JPH0328371B2 - - Google Patents
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- Publication number
- JPH0328371B2 JPH0328371B2 JP23823684A JP23823684A JPH0328371B2 JP H0328371 B2 JPH0328371 B2 JP H0328371B2 JP 23823684 A JP23823684 A JP 23823684A JP 23823684 A JP23823684 A JP 23823684A JP H0328371 B2 JPH0328371 B2 JP H0328371B2
- Authority
- JP
- Japan
- Prior art keywords
- gas
- reaction
- silicon
- sif
- fluorochlorosilanes
- 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.)
- Expired
Links
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 description 35
- 238000006243 chemical reaction Methods 0.000 description 26
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 19
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 17
- 239000002994 raw material Substances 0.000 description 15
- 239000000460 chlorine Substances 0.000 description 14
- 238000000034 method Methods 0.000 description 14
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 12
- 239000005049 silicon tetrachloride Substances 0.000 description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 238000009835 boiling Methods 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000005660 chlorination reaction Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229910000676 Si alloy Inorganic materials 0.000 description 5
- 239000001307 helium Substances 0.000 description 5
- 229910052734 helium Inorganic materials 0.000 description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- ODNBVEIAQAZNNM-UHFFFAOYSA-N 1-(6-chloroimidazo[1,2-b]pyridazin-3-yl)ethanone Chemical compound C1=CC(Cl)=NN2C(C(=O)C)=CN=C21 ODNBVEIAQAZNNM-UHFFFAOYSA-N 0.000 description 3
- GUNJVIDCYZYFGV-UHFFFAOYSA-K Antimony trifluoride Inorganic materials F[Sb](F)F GUNJVIDCYZYFGV-UHFFFAOYSA-K 0.000 description 3
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 3
- 229910003902 SiCl 4 Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 3
- SDNBGJALFMSQER-UHFFFAOYSA-N trifluoro(trifluorosilyl)silane Chemical compound F[Si](F)(F)[Si](F)(F)F SDNBGJALFMSQER-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910004014 SiF4 Inorganic materials 0.000 description 1
- MKPXGEVFQSIKGE-UHFFFAOYSA-N [Mg].[Si] Chemical compound [Mg].[Si] MKPXGEVFQSIKGE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- WOLDFAYTXKMDAQ-UHFFFAOYSA-N chlorotrifluorosilane Chemical compound F[Si](F)(F)Cl WOLDFAYTXKMDAQ-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- LNUZHCSQTRPPPK-UHFFFAOYSA-N dichloro(difluoro)silane Chemical compound F[Si](F)(Cl)Cl LNUZHCSQTRPPPK-UHFFFAOYSA-N 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000012025 fluorinating agent Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003701 inert diluent Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- PGHWHQUVLXTFLZ-UHFFFAOYSA-N trichloro(fluoro)silane Chemical compound F[Si](Cl)(Cl)Cl PGHWHQUVLXTFLZ-UHFFFAOYSA-N 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は珪素化合物の中間原料として有用なフ
ルオロクロロシラン類SiFnCl4-o（ｎ＝１、２、
３）の製造法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention provides fluorochlorosilanes SiFnCl 4-o (n=1, 2,
3) Regarding the manufacturing method.
フルオロクロロシラン類の製造法としては次の
各法が公知である。
The following methods are known as methods for producing fluorochlorosilanes.
四塩化珪素を三弗化アンチモンを用いて部分
弗素化する方法。例えばH.S.Booth et al.〔J.
A.C.S.54−4750（1932）〕がある。 A method for partially fluorinating silicon tetrachloride using antimony trifluoride. For example, HS Booth et al. [J.
ACS54-4750 (1932)].
ヘキサフルオロジシラン（Si2F6）と塩素ガ
スとの反応による方法。例えばW.C.Schumbet
al.〔J.A.C.S.54−3943（1932）〕がある。 A method based on the reaction of hexafluorodisilane (Si 2 F 6 ) with chlorine gas. For example WCShumbet
al. [JACS54-3943 (1932)].
