JPH04164814A - Production of ultra-fine zinc oxide powder having excellent dispersibility - Google Patents
Production of ultra-fine zinc oxide powder having excellent dispersibilityInfo
- Publication number
- JPH04164814A JPH04164814A JP29242690A JP29242690A JPH04164814A JP H04164814 A JPH04164814 A JP H04164814A JP 29242690 A JP29242690 A JP 29242690A JP 29242690 A JP29242690 A JP 29242690A JP H04164814 A JPH04164814 A JP H04164814A
- Authority
- JP
- Japan
- Prior art keywords
- zinc oxide
- aqueous solution
- oxide powder
- zinc
- ultra
- 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 58
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 28
- 239000002245 particle Substances 0.000 claims abstract description 17
- 239000011787 zinc oxide Substances 0.000 claims abstract description 16
- 150000003751 zinc Chemical class 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 9
- 239000003513 alkali Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 3
- 239000002537 cosmetic Substances 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract description 3
- 230000003287 optical effect Effects 0.000 abstract description 3
- 239000011882 ultra-fine particle Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000011701 zinc Substances 0.000 description 7
- 229910052725 zinc Inorganic materials 0.000 description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 6
- 238000004438 BET method Methods 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 4
- 239000011163 secondary particle Substances 0.000 description 4
- 238000004381 surface treatment Methods 0.000 description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 4
- 229960001763 zinc sulfate Drugs 0.000 description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000011592 zinc chloride Substances 0.000 description 3
- 235000005074 zinc chloride Nutrition 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 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 2
- 230000001681 protective effect Effects 0.000 description 2
- 230000000475 sunscreen effect Effects 0.000 description 2
- 239000000516 sunscreening agent Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 2
- 229940007718 zinc hydroxide Drugs 0.000 description 2
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- ZPEJZWGMHAKWNL-UHFFFAOYSA-L zinc;oxalate Chemical compound [Zn+2].[O-]C(=O)C([O-])=O ZPEJZWGMHAKWNL-UHFFFAOYSA-L 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 239000012965 benzophenone Substances 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 230000036556 skin irritation Effects 0.000 description 1
- 231100000475 skin irritation Toxicity 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は分散性に優れた超微粒子酸化亜鉛粉末の製造方
法に関する。本発明に係る酸化亜鉛粉末を分散させた膜
あるいは成形体及びペーストは、透明でかつ紫外線遮断
効果を有するので１例えば。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing ultrafine zinc oxide powder with excellent dispersibility. For example, the film or molded body and paste in which zinc oxide powder according to the present invention is dispersed is transparent and has an ultraviolet blocking effect.
日焼は止め化粧料、自動車、家具、光学材料等の紫外線
遮断保護膜に利用できる。It can be used in sunscreen cosmetics, UV-blocking protective films for automobiles, furniture, optical materials, etc.
紫外線遮断効果を有する材料は昔から良く知られており
、有機系ではベンゾトリアゾール、ベンゾフェノン等が
あり、また無機系では酸化チタン、酸化亜鉛などがある
。これらの中で有機系は皮膚刺激性やそれ自身の光分解
等の問題があり、また無機系は粒子が大きく透明性を比
すことができない。最近無機粉体の透明性を出すため超
微粒子化が検討され、光の散乱を小さくして透明性を向
上させた超微粒子酸化チタン、超微粒子酸化亜鉛が市販
されている。しかし超微粒子化により透明性は向上した
が、粉末の表面処理、分散方法等多くの問題がまだ残さ
れており、また透明性も十分とは言えない。Materials that have an ultraviolet blocking effect have been well known for a long time, and organic materials include benzotriazole and benzophenone, and inorganic materials include titanium oxide and zinc oxide. Among these, organic types have problems such as skin irritation and photodecomposition, and inorganic types have large particles and cannot be compared in transparency. Recently, ultrafine particles have been studied to improve the transparency of inorganic powders, and ultrafine titanium oxide and zinc oxide, which reduce light scattering and improve transparency, are commercially available. However, although transparency has improved due to ultrafine particle size, many problems still remain, such as surface treatment of powder and dispersion method, and transparency cannot be said to be sufficient.
