JPH02217308A - Production of oxide powder - Google Patents
Production of oxide powderInfo
- Publication number
- JPH02217308A JPH02217308A JP3974889A JP3974889A JPH02217308A JP H02217308 A JPH02217308 A JP H02217308A JP 3974889 A JP3974889 A JP 3974889A JP 3974889 A JP3974889 A JP 3974889A JP H02217308 A JPH02217308 A JP H02217308A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- oxide powder
- gas
- metal powder
- combustion chamber
- 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.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 119
- 238000004519 manufacturing process Methods 0.000 title claims description 23
- 239000007789 gas Substances 0.000 claims abstract description 45
- 229910052751 metal Inorganic materials 0.000 claims abstract description 38
- 239000002184 metal Substances 0.000 claims abstract description 38
- 238000002485 combustion reaction Methods 0.000 claims abstract description 37
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000012159 carrier gas Substances 0.000 claims abstract description 21
- 230000001590 oxidative effect Effects 0.000 claims abstract description 10
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000003085 diluting agent Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005188 flotation Methods 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 9
- 239000001301 oxygen Substances 0.000 abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 abstract description 9
- 239000000377 silicon dioxide Substances 0.000 abstract description 8
- 229910052681 coesite Inorganic materials 0.000 abstract description 7
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 7
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 7
- 229910052682 stishovite Inorganic materials 0.000 abstract description 7
- 229910052905 tridymite Inorganic materials 0.000 abstract description 7
- 230000007935 neutral effect Effects 0.000 abstract description 6
- 238000007865 diluting Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 239000011863 silicon-based powder Substances 0.000 abstract description 5
- 239000001257 hydrogen Substances 0.000 abstract description 4
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 4
- 229910001873 dinitrogen Inorganic materials 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 238000010790 dilution Methods 0.000 abstract description 2
- 239000012895 dilution Substances 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 229910044991 metal oxide Inorganic materials 0.000 abstract 1
- 150000004706 metal oxides Chemical class 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 30
- 238000000034 method Methods 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000009841 combustion method Methods 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000011449 brick Substances 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000011144 upstream manufacturing Methods 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- -1 etc. Chemical compound 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Oxygen, Ozone, And Oxides In General (AREA)
- Silicon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、金属粉末燃焼法により酸化物粉末を製造する
酸化物粉末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 oxide powder by producing oxide powder by a metal powder combustion method.
［従来の技術］
従来の金属粉末燃焼法による酸化物粉末の製造方法が特
開昭６３−７９７１２号公報に開示されている。この製
造方法は、燃焼室にキャリアガスとともに金属粉末を供
給する金属粉末供給工程と、燃焼室内において酸化性雰
囲気下で金属粉末の酸化反応による化学炎を形成して酸
化物粉末を１ｑる燃焼工程と、得られた酸化物粉末を捕
集する捕集工程とからなるものである。この製造方法に
よって、高純度のＡＱ２０３粉末やＳｉＯ２粉末等を粒
度分布にばらつきなく、安価に、かつ連続的に製造する
ことができる。[Prior Art] A method for producing oxide powder using a conventional metal powder combustion method is disclosed in JP-A-63-79712. This manufacturing method consists of a metal powder supply step in which metal powder is supplied together with a carrier gas into a combustion chamber, and a combustion step in which 1q of oxide powder is produced by forming a chemical flame through an oxidation reaction of the metal powder in an oxidizing atmosphere in the combustion chamber. and a collection step of collecting the obtained oxide powder. By this manufacturing method, high purity AQ203 powder, SiO2 powder, etc. can be manufactured inexpensively and continuously without variation in particle size distribution.