四塩化珪素と四弗化珪素との再分配反応
（Redistribution）による方法。例えばH.H.
Anderson〔J.A.C.S72−2091（1950）〕あるいは
USP2395826などがある。 A method using redistribution reaction between silicon tetrachloride and silicon tetrafluoride. For example HH
Anderson [JACS72-2091 (1950)] or
Examples include USP2395826.
しかしながらの方法では弗素化剤である三弗
化アンチモンの吸湿性が強いことおよび三弗化ア
ンチモンの純度を良くするために昇華による精製
が必要であることなど取扱いが煩雑となる欠点を
有している。の方法ではヘキサフルオロジシラ
ンと塩素ガスとのマイルドな爆発反応であり、工
業的規模の製造には不向きである。また原料ヘキ
サフルオロジシランの入手も難かしく、好ましい
方法とは言えない。の四塩化珪素と四弗化珪素
とを600〜700℃で再分配反応させる方法が三つの
方法のうちでは工業的規模の製造に適していると
考えられる。 However, this method has drawbacks such as the strong hygroscopicity of the fluorinating agent, antimony trifluoride, and the need for purification by sublimation to improve the purity of antimony trifluoride, making it complicated to handle. There is. The method involves a mild explosive reaction between hexafluorodisilane and chlorine gas, and is unsuitable for industrial scale production. Furthermore, it is difficult to obtain the raw material hexafluorodisilane, so this method cannot be said to be preferable. Of the three methods, the method of redistributing silicon tetrachloride and silicon tetrafluoride at 600 to 700°C is considered to be suitable for industrial scale production.
しかしながら、一方の原料である四塩化珪素は
一般的には珪素合金に塩素ガスを約400℃で作用
させて得られるものであり、塩素化反応のために
相当量の熱エネルギーが必要である。この四塩化
珪素原料を製造するための熱エネルギーと前記
600〜700℃で再分配反応をおこなわせるための熱
エネルギーが二重に必要となり、熱エネルギーの
損失は大となる欠点を有している。また再分配反
応時の四塩化珪素の流量の制御は液体のままで
も、気化させた気体状でも精度が得にくいと言う
欠点を有する。
However, silicon tetrachloride, one of the raw materials, is generally obtained by applying chlorine gas to a silicon alloy at about 400°C, and a considerable amount of thermal energy is required for the chlorination reaction. Thermal energy and the above for producing this silicon tetrachloride raw material
The disadvantage is that double thermal energy is required to carry out the redistribution reaction at 600 to 700°C, resulting in a large loss of thermal energy. Furthermore, it is difficult to control the flow rate of silicon tetrachloride during the redistribution reaction, whether it is in the liquid state or in the vaporized gas state.
本発明者らは前記の方法の欠点を排除するた
め鋭意検討した結果、四塩化珪素合成反応と同時
に再分配反応をおこなわせる方法を見出し、本発
明の到つたものである。すなわち本発明は金属珪
素あるいは珪素合金に塩素ガスと四弗化珪素ガス
を作用させることを特徴とするフルオロクロロシ
ラン類の製造法である。
The present inventors have made extensive studies to eliminate the drawbacks of the above-mentioned methods, and as a result have found a method in which the redistribution reaction is carried out simultaneously with the silicon tetrachloride synthesis reaction, and the present invention has been achieved. That is, the present invention is a method for producing fluorochlorosilanes, which is characterized by causing chlorine gas and silicon tetrafluoride gas to act on metallic silicon or a silicon alloy.
本発明の方法によればフルオロクロロシラン類
の製造時にのみ熱エネルギーを加えればよく、前
記熱エネルギー損失の欠点が排除できる。また塩
素ガスおよび四弗化珪素ガスの流量制御はどちら
も常温ではガス体であるため非常に容易となるば
かりでなく、精度も著しく向上させることができ
る。 According to the method of the present invention, it is only necessary to apply thermal energy during the production of fluorochlorosilanes, thereby eliminating the disadvantage of thermal energy loss. Furthermore, since both chlorine gas and silicon tetrafluoride gas are gaseous at room temperature, flow rate control is not only extremely easy, but also significantly improved in accuracy.