更に従来の超微粒子酸化亜鉛粉末は、塩基性炭酸亜鉛、
シュウ酸亜鉛、水酸化亜鉛等を生成させ、これを脱水乾
燥後、焼成することにより製造しているため、ｉｊ集し
やすく分散性に劣る。Furthermore, conventional ultrafine zinc oxide powder contains basic zinc carbonate,
Since it is manufactured by generating zinc oxalate, zinc hydroxide, etc., dehydrating it, drying it, and then firing it, it tends to aggregate and has poor dispersibility.
亜鉛塩の水溶液は、アルカリ性下で加水分解して亜鉛の
ヒドロシルが生成することが知られている。本発明者は
、可視域での高い透明性と優れた紫外線遮断効果を有す
る超微粒子酸化亜鉛粉末の製造法につき鋭意検討し１強
アルカリ性下で、かつ６０℃以上の温度で反応させるこ
とにより焼成工程を経ることなく、分散性に優れた超微
粒子酸化亜鉛粉末を製造できることを見出した。It is known that an aqueous solution of zinc salt is hydrolyzed under alkaline conditions to produce zinc hydrosyl. The present inventor has conducted extensive studies on a method for producing ultrafine zinc oxide powder that has high transparency in the visible range and excellent UV blocking effect, and has developed a method for producing ultrafine zinc oxide powder, which is fired by reacting it under strongly alkaline conditions and at a temperature of 60°C or higher. We have discovered that it is possible to produce ultrafine zinc oxide powder with excellent dispersibility without going through any process.
［１１８！の解決手段：発明の構成〕
本発明によれば、６０℃以上の温度下で、アルカリ水溶
液に亜鉛塩の水溶液を滴下し、最終ＰＨ９以上で酸化亜
鉛の沈澱を生成させて平均粒径０．０２〜０．０５μ園
の超微粒子酸化亜鉛粉末を製造することを特−徴とする
方法が提供される。[118! According to the present invention, an aqueous solution of zinc salt is dropped into an alkaline aqueous solution at a temperature of 60° C. or higher, and zinc oxide precipitates are formed at a final pH of 9 or higher, so that the average particle size is 0. A method is provided for producing ultrafine zinc oxide powder having a particle size of 0.02 to 0.05 μm.
またその好適な態様として、アルカリ水溶液に亜鉛塩の
水溶液を滴下した後に、３０分以上反応温度を６０℃以
上に保持する方法が提供される。A preferred embodiment thereof is a method in which the aqueous zinc salt solution is dropped into the alkaline aqueous solution and then the reaction temperature is maintained at 60° C. or higher for 30 minutes or more.
本発明に使用される亜鉛塩の水溶液は、硫酸亜鉛、塩化
亜鉛、硝酸亜鉛等を水に溶かして調製される。また、本
発明に使用されるアルカリ溶液は、水酸化ナトリウム、
水酸化カリウム、水酸化リチウム等の強アルカリを水に
溶かして調製される。The aqueous solution of zinc salt used in the present invention is prepared by dissolving zinc sulfate, zinc chloride, zinc nitrate, etc. in water. In addition, the alkaline solution used in the present invention includes sodium hydroxide,
It is prepared by dissolving a strong alkali such as potassium hydroxide or lithium hydroxide in water.
なお、アンモニア水溶液は、亜鉛のヒドロシルを生成し
やすいため、更に、上記強アルカリ剤を加えて液性を調
整する必要がある。Since the ammonia aqueous solution tends to generate zinc hydrosil, it is necessary to further adjust the liquid properties by adding the strong alkaline agent mentioned above.
前記亜鉛塩およびアルカリ原料はいずれも市販品をその
まま用いることができる。反応に用いるこれらの亜鉛塩
およびアルカリの水溶液の濃度は０．０１〜１０モル／
１が好ましい。０．０１モル／〕未満の濃度では生産効
率が低下するため好ましくなく、また１０モル／１を超
えると反応効率が低下するので好ましくない。Commercially available products can be used as they are for both the zinc salt and the alkali raw material. The concentration of the zinc salt and alkali aqueous solution used in the reaction is 0.01 to 10 mol/
1 is preferred. A concentration of less than 0.01 mol/1 is undesirable because the production efficiency decreases, and a concentration of more than 10 mol/1 is undesirable because the reaction efficiency decreases.