［発明が解決しようとする課題］
ところが、前記従来の製造方法で製造された酸化物粉末
は、ＰＨ４〜５の酸性を示すことが確認された。このた
め、前記従来の製造方法で製造されたＡ９２０３粉末や
ＳｉＯ２粉末等をエポキシ樹脂等のポリマーに対する充
填材として使用すると、これらの粉末がポリマーと反応
しにくく、ポリマー中で均一に混合できないという不具
合があった。一般に、バイヤ法で製造されたＡ５？ ２
０３粉末やカセイソーダ法で製造されたＳｉＯ２粉末は
アルカリ性を示し、天然のシリカは中性を示すように、
金属粉末燃焼法以外の方法で製造された酸化物粉末はア
ルカリ性又は中性である。こうした金属粉末燃焼法以外
の方法で製造された中性の酸化物粉末を充填材とすれば
、ポリマー中で均一に混合できないなどという不具合は
ない。したがって、上記従来の金属粉末燃焼法による製
造方法で製造された酸化物粉末は充填材として用いるこ
とが困難であった。[Problems to be Solved by the Invention] However, it has been confirmed that the oxide powder produced by the conventional production method exhibits acidity with a pH of 4 to 5. For this reason, when A9203 powder, SiO2 powder, etc. manufactured by the conventional manufacturing method are used as fillers for polymers such as epoxy resins, these powders are difficult to react with the polymer, and there is a problem that they cannot be mixed uniformly in the polymer. was there. In general, A5 manufactured by the Bayer method? 2
03 powder and SiO2 powder manufactured by the caustic soda method show alkalinity, while natural silica shows neutrality.
Oxide powders produced by methods other than metal powder combustion are alkaline or neutral. If a neutral oxide powder produced by a method other than the metal powder combustion method is used as a filler, there will be no problem such as inability to uniformly mix it in the polymer. Therefore, it has been difficult to use the oxide powder produced by the conventional metal powder combustion method as a filler.
本発明は上記のような従来の不具合に鑑みてなされたも
のであって、中性で高純度の酸化物粉末を粒度分布にば
らつきなく、安価に、かつ連続的に製造することができ
る製造方法を提供することを目的とする。The present invention has been made in view of the above-mentioned conventional problems, and provides a manufacturing method that can inexpensively and continuously manufacture neutral, high-purity oxide powder without variation in particle size distribution. The purpose is to provide
［課題を解決するための手段］
本発明に係る酸化物粉末の製造方法は、燃焼室に窒素を
含有するキャリアガスとともに金属粉末を供給する金属
粉末供給工程と、該燃焼室内においてキャリアガスとと
もに該金属粉末を酸化性雰囲気下で燃焼させることによ
り第１酸化物粉末を得る燃焼工程と、該燃焼室の下流側
において、窒素を含有する雰囲気を希釈する希釈ガスを
供給するとともに該第１酸化物粉末を加熱してＮＯｘの
付着量が減少した酸化物粉末を得る浮遊工程と、該酸化
物粉末を捕集する捕集工程とからなることを特徴とする
ものである。[Means for Solving the Problems] The method for producing oxide powder according to the present invention includes a metal powder supply step of supplying metal powder together with a carrier gas containing nitrogen into a combustion chamber, and a step of supplying metal powder together with a carrier gas containing nitrogen in the combustion chamber. a combustion step of obtaining a first oxide powder by burning metal powder in an oxidizing atmosphere; supplying a diluent gas to dilute a nitrogen-containing atmosphere on the downstream side of the combustion chamber; This method is characterized by comprising a floating step in which the powder is heated to obtain an oxide powder with a reduced amount of attached NOx, and a collecting step in which the oxide powder is collected.
金属粉末供給工程は、窒素を含有するキャリアガスとと
もに金属粉末を燃焼室に供給する工程である。この金属
粉末供給工程としては、従来の方法を実施することがで
きる。窒素を含有するキャリアガスとしては、Ｎ２ガス
や空気を用いることができる。金属粉末としては、アル
ミニウム、マグネシウム、シリコン、ジルコニウム、チ
タン等の粉末、その他ムライト組成に調合したアルミニ
ウム粉末とシリコン粉末、スピネル組成に調合したマグ
ネシウム粉末とアルミニウム粉末、コージェライト組成
に調合したアルミニウム粉末、マグネシウム粉末及びシ
リコン粉末等を用いることができる。The metal powder supply step is a step of supplying metal powder to the combustion chamber together with a carrier gas containing nitrogen. A conventional method can be implemented as this metal powder supply step. As the carrier gas containing nitrogen, N2 gas or air can be used. Metal powders include powders of aluminum, magnesium, silicon, zirconium, titanium, etc., aluminum powder and silicon powder blended in a mullite composition, magnesium powder and aluminum powder blended in a spinel composition, aluminum powder blended in a cordierite composition, Magnesium powder, silicon powder, etc. can be used.