以下、本発明をさらに詳しく説明する。 The present invention will be explained in more detail below.
フルオロクロロシラン類製造のSi原料としては
金属珪素あるいは珪素合金を使用する。金属珪素
としては一般的な珪石の炭素還元で得られるもの
あるいはこれを粉砕した後、酸処理して粒界に折
出した不純物を除いたものなどを使用する。珪素
合金としては一般的なフエロシリコン（Fe−
Si）、カルシウムシリコン（Ca−Si）、マグネシ
ウムシリコン（Mg−Si）などが使用できる。反
応の形式としては固定床、流動層、移動層などい
ずれを採用しても良い。 Metallic silicon or a silicon alloy is used as the Si raw material for producing fluorochlorosilanes. As the metallic silicon, one obtained by carbon reduction of general silica stone, or one obtained by crushing it and treating it with an acid to remove impurities precipitated at grain boundaries, etc. is used. Ferrosilicon (Fe-
Si), calcium silicon (Ca-Si), magnesium silicon (Mg-Si), etc. can be used. As for the reaction format, any of fixed bed, fluidized bed, moving bed, etc. may be employed.
Si原料の使用に際しては反応の形式に合致した
適当な粒度範囲のものに調整して用いる。例えば
固定床の場合には１×１mm〜10×10mm程度の範囲
が好ましい。一方、塩素ガスおよび四弗化珪素ガ
スは市販のものがそのまま使用できる。また精製
前の粗製ガスを使用しても良いが塩素ガスは充分
脱水して使用する必要がある。また、必要に応じ
て反応系に窒素、ヘリウム、アルゴンなどの不活
性な希釈ガスを長しても良い。また、塩素ガスと
四弗化珪素ガスは混合して反応系に導入してもよ
いし、別々に導入してもよく、塩素化ゾーンと再
分配反応ゾーンに分けてもよい。 When using a Si raw material, it is adjusted to have a particle size within an appropriate particle size range that matches the type of reaction. For example, in the case of a fixed bed, the preferred range is about 1 x 1 mm to 10 x 10 mm. On the other hand, commercially available chlorine gas and silicon tetrafluoride gas can be used as they are. Further, crude gas before purification may be used, but chlorine gas must be sufficiently dehydrated before use. Furthermore, if necessary, an inert diluent gas such as nitrogen, helium, or argon may be added to the reaction system. Further, chlorine gas and silicon tetrafluoride gas may be introduced into the reaction system as a mixture, or may be introduced separately, or may be divided into a chlorination zone and a redistribution reaction zone.
金属珪素をSi原料とする場合には四弗化珪素ガ
スと塩素ガスのモル比MR（MR＝SiF4／Cl2）は
0.05〜５の範囲から選らばれる。 When metallic silicon is used as the Si raw material, the molar ratio MR of silicon tetrafluoride gas and chlorine gas (MR=SiF 4 /Cl 2 ) is
Selected from the range of 0.05 to 5.
フルオロクロロシラン類SiFnCl4-oには
モノフルオロトリクロロシランSiFCl3（ｎ−１）
沸点12.2℃
ジフルオロジクロロシランSiF2Cl2（ｎ−２）沸
点−32.2℃
トリフルオロモノクロロシランSiF3Cl（ｎ−３）
沸点−70.0℃
の三種があるが、MRを大きくするとSiF3Clリツ
チの混合ガスが、またMRを小さくするとSiFCl3
リツチな混合ガスが得られる。MRが0.05以下あ
るいは５以上の場合、いずれも反応の収率の低下
をまねくので好ましくない。 For fluorochlorosilanes SiFnCl 4-o , monofluorotrichlorosilane SiFCl 3 (n-1)
Boiling point 12.2℃ Difluorodichlorosilane SiF 2 Cl 2 (n-2) Boiling point -32.2℃ Trifluoromonochlorosilane SiF 3 Cl (n-3)
There are three types with a boiling point of -70.0°C; increasing the MR produces a mixture gas rich in SiF 3 Cl, while decreasing MR produces a mixed gas rich in SiFCl 3
A rich gas mixture is obtained. If the MR is less than 0.05 or more than 5, this is not preferable as both lead to a decrease in the reaction yield.
