JPH01286919A - Production of fine particle of zinc oxide - Google Patents
Production of fine particle of zinc oxideInfo
- Publication number
- JPH01286919A JPH01286919A JP11472288A JP11472288A JPH01286919A JP H01286919 A JPH01286919 A JP H01286919A JP 11472288 A JP11472288 A JP 11472288A JP 11472288 A JP11472288 A JP 11472288A JP H01286919 A JPH01286919 A JP H01286919A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- metallic
- temperature
- zinc oxide
- jetted
- 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 44
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 22
- 239000010419 fine particle Substances 0.000 title claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000011701 zinc Substances 0.000 claims abstract description 40
- 239000007789 gas Substances 0.000 claims abstract description 24
- 238000002485 combustion reaction Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000011261 inert gas Substances 0.000 claims abstract description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 32
- 229910052725 zinc Inorganic materials 0.000 claims description 32
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000012159 carrier gas Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 description 17
- 239000002184 metal Substances 0.000 description 17
- 239000002245 particle Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000007664 blowing Methods 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910000809 Alumel Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 244000261422 Lysimachia clethroides Species 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000013040 rubber vulcanization Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 230000000475 sunscreen effect Effects 0.000 description 1
- 239000000516 sunscreening agent Substances 0.000 description 1
- 229910000859 α-Fe 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、比表面積が大きく、かつ、過剰亜鉛が少ない
酸化亜鉛微粒子の製造方法の改良に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to an improvement in a method for producing zinc oxide fine particles having a large specific surface area and a small amount of excess zinc.
酸化亜鉛粒子は、広い用途を有する工業製品で、例えば
、ゴムの加硫促進剤、塗料、触媒、医薬品、電子写真用
感光材料、ファンデーション、クリーム等の化粧品、バ
リスター、フェライト等の電子部品材料などに用いられ
ている。Zinc oxide particles are industrial products with a wide range of uses, such as rubber vulcanization accelerators, paints, catalysts, pharmaceuticals, electrophotographic photosensitive materials, cosmetics such as foundations and creams, and electronic component materials such as varistors and ferrites. It is used for such things.
このような用途に用いられる酸化亜鉛はできるだけ微粒
であること、即ち粒子の比表面積が大きいこと、及びそ
の純度が高いことが必要である。Zinc oxide used for such purposes needs to be as fine as possible, that is, the particles need to have a large specific surface area and have high purity.
従来、酸化亜鉛の製造方法としては次に述べる乾式法が
知られている。即ち、この方法は、酸素を含有する雰囲
気中に金属亜鉛蒸気をキャリアガスとしての不活性ガス
と共に噴出させて導入して金属亜鉛を酸化燃焼させ、得
られた酸化亜鉛を急冷するというものである。Conventionally, the following dry method is known as a method for producing zinc oxide. That is, in this method, metallic zinc vapor is jetted and introduced together with an inert gas as a carrier gas into an oxygen-containing atmosphere to oxidize and burn metallic zinc, and the obtained zinc oxide is rapidly cooled. .
しかし、上記方法によって得られる酸化亜鉛の粒子は、
比表面積が２５ｒｒｆ／ｇより小さく、また、含有され
る過剰亜鉛が重量にて２０ｐ９ｒａより大きいために、
粒度においても純度においても充分満足し得るものでは
なかった。However, the zinc oxide particles obtained by the above method are
Since the specific surface area is smaller than 25rrf/g and the excess zinc contained is larger than 20p9ra by weight,
Both particle size and purity were not fully satisfactory.
本発明の目的は、このような従来の方法を改良して、こ
の方法の問題点を解決し、比表面積が２５ｏｆ／ｇ以上
で、含有される過剰亜鉛が重量にて２０ｐｐｍ以下の酸
化亜鉛微粒子を製造し得る方法を提供することにある。The purpose of the present invention is to improve the conventional method, solve the problems of this method, and produce zinc oxide fine particles with a specific surface area of 25 of/g or more and an excess zinc content of 20 ppm or less by weight. The objective is to provide a method for manufacturing.
本発明は、前記問題点を解決するものとして、酸素を含
有する雰囲気中に金属亜鉛蒸気をキャリアガスとしての
不活性ガスと共に噴出させて金属亜鉛を酸化燃焼させ、
得られた酸化亜鉛を急冷する方法において、該噴出ガス
に該金属亜鉛蒸気以外の可燃性ガスを含有させることな
く、該噴出ガスの温度を８００℃以上とし、がっ、該燃
焼の温度を１３００〜１６００℃とすることを特徴とす
るものである。The present invention solves the above-mentioned problems by oxidizing and burning metal zinc by spouting metal zinc vapor together with an inert gas as a carrier gas into an oxygen-containing atmosphere.