燃焼工程は、燃焼室内においてキャリアが又とともに金
属粉末を酸化性雰囲気下で燃焼させ、第１酸化物粉末を
得る工程である。この燃焼工程としては、従来の方法を
実施することができる。The combustion step is a step in which the metal powder is burned in an oxidizing atmosphere together with the carrier in the combustion chamber to obtain the first oxide powder. This combustion step can be carried out using conventional methods.
浮遊工程は、燃焼室の下流側において窒素を含有する雰
囲気を希釈する希釈ガスを供給するとともに第１酸化物
粉末を加熱し、ＮＯＸの付＠聞が減少した酸化物粉末を
得る工程である。希釈ガスとしては、キャリアガスにＮ
２ガスを用いた場合には空気やアルゴンガス等の不活性
ガスを用いることができ、キャリアガスに空気を用いた
場合には不活性ガスを用いることができる。第１酸化物
粉末を加熱する温度は、燃焼工程における温度より低温
であるが、窒素酸化物が容易に粒子から分離するような
高温であることが好ましい。ただし、第１酸化物粉末が
互いに衝突して焼結又は溶融する程高温に加熱すること
は好ましくないため、製造する酸化物粉末の焼結又は溶
融温度の２／３以下の温度に加熱することが好ましい。The flotation process is a process in which a diluent gas is supplied to dilute the nitrogen-containing atmosphere on the downstream side of the combustion chamber, and the first oxide powder is heated to obtain an oxide powder with reduced NOx content. As a diluent gas, N is added to the carrier gas.
When two gases are used, an inert gas such as air or argon gas can be used, and when air is used as a carrier gas, an inert gas can be used. The temperature at which the first oxide powder is heated is lower than the temperature during the combustion step, but preferably at a high temperature such that the nitrogen oxides are easily separated from the particles. However, it is not preferable to heat the first oxide powder to such a high temperature that it collides with each other and sinters or melts, so it should be heated to a temperature that is 2/3 or less of the sintering or melting temperature of the oxide powder to be manufactured. is preferred.
例えば、Ｓ０２粉末を製造する場合には約１０００℃以
下、ＡＱ ２０３粉末を製造する場合には約１４００℃
以下が好ましい。For example, when manufacturing S02 powder, the temperature is about 1000°C or less, and when manufacturing AQ 203 powder, it is about 1400°C.
The following are preferred.
捕集工程は酸化物粉末を捕集する工程である。The collection process is a process of collecting oxide powder.
この捕集工程としては、従来の方法を実施することがで
きる。A conventional method can be implemented as this collection step.
本発明の製造方法を実施するための製造装置としては、
燃焼室を内部に形成する第１反応容器と、燃焼室にキャ
リアガスとともに金属粉末を供給する金属粉末供給装置
と、燃焼室内へ着火用ガス等を供給する着火用ガス供給
装置と、燃焼室の下流側において浮遊工程を実施する浮
遊室を内部に形成する第２反応容器と、浮遊室内へ希釈
ガスを供給する希釈ガス供給装置と、浮遊室内を加熱す
る加熱装置と、製造した酸化物粉末を捕集する捕集装置
とから構成することができる。Manufacturing equipment for carrying out the manufacturing method of the present invention includes:
a first reaction vessel that forms a combustion chamber therein; a metal powder supply device that supplies metal powder together with a carrier gas to the combustion chamber; an ignition gas supply device that supplies ignition gas and the like into the combustion chamber; A second reaction vessel in which a floating chamber is formed in which a floating process is carried out on the downstream side, a diluting gas supply device that supplies diluent gas into the floating chamber, a heating device that heats the inside of the floating chamber, and the produced oxide powder. It can be composed of a collection device that collects the water.
第１及び第２反応容器は、アルミナレンガなどの断熱材
料で内張すされていることが好ましい。Preferably, the first and second reaction vessels are lined with a heat insulating material such as alumina brick.
なお、第１及び第２反応容器を一体とし、燃焼室と浮遊
室とを一つの反応容器で形成することもできる。Note that the first and second reaction vessels may be integrated to form the combustion chamber and the floating chamber in one reaction vessel.
金属粉末供給装置は、金属粉末を収納するホッパなどの
供給源と、キャリアガスを供給するキャリアガス供給管
と、燃焼室にキャリアガスとともに金属粉末を供給する
供給パイプとから構成することができる。The metal powder supply device can be composed of a supply source such as a hopper that stores metal powder, a carrier gas supply pipe that supplies carrier gas, and a supply pipe that supplies the metal powder together with the carrier gas to the combustion chamber.