珪素合金をSi原料とする場合、例えばフエロシ
リコンではFeCl3が副生するので反応系にチヤー
ジする四弗化珪素ガスと塩素ガスのモル比MRは
当然のことながら金属珪素の場合よりは小さくす
る必要がある。 When a silicon alloy is used as a Si raw material, for example, in ferrosilicon, FeCl 3 is produced as a by-product, so the molar ratio MR of silicon tetrafluoride gas and chlorine gas charged to the reaction system is naturally smaller than in the case of metallic silicon. There is a need to.
塩素ガスと四弗化珪素ガスの流量は反応形式に
より異なるがSi原料と充分なる接触時間を与えな
ければならない。反応温度としてはSi原料の塩素
化反応が進行する180〜1000℃の温度範囲が好ま
しく、より好適には350〜800℃の範囲が選ばれ
る。180℃以下ではSi原料の塩素化速度が遅すぎ
るし、また1000℃以上にしても高温にすることに
よる特別な利益は得られない。従来の四塩化珪素
と四弗化珪素の再分配反応では十分な収率を得る
ためには比較的高温での反応が必要であつたが、
本発明方法では、その理由は明確ではないが、よ
り低温で十分な収率を得ることができる。反応系
から排出する生成ガス中には上記三種のフルオロ
クロロシラン類とともに少量の四塩化珪素ガスと
未反応の四弗化珪素ガスを含有する。フルオロク
ロロシラン類だけを捕集するためにはまず高沸点
の四塩化珪素ガス（沸点57℃）を除去するため０
〜−20℃の冷却トラツプを通す。次に−80〜−
110℃の冷却トラツプを通してフルオロクロロシ
ラン類を捕集する。最後に低沸点の四弗化珪素ガ
ス（沸点−95℃）を−196℃の冷却トラツプで捕
集する。捕集したフルオロクロロシラン類は低温
蒸留あるいは加圧蒸留などの蒸留操作により
SiFCl3、SiF2Cl2並びにSiF3Clに単離できる。 Although the flow rates of chlorine gas and silicon tetrafluoride gas vary depending on the reaction type, sufficient contact time with the Si raw material must be provided. The reaction temperature is preferably in the range of 180 to 1000°C, at which the chlorination reaction of the Si raw material proceeds, and more preferably in the range of 350 to 800°C. If the temperature is below 180°C, the rate of chlorination of the Si raw material is too slow, and even if the temperature is above 1000°C, no special benefit can be obtained by increasing the temperature. In the conventional redistribution reaction between silicon tetrachloride and silicon tetrafluoride, a reaction at a relatively high temperature was necessary to obtain a sufficient yield.
In the method of the present invention, a sufficient yield can be obtained at a lower temperature, although the reason is not clear. The generated gas discharged from the reaction system contains a small amount of silicon tetrachloride gas and unreacted silicon tetrafluoride gas along with the above three types of fluorochlorosilanes. In order to collect only fluorochlorosilanes, first remove the high boiling point silicon tetrachloride gas (boiling point 57℃).
Pass through a cooling trap at ~-20°C. Next -80~-
Fluorochlorosilanes are collected through a cooling trap at 110°C. Finally, low boiling point silicon tetrafluoride gas (boiling point -95°C) is collected in a cooling trap at -196°C. The collected fluorochlorosilanes are removed by distillation operations such as low-temperature distillation or pressure distillation.
It can be isolated as SiFCl 3 , SiF 2 Cl 2 and SiF 3 Cl.
塩素化と再分配の同時反応の反応式の例として
は
Si＋2Cl2＋SiF4→2SiF2Cl2 (1)
Si＋2Cl2＋3SiF4→4SiF3Cl (2)
3Si＋6Cl2＋SiF4→4SiFCl3 (3)
が考えられる。 An example of a reaction equation for the simultaneous reaction of chlorination and redistribution is: Si+2Cl 2 +SiF 4 →2SiF 2 Cl 2 (1) Si+2Cl 2 +3SiF 4 →4SiF 3 Cl (2) 3Si+6Cl 2 +SiF 4 →4SiFCl 3 (3) It will be done.