In the method of rapidly cooling the obtained zinc oxide, the temperature of the ejected gas is set to 800°C or higher without causing the ejected gas to contain any flammable gas other than the metal zinc vapor, and the temperature of the combustion is increased to 1300°C. It is characterized by a temperature of ~1600°C.
金属亜鉛を加熱して蒸発させて得られた金属亜鉛蒸気は
ノズルからキャリアガスとして窒素、アルゴン等の不活
性ガスと共に燃焼室へ噴出する。Metal zinc vapor obtained by heating and evaporating metal zinc is ejected from a nozzle into a combustion chamber as a carrier gas together with an inert gas such as nitrogen or argon.
燃焼室の雰囲気は酸素を含有するものであり、空気又は
酸素を前記ノズルとは別のノズルより供給する。このよ
うな雰囲気中に噴出された前記金属亜鉛蒸気は直ちに酸
化燃焼して酸化亜鉛を生成する。生成した酸化亜鉛は冷
却するまでに団塊状粒子に焼結するのを抑制するため急
冷した後、捕集される。The atmosphere in the combustion chamber contains oxygen, and air or oxygen is supplied from a nozzle different from the above-mentioned nozzle. The metallic zinc vapor ejected into such an atmosphere is immediately oxidized and burned to produce zinc oxide. The generated zinc oxide is rapidly cooled to prevent it from sintering into nodular particles before being cooled, and then collected.
本発明においては、前記燃焼室に噴出される金属亜鉛蒸
気および不活性ガスに該金属亜鉛蒸気以外の可燃性ガス
を含有させない。本出願人は、先に、この可燃性ガスを
含有させることにより、比表面積が大きく、過剰亜鉛が
少ない酸化亜鉛微粒子の製造方法を出願した（特願昭６
ｌ−２９４７５２）。しかし、本発明は、金属亜鉛蒸気
以外の可燃性ガスを含有させることなく、前記目的を達
成することができる。そのためには、（１）噴出ガスの
温度を８００℃以上とすること、（２）燃焼の温度を１
３００〜１６００℃とすることが必要である。噴出ガス
は、金属亜鉛蒸気と不活性ガスとを、適宜混合した後加
熱するか、あるいは別々に加熱した後混合するかされる
が、この噴出ガスの温度が８００℃未満では、前記目的
である比表面積および過剰亜鉛の条件のうち高々、いず
れか１つしか達成され得ない場合が多くなる。また、燃
焼の温度は、前記噴出ガスの温度、噴出ガス中の金属亜
鉛蒸気と不活性ガスの割合などを調整することにより制
御できるが、この温度が１３００℃未満では、金属亜鉛
蒸気の酸化反応が充分でなく、生成する粒子中の過剰亜
鉛が多くなり易い。一方、この温度が１６００’Ｃを超
えると、粒子の成長速度が増大し過ぎ、生成する粒子の
比表面積が小さくなり易い、この温度を１３００〜１６
００℃に制御するためには、噴出ガス中の金属亜鉛蒸気
（重量）と不活性ガス（容ｉｔ）の比は１７６〜３／２
ｇ／ｊ！とするのが好ましい。In the present invention, the metal zinc vapor and inert gas ejected into the combustion chamber do not contain any combustible gas other than the metal zinc vapor. The present applicant previously filed an application for a method for producing zinc oxide fine particles that have a large specific surface area and a small amount of excess zinc by containing this flammable gas (patent application filed in 1983).
l-294752). However, the present invention can achieve the above object without containing any flammable gas other than metal zinc vapor. To achieve this, (1) the temperature of the ejected gas must be set to 800°C or higher, and (2) the combustion temperature must be set to 1.
It is necessary to set it as 300-1600 degreeC. The ejected gas is heated after appropriately mixing metal zinc vapor and inert gas, or heated separately and then mixed, but if the temperature of this ejected gas is less than 800 ° C., the above purpose is not met. In many cases, only one of the specific surface area and excess zinc conditions can be achieved. Furthermore, the combustion temperature can be controlled by adjusting the temperature of the ejected gas, the ratio of metal zinc vapor and inert gas in the ejected gas, etc., but if this temperature is less than 1300°C, the oxidation reaction of the metal zinc vapor will occur. is insufficient, and the resulting particles tend to contain a large amount of excess zinc. On the other hand, if this temperature exceeds 1600'C, the growth rate of particles increases too much and the specific surface area of the generated particles tends to become small.