着火用ガス供給装置が供給する着火用ガスとしては、メ
タンガス、プロパンガス等の炭化水素系ガスや一酸化炭
素ガス、ガス状に噴霧した重油等の液体燃料を用いるこ
とができる。着火用ガス供給装置は、空気や酸素ガス等
の酸化物粉末を構成する酸化性ガスを着火用ガスと同時
に供給することもできる。As the ignition gas supplied by the ignition gas supply device, a hydrocarbon gas such as methane gas or propane gas, carbon monoxide gas, or a liquid fuel such as heavy oil sprayed in a gaseous state can be used. The ignition gas supply device can also supply an oxidizing gas constituting the oxide powder, such as air or oxygen gas, at the same time as the ignition gas.
希釈ガス供給装置が供給する希釈ガスによって、第１酸
化物粉末を加熱する所定温度まで浮遊室内を下げること
もできる。The inside of the floating chamber can be lowered to a predetermined temperature at which the first oxide powder is heated by the diluting gas supplied by the diluting gas supply device.
加熱装置としては、Ｈ２と０２との反応により加熱する
装置を使用することが好ましい。As the heating device, it is preferable to use a device that heats by a reaction between H2 and 02.
捕集装置は集塵機を用いることができる。集塵機として
は、電気式集塵機、バグフィルタ、捕集ドラム式微粉末
捕集装置などを用いることができる。A dust collector can be used as the collection device. As the dust collector, an electric dust collector, a bag filter, a collection drum type fine powder collection device, etc. can be used.
［作用］
金属粉末供給工程においてキャリアガスとともに燃焼室
に供給された金属粉末は、燃焼工程によって酸化性雰囲
気下で金属粉末の酸化反応による化学炎を形成して燃焼
され、第一酸化物粉末となる。この第１１１化物粉末は
ＰＨ４〜５の酸性を示す。発明者は、鋭意研究の結果、
第１酸化物粉末が酸性である原因が表面に付着するＮＯ
Ｘにあることを発見した。ここに、ＮＯＸは、Ｎ０１Ｎ
０２、Ｎ２０などの窒素酸化物をいい、２０００℃程度
以上の高温で発生しやすい。つまり、金属粉末の燃焼と
同時に燃焼室に供給された窒素を含有するキャリアガス
は、酸化性雰囲気下、金属粉末が燃焼するときに発する
高温の熱によって酸化され、ＮＯＸを生じる。このため
、燃焼室内はＮＯｘを含有する雰囲気となっている。し
たがって、製造された第１酸化物粉末の表面にはＮＯＸ
が付着する。このとき、第１酸化物粉末に付着するＮＯ
ｘは、雰囲気中のＮＯＸの濃度に比例して太きくなる。[Function] The metal powder supplied to the combustion chamber together with the carrier gas in the metal powder supply process is combusted by forming a chemical flame due to the oxidation reaction of the metal powder in an oxidizing atmosphere in the combustion process, and becomes the first oxide powder. Become. This 111th compound powder exhibits acidity with a pH of 4 to 5. As a result of intensive research, the inventor discovered
The reason why the first oxide powder is acidic is NO adhering to the surface.
I discovered something about X. Here, NOX is N01N
It refers to nitrogen oxides such as 02, N20, etc., and is likely to be generated at high temperatures of about 2000°C or higher. That is, the nitrogen-containing carrier gas supplied to the combustion chamber at the same time as the metal powder is combusted is oxidized by the high temperature heat generated when the metal powder is combusted in an oxidizing atmosphere, producing NOx. Therefore, the inside of the combustion chamber has an atmosphere containing NOx. Therefore, NOx is present on the surface of the first oxide powder produced.
is attached. At this time, NO attached to the first oxide powder
x increases in proportion to the concentration of NOX in the atmosphere.
