverization, and is not particularly limited. Water is suitable as the medium for wet grinding, and the grinding is carried out at room temperature.
湿式粉砕が終った後、上澄液の電気伝導度が５μｓ以下
になるまでデカンテーションを行なって、粉砕により溶
出した不純物を洗浄除去する。次いで固液を分離し、１
００〜１１０℃で乾燥した後焼成して微粒子酸化亜鉛（
２ｎＯ）とする。焼成温度は３５０〜４５０℃で行なう
のが好適である。３５０℃以下では焼成が十分でなく、
４５０℃以上になると粒子が粗大化する傾向があり１本
発明の目的とする比表面積２５ｒｒｒ／ｇ以上の微粒子
は得られない。焼成は加熱炉を用いて公知の方法で行な
われ特に限定されない、また静置法でもよく流動層方式
でもよい。After the wet pulverization is completed, decantation is performed until the electrical conductivity of the supernatant becomes 5 μs or less to wash and remove impurities eluted by the pulverization. Then the solid and liquid are separated and 1
Fine particles of zinc oxide (
2nO). The firing temperature is preferably 350 to 450°C. If the temperature is below 350℃, the firing will not be sufficient.
If the temperature exceeds 450° C., the particles tend to become coarse, making it impossible to obtain fine particles having a specific surface area of 25 rrr/g or more, which is the object of the present invention. Firing is performed by a known method using a heating furnace and is not particularly limited, and may be a stationary method or a fluidized bed method.
このようにして得られた微粒子酸化亜鉛は、Ｘ線回折、
ＢＥＴ法による表面積測定および不純物分析を行なっ
た結果比表面積２５ｍ／ｇ以上、不純物（ｓｏ４２−等
）７０ｐｐｍ以下であり、従来法で得られたものと比べ
極めて高純度の微粒子酸化亜鉛であることが確認された
。The fine particles of zinc oxide thus obtained can be analyzed by X-ray diffraction,
The results of surface area measurement and impurity analysis using the BET method revealed a specific surface area of 25 m/g or more and impurities (so42-, etc.) of 70 ppm or less, indicating that the zinc oxide particles were extremely purified compared to those obtained using conventional methods. confirmed.
上記のように本発明によればｌｎＣ，０４を湿式粉砕す
ることにより、微粒子化すると同時に粒子に吸着・吸蔵
された不純物を除去し、さらに低い温度で焼成すること
により、比表面積が２５ ｒｒｒ７ｇ以上の高純度微粒
子酸化亜鉛を得ることができる。この酸化亜鉛は電子材
料、融媒、化粧料、医薬品基材等の原料として最適であ
る。As described above, according to the present invention, by wet-pulverizing lnC,04, the impurities adsorbed and occluded in the particles are removed at the same time as they are made into fine particles, and the impurities adsorbed and occluded in the particles are removed, and the specific surface area is increased to 25 rrr7 g or more by firing at a lower temperature. High purity fine particle zinc oxide can be obtained. This zinc oxide is optimal as a raw material for electronic materials, fluxes, cosmetics, pharmaceutical base materials, etc.
以下実施例を用いて本発明をより具体的に説明する。 The present invention will be described in more detail below using Examples.
実施例ｌ
ＺｎＳＯ４・７Ｈ２０の５０ｗｔ％水溶液１０００ｇと
Ｃ，０４Ｈ，１００ｇ＃１の水溶液２Ｑとを混合し、Ｚ
ｎＣ，０４沈澱を得た。副生したＨ、 ＳＯ２をデカン
テーションにより十分洗浄した後、ハンマーミルでＺｎ
Ｃ２Ｏ４を湿式粉砕した。Example 1 1000g of a 50wt% aqueous solution of ZnSO4.7H20 and 2Q of an aqueous solution of C,04H,100g #1 were mixed,
nC,04 precipitate was obtained. After thoroughly cleaning the by-produced H and SO2 by decantation, Zn is removed using a hammer mill.
C2O4 was wet milled.
次いで上澄液の電気伝導度が５μＳ以下になるまでデカ
ンテーションを行なった後置液分離し１００℃で乾燥し
た。乾燥したＺｎＣ，０４を４００℃で３時間焼成して
得られたものについてｘｔｌ＠回折、 ＢＥＴ法測定お
よび不純物分析を行なった結果表に示す表面積、純度等
のＺｎＯであることが確認された。Next, the supernatant liquid was decanted until the electrical conductivity became 5 μS or less, and the supernatant liquid was separated and dried at 100°C. The dried ZnC,04 was baked at 400° C. for 3 hours, and as a result of xtl@ diffraction, BET measurement and impurity analysis, it was confirmed that it was ZnO with the surface area, purity, etc. shown in the table.
実施例２．３
焼成温度を３５０℃および４５Ｑ’Ｃとして実施例１と
同様の操作を行なった結果得られたＺｎＯについてのデ
ータを表に掲げた。Example 2.3 Data regarding ZnO obtained as a result of performing the same operation as in Example 1 with the firing temperature of 350°C and 45Q'C are listed in the table.
実施例４
Ｚｎ源としてＺｎＣらを用いて実施例１と同様の操作を
行ない、得られたＺｎＯについての測定結果を表に示し
た。Example 4 The same operation as in Example 1 was performed using ZnC etc. as the Zn source, and the measurement results for the obtained ZnO are shown in the table.