In order to control the temperature to 00℃, the ratio of metal zinc vapor (weight) to inert gas (volume) in the ejected gas should be 176 to 3/2.
g/j! It is preferable that
このようにすることにより、比表面積および過剰亜鉛の
いずれの条件をも満足させ得るのは、微粒子成長の出発
点である臨界核の径および生成頻度が夫々より小に、よ
り大になったことによるものと推察される。By doing this, both the specific surface area and excess zinc conditions can be satisfied because the diameter and generation frequency of critical nuclei, which are the starting point for fine particle growth, have become smaller and larger, respectively. It is assumed that this is due to the following.
このような乾式法で得られた微粒で純度の高い酸化亜鉛
粒子は、電子写真用感光材料として好適である。また、
ノビが良いことや皮膚の紫外線防御等に好適である点で
、ファンデーション、日焼は止めクリーム等の化粧品の
原料としても最適である。Fine and highly pure zinc oxide particles obtained by such a dry method are suitable as a light-sensitive material for electrophotography. Also,
It is also ideal as a raw material for cosmetics such as foundations and sunscreen creams because of its good elasticity and its ability to protect the skin from ultraviolet rays.
以下、本発明を実施例および比較例によって具体的に説
明する。Hereinafter, the present invention will be specifically explained using Examples and Comparative Examples.
実施例１
第１図は本発明方法の実施に用いた装置の概略図である
。図において、燃焼室１は、抵抗発熱体を取り付けた電
気炉２の上に断熱レンガにより内部を一辺５０ｃｌｌの
立方体状に形成した。電気炉２には、上部に金属亜鉛蒸
気を噴出するノズル３を有する黒鉛ルツボ４が載置され
る。この黒鉛ルツボ４内に装入された金属亜鉛（純度９
９．９９重量％）が、電気炉２により加熱され溶解され
る。溶解した金属亜鉛浴面上にキャリアガスとしての窒
素を導入することができる導入管５が、黒鉛ルツボ４に
設けられている。窒素が導入管５により導入されると、
黒鉛ルツボ４内の金属亜鉛浴面上で金属亜鉛蒸気と混合
されると同時に、電気炉２により所望温度に加熱された
後、ノズル３から噴出する。ノズル３の周囲には、燃焼
室１内を酸素を含有する雰囲気に維持するために旋回流
の酸素を吹き込むための風箱６が、また、ノズル３付近
で着火して生じたフレームの直上には、生成した酸化亜
鉛を急冷するための冷却用空気吹込管７が設けである。Example 1 FIG. 1 is a schematic diagram of an apparatus used to carry out the method of the present invention. In the figure, a combustion chamber 1 was formed into a cubic shape of 50 cl on each side using insulating bricks on an electric furnace 2 equipped with a resistance heating element. A graphite crucible 4 is placed in the electric furnace 2 and has a nozzle 3 at the top for spouting metallic zinc vapor. The metal zinc charged in this graphite crucible 4 (purity 9
9.99% by weight) is heated and melted in the electric furnace 2. The graphite crucible 4 is provided with an introduction pipe 5 that can introduce nitrogen as a carrier gas onto the surface of the molten metal zinc bath. When nitrogen is introduced through the introduction pipe 5,
It is mixed with metal zinc vapor on the surface of the metal zinc bath in the graphite crucible 4, heated to a desired temperature by the electric furnace 2, and then jetted out from the nozzle 3. Around the nozzle 3, there is a wind box 6 for blowing swirling oxygen into the combustion chamber 1 to maintain an oxygen-containing atmosphere. A cooling air blowing pipe 7 is provided for rapidly cooling the produced zinc oxide.
燃焼室１の出口８は、グーズネック煙道９、分級ボック
ス１０、捕集装置を介して吸引ファンに接続している（
捕集装置と吸引ファンは図示せず）。The outlet 8 of the combustion chamber 1 is connected to a suction fan via a gooseneck flue 9, a classification box 10 and a collection device (
(Collection device and suction fan not shown).
第１図の装置によって、金属亜鉛を１０ｋｇ溶解し、風
箱６より酸素を５０１／分吹き込み、冷却用空気吹込管
７より空気を１６７１７分吹き込むことによって酸化亜
鉛を製造する実験を行なった。Using the apparatus shown in FIG. 1, an experiment was conducted to produce zinc oxide by melting 10 kg of metallic zinc, blowing oxygen at 501/min from the air box 6, and blowing air at 16,717 min from the cooling air blowing pipe 7.
その他の酸化亜鉛製造条件および実験により得られた酸
化亜鉛の品質特性を第１表に示す。Other zinc oxide production conditions and quality characteristics of zinc oxide obtained through experiments are shown in Table 1.