また、第１酸化物粉末の表面に存在するＮＯｘと雰囲気
中のＮＯｘとの平衡状態は、高温では「囲気中にＮＯｘ
が浮遊した状態で安定となる。このため、本発明では、
燃焼室の下流側における浮遊工程において、希釈ガスを
供給することによってＮＯｘを含有する雰囲気中のＮＯ
ｘ８度を希釈し、これにより第１酸化物粉末に付着した
ＮＯｘをＮＯｘの濃度の低い雰囲気中に飛散させる。こ
うして、ＮＯｘの付着最が減少した酸化物粉末が得られ
る。次いで、捕集工程によって酸化物粉末を捕集する。Furthermore, at high temperatures, the equilibrium state between NOx present on the surface of the first oxide powder and NOx in the atmosphere is
becomes stable in a floating state. Therefore, in the present invention,
In the flotation process downstream of the combustion chamber, NO in the NOx-containing atmosphere is removed by supplying diluent gas.
By diluting the first oxide powder by 8 degrees, NOx adhering to the first oxide powder is scattered into an atmosphere with a low NOx concentration. In this way, an oxide powder with reduced NOx adhesion is obtained. Next, the oxide powder is collected by a collection process.
なお、前述のようにＮＯｘはキャリアガス中の窒素が燃
焼室内において金属粉末とともに酸化性雰囲気下で燃焼
するために酸化物粉末、相付着する。Note that, as described above, NOx is attached to the oxide powder because nitrogen in the carrier gas burns in an oxidizing atmosphere together with the metal powder in the combustion chamber.
したがって、キャリアガスとして、例えば、アルゴンガ
ス等の窒素を含有しないガスを使用すれば酸化物粉末が
酸性になることを防止できる。しかし、アルゴンガス等
は非常に高価であり、入手も困難な場合があるため、キ
ャリアガスにアルゴンガス等を用いることは生産上はと
んど行なわれず、安価な窒素ガスや空気をキャリアガス
として使用することが多い。このため、発明者は、キャ
リアガスとして安価で入手が容易な空気、窒素ガス等を
使用しつつ、中性の酸化物粉末を製造できる製造方法を
発明したのである。Therefore, if a gas not containing nitrogen, such as argon gas, is used as the carrier gas, the oxide powder can be prevented from becoming acidic. However, argon gas is very expensive and sometimes difficult to obtain, so argon gas is rarely used as a carrier gas in production, and cheap nitrogen gas or air is used as a carrier gas. Often used. For this reason, the inventor invented a manufacturing method that can produce neutral oxide powder while using cheap and easily available air, nitrogen gas, etc. as a carrier gas.
［実施例］
以下、本発明を具体化した実施例を図面を参照しつつ説
明する。[Example] Hereinafter, an example embodying the present invention will be described with reference to the drawings.
まず、本実施例を実施するためのｌ造装置について説明
する。この製造装置は、第１図に概略構成図を示すよう
に、第１反応容器１と、この第１反応容器１の上流側に
連結された供給パイプ２０をもつ金属粉末供給装置２と
、供給パイプ２０と同軸的に反応容器１の上流側に設け
られたガス供給路３０をもつ着火用ガス供給装置３と、
第１反応容器１の下流側に設けられた第２反応容器４と
、第１反応容器１と第２反応容器４との連絡路に設けら
れた希釈ガス供給装置５と、第２反応容器４の上流側に
設けられた加熱装置６と、第２反応容器４の下流側の設
けられた捕集装置７とから構成されている。First, a manufacturing apparatus for carrying out this embodiment will be explained. As shown in a schematic diagram in FIG. 1, this manufacturing apparatus includes a first reaction vessel 1, a metal powder supply apparatus 2 having a supply pipe 20 connected to the upstream side of the first reaction vessel 1, an ignition gas supply device 3 having a gas supply path 30 provided on the upstream side of the reaction vessel 1 coaxially with the pipe 20;
A second reaction container 4 provided on the downstream side of the first reaction container 1, a diluent gas supply device 5 provided in a communication path between the first reaction container 1 and the second reaction container 4, and a second reaction container 4. A heating device 6 is provided on the upstream side of the second reaction vessel 4, and a collection device 7 is provided on the downstream side of the second reaction vessel 4.
第１反応容器１は、内壁が耐熱レンガで囲まれた燃焼室
１０を形成している。この第１反応容器１の土壁には、
供給パイプ２０に連絡する粉末開口と、ガス供給路３０
が粉末開口と同心的かつ二重に連絡するガス開口とが設
けられている。The first reaction vessel 1 forms a combustion chamber 10 whose inner wall is surrounded by heat-resistant bricks. On the earthen wall of this first reaction vessel 1,
A powder opening communicating with the supply pipe 20 and a gas supply path 30
A gas opening is provided which is concentric and in dual communication with the powder opening.