次に本発明を実施例で示す。 Next, the present invention will be illustrated by examples.
実施例 １
内径34φ、長さ550mmの石英管に粒度２×２mm
〜５×５mm程度の金属珪素を反応に充分な量450
ｇ充てんした。この石英管を管状炉にセツトし、
入口側よりヘリウムを長しながら昇温し、管内の
空気、水分をほぼ完全にパージしたのち管状炉の
温度を700℃に設定した。次に原料ガスとして乾
燥塩素ガス80c.c.／min、四弗化珪素ガス40c.c.／
minおよび希釈用としてヘリウム20c.c.／minの混
合ガスを入口側よりチヤージし、塩素化反応と再
分配反応を同時におこなつた。（MR＝SiF4／Cl2
＝0.5に相当）石英管出口ガスのうち四塩化珪素
ガスは−10℃のトラツプで捕集し、フルオロクロ
ロシラン類は−100℃のトラツプで捕集した。未
反応の四弗化珪素ガスは−196℃のトラツプで捕
集した。反応時間は２時間とし、原料ガスのチヤ
ージを停止したのち、石英管内に残存するガスを
充分にトラツプするため、ヘリウムを100c.c.／
minで２時間流した。反応終了後、−100℃のトラ
ツプ内に捕集したフルオロクロロシラン類を別の
真空容器に気化させ、生成したフルオロクロロシ
ラン類を測定したところ43.0ｇとなり、原料ガス
の四弗化珪素量と塩素ガス量を四塩化珪素に換算
した量との合計量をベースとした収率は80％であ
つた。また、気化させた混合ガスをガスクロマト
グラフイーで分析した結果、平均的な組成は
SiCl4 trace
SiFCl3 20 mole％
SiF2Cl2 35 mole％
SiF3Cl 45 mole％
SiF4 trace
であつた。Example 1 Particle size 2 x 2 mm in a quartz tube with an inner diameter of 34φ and a length of 550 mm
~ 5 x 5 mm metal silicon in sufficient amount for reaction 450
I filled up with g. Set this quartz tube in a tube furnace,
The temperature of the helium was raised from the inlet side while being extended, and after almost completely purging the air and moisture inside the tube, the temperature of the tube furnace was set to 700℃. Next, as raw material gases, dry chlorine gas 80c.c./min and silicon tetrafluoride gas 40c.c./min.
A mixed gas of 20 c.c./min of helium was charged from the inlet side for dilution and chlorination reaction and redistribution reaction were performed simultaneously. (MR= SiF4 / Cl2
= 0.5) Of the quartz tube outlet gas, silicon tetrachloride gas was collected in a -10°C trap, and fluorochlorosilanes were collected in a -100°C trap. Unreacted silicon tetrafluoride gas was collected in a trap at -196°C. The reaction time was 2 hours, and after stopping the charging of the raw material gas, 100 c.c./h of helium was added to sufficiently trap the gas remaining in the quartz tube.
It was run for 2 hours at min. After the reaction, the fluorochlorosilanes collected in the trap at -100°C were vaporized in another vacuum container, and the amount of fluorochlorosilanes produced was 43.0 g, which was the same as the amount of silicon tetrafluoride in the raw material gas and the chlorine gas. The yield was 80% based on the total amount including the amount converted to silicon tetrachloride. Further, as a result of analyzing the vaporized mixed gas by gas chromatography, the average composition was SiCl 4 trace SiFCl 3 20 mole% SiF 2 Cl 2 35 mole% SiF 3 Cl 45 mole% SiF 4 trace.
