JPH0471008B2 - - Google Patents
Info
- Publication number
- JPH0471008B2 JPH0471008B2 JP3122885A JP3122885A JPH0471008B2 JP H0471008 B2 JPH0471008 B2 JP H0471008B2 JP 3122885 A JP3122885 A JP 3122885A JP 3122885 A JP3122885 A JP 3122885A JP H0471008 B2 JPH0471008 B2 JP H0471008B2
- Authority
- JP
- Japan
- Prior art keywords
- reaction
- silane compound
- raw material
- disproportionation
- stage
- 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
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 239000003054 catalyst Substances 0.000 claims description 13
- 238000007323 disproportionation reaction Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 11
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 9
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 8
- DESGIDRJCLIWRS-UHFFFAOYSA-N [SiH]Cl Chemical compound [SiH]Cl DESGIDRJCLIWRS-UHFFFAOYSA-N 0.000 claims description 6
- 150000004756 silanes Chemical class 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 238000011437 continuous method Methods 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims 6
- -1 silane compound Chemical class 0.000 claims 6
- 239000006227 byproduct Substances 0.000 claims 2
- 125000001309 chloro group Chemical group Cl* 0.000 claims 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 2
- 238000000066 reactive distillation Methods 0.000 claims 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical class Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims 2
- 150000001875 compounds Chemical class 0.000 claims 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 11
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 10
- 239000005052 trichlorosilane Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 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 4
- 239000005046 Chlorosilane Substances 0.000 description 4
- 238000004817 gas chromatography Methods 0.000 description 4
- 239000005049 silicon tetrachloride Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000003512 tertiary amines Chemical class 0.000 description 3
- 239000003957 anion exchange resin Substances 0.000 description 2
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 238000003541 multi-stage reaction Methods 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- ICSWLKDKQBNKAY-UHFFFAOYSA-N 1,1,3,3,5,5-hexamethyl-1,3,5-trisilinane Chemical compound C[Si]1(C)C[Si](C)(C)C[Si](C)(C)C1 ICSWLKDKQBNKAY-UHFFFAOYSA-N 0.000 description 1
- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 description 1
- AVQQQNCBBIEMEU-UHFFFAOYSA-N 1,1,3,3-tetramethylurea Chemical compound CN(C)C(=O)N(C)C AVQQQNCBBIEMEU-UHFFFAOYSA-N 0.000 description 1
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- YKFRUJSEPGHZFJ-UHFFFAOYSA-N N-trimethylsilylimidazole Chemical compound C[Si](C)(C)N1C=CN=C1 YKFRUJSEPGHZFJ-UHFFFAOYSA-N 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- OAGOUCJGXNLJNL-UHFFFAOYSA-N dimethylcyanamide Chemical compound CN(C)C#N OAGOUCJGXNLJNL-UHFFFAOYSA-N 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 description 1
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Description
〔産業上の利用分野〕
本発明は、水素化塩化珪素を反応塔に供給し
て、触媒の存在下で不均斉化反応させると共に蒸
留効果による分離を同時に行わせて、ジクロルシ
ラン、モノクロルシラン、モノシラン等のシラン
化合物を連続的に取得するシラン化合物の連続的
製法に関するものである。
〔従来技術と問題点〕
ジクロルシラン、モノクロルシラン及びモノシ
ラン等は半導体や太陽電池等の素子に使用される