粉末供給装置２は、バルブ２１を介してＮ２ガスボンベ
（図示せず）に接続された窒素供給管２２と、窒素供給
管２２が内部に装着された供給パイプ２０と、供給パイ
プ２０に下端が連結されＳｉ粉末を収納したホッパ２３
とをもつ。The powder supply device 2 includes a nitrogen supply pipe 22 connected to an N2 gas cylinder (not shown) via a valve 21, a supply pipe 20 in which the nitrogen supply pipe 22 is installed, and a lower end connected to the supply pipe 20. Hopper 23 containing Si powder
has.
着火用ガス供給装置３は、供給パイプ２０を二重にとり
まくガス供給路３０と、このガス供給路３０の内側に連
結されバルブ３１を介して酸素ボンベ（図示せず）に接
続された酸素供給管３２と、ガス供給路３０の外側に連
結されバルブ３３を介してＬＰＧボンベ（図示せず）に
接続されたＬＰＧ供給管３４とを備えている。The ignition gas supply device 3 includes a gas supply path 30 doubly surrounding the supply pipe 20, and an oxygen supply path connected to the inside of the gas supply path 30 and connected to an oxygen cylinder (not shown) via a valve 31. A pipe 32 and an LPG supply pipe 34 connected to the outside of the gas supply path 30 and connected to an LPG cylinder (not shown) via a valve 33 are provided.
第２反応容器４は、内壁が耐熱レンガで囲まれた浮遊室
４０を形成している。The second reaction vessel 4 forms a floating chamber 40 whose inner wall is surrounded by heat-resistant bricks.
希釈ガス供給装置５は、第１反応容器１と第２反応容器
４との連絡路に連結されバルブ５０を介して空気ボンベ
（図示せず）に接続された空気供給管５１をもつ。なお
、バルブ５０は第２反応容器４に配置された熱電対（図
示せず）に接続されている。The diluent gas supply device 5 has an air supply pipe 51 connected to a communication path between the first reaction vessel 1 and the second reaction vessel 4 and connected to an air cylinder (not shown) via a valve 50. Note that the valve 50 is connected to a thermocouple (not shown) placed in the second reaction vessel 4.
加熱装置６は、第１反応容器４の接線方向から浮遊室４
０内に向かって装着された２本のバーナ６０と、これら
バーナ６０に連結されバルブ６１を介して水素ボンベ（
図示せず〉に接続された水素供給管６２と、バーナ６０
に連結されバルブ６３を介して酸素ボンベ（図示せず）
に接続された酸素供給管６４とを備えている。The heating device 6 connects the floating chamber 4 from the tangential direction of the first reaction vessel 4.
Two burners 60 are installed toward the inside of the hydrogen cylinder (
A hydrogen supply pipe 62 and a burner 60 connected to
is connected to an oxygen cylinder (not shown) via a valve 63.
The oxygen supply pipe 64 is connected to the oxygen supply pipe 64.
捕集装置７は、第２反応容器４の側壁に開口する排出通
路７０と、この排出通路７０の下流側に設けられたバグ
フィルタ７１と、このバグフィルタ７１の下流側に設け
られたブロア７２とからなる。The collection device 7 includes a discharge passage 70 opening to the side wall of the second reaction vessel 4, a bag filter 71 provided downstream of the discharge passage 70, and a blower 72 provided downstream of the bag filter 71. It consists of
上記のように構成された製造装置により、３５０メツシ
ユアンダーの３ｉ粉末から５ｉ０２粉末を製造するため
、以下のような操作を行なった。The following operations were performed to produce 5i02 powder from 3i powder of 350 mesh under using the production apparatus configured as described above.
