JPS58213625A - Novel process for preparation of mixture of carbon and elemental silicon or silicon oxide - Google Patents
Novel process for preparation of mixture of carbon and elemental silicon or silicon oxideInfo
- Publication number
- JPS58213625A JPS58213625A JP57159516A JP15951682A JPS58213625A JP S58213625 A JPS58213625 A JP S58213625A JP 57159516 A JP57159516 A JP 57159516A JP 15951682 A JP15951682 A JP 15951682A JP S58213625 A JPS58213625 A JP S58213625A
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- Japan
- Prior art keywords
- silicon
- carbon
- mixture
- elemental
- hot gas
- 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.)
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- Carbon And Carbon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
本発明はすぐれた高温強度と耐熱耐蝕性をもつセラミッ
ク材料として注目を集めている炭化ケイ素の中間原料と
なる単体ケイ素あるいはケイ素酸化物と炭素との混合物
を製造する新しい方法に関する。更に詳しくは、ケイ素
化合物と炭化水素を熱ガス中に同時に注入して単体ケイ
素もしくは酸化ケイ素と炭素との混合物を製造する方法
に関するものである。[Detailed Description of the Invention] The present invention is a novel method for producing silicon or a mixture of silicon oxide and carbon, which is an intermediate raw material for silicon carbide, which is attracting attention as a ceramic material with excellent high-temperature strength and heat and corrosion resistance. Regarding the method. More particularly, the present invention relates to a method for producing elemental silicon or a mixture of silicon oxide and carbon by simultaneously injecting a silicon compound and a hydrocarbon into hot gas.
従来炭化ケイ素はケイ砂などの様な二酸化ケイ素とコー
クスなどの様な炭素系物質とを粉砕混合し、例えばアチ
ソン型の直接通電抵抗炉などによシ高温下で(1)式に
示す固相反応によって得る方法が一般的である。Conventionally, silicon carbide is produced by pulverizing and mixing silicon dioxide such as silica sand with a carbonaceous material such as coke, and then forming the solid phase shown in equation (1) under high temperature using, for example, an Acheson-type direct current resistance furnace. A common method is to obtain it by reaction.
SiO,’+30−+ Sio+200・・・・・・
・・・ (1)この方法では原料とする例えばケイ砂と
コークスの粉砕混合はボールミルなどを用いた機械的な
方法が用いられており、一般にバッチ方式が採用されて
いる。従って原料の混合装入時、搬出時における作業工
程の繁雑さ、及び粉塵の移しい発生や粉砕混合時の騒音
といった作業環境上の問題がある。またケイ砂、コーク
スには通常AL、 F e、 N i、 N a、 M
fなどが不純物として含まれているので、この方法では
これら不純物は結局そのまま除去されることなく製品炭
化ケイ素中に含まれるため、純度の高い炭化ケイ素を得
るためにはさらに後工程を設は化学洗浄などを行なう必
要があった。SiO,'+30-+ Sio+200...
(1) In this method, a mechanical method using a ball mill or the like is used to grind and mix the raw materials, for example, silica sand and coke, and a batch method is generally adopted. Therefore, there are problems in the work environment, such as complicated work processes during mixing and charging of raw materials and when taking them out, as well as generation of moving dust and noise during pulverization and mixing. Also, silica sand and coke usually contain AL, Fe, Ni, Na, M
In this method, these impurities are ultimately included in the product silicon carbide without being removed as they are, so in order to obtain highly pure silicon carbide, further post-processing is required. I had to do some cleaning etc.
本発明者等は炭化ケイ素の製造方法について研究してい
たところ、従来技術とは全く異なる技術に至り、それに
関係して単体ケイ素あるいはケイ素酸化物と炭素との混
合物を製造する新規な方法に到達した。While researching methods for producing silicon carbide, the present inventors came up with a technology that is completely different from conventional technology, and related to this, they also came up with a new method for producing silicon or a mixture of silicon oxide and carbon. did.