高純度シリコンの原料として益々需要の増加が見
込まれており、特にジクロルシランおよびモノシ
ランを大量に効率よく製造することが要望されて
いる。
従来から、クロルシラン類の不均斉化反応は公
知であり、またその触媒についても種々提案され
ている。例えば第３級アミン又は第４級アンモニ
ウムを含む網目状陰イオン交換樹脂、Ｎメチル２
ピロリドン、メチルイミダゾール、テトラメチル
尿素、ジメチルシアナミド、テトラメチルグアニ
ジン、トリメチルシリルイミダゾール、ベンゾチ
アゾール、NNジメチルアセトアミド等があげら
れる。これらの触媒とトリクロルシランと接触さ
せると、次の(1)、(2)及び(3)の不均斉化反応式に従
つてジクロルシラン、モノクロルシランおよびモ
ノシランが生成する。
2SiHCl2SiCl4＋SiH2Cl2 (1)
2SiH2Cl2SiHCl3＋SiH3Cl (2)
2SiH2ClSiH2Cl2＋SiH4 (3)
これについてさらに詳しく説明する。
例えば触媒として第３級アミンを含む陰イオン
交換樹脂を充填した固定床式の反応器において、
反応温度30〜200℃、圧力１〜30atmの条件下で
反応器の一方の口よりトリクロルシラン又はジク
ロルシラン等の原料水素化塩化珪素を液状で供給
すると、反応器の他方の口よりモノシラン、モノ
クロルシラン、ジクロルシラン、トリクロルシラ
ン及び四塩化珪素からなる反応生成物が得られ
る。しかし前記不均斉化反応式(1)、(2)および(3)は
平衡反応であるので、たとえ反応時間を大きくと
つたにしても原料水素化塩化珪素を100％反応完
結させることは出来ない。トリクロルシランおよ
びジクロルシランを原料として不均斉化反応させ
た場合に反応が平衡状態に到達した時のそれぞれ
モノシラン、モノクロルシラン、ジクロルシラ
ン、トリクロルシランおよび四塩化珪素の温度80
℃における不均斉化反応の平衡組成を表１に示
す。
[Industrial Application Field] The present invention supplies silicon hydride chloride to a reaction column, causes a disproportionation reaction in the presence of a catalyst, and simultaneously performs separation by a distillation effect to produce dichlorosilane, monochlorosilane, and monosilane. This invention relates to a continuous method for producing silane compounds, which continuously obtains silane compounds such as silane compounds. [Prior art and problems] Demand for dichlorosilane, monochlorosilane, monosilane, etc. is expected to increase as raw materials for high-purity silicon used in devices such as semiconductors and solar cells. There is a demand for good manufacturing. The disproportionation reaction of chlorosilanes has been known, and various catalysts have been proposed. For example, reticulated anion exchange resins containing tertiary amines or quaternary ammonium, N-methyl 2
Examples include pyrrolidone, methylimidazole, tetramethylurea, dimethylcyanamide, tetramethylguanidine, trimethylsilylimidazole, benzothiazole, and NN dimethylacetamide. When these catalysts are brought into contact with trichlorosilane, dichlorosilane, monochlorosilane and monosilane are produced according to the following disproportionation reaction formulas (1), (2) and (3). 2SiHCl 2 SiCl 4 +SiH 2 Cl 2 (1) 2SiH 2 Cl 2 SiHCl 3 +SiH 3 Cl (2) 2SiH 2 ClSiH 2 Cl 2 +SiH 4 (3) This will be explained in more detail. For example, in a fixed bed reactor filled with an anion exchange resin containing a tertiary amine as a catalyst,
When silicon hydride chloride, such as trichlorosilane or dichlorosilane, is supplied in liquid form from one port of the reactor at a reaction temperature of 30 to 200°C and a pressure of 1 to 30 atm, monosilane and monochlorosilane are supplied from the other port of the reactor. , dichlorosilane, trichlorosilane and silicon tetrachloride are obtained. However, since the disproportionation reactions (1), (2), and (3) are equilibrium reactions, even if the reaction time is increased, it is not possible to complete the reaction of the raw material silicon hydride chloride to 100%. . Temperatures of monosilane, monochlorosilane, dichlorosilane, trichlorosilane, and silicon tetrachloride when the reaction reaches an equilibrium state when a disproportionation reaction is performed using trichlorosilane and dichlorosilane as raw materials80
Table 1 shows the equilibrium composition of the disproportionation reaction at °C.