バルブ３１．３３を開いて、酸素供給管３２がら酸素ガ
スを１５Ｎｍｌ ／ｈｒの流出で供給するとともにＬＰ
Ｇ供給管３４からＬＰＧを０．７Ｎｍ’、”ｈｒの流量
で供給し、図示しない着火手段にＪ：り着火して種火を
形成する。バルブ２１を聞いてキャリアガスとしての窒
素ガスを２ Ｋ９ ／ ｃｔｔｔ、６Ｎ１７ｕ／ｈｒの
流量で窒素供給管２２から供給パイプ２０内へ流出させ
るとともに、ホッパ２３からＳｉ粉末を５Ｎｇ／ｈｒの
流量で供給した。流出した窒素ガスは３ｉ粉末を搬送し
て３ｉ粉末を燃焼室１０の種火と接触させる。３ｉ粉末
は種火と接触することにより化学炎を形成し、第１酸化
物粉末たる第１３ｉ０２粉末となる。第１ＳｉＯ２ｆｆ
Ａ末は、ブロア７２の吸引力により燃焼排ガス（雰囲気
）とともに第２反応容器４の浮遊室４０へ搬送される。Open the valves 31 and 33 to supply oxygen gas from the oxygen supply pipe 32 at a flow rate of 15 Nml/hr, and at the same time
LPG is supplied from the G supply pipe 34 at a flow rate of 0.7 Nm', hr, and ignited by an ignition means (not shown) to form a pilot flame. K9/cttt, 6N was flown into the supply pipe 20 at a flow rate of 17u/hr, and Si powder was supplied from the hopper 23 at a flow rate of 5Ng/hr. The 3i powder is brought into contact with the pilot flame in the combustion chamber 10. The 3i powder forms a chemical flame by contacting the pilot flame, and becomes the 13i02 powder, which is the first oxide powder. The first SiO2ff
The A powder is conveyed to the floating chamber 40 of the second reaction vessel 4 together with the combustion exhaust gas (atmosphere) by the suction force of the blower 72 .
バルブ５０を開いて、空気供給管５１がら空気を１ＯＮ
ｍｌ／ｈｒ（７）流ｍで供給シ、第１反応容器１から流
出する雰囲気を希釈するとともに１０００℃まで温度を
下げて第２反応容器４へ供給する。同時に、バルブ６１
．６３を開いて、水素供給管６２から水素ガスを６Ｎｍ
” ／ｈｒの流量で供給するとともにｒ！ａ素供素管給
管６４酸素ガスを４Ｎｍ、１／ｈｒの流量で供給し、図
示しない着火手段でバーナ６０を点火する。このとき、
バーナ６０がそれぞれ第２反応容器４の接線方向から浮
遊室４０内へ装着されているため、浮遊室４０に熱の旋
回流が形成されている。第１８ｉＯ２粉末は、旋回流に
より浮遊室４０に長時間）ｍ在する。こうして、付着し
たＮＯＸの付着量が減少したＳｉＯ２粉末となる。なお
、浮遊室４０の温度が高くなりすぎたとき及び低くなり
すぎたときは熱電対によりバルブ５０を操作する。そし
て、ＳｉＯ２粉末を含む燃焼排ガスを吸引し、バグフィ
ルタ７１により５ｉ０２粉末を捕集した。Open the valve 50 and turn on the air from the air supply pipe 51.
The atmosphere flowing out from the first reaction vessel 1 is diluted and the temperature is lowered to 1000° C. before being supplied to the second reaction vessel 4 at a flow rate of ml/hr (7). At the same time, valve 61
．． 63, and hydrogen gas is supplied from the hydrogen supply pipe 62 at 6Nm.
"/hr, and r!a oxygen supply pipe 64 is supplied at a flow rate of 4 Nm and 1/hr, and the burner 60 is ignited by an ignition means (not shown). At this time,
Since the burners 60 are each installed into the floating chamber 40 from the tangential direction of the second reaction vessel 4, a swirling flow of heat is formed in the floating chamber 40. The 18th iO2 powder remains in the floating chamber 40 for a long time due to the swirling flow. In this way, the SiO2 powder has a reduced amount of attached NOX. Note that when the temperature of the floating chamber 40 becomes too high or too low, the valve 50 is operated by a thermocouple. Then, the combustion exhaust gas containing SiO2 powder was sucked, and the 5i02 powder was collected by the bag filter 71.
以上のようにして得られた５ｉ０２粉末のＰＨと浮遊室
の温度との関係を求めた。この結果を第２図に示す。第
２図に示されるように、浮遊室の温度が８００〜１００
０’Ｃと高いほど中性（ＰＨ７）に近づくため好ましい
ことがわかる。The relationship between the pH of the 5i02 powder obtained as described above and the temperature of the floating chamber was determined. The results are shown in FIG. As shown in Figure 2, the temperature of the floating chamber is between 800 and 100.