即ち本発明は単体ケイ素あるいはケイ素酸化物と炭素と
の混合物を製造する新しい方法であって、ケイ素化合物
と炭化水素を同時に熱ガス中に装入して、少なくとも単
体ケイ素あるいはケイ素酸化物と炭素を含む粉体を熱ガ
ス中に生成させて、その粉体を捕集して得ることを特徴
とするものである。本発明ではケイ素化合物と炭化水素
を熱ガス中で化学反応させ、即ち熱分解、酸化、加水分
解等によシ粉体を発生させる方法であるので、従来の機
械的な混合法とは全く異なり粉塵、騒音などの作業環境
上の問題がなく、バッチ方式と異なり連続的に混合物を
得ることができるため、従来の作業工程の繁雑さが著し
く低減され、更に混合機自身も摩耗による不純物の混入
といった問題もない。That is, the present invention is a new method for producing elemental silicon or a mixture of silicon oxide and carbon, in which a silicon compound and a hydrocarbon are simultaneously charged into hot gas to produce at least elemental silicon or silicon oxide and carbon. It is characterized in that it is obtained by generating powder contained in hot gas and collecting the powder. The present invention is a method in which a silicon compound and a hydrocarbon are chemically reacted in hot gas, that is, a powder is generated through thermal decomposition, oxidation, hydrolysis, etc., which is completely different from conventional mechanical mixing methods. There are no working environment problems such as dust or noise, and unlike batch systems, the mixture can be obtained continuously, which significantly reduces the complexity of the conventional work process, and also eliminates the possibility of contamination with impurities due to wear of the mixer itself. There is no such problem.
本発明の実施の結果得られる混合物は、これを強熱する
ことにより不純物の少い炭化ケイ素を容易に与えるもの
である。The mixture obtained as a result of the practice of the present invention easily provides silicon carbide with few impurities by igniting the mixture.
本発明の詳細な説明すると、熱ガス中に好ましくは一般
式5inX2n+2(nは1から4の整数)で表わされ
るケイ素化合物と炭化水素を装入する。この一般式でX
は水素もしくはノ・ロゲン原子またはアルキル基もしく
はアルコキシル基であり、具体的なケイ素化合物を挙げ
ればS i OZ4、H810t3、SiHい(−0H
3)、8 i、(OH+)2siOA2、CH3S i
Ot3、S i F4 、8 i (002H11)
4 などであり、またこれらの混合物であっても本発
明には何等の支障もない。To explain the present invention in detail, a silicon compound preferably represented by the general formula 5inX2n+2 (n is an integer from 1 to 4) and a hydrocarbon are charged into hot gas. In this general formula,
is a hydrogen or nitrogen atom, an alkyl group, or an alkoxyl group, and specific examples of silicon compounds include SiOZ4, H810t3, SiH(-0H
3), 8 i, (OH+)2siOA2, CH3S i
Ot3, S i F4, 8 i (002H11)
4, etc., and even if these are mixed, there is no problem in the present invention.
炭化水素も広範囲に選択可能である。例えばナフサ、プ
ロパン、灯油、軽油、重油などの石油類は勿論、石油ピ
ッチ、メチル油、アントラセン油、クレオソート油など
の精製残留物、エチレンボトムなどの石油化学精留残物
でさえも使用可能である。しかし本発明の実施の結果得
られる混合物の用途によって、特定の不純物の挟在を排
除する必要がある場合には原料とするケイ素化合物及び
炭化水素をこの見地から選択する必要がある。この見地
から排除する必要がある不純物は本発明においては少な
くともケイ素化合物、炭化水素からは排除されていなけ
ればならない。このような目的の為の特定不純物の排除
は蒸溜、吸着、洗滌などの簡便な操作で容易に達成でき
る。There is also a wide range of hydrocarbons to choose from. For example, not only petroleum products such as naphtha, propane, kerosene, light oil, and heavy oil, but also refining residues such as petroleum pitch, methyl oil, anthracene oil, creosote oil, and even petrochemical distillation residues such as ethylene bottoms can be used. It is. However, depending on the use of the mixture obtained as a result of implementing the present invention, if it is necessary to eliminate the inclusion of specific impurities, it is necessary to select the silicon compounds and hydrocarbons used as raw materials from this viewpoint. From this point of view, impurities that need to be excluded must be excluded from at least silicon compounds and hydrocarbons in the present invention. Removal of specific impurities for this purpose can be easily accomplished by simple operations such as distillation, adsorption, and washing.