以上実施例１〜４は何れも本発明の方法により製造され
たＺｎＯであって、比表面積２５ｒｎ’／ｇ以上の微粒
子ＺｎＯであり、不純物含有量も６０ｐｐｍ以下の高純
度品である。All of Examples 1 to 4 are fine particle ZnO produced by the method of the present invention, with a specific surface area of 25 rn'/g or more, and high purity products with an impurity content of 60 ppm or less.
比較例１〜２
実施例１において、ＺｎＣ，０４を湿式粉砕しないまま
デカンテーション後分離し１／２を４００℃、残る１／
２を６００℃で夫々３時間焼成した結果、４００℃で焼
成したものはＺｎＣ２Ｏ４が完全に分解しながった。Comparative Examples 1 to 2 In Example 1, ZnC,04 was separated after decantation without wet grinding, 1/2 was separated at 400°C, and the remaining 1/2
2 were fired at 600°C for 3 hours each, and as a result, ZnC2O4 was not completely decomposed in those fired at 400°C.
６００℃で焼成したものはＺｎＯであったが、比表面積
６．８ｒｒｔ／ｇ、濃度Ｓｏ４２−５３２ｐｐｍで、粒
子、純度共レベルの低いものであった。実施例と併記し
て表に比較した。The ZnO fired at 600°C had a specific surface area of 6.8 rrt/g, a concentration of So42-532 ppm, and had low levels of particles and purity. A comparison is made in the table along with the examples.
表table
Claims (1)
おいて、予めシュウ酸亜鉛を湿式粉砕し、３５０〜４５
０℃で焼成することを特徴とする高純度微粒子酸化亜鉛
の製造方法。In the method of manufacturing zinc oxide powder by baking zinc oxalate, zinc oxalate is wet-pulverized in advance to give a
A method for producing high-purity particulate zinc oxide, characterized by firing at 0°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18459789A JPH0350119A (en) | 1989-07-19 | 1989-07-19 | Production of fine zinc oxide particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18459789A JPH0350119A (en) | 1989-07-19 | 1989-07-19 | Production of fine zinc oxide particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0350119A true JPH0350119A (en) | 1991-03-04 |
Family
ID=16155996
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18459789A Pending JPH0350119A (en) | 1989-07-19 | 1989-07-19 | Production of fine zinc oxide particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0350119A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2703349A1 (en) * | 1993-04-01 | 1994-10-07 | France Pharmacie Centrale | Zinc oxide powder doped, manufacturing process and ceramic obtained from said powder. |
| WO2005033355A1 (en) * | 2003-09-30 | 2005-04-14 | Nikko Materials Co., Ltd. | High purity zinc oxide powder and method for production thereof, and high purity zinc oxide target and thin film of high purity zinc oxide |
| JP4966447B2 (en) * | 1998-05-15 | 2012-07-04 | アドバンスド ナノ テクノロジーズ プロプライエタリー リミテッド | Method for producing ultrafine powder |
| JP2012166967A (en) * | 2011-02-10 | 2012-09-06 | Sumitomo Metal Mining Co Ltd | Nickel oxide fine powder and method for producing the same |
| 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 |
| WO2019088130A1 (en) * | 2017-10-31 | 2019-05-09 | 住友大阪セメント株式会社 | Zinc oxide powder, dispersion, cosmetic material, and method for producing zinc oxide powder |
| CN110357145A (en) * | 2019-08-15 | 2019-10-22 | 昆明理工大学 | A method of zinc oxalate is prepared using zinc oxide fumes and prepares nano zine oxide |
-
1989
- 1989-07-19 JP JP18459789A patent/JPH0350119A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2703349A1 (en) * | 1993-04-01 | 1994-10-07 | France Pharmacie Centrale | Zinc oxide powder doped, manufacturing process and ceramic obtained from said powder. |
| WO1994022765A1 (en) * | 1993-04-01 | 1994-10-13 | Pharmacie Centrale De France | Doped zinc oxide powder, preparation thereof and ceramic produced therefrom |
| JP4966447B2 (en) * | 1998-05-15 | 2012-07-04 | アドバンスド ナノ テクノロジーズ プロプライエタリー リミテッド | Method for producing ultrafine powder |
| WO2005033355A1 (en) * | 2003-09-30 | 2005-04-14 | Nikko Materials Co., Ltd. | High purity zinc oxide powder and method for production thereof, and high purity zinc oxide target and thin film of high purity zinc oxide |
| US7510635B2 (en) | 2003-09-30 | 2009-03-31 | Nippon Mining & Metals Co., Ltd. | High purity zinc oxide powder and method for production thereof, and high purity zinc oxide target and thin film of high purity zinc oxide |
| JP2012166967A (en) * | 2011-02-10 | 2012-09-06 | Sumitomo Metal Mining Co Ltd | Nickel oxide fine powder and method for producing the same |
| 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 |
| WO2019088130A1 (en) * | 2017-10-31 | 2019-05-09 | 住友大阪セメント株式会社 | Zinc oxide powder, dispersion, cosmetic material, and method for producing zinc oxide powder |
| CN110357145A (en) * | 2019-08-15 | 2019-10-22 | 昆明理工大学 | A method of zinc oxalate is prepared using zinc oxide fumes and prepares nano zine oxide |
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