It can be seen that the higher the temperature is, 0'C, the closer it is to neutrality (PH7), which is preferable.
［発明の効果］
本発明の酸化物粉末の製造方法は、表面に付着したＮＯ
Ｘを雰囲気中に浮遊させるため、中性で高純度の酸化物
粉末を粒度分布にばらつきなく、安価に、かつ連続的に
製造することができる。[Effect of the invention] The method for producing oxide powder of the present invention eliminates NO adhering to the surface.
Since X is suspended in the atmosphere, neutral and highly pure oxide powder can be produced continuously at low cost without variation in particle size distribution.
したがって、本発明の製造方法で製造された酸化物粉末
を何等支障なくポリマーに対する充填材として用いるこ
とができる。Therefore, the oxide powder produced by the production method of the present invention can be used as a filler for polymers without any problems.
第１図は本発明の実施例で用いた製造装置の模式断面図
、第２図はＳｉＯ２のＰＨと温度との関係を示す線図で
ある。
１・・・第１反応容器 １０・・・燃焼室２・・
・粉末供給装置 ２０・・・供給パイプ３・・・
着火用ガス供給装置
４・・・第２反応容器 ４０・・・浮遊室５・・
・希釈ガス供給装置 ６・・・加熱装置７・・・捕集
装置FIG. 1 is a schematic sectional view of a manufacturing apparatus used in an example of the present invention, and FIG. 2 is a diagram showing the relationship between PH of SiO2 and temperature. 1... First reaction vessel 10... Combustion chamber 2...
・Powder supply device 20... Supply pipe 3...
Ignition gas supply device 4...Second reaction vessel 40...Floating chamber 5...
・Dilution gas supply device 6... Heating device 7... Collection device
Claims (1)
属粉末を供給する金属粉末供給工程と、該燃焼室内にお
いてキャリアガスとともに該金属粉末を酸化性雰囲気下
で燃焼させることにより第１酸化物粉末を得る燃焼工程
と、 該燃焼室の下流側において窒素を含有する雰囲気を希釈
する希釈ガスを供給するとともに該第１酸化物粉末を加
熱してＮＯｘの付着量が減少した酸化物粉末を得る浮遊
工程と、 該酸化物粉末を捕集する捕集工程と、 からなることを特徴とする酸化物粉末の製造方法。(1) A metal powder supply step in which metal powder is supplied together with a carrier gas containing nitrogen into a combustion chamber, and a first oxide powder is produced by burning the metal powder together with a carrier gas in the combustion chamber in an oxidizing atmosphere. and a flotation step of supplying a diluent gas to dilute the nitrogen-containing atmosphere on the downstream side of the combustion chamber and heating the first oxide powder to obtain an oxide powder with a reduced amount of NOx deposited. A method for producing oxide powder, comprising: and a collection step of collecting the oxide powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3974889A JP2679216B2 (en) | 1989-02-20 | 1989-02-20 | Method for producing oxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3974889A JP2679216B2 (en) | 1989-02-20 | 1989-02-20 | Method for producing oxide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02217308A true JPH02217308A (en) | 1990-08-30 |
| JP2679216B2 JP2679216B2 (en) | 1997-11-19 |
Family
ID=12561584
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3974889A Expired - Lifetime JP2679216B2 (en) | 1989-02-20 | 1989-02-20 | Method for producing oxide powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2679216B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107285321A (en) * | 2017-06-29 | 2017-10-24 | 苏州吉云新材料技术有限公司 | A kind of preparation method of sub- nanometer spherical silicon powder |
| CN111320139A (en) * | 2019-02-27 | 2020-06-23 | 株式会社亚都玛科技 | Method for producing metal oxide particle material |
-
1989
- 1989-02-20 JP JP3974889A patent/JP2679216B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107285321A (en) * | 2017-06-29 | 2017-10-24 | 苏州吉云新材料技术有限公司 | A kind of preparation method of sub- nanometer spherical silicon powder |
| CN111320139A (en) * | 2019-02-27 | 2020-06-23 | 株式会社亚都玛科技 | Method for producing metal oxide particle material |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2679216B2 (en) | 1997-11-19 |
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