本発明の実施に用いる炭化水素も特定のケイ素化合物も
、そのまますでに又は容易に流体となし得るものである
から、これら化合物の熱ガス中への注入は単にノズルか
ら所望の量を注入するだけですむ。Since both the hydrocarbons and the specific silicon compounds used in the practice of this invention can already or easily be made into fluids, injection of these compounds into the hot gas is simply a matter of injecting the desired amount through a nozzle. nothing.
熱ガスの温度は700C以上が望ましい。この程度の温
度以上であれば、本発明で特定する前記一般式で示され
るケイ素化合物から単体ケイ素または二酸化ケイ素が、
また炭化水素からは単体炭素がそれぞれ固体となって熱
気流中に得られる。なおこの条件下で二酸化ケイ素の他
に酸化ケイ素も生成し粉体中に含まれるがこれは容易に
二酸化ケイ素となるので本発明の実施の妨げとはならな
い。しかしこの温度以下の条件は単体ケイ素又は単体炭
素の充分な生成が不十分となって望ましい混合物を得る
ことが次第に困難となる。The temperature of the hot gas is preferably 700C or higher. At temperatures above this level, elemental silicon or silicon dioxide can be extracted from the silicon compound represented by the general formula specified in the present invention.
In addition, elemental carbons from hydrocarbons are obtained in the form of solids in hot air streams. Note that under these conditions, silicon oxide is also produced in addition to silicon dioxide and is contained in the powder, but this does not interfere with the practice of the present invention because it easily becomes silicon dioxide. However, if the temperature is below this temperature, sufficient formation of elemental silicon or elemental carbon becomes insufficient, and it becomes increasingly difficult to obtain a desired mixture.
熱ガスを得る方法としては、通常行われている種々の方
法が採用できるが水素、メタン、アセチレンなど、ある
いは原料とする炭化水素そのものを空気で燃焼させる方
法が簡便である。なお本発明の実施に用いられるケイ素
化合物には700C以下の温度でも水蒸気を含んだガス
と接触して加水分解反応によって酸化ケイ素の粉体を生
成するものも含まれているが、これらが予め低温で酸化
ケイ素となシ更にこれが熱ガス中で単体ケイ素あるいは
二酸化ケイ素となる経路であっても本発明の実施の妨げ
とはならない。Various commonly used methods can be used to obtain the hot gas, but a simple method is to combust hydrogen, methane, acetylene, etc., or a hydrocarbon itself as a raw material with air. Note that the silicon compounds used in the practice of the present invention include those that generate silicon oxide powder through a hydrolysis reaction when they come into contact with gas containing water vapor even at temperatures below 700C; Furthermore, even if silicon oxide is formed in the hot gas, the process of converting it into elemental silicon or silicon dioxide does not impede the implementation of the present invention.
熱ガス中妬形成され澤粉体は反応の系外に誘導した後、
含まれる粉体をバグフィルタ−、サイクロン、電気収塵
機等の捕集装置で捕集する。After the powder is formed in the hot gas and guided out of the reaction system,
The contained powder is collected using a collection device such as a bag filter, cyclone, or electric dust collector.
捕集装置での熱負荷を軽減するためには予め熱ガスを冷
却することが望ましい。冷却の方法としては反応後の帯
域を冷却するとか又は水を注入してもよい。In order to reduce the heat load on the collection device, it is desirable to cool the hot gas in advance. As a method of cooling, the zone after the reaction may be cooled or water may be injected.
捕集された粉体は炉、例えばアチソン型直接通電抵抗炉
、高周波加熱炉などを用いて強熱することにより炭化ケ
イ素粉体を得ることができる。Silicon carbide powder can be obtained by igniting the collected powder using a furnace, such as an Acheson-type direct current resistance furnace or a high-frequency heating furnace.
また、粉体そのものを成型するかあるいは炭化ケイ素粉
とを混合したものを成型し、これをホットプレスなどの
焼結機を用いて炭化ケイ素成型体とすることも可能であ
Σ。It is also possible to mold the powder itself or mold a mixture with silicon carbide powder, and use a sintering machine such as a hot press to form a silicon carbide molded body.