また本発明において、結晶性の高い超微粒子酸化亜鉛粉
末を得るためには、亜鉛の水溶液をアルカリ水溶液に滴
下する際、最終ｐＨを９以上に調整する。ｐＨ９未満の
領域では亜鉛のヒドロシルが混在するため本発明の目的
とする良好な酸化亜鉛粉末が得られない。更に、本発明
においては、反応液中の加水分解を促進するために反応
温度を６０℃以上に調整する。６０℃未満では、亜鉛の
ヒドロシルが混合し、純度の高い超微粒子酸化亜鉛粉末
を得ることはできない。Further, in the present invention, in order to obtain ultrafine zinc oxide powder with high crystallinity, the final pH is adjusted to 9 or higher when dropping the zinc aqueous solution into the alkaline aqueous solution. In a pH range of less than 9, zinc hydrosyl is present, making it impossible to obtain a good zinc oxide powder, which is the object of the present invention. Furthermore, in the present invention, the reaction temperature is adjusted to 60°C or higher in order to promote hydrolysis in the reaction solution. If the temperature is lower than 60° C., zinc hydrosil will be mixed, making it impossible to obtain ultrafine zinc oxide powder with high purity.
亜鉛塩の水溶液の滴下が終った後さらに３０分以上反応
温度を保持することが好ましい。It is preferable to maintain the reaction temperature for an additional 30 minutes or more after the dropwise addition of the zinc salt aqueous solution is completed.
なお、亜鉛塩の水溶液にアルカリ水溶液を滴下すると生
成する酸化亜鉛の粒子が０．０５μｌより大きくなる傾
向があり、 ０．０２〜０．０５μ鰯の粒径を有する酸
化亜鉛粉末を得るのが難しい。Furthermore, when an alkaline aqueous solution is dropped into an aqueous solution of zinc salt, the particles of zinc oxide produced tend to be larger than 0.05 μl, making it difficult to obtain zinc oxide powder having a particle size of 0.02 to 0.05 μl. .
ここで得られた酸化亜鉛は平均粒径０．０２〜０．０５
μ■の超微粒子酸化亜鉛であり、水洗して塩類を除去し
た後、乾燥工程を経ることなく直接、水あるいは溶媒に
分散させて塗料、ペーストなどの添加材として利用する
ことができる。また、必要に応じて表面処理することに
より、更に分散性を高めることもできる。この場合にお
いても、乾燥工程を必要としないため液中での表面処理
が容易に行える。なお、表面処理は従来公知の方法を適
用することができる。The zinc oxide obtained here has an average particle size of 0.02 to 0.05
It is ultrafine zinc oxide with a particle size of μ■. After washing with water to remove salts, it can be directly dispersed in water or a solvent without going through a drying process and used as an additive for paints, pastes, etc. Moreover, the dispersibility can be further improved by surface treatment as necessary. Even in this case, surface treatment in liquid can be easily performed since no drying step is required. Note that a conventionally known method can be applied to the surface treatment.
本発明による酸化亜鉛粉末の製造方法によれば、焼成工
程を経ることなく、分散性に優れた超ｌＩＩ粒子酸化亜
鉛粉末を得ることができ、この粉末を利用すれば、可視
域での高い透明性と優れた紫外線遮断効果を有する塗膜
を製造することができる。According to the method for producing zinc oxide powder according to the present invention, it is possible to obtain a super lII particle zinc oxide powder with excellent dispersibility without going through a firing process. It is possible to produce a coating film that has high properties and excellent ultraviolet blocking effects.
更に１本発明による超微粒子酸化亜鉛粉末は５日焼は止
め化粧料、自動車、家具、光学材料等の紫外線遮断保護
膜に利用することができる。また、この粉末の分散液を
利用すると、塗料化、ペースト化を容易に行うことがで
きる。Furthermore, the ultrafine zinc oxide powder according to the present invention can be used in UV-blocking protective films for sunscreen cosmetics, automobiles, furniture, optical materials, etc. Further, by using this powder dispersion, it can be easily made into a paint or a paste.
前述の如く、従来の製造方法によって得られる酸化亜鉛
粉末は、塩基性炭酸亜鉛、シュウ酸亜鉛、水酸化亜鉛等
を脱水乾燥して焼成するために凝集し易く５分散性に劣
る。一方１本発明によって得られる超微粒子酸化亜鉛粉
末は、焼成しなくても高い結晶性を有し分散性に優れる
。As mentioned above, zinc oxide powder obtained by conventional manufacturing methods tends to aggregate and has poor dispersibility because basic zinc carbonate, zinc oxalate, zinc hydroxide, etc. are dehydrated and dried and then fired. On the other hand, the ultrafine zinc oxide powder obtained by the present invention has high crystallinity and excellent dispersibility even without firing.