実施例 １
第１図で示す段塔式蒸留塔にて反応を行なつ
た。第１図に示す内容積10の分離槽９に予め触
媒としてトリｎ−オクチルアミンを２充填し、
触媒液温度を100℃に保つた。又、反応器上部凝
縮器３は温度−10℃に冷却した。反応器下部リボ
イラ２を加熱し、反応塔１にトリクロルシラン
2.0Kg／hrの速度で原料供給導管４から、又分離
槽９内の触媒を520ｇ／hrの速度で反応塔１に供
給した。反応塔１は20段のシーブトレイ（開口比
0.05）方式の塔である。圧力は調整器５より４
Kg／cm2Ｇに保ち、リボイラ２の液面は調節弁８に
より一定になる様に調整した。
反応塔１の塔頂温度は58℃、塔底のリボイラは
温度110℃に保持し、50時間連続運転した。塔頂
からはモノシラン92％、モノクロルシラン5.4％、
ジクロルシラン2.6％の混合ガスが90ｇ／hrの速
度で得られた。又、分離槽９から蒸発分離したク
ロルシランを凝縮器１０で冷却し、1.9Kg／hrの
速度で貯槽１１に回収した。回収液の組成をガス
クロマトグラフイーで分析した結果トリクロルシ
ラン53％、四塩化珪素47％であつた。（モル％）
実施例 ２
第１図に示す反応塔１（内容積60）に予じめ
触媒を担持したモレキユラシーブを充填した。触
媒はトリｎ−ブチルアミンを平均粒径２mmのモレ
キユラーシーブに浸漬することにより得た。反応
器上部の凝縮器３は温度−10℃に冷却した。反応
器下部のリボイラ２を加熱し、反応塔１にトリク
ロルシラン2.5Kg／hrの速度で原料供給導管４か
ら反応塔１に供給した。圧力は調整器５より３
Kg／sin2Gに保ち、リボイラ２の液面は調節弁８
により一定になる様に調整した。
反応塔１の塔頂温度は55℃、塔底リボイラ２を
温度105℃に保持し100時間連続運転した。塔頂か
らモノシラン88％、モノクロルシラン５％、シク
ロルシラン７％の混合ガスが120ｇ／hrの速度で
得られた。又分離槽９から蒸発したクロルシラン
を凝縮器１０で冷却し2.2Kg／hrの速度で貯槽１
１に回収した。回収液の組成をガスクロマトグラ
フイーで分析した結果トリクロルシラン55％、四
塩化珪素45％であつた（モル％）
実施例 ３
第２図に示す多段式反応蒸発缶１ａ，１ｂ，１
ｃ，１ｄを用いてモノシランの製造を行なつた。
触媒として、第３級アミンを担持したイオン交
換樹脂を各々の反応蒸発缶１ａ，１ｂ，１ｃ，１
ｄに500ｇづつ投入した。なお反応蒸発缶１ａ，
１ｂ，１ｃ，１ｄは各々２の内容積のものを用
いた。温度・圧力を表２に示す条件に設定後、ト
リクロルシランを1.0Kg／hrの速度で原料供給導
管６から導入し、反応を開始した。触媒とクロル
シランの接触を良くするため撹拌器２ａ，２ｂ，
２ｃ，２ｄにより撹拌した。不均斉化反応により
生成した低沸分は凝縮器３，３ｂ，３ｃ，３ｄ、
圧力調節弁４ａ，４ｂ，４ｃ，４ｄを介して後段
の反応器に送り、高沸分はフイルター５ａ，５
ｂ，５ｃ，５ｄを介し前段に戻した。各蒸発缶の
反応率は調節弁後のサンプリング口７ａ，７ｂ，
７ｃ，７ｄからサンプルを抜き出しガスクロマト
グラフイーにより組成分析して求めた。各蒸発缶
の反応条件及びガスクロによる組成分析の結果を
表２に示す。
Example 1 A reaction was carried out in a tray column type distillation column shown in FIG. Separation tank 9 with an internal volume of 10 shown in FIG. 1 was filled with two tri-n-octylamine catalysts in advance,
The catalyst liquid temperature was maintained at 100°C. Further, the reactor upper condenser 3 was cooled to a temperature of -10°C. The lower reboiler 2 of the reactor is heated, and trichlorosilane is added to the reaction column 1.