実施例 ２
MRを0.35とし、管状炉の温度を500℃とした
以外は実施例１と同様にして反応をおこなつた。
すなわち原料ガスとして乾燥塩素ガス88.9c.c.／
min、四弗化珪素ガス31.1c.c.／min.ヘリウム20
c.c.／minの混合ガスを入口側よりチヤージし、反
応させたところ生成したフルオロクロロシラン類
は41.3ｇとなり、前記収率は78％であつた。また
気化させた混合ガスをガスクロマトグラフイーで
分析した結果、平均的な組成は
SiCl4 trace
SiFCl3 27 mole％
SiF2Cl2 38 mole％
SiF3Cl 35 mole％
SiF4 trace
であつた。Example 2 A reaction was carried out in the same manner as in Example 1, except that MR was 0.35 and the temperature of the tube furnace was 500°C.
In other words, 88.9cc/dry chlorine gas is used as raw material gas.
min, silicon tetrafluoride gas 31.1cc/min. helium 20
A mixed gas of cc/min was charged from the inlet side to cause a reaction, and the amount of fluorochlorosilanes produced was 41.3 g, and the yield was 78%. Further, as a result of analyzing the vaporized mixed gas by gas chromatography, the average composition was found to be SiCl 4 trace SiFCl 3 27 mole% SiF 2 Cl 2 38 mole% SiF 3 Cl 35 mole% SiF 4 trace.
実施例 ３
粒度２×２mm〜５×５mmに調整したフエロシリ
コン（Si；90％）を用い、乾燥塩素ガス80c.c.／
min、四弗化珪素ガス30c.c.／minとする以外は実
施例１と同様に反応をおこなつた。その結果２時
間反応後の収率は82％であつた。また得られたガ
スをガスクロマトグラフイーで分析した結果、平
均的な組成は
SiCl4 trace
SiFCl3 21 mole％
SiF2Cl2 36 mole％
SiF3Cl 43 mole％
SiF4 trace
であつた。Example 3 Using ferrosilicon (Si; 90%) adjusted to a particle size of 2 x 2 mm to 5 x 5 mm, dry chlorine gas 80 c.c./
The reaction was carried out in the same manner as in Example 1 except that the amount of silicon tetrafluoride gas was 30 c.c./min. As a result, the yield after 2 hours of reaction was 82%. Further, as a result of analyzing the obtained gas by gas chromatography, the average composition was as follows: SiCl 4 trace SiFCl 3 21 mole% SiF 2 Cl 2 36 mole% SiF 3 Cl 43 mole% SiF 4 trace.
本発明によれば金属珪素、珪素合金に塩素ガス
と四弗化珪素ガスを作用させることで容易にフル
オロクロロシラン類を得ることができ、エネルギ
ー効率もよく、また原料の導入量制御も容易であ
り、極めて工業的に有利にフルオロクロロシラン
類を得ることができる。
According to the present invention, fluorochlorosilanes can be easily obtained by causing chlorine gas and silicon tetrafluoride gas to act on metallic silicon or silicon alloys, and the energy efficiency is good, and the amount of raw materials introduced can be easily controlled. , it is possible to obtain fluorochlorosilanes in a very industrially advantageous manner.
Claims (1)
と四弗化珪素ガスを作用させ反応させることを特
徴とするフルオロクロロシラン類SiFnCl4-o（ｎ−
１、２、３）の製造法。1. Fluorochlorosilanes SiFnCl 4-o (n-
1, 2, 3) manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23823684A JPS61117112A (en) | 1984-11-14 | 1984-11-14 | Preparation of fluorochlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23823684A JPS61117112A (en) | 1984-11-14 | 1984-11-14 | Preparation of fluorochlorosilane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61117112A JPS61117112A (en) | 1986-06-04 |
| JPH0328371B2 true JPH0328371B2 (en) | 1991-04-18 |
Family
ID=17027163
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23823684A Granted JPS61117112A (en) | 1984-11-14 | 1984-11-14 | Preparation of fluorochlorosilane |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61117112A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20040096628A (en) | 2002-02-27 | 2004-11-16 | 허니웰 인터내셔널 인코포레이티드 | Preparation of Mixed-Halogen Halo-Silanes |
-
1984
- 1984-11-14 JP JP23823684A patent/JPS61117112A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61117112A (en) | 1986-06-04 |
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