実施例１
１００℃の水酸化ナトリウム水溶液（１モル／ｌ） １
９０ｃｃに硫酸亜鉛水溶液（１モル／１）ｌｏｏｃｃを
滴下した後、３０分間温度を１００℃に保持して超微粒
子酸化亜鉛を生成させた。このときの溶液のｐＨは９で
あった。Example 1 100°C sodium hydroxide aqueous solution (1 mol/l) 1
After dropping an aqueous zinc sulfate solution (1 mol/1) LOOC into 90 cc, the temperature was maintained at 100° C. for 30 minutes to generate ultrafine zinc oxide particles. The pH of the solution at this time was 9.
反応後、水洗により塩類を除去し、濾別、風乾した。こ
の粉末の比表面積をＢＥＴ法により測定したところ、比
表面積４０ｒｌ／ｇ、−次粒子径０．０３μ■の分散性
に優れた超微粒子酸化亜鉛粉末が得られた。After the reaction, salts were removed by washing with water, filtered, and air-dried. When the specific surface area of this powder was measured by the BET method, an ultrafine zinc oxide powder with excellent dispersibility and a specific surface area of 40 rl/g and a secondary particle size of 0.03 μm was obtained.
この粉末は、第１図の透過型電子顕微鏡写真に示すよう
に、粒子の凝集もなく分散性に優れている。As shown in the transmission electron micrograph of FIG. 1, this powder has excellent dispersibility without particle agglomeration.
また、これをＸ線回折法により測定したところ、第２図
に示すように、亜鉛のヒドロシルの生成もなく酸化亜鉛
の高い結晶性を示した。Furthermore, when this was measured by X-ray diffraction method, as shown in FIG. 2, no zinc hydrosyl was formed and the zinc oxide exhibited high crystallinity.
実施例２
６０℃の水酸化リチウム水溶液（１モル／Ｌ）２２０ｃ
ｃに硫酸亜鉛水溶液（１モル／ｌ） １００ｃｃを滴下
した後、３０分間温度を６０℃に保持して超微粒子酸化
亜鉛を生成させた。このときの溶液のｐＨは１２であっ
た。反応後、水洗により塩類を除去し濾別、風乾した。Example 2 Lithium hydroxide aqueous solution (1 mol/L) 220c at 60°C
After dropping 100 cc of an aqueous zinc sulfate solution (1 mol/l) into C, the temperature was maintained at 60° C. for 30 minutes to generate ultrafine zinc oxide particles. The pH of the solution at this time was 12. After the reaction, salts were removed by washing with water, filtered, and air-dried.
この粉末の比表面積をＢＥＴ法により測定したところ、
比表面積２５ｍ／ｇ、−次粒子径０．０４μｍの分散性
に優れた超微粒子酸化亜鉛粉末が得られた。When the specific surface area of this powder was measured by the BET method,
Ultrafine zinc oxide powder with excellent dispersibility and a specific surface area of 25 m/g and a secondary particle size of 0.04 μm was obtained.
実施例３
８０℃の水酸化カリウム水溶液（１モル／１）２２０ｃ
ｃに塩化亜鉛水溶液（１モル／１ＨＯＯｃｃを滴下した
後、３０分間温度を８０℃に保持して超微粒子酸化亜鉛
を生成させ、水洗により塩類を除去し濾別、風乾した。Example 3 Potassium hydroxide aqueous solution (1 mol/1) 220c at 80°C
After adding a zinc chloride aqueous solution (1 mol/1 HOOcc) dropwise to c, the temperature was maintained at 80° C. for 30 minutes to produce ultrafine zinc oxide particles. Salts were removed by washing with water, filtered, and air-dried.
この粉末の比表面積をＢＥＴ法により測定したところ、
比表面積２０ｍ／ｇ、−次粒子径０．０５μｍの分散性
に優れた超微粒子酸化亜鉛粉末が得られた。When the specific surface area of this powder was measured by the BET method,
Ultrafine zinc oxide powder with excellent dispersibility and a specific surface area of 20 m/g and a secondary particle size of 0.05 μm was obtained.