The catalyst in the separation tank 9 was supplied to the reaction column 1 at a rate of 520 g/hr from the raw material supply conduit 4 at a rate of 2.0 kg/hr. Reaction tower 1 has 20 sieve trays (opening ratio
0.05) method tower. Pressure is 4 from regulator 5
Kg/cm 2 G, and the liquid level in the reboiler 2 was adjusted using the control valve 8 to be constant. The temperature at the top of the reaction column 1 was maintained at 58°C, and the reboiler at the bottom of the column was maintained at a temperature of 110°C, and the reactor was operated continuously for 50 hours. From the top of the tower, 92% monosilane, 5.4% monochlorosilane,
A mixed gas containing 2.6% dichlorosilane was obtained at a rate of 90 g/hr. Further, the chlorosilane evaporated and separated from the separation tank 9 was cooled in a condenser 10 and recovered into a storage tank 11 at a rate of 1.9 kg/hr. The composition of the recovered liquid was analyzed by gas chromatography and found to be 53% trichlorosilane and 47% silicon tetrachloride. (mol %) Example 2 The reaction tower 1 (inner volume: 60) shown in FIG. 1 was filled with a molecular sieve on which a catalyst was supported in advance. The catalyst was obtained by soaking tri-n-butylamine in a molecular sieve having an average particle size of 2 mm. The condenser 3 at the top of the reactor was cooled to a temperature of -10°C. The reboiler 2 at the bottom of the reactor was heated, and trichlorosilane was supplied to the reaction tower 1 from the raw material supply conduit 4 at a rate of 2.5 kg/hr. Pressure is 3 from regulator 5
Kg/sin 2 G, and the liquid level in reboiler 2 is controlled by control valve 8.
Adjusted to be more constant. The top temperature of the reaction column 1 was maintained at 55°C, and the bottom reboiler 2 was maintained at a temperature of 105°C, and the reactor was operated continuously for 100 hours. A mixed gas containing 88% monosilane, 5% monochlorosilane, and 7% cyclosilane was obtained from the top of the column at a rate of 120 g/hr. In addition, the chlorosilane evaporated from the separation tank 9 is cooled in the condenser 10 and transferred to the storage tank 1 at a rate of 2.2 kg/hr.
It was collected at 1. The composition of the recovered liquid was analyzed by gas chromatography and found to be 55% trichlorosilane and 45% silicon tetrachloride (mol%).Example 3 Multi-stage reaction evaporator 1a, 1b, 1 shown in FIG.
Monosilane was produced using silanes c and 1d. As a catalyst, an ion exchange resin supporting a tertiary amine was added to each reaction evaporator 1a, 1b, 1c, 1.
500g each was added to d. Note that the reaction evaporator 1a,
1b, 1c, and 1d each had an internal volume of 2. After setting the temperature and pressure to the conditions shown in Table 2, trichlorosilane was introduced from the raw material supply conduit 6 at a rate of 1.0 kg/hr to start the reaction. In order to improve the contact between the catalyst and chlorosilane, stirrers 2a, 2b,
The mixture was stirred using 2c and 2d. The low-boiling components generated by the disproportionation reaction are sent to condensers 3, 3b, 3c, 3d,
It is sent to the subsequent reactor via pressure regulating valves 4a, 4b, 4c, 4d, and high boiling components are passed through filters 5a, 5.
It was returned to the previous stage via b, 5c, and 5d. The reaction rate of each evaporator is determined by sampling ports 7a, 7b after the control valve.
Samples were extracted from 7c and 7d, and the composition was analyzed by gas chromatography. Table 2 shows the reaction conditions of each evaporator and the results of composition analysis by gas chromatography.