以下実施例によシ本発明を具体的に説明する。The present invention will be specifically explained below using examples.
実施例1゜
図面に示す反応装置(直径300mm長さ3 m )を
用いて、ダクト(3)より空気を100 Nnl/ h
で連続的に送入し、燃焼バーナー(4)よりプロパンガ
スを3Nm’/h供給燃焼させて、1600〜1800
rの熱ガス流を発生させた。次にノズル(5)よシケ
イ素化合物として5iCt4を10Kg/ h で、
またノズル(6)より炭化水素としてA重油を6Kq/
h で夫々注入すると共に、ノズル(7)より水を5
5 t / bで注入して得られた粉体をバッグフィル
ターで20分間捕集し、約2 Kf得た。捕集した粉体
は化学分析により、炭素と二酸化ケイ素よりなると六が
確認され、酸化重量法によるその重量比(0/5iO2
)は3.2であった。Example 1 Using the reaction apparatus shown in the drawing (diameter 300 mm, length 3 m), air was supplied from duct (3) at a rate of 100 Nnl/h.
Propane gas is continuously fed in at 3 Nm'/h from the combustion burner (4) and burned at 1,600 to 1,800
A hot gas flow of r was generated. Next, through the nozzle (5), 5iCt4 was applied as a silica compound at 10 kg/h.
In addition, 6Kq/A heavy oil is added as hydrocarbon from the nozzle (6).
At the same time, water is injected at 5 h from the nozzle (7).
The powder obtained by injection at 5 t/b was collected on a bag filter for 20 minutes, yielding approximately 2 Kf. Chemical analysis of the collected powder confirmed that it was composed of carbon and silicon dioxide, and the weight ratio (0/5iO2) was determined by the oxidation gravimetric method.
) was 3.2.
実施例2
実施例1と全く同様にして発生させた熱ガス流に、ノズ
ル(5)よシ予めA重油と5iC4,をl対3.5の重
量比で混合させた混合液を45 K9/hの割合で注入
すると共に、ノズル(7)より水を55t/hで注入し
て得た粉体をバッグフィルターで10分間捕集し、約3
K9得た。Example 2 A mixture of heavy oil A and 5iC4 in a weight ratio of 1 to 3.5 was added to the hot gas flow generated in the same manner as in Example 1 through the nozzle (5). At the same time, the powder obtained by injecting water at a rate of 55 t/h from the nozzle (7) was collected with a bag filter for 10 minutes, and the powder was collected at a rate of about 3
Got K9.
捕集した粉体は化学分析によシ、炭素と二酸化ケイ素よ
シなることが確認され、酸化重量法によるその重量比(
0/ S i 02 )は2.0であった。The collected powder was confirmed to be composed of carbon and silicon dioxide through chemical analysis, and their weight ratio (
0/S i 02 ) was 2.0.
実施例3
実施例1と同じ反応装置を用いて、ダクト(3)より空
気を100 Nm/ hで連続的に送太し、燃焼バーナ
ー(4)より水素を25N?I/h供給燃焼させて、1
400〜1600rの熱ガス流を発生させた。次にノズ
ル(5ンよシ炭7ヒ水素としてエチレンボトムを10K
g/hで、葦だノズル(6)よりケイ素化合物としてH
2S1c42を9 Kg/hで夫々装入すると共に、ノ
ズル(7)より水を55 L/ hで注入して得た粉体
をバッグフィルターで15分間捕集し、約2 K9得た
。Example 3 Using the same reactor as in Example 1, air was continuously fed from the duct (3) at 100 Nm/h, and hydrogen was fed from the combustion burner (4) at 25 Nm/h. I/h supply combustion, 1
A hot gas flow of 400-1600 r was generated. Next, the nozzle (5 mm, 7 carbon, 7 arsenic, 10K ethylene bottom)
g/h as silicon compounds from the reed nozzle (6).
2S1c42 was charged at 9 Kg/h, and water was injected from the nozzle (7) at 55 L/h, and the resulting powder was collected with a bag filter for 15 minutes to obtain about 2K9.