比較例１
４０℃の水酸化ナトリウム水溶液（１モル／１）２２０
ｃｃに硫酸亜鉛水溶液（１モル／１）１００ｃｃを滴下
した後、３０分間温度を４０℃に保持して沈澱を生成さ
せた。このときの溶液のｐＨは１２であった。反応後水
洗により塩類を除去し濾別、風乾した。この沈澱をＸ線
回折法により測定したとろ、酸化亜鉛とともに亜鉛のヒ
ドロシルの生成が見られた。Comparative Example 1 40°C sodium hydroxide aqueous solution (1 mol/1) 220
After dropping 100 cc of an aqueous zinc sulfate solution (1 mol/1) into the cc, the temperature was maintained at 40° C. for 30 minutes to form a precipitate. The pH of the solution at this time was 12. After the reaction, salts were removed by washing with water, filtered, and air-dried. When this precipitate was measured by X-ray diffraction, it was found that zinc oxide and zinc hydrosyl were formed.
比較例２
６０℃の塩化亜鉛水溶液（１モル／１）１００ｃｃに水
酸化ナトリウム水溶液（１モル／１）２２０ｃｃを滴下
した後、３０分間温度を６０℃に保持して酸化亜鉛を生
成させ（ρ旧２）、水洗により塩類を除去し濾別、風乾
した。Comparative Example 2 After dropping 220 cc of sodium hydroxide aqueous solution (1 mol/1) into 100 cc of zinc chloride aqueous solution (1 mol/1) at 60°C, the temperature was maintained at 60°C for 30 minutes to generate zinc oxide (ρ Former 2), salts were removed by washing with water, filtered, and air-dried.
この粉末の比表面積をＢＥＴ法により測定したところ、
比表面積１０ ｍ ／ ｇ 、−次粒子径０．１μｍで
あり。When the specific surface area of this powder was measured by the BET method,
It has a specific surface area of 10 m/g and a secondary particle size of 0.1 μm.
ここで得られた酸化亜鉛の粒子径は、実施例と比較して
大きかった。The particle size of the zinc oxide obtained here was larger than that in Examples.
第１図は実施例１で得られた超微粒子酸化亜鉛粉末の粒
子構造を示す透過型電子顕微鏡写真、第２図は同じ試料
のＸ線回折チャートである。FIG. 1 is a transmission electron micrograph showing the particle structure of the ultrafine zinc oxide powder obtained in Example 1, and FIG. 2 is an X-ray diffraction chart of the same sample.
Claims (2)
の水溶液を滴下し、最終ｐＨ９以上で酸化亜鉛の沈澱を
生成させて平均粒径０．０２〜０．０５μｍの超微粒子
酸化亜鉛粉末を製造することを特徴とする方法。(1) At a temperature of 60°C or higher, an aqueous solution of zinc salt is dropped into an aqueous alkaline solution, and at a final pH of 9 or higher, zinc oxide precipitates are formed to produce ultrafine zinc oxide powder with an average particle size of 0.02 to 0.05 μm. A method characterized by manufacturing.