本発明によれば、反応塔内で不均斉化反応と分
離が同時に起つているので表１に示したような平
衡組成の制限を受けず、従来法に比べてはるかに
効率よくシラン化合物が得られるという効果があ
る。
According to the present invention, since the disproportionation reaction and separation occur simultaneously in the reaction column, there is no restriction on the equilibrium composition shown in Table 1, and silane compounds can be obtained much more efficiently than in conventional methods. It has the effect of being
図面は本発明の実施例に用いる装置の説明図で
あつて、第１図は段塔式蒸留塔、第２図は多段式
反応蒸発缶の説明図である。
符号、１……反応塔、２……リボイラ、３……
凝縮器、４……原料供給導管、５……調節弁、６
……凝縮器、７……補集貯槽、８……調節弁、９
……分離槽、１０……凝縮器、１１……貯槽、１
ａ，１ｂ，１ｃ，１ｄ……反応蒸発缶、２ａ，２
ｂ，２ｃ，２ｄ……撹拌器、３ａ，３ｂ，３ｃ，
３ｄ……凝縮器、４ａ，４ｂ，４ｃ，４ｄ……圧
力調節弁、５ａ，５ｂ，５ｃ，５ｄ……フイルタ
ー、６……原料供給導管、７ａ，７ｂ，７ｃ，７
ｄ……ガスクロマトグラフサンプルリング口。
The drawings are explanatory diagrams of the apparatus used in the embodiments of the present invention, in which FIG. 1 is an explanatory diagram of a tray-type distillation column, and FIG. 2 is an explanatory diagram of a multi-stage reaction evaporator. Code, 1... Reaction tower, 2... Reboiler, 3...
Condenser, 4... Raw material supply conduit, 5... Control valve, 6
... Condenser, 7 ... Collection storage tank, 8 ... Control valve, 9
... Separation tank, 10 ... Condenser, 11 ... Storage tank, 1
a, 1b, 1c, 1d...reaction evaporator, 2a, 2
b, 2c, 2d... stirrer, 3a, 3b, 3c,
3d... Condenser, 4a, 4b, 4c, 4d... Pressure control valve, 5a, 5b, 5c, 5d... Filter, 6... Raw material supply conduit, 7a, 7b, 7c, 7
d...Gas chromatograph sample ring port.
Claims (1)
ランあるいはジクロルシラン等のシラン化合物を
連続的に製造するにあたり、不均斉化触媒を保持
し、かつ蒸留分離機能を有する反応装置に原料水
素化塩化珪素を供給して反応蒸留させ、反応装置
の上部より原料水素化塩化珪素より水素原子の多
いシラン化合物を取得し、一方反応装置の底部よ
り副生する塩素原子の多いシラン化合物を抜き取
るか、又は前記反応装置を多段に分け、各段に不
均斉化触媒を保持させた後、第１段反応装置に原
料水素化塩化珪素を供給して不均斉化反応させ、
第１段反応装置上部から排出される原料水素化塩
化珪素より水素原子の多いシラン化合物を第２段
反応装置に供給して反応蒸留させ、その反応装置
の底部より副生する塩素原子の多いシラン化合物
を第１段に供給し、以下この手段を次段の反応装
置に繰り返すことを特徴とするシラン化合物の連
続的製造方法。 ２ 不均斉化反応は、反応温度10〜200℃、反応
圧力（ゲージ圧）０〜30Kg／cm2である特許請求の
範囲第１項記載のシラン化合物の連続的製造方
法。[Scope of Claims] 1. A reaction apparatus that holds a disproportionation catalyst and has a distillation separation function for continuously producing silane compounds such as monosilane or dichlorosilane by subjecting silicon hydride chloride to a disproportionation reaction. The raw material hydrogenated silicon chloride is supplied and subjected to reactive distillation, and a silane compound containing more hydrogen atoms than the raw material hydrogenated silicon chloride is obtained from the upper part of the reaction apparatus, while a by-product silane compound containing many chlorine atoms is obtained from the bottom of the reaction apparatus. After extracting or dividing the reaction apparatus into multiple stages and holding a disproportionation catalyst in each stage, supplying the raw material silicon hydride chloride to the first stage reaction apparatus and causing a disproportionation reaction,
A silane compound containing more hydrogen atoms than the raw material silicon hydride chloride discharged from the upper part of the first stage reactor is supplied to the second stage reactor and subjected to reactive distillation, and a silane compound containing many chlorine atoms is produced as a by-product from the bottom of the reactor. A method for continuously producing a silane compound, characterized in that the compound is supplied to the first stage, and this process is then repeated to the next stage reactor. 2. The continuous method for producing a silane compound according to claim 1, wherein the disproportionation reaction is performed at a reaction temperature of 10 to 200°C and a reaction pressure (gauge pressure) of 0 to 30 Kg/cm 2 .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3122885A JPS61191513A (en) | 1985-02-19 | 1985-02-19 | Continuous production of silane compounds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3122885A JPS61191513A (en) | 1985-02-19 | 1985-02-19 | Continuous production of silane compounds |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61191513A JPS61191513A (en) | 1986-08-26 |