捕集した粉体は化学分析により、炭素と二酸化ケイ素よ
シなることが確認され、酸化重量法によるその重量比(
C/5iO2)は4.3であった。Chemical analysis of the collected powder confirmed that it was composed of carbon and silicon dioxide, and the weight ratio (
C/5iO2) was 4.3.
以上の結果をまとめたものが第1表である。Table 1 summarizes the above results.
第1表Table 1
図面は本発明の実施に使用する反応装置の断面図の一例
を示したものである。
図面において
■ ・・・・・・・・・・・・・・・ 炉壁2 ・・・
・・・・・・・・・・・・ 炉壁に内接する炉材3 ・
・・・・・・・・・・・・・・ ダクト4 ・・・・・
・・・・・・・・・・燃焼バーナー5 ・・・・・・・
・・・・・・・・ ノズル6 ・・・・・・・・・・・
川・ ノズル7 ・・・・・・・・・・・・・・・ ノ
ズル8 ・・・・・・・・・・・・・・・ ダクトをそ
れぞれ示す。
特許出願人 三井東圧化学株式会社The drawing shows an example of a cross-sectional view of a reaction apparatus used in carrying out the present invention. In the drawing ■ ・・・・・・・・・・・・ Furnace wall 2 ・・・
・・・・・・・・・ Furnace material 3 inscribed in the furnace wall ・
・・・・・・・・・・・・・・・ Duct 4 ・・・・・・
・・・・・・・・・ Combustion burner 5 ・・・・・・・・・
・・・・・・・・・ Nozzle 6 ・・・・・・・・・・・・
River/ Nozzle 7 ・・・・・・・・・・・・・・・ Nozzle 8 ・・・・・・・・・・・・・・・ The ducts are shown respectively. Patent applicant Mitsui Toatsu Chemical Co., Ltd.
Claims (1)
は二酸化ケイ素を生成するケイ素化合物と、熱分解によ
シ単体炭素を生成する炭化水素を熱ガス中に同時に注入
することを特徴とする単体ケイ素あるいはケイ素酸化物
と炭素との混合物の新しい製造法Elemental silicon or silicon, which is characterized by simultaneously injecting into hot gas a silicon compound that produces elemental silicon or silicon dioxide through thermal decomposition, oxidation, or hydrolysis, and a hydrocarbon that produces elemental carbon through thermal decomposition. New method for producing mixtures of silicon oxide and carbon
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP57159516A JPS58213625A (en) | 1982-09-16 | 1982-09-16 | Novel process for preparation of mixture of carbon and elemental silicon or silicon oxide |
US06/886,768 US4752456A (en) | 1982-06-01 | 1983-06-01 | Process for preparing metal carbides and precursors thereof |
DE8383901729T DE3381007D1 (en) | 1982-06-01 | 1983-06-01 | METHOD OF PRODUCING METAL CARBIDES AND THEIR PRE-PRODUCTS. |
PCT/JP1983/000180 WO1983004188A1 (en) | 1982-06-01 | 1983-06-01 | Process for manufacturing metal carbides and their precursors |
EP83901729A EP0111008B1 (en) | 1982-06-01 | 1983-06-01 | Process for manufacturing metal carbides and their precursors |
CA000436445A CA1214309A (en) | 1982-09-14 | 1983-09-12 | Process for preparing metal carbides and precursors thereof |
IT48972/83A IT1170492B (en) | 1982-09-14 | 1983-09-13 | Metal carbide and metal carbide precursor mfr. |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP57159516A JPS58213625A (en) | 1982-09-16 | 1982-09-16 | Novel process for preparation of mixture of carbon and elemental silicon or silicon oxide |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP57092215A Division JPS58213621A (en) | 1982-06-01 | 1982-06-01 | Preparation of slicon carbide powder having large specific surface area |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS58213625A true JPS58213625A (en) | 1983-12-12 |
Family
ID=15695475
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP57159516A Pending JPS58213625A (en) | 1982-06-01 | 1982-09-16 | Novel process for preparation of mixture of carbon and elemental silicon or silicon oxide |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS58213625A (en) |
-
1982
- 1982-09-16 JP JP57159516A patent/JPS58213625A/en active Pending
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