なお、第１表中、噴出ガスの温度および燃焼の温度は夫
々黒鉛ルツボ４内のノズル３直下でクロメル−アルメル
熱電対を使用して、ノズル３付近で着火して生じたフレ
ーム内で白金−白金ロジウム熱電対を使用して測定した
もので、燃焼の温度は得られた測定値のうち最も高いも
のである。In Table 1, the temperature of the ejected gas and the temperature of combustion are determined using a chromel-alumel thermocouple directly below the nozzle 3 in the graphite crucible 4, and a platinum-alumel thermocouple is used in the flame produced by ignition near the nozzle 3. Measured using a platinum-rhodium thermocouple, the temperature of combustion is the highest measured value obtained.
以上から明らかなように、本発明方法によれば、乾式法
により比表面積が２５ｒｒｒ／ｇ以上で、含有される過
剰亜鉛が重量にて２０ｐｐｍ以下の酸化亜鉛微粒子を製
造することができ、この方法は工業的実用性の高いもの
である。As is clear from the above, according to the method of the present invention, zinc oxide fine particles having a specific surface area of 25 rrr/g or more and containing 20 ppm or less of excess zinc by weight can be produced by a dry method. is of high industrial practicality.
第１図は本発明の実施例に用いた実験装置の概略図であ
る。
１・・・燃焼室、２・・・電気炉、３・・・ノズル、４
・・・黒鉛ルツボ、５・・・導入管、６・・・風箱、７
川冷却用空気吹込管。
特許出願人 住友金属鉱山株式会社
第１図FIG. 1 is a schematic diagram of an experimental apparatus used in an example of the present invention. 1... Combustion chamber, 2... Electric furnace, 3... Nozzle, 4
...Graphite crucible, 5...Introduction pipe, 6...Wind box, 7
Air blowing pipe for river cooling. Patent applicant Sumitomo Metal Mining Co., Ltd. Figure 1
Claims (1)
アガスとしての不活性ガスと共に噴出させて金属亜鉛を
酸化燃焼させ、得られた酸化亜鉛を急冷する方法におい
て、該噴出ガスに該金属亜鉛蒸気以外の可燃性ガスを含
有させることなく、該噴出ガスの温度を８００℃以上と
し、かつ、該燃焼の温度を１３００〜１６００℃とする
ことを特徴とする酸化亜鉛微粒子の製造方法。(1) In a method in which metallic zinc vapor is ejected together with an inert gas as a carrier gas into an oxygen-containing atmosphere to oxidize and burn the metallic zinc, and the resulting zinc oxide is rapidly cooled, the ejected gas is mixed with the metallic zinc. A method for producing zinc oxide fine particles, characterized in that the temperature of the ejected gas is 800°C or higher, and the combustion temperature is 1300 to 1600°C, without containing any flammable gas other than steam.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11472288A JPH01286919A (en) | 1988-05-13 | 1988-05-13 | Production of fine particle of zinc oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11472288A JPH01286919A (en) | 1988-05-13 | 1988-05-13 | Production of fine particle of zinc oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01286919A true JPH01286919A (en) | 1989-11-17 |
Family
ID=14644983
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11472288A Pending JPH01286919A (en) | 1988-05-13 | 1988-05-13 | Production of fine particle of zinc oxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01286919A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5618580A (en) * | 1992-12-28 | 1997-04-08 | Kao Corporation | Method for producing ceramic fine particles and apparatus used therefor |
| WO2000046152A1 (en) * | 1999-02-05 | 2000-08-10 | Showa Denko K.K. | Ultra-fine particles of zinc oxide, method for preparing the same and cosmetic comprising the same |
| US6827758B2 (en) | 2001-05-30 | 2004-12-07 | Tdk Corporation | Method for manufacturing magnetic metal powder, and magnetic metal powder |
| JP2010105907A (en) * | 2008-09-30 | 2010-05-13 | Ube Material Industries Ltd | Method and apparatus for producing zinc oxide |
-
1988
- 1988-05-13 JP JP11472288A patent/JPH01286919A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5618580A (en) * | 1992-12-28 | 1997-04-08 | Kao Corporation | Method for producing ceramic fine particles and apparatus used therefor |
| WO2000046152A1 (en) * | 1999-02-05 | 2000-08-10 | Showa Denko K.K. | Ultra-fine particles of zinc oxide, method for preparing the same and cosmetic comprising the same |
| JP4462523B2 (en) * | 1999-02-05 | 2010-05-12 | 昭和電工株式会社 | Ultrafine zinc oxide, method for producing the same, and cosmetics using the same |
| US6827758B2 (en) | 2001-05-30 | 2004-12-07 | Tdk Corporation | Method for manufacturing magnetic metal powder, and magnetic metal powder |
| US7416795B2 (en) | 2001-05-30 | 2008-08-26 | Tdk Corporation | Method for manufacturing magnetic metal powder, and magnetic metal powder |
| JP2010105907A (en) * | 2008-09-30 | 2010-05-13 | Ube Material Industries Ltd | Method and apparatus for producing zinc oxide |
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