、３０分以上反応温度を６０℃以上に保持する第１請求
項の製造方法。(2) The manufacturing method according to claim 1, wherein the reaction temperature is maintained at 60° C. or higher for 30 minutes or more after dropping the zinc salt aqueous solution into the alkaline aqueous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29242690A JPH04164814A (en) | 1990-10-30 | 1990-10-30 | Production of ultra-fine zinc oxide powder having excellent dispersibility |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29242690A JPH04164814A (en) | 1990-10-30 | 1990-10-30 | Production of ultra-fine zinc oxide powder having excellent dispersibility |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04164814A true JPH04164814A (en) | 1992-06-10 |
Family
ID=17781638
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29242690A Pending JPH04164814A (en) | 1990-10-30 | 1990-10-30 | Production of ultra-fine zinc oxide powder having excellent dispersibility |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04164814A (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH684387A5 (en) * | 1993-04-22 | 1994-09-15 | Greiter Ag | Cosmetic or pharmaceutical product for topical application to the skin and the mucous membranes |
| US5945211A (en) * | 1996-02-22 | 1999-08-31 | Mitsui Mining And Smelting Co., Ltd. | Composite material carrying zinc oxide fine particles adhered thereto and method for preparing same |
| EP1172334A1 (en) * | 1999-02-05 | 2002-01-16 | Showa Denko K K | Ultra-fine particles of zinc oxide, method for preparing the same and cosmetic comprising the same |
| WO2003048047A1 (en) * | 2001-12-07 | 2003-06-12 | Sung Park | A METHOD FOR PREPARING ZnO NANOPOWDER |
| US6710091B1 (en) | 1999-02-23 | 2004-03-23 | Bayer Aktiengesellschaft | Nanoparticulate, redispersible zinc oxide gels |
| US7371337B2 (en) * | 2003-09-22 | 2008-05-13 | Evonik Degussa Gmbh | Zinc oxide powder aggregates present in circular, ellipsoidal, linear and branched form |
| JP2009132599A (en) * | 2007-11-07 | 2009-06-18 | Sumitomo Metal Mining Co Ltd | Method for producing ultraviolet shielding material fine particle, ultraviolet shielding material fine particle dispersion, and ultraviolet shielding body |
| US7666506B2 (en) | 2005-06-03 | 2010-02-23 | Basf Se | Surface-modified metal oxides prepared by precipitation in the presence of a copolymer having N-vinylamide units, production processes and use thereof in cosmetic preparations |
| CN103408061A (en) * | 2013-07-25 | 2013-11-27 | 南京航空航天大学 | Preparation method for zinc oxide nanocrystalline |
| CN103482681A (en) * | 2013-09-22 | 2014-01-01 | 常州大学 | Method for preparing monodisperse spherical nano ZnO |
| CN104843764A (en) * | 2015-03-31 | 2015-08-19 | 南京工业大学 | Method for preparing nano zinc oxide by using fluidized calcinated alkali zinc carbonate |
-
1990
- 1990-10-30 JP JP29242690A patent/JPH04164814A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH684387A5 (en) * | 1993-04-22 | 1994-09-15 | Greiter Ag | Cosmetic or pharmaceutical product for topical application to the skin and the mucous membranes |
| US5945211A (en) * | 1996-02-22 | 1999-08-31 | Mitsui Mining And Smelting Co., Ltd. | Composite material carrying zinc oxide fine particles adhered thereto and method for preparing same |
| EP1172334A1 (en) * | 1999-02-05 | 2002-01-16 | Showa Denko K K | Ultra-fine particles of zinc oxide, method for preparing the same and cosmetic comprising the same |
| EP1172334A4 (en) * | 1999-02-05 | 2005-03-16 | Showa Denko Kk | Ultra-fine particles of zinc oxide, method for preparing the same and cosmetic comprising the same |
| JP4864205B2 (en) * | 1999-02-23 | 2012-02-01 | ランクセス・ドイチュランド・ゲーエムベーハー | Method for producing nano-sized zinc oxide particles |
| US6710091B1 (en) | 1999-02-23 | 2004-03-23 | Bayer Aktiengesellschaft | Nanoparticulate, redispersible zinc oxide gels |
| WO2003048047A1 (en) * | 2001-12-07 | 2003-06-12 | Sung Park | A METHOD FOR PREPARING ZnO NANOPOWDER |
| US7371337B2 (en) * | 2003-09-22 | 2008-05-13 | Evonik Degussa Gmbh | Zinc oxide powder aggregates present in circular, ellipsoidal, linear and branched form |
| US7666506B2 (en) | 2005-06-03 | 2010-02-23 | Basf Se | Surface-modified metal oxides prepared by precipitation in the presence of a copolymer having N-vinylamide units, production processes and use thereof in cosmetic preparations |
| JP2009132599A (en) * | 2007-11-07 | 2009-06-18 | Sumitomo Metal Mining Co Ltd | Method for producing ultraviolet shielding material fine particle, ultraviolet shielding material fine particle dispersion, and ultraviolet shielding body |
| CN103408061A (en) * | 2013-07-25 | 2013-11-27 | 南京航空航天大学 | Preparation method for zinc oxide nanocrystalline |
| CN103482681A (en) * | 2013-09-22 | 2014-01-01 | 常州大学 | Method for preparing monodisperse spherical nano ZnO |
| CN104843764A (en) * | 2015-03-31 | 2015-08-19 | 南京工业大学 | Method for preparing nano zinc oxide by using fluidized calcinated alkali zinc carbonate |
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