| JPH0471008B2 true JPH0471008B2 (en) | 1992-11-12 |
Family
ID=12325555
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3122885A Granted JPS61191513A (en) | 1985-02-19 | 1985-02-19 | Continuous production of silane compounds |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61191513A (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19860146A1 (en) | 1998-12-24 | 2000-06-29 | Bayer Ag | Process and plant for the production of silane |
| DE10017168A1 (en) * | 2000-04-07 | 2001-10-11 | Bayer Ag | Continuous production of silane, useful in production of silicon for semiconductors, involves catalytic disproportionation of trichlorosilane over solid catalyst in 2 or more zones with intermediate condensation |
| DE102004045245B4 (en) * | 2004-09-17 | 2007-11-15 | Degussa Gmbh | Apparatus and process for the production of silanes |
| DE102005046105B3 (en) * | 2005-09-27 | 2007-04-26 | Degussa Gmbh | Process for the preparation of monosilane |
| TWI404676B (en) * | 2006-09-27 | 2013-08-11 | Denki Kagaku Kogyo Kk | Single Silane Continuous Manufacturing Method |
| CN101798085B (en) * | 2010-04-21 | 2012-10-17 | 江苏扬农化工集团有限公司 | Preparation process of magnesium silicide method silane |
| EP2426089A1 (en) | 2010-09-03 | 2012-03-07 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Process for separating monosilane from chlorosilanes-rich mixture |
| EP2426088A1 (en) * | 2010-09-03 | 2012-03-07 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Process for producing monosilane from dichlorosilane |
-
1985
- 1985-02-19 JP JP3122885A patent/JPS61191513A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61191513A (en) | 1986-08-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US4610858A (en) | Chlorosilane disproportionation catalyst and method for producing a silane compound by means of the catalyst | |
| US20100296994A1 (en) | Catalyst and method for dismutation of halosilanes containing hydrogen | |
| US20100150809A1 (en) | enhancements for a chlorosilane redistribution reactor | |
| JPH01283817A (en) | Evaporation of semiconductor silicon by cvd | |
| TWI755148B (en) | Process for removing an impurity from a chlorosilane mixture | |
| RU2368568C2 (en) | Method of obtaining silicon | |
| KR20110015527A (en) | Manufacturing method and system of pure silicon | |
| KR20150119084A (en) | Method for producing trichlorosilane | |
| CN102264642A (en) | Process for producing chlorosilane | |
| JPH0471008B2 (en) | ||
| US8404205B2 (en) | Apparatus and method for producing polycrystalline silicon having a reduced amount of boron compounds by forming phosphorus-boron compounds | |
| JPS641406B2 (en) | ||
| TWI853194B (en) | Process for removing an impurity from a chlorosilane mixture | |
| JPS643804B2 (en) | ||
| CN223069100U (en) | Chlorosilane raw material purification system for reducing donor impurities and acceptor impurities in polycrystalline silicon | |
| US3980686A (en) | Process for the preparation of chlorosilane | |
| US20240182497A1 (en) | Method and system for selective recovery of monochlorosilane and dichlorosilane in polysilicon production process | |
| JPH0472764B2 (en) | ||
| JPH0470249B2 (en) | ||
| CN108586515B (en) | Synthesis method of trisilylamine | |
| JPS6333422B2 (en) | ||
| EP0213215B2 (en) | Chlorosilane disproportionation catalyst and method for producing a silane compound by means of the catalyst | |
| JPS59121110A (en) | Continuous preparation of silane compound | |
| TWI773121B (en) | Process for obtaining hexachlorodisilane | |
| CN116102018B (en) | Method for separating hexachlorodisilane from polysilicon byproduct oligomeric chlorosilane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |