JPS6270425A - Manufacturing method of chloropolysilane - Google Patents
Manufacturing method of chloropolysilaneInfo
- Publication number
- JPS6270425A JPS6270425A JP21026485A JP21026485A JPS6270425A JP S6270425 A JPS6270425 A JP S6270425A JP 21026485 A JP21026485 A JP 21026485A JP 21026485 A JP21026485 A JP 21026485A JP S6270425 A JPS6270425 A JP S6270425A
- Authority
- JP
- Japan
- Prior art keywords
- chloropolysilane
- catalyst
- results
- activated alumina
- manufacturing
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 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 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- -1 SiC14 Chemical compound 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 229910021346 calcium silicide Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910001947 lithium oxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 description 1
- PZKOFHKJGUNVTM-UHFFFAOYSA-N trichloro-[dichloro(trichlorosilyl)silyl]silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)[Si](Cl)(Cl)Cl PZKOFHKJGUNVTM-UHFFFAOYSA-N 0.000 description 1
- VEDJZFSRVVQBIL-UHFFFAOYSA-N trisilane Chemical compound [SiH3][SiH2][SiH3] VEDJZFSRVVQBIL-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Catalysts (AREA)
- Silicon Polymers (AREA)
- Silicon Compounds (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
く技術分野〉
本願発明はクロロポリシランの新規な製造方法に関する
。DETAILED DESCRIPTION OF THE INVENTION Technical Field The present invention relates to a novel method for producing chloropolysilane.
ヘキサクロロジシラン（Ｓｉ２ Ｇ＋６ ） 、 オク
タクロロトリシラン（Ｓｉ３ ＣＩＢ ）等のクロロポ
リシラは、集積回路のエピタキシャルシリコン層、太陽
電池のアモルファスシリコン層、ゼログラフ複写機のア
モルファスシリコン感光層、あるいは各種珪化物セラミ
ックス、等の製造原料として注目されているジシラン（
Ｓｉ２．）１６）やトリシラン（Ｓｔ３Ｈｅ）ようなポ
リシランを製造するための中間体として、またオルガノ
シラン、珪酸エステルの原料して重要である。Chloropolysilanes such as hexachlorodisilane (Si2 G+6) and octachlorotrisilane (Si3 CIB) are used in epitaxial silicon layers of integrated circuits, amorphous silicon layers of solar cells, amorphous silicon photosensitive layers of xerographic copying machines, various silicide ceramics, etc. Disilane (
Si2. )16) and trisilane (St3He), and as a raw material for organosilanes and silicate esters.
〈従来技術とその問題点〉
従来クロロポリシランの製法は珪化カルシウムと塩素の
反応によるものであるが、収率は高々２０％と非常に低
く、また副生物として多量の塩化カルシウムが生じ、こ
れが珪化カルシウムの表面を覆い、反応の進行を妨害す
るので、これを頗繁に除去しなければならないことが難
点である。<Prior art and its problems> The conventional method for producing chloropolysilane is based on the reaction of calcium silicide and chlorine, but the yield is very low at 20% at most, and a large amount of calcium chloride is produced as a by-product, which is caused by silicification. The problem is that it covers the surface of calcium and obstructs the progress of the reaction, so it must be removed frequently.
それゆえに、収率のよい、副生物の生成のないクロロポ
リシランの製法の開発が望まれている。Therefore, it is desired to develop a method for producing chloropolysilane with good yield and without the formation of by-products.
〈発明の構成〉
本発明によれば、リチウムとマグネシウムの複合酸化物
を触媒として、２００℃〜７００°Ｃの温度でクロロモ
ノシラン、 即ち、Ｓ ｉＣ１４，５ｉＨＣ１３，５ｊ
Ｈ７Ｃ１２，５ｉＨ３ＣＩまたはこれらの程合物を重合
させることを特徴とするクロロポリシランの製造方法が
提供される。<Configuration of the Invention> According to the present invention, chloromonosilane, i.e., SiC14,5iHC13,5j, is produced at a temperature of 200°C to 700°C using a composite oxide of lithium and magnesium as a catalyst.
A method for producing chloropolysilane is provided, which comprises polymerizing H7C12,5iH3CI or a compound thereof.
本発明方法において、触媒物質は通常触媒効果を高める
ために、担体に担持させる。担体は特に限定されないが
、活性アルミナ、シリカゲル、モレキュラーシーブ等が
好適である。In the method of the present invention, the catalytic material is usually supported on a carrier in order to enhance the catalytic effect. The carrier is not particularly limited, but activated alumina, silica gel, molecular sieve, etc. are suitable.
反応温度は２００℃未満では重合が起らず、また７００
℃を越えると、生成したクロロポリシランが分解し始め
る。Polymerization does not occur at a reaction temperature of less than 200°C;
When the temperature exceeds ℃, the chloropolysilane produced begins to decompose.
生成混合物は蒸留によって目的のクロロポリシランを分
別採取することができる。The desired chloropolysilane can be fractionated from the resulting mixture by distillation.
〈実施態様〉 以下本発明を実施例により具体的に例示する。<Embodiment> The present invention will be specifically illustrated below with reference to Examples.
実施例１
Ｌｉ とＭｇを酸化物に換算して１：２の割合で含む複
合酸化物を含浸法により５％担持させた活性アルミナ（
硝酸リチウム４．６ｇ及び硝酸マグネシウム１２．８ｇ
を溶解した水２００ ｍ ｌを活性アルミナ（直径２〜
３＋ａｍの球状）に含浸させ、この活性アルミナを酸素
雰囲気で５時間焙焼した。）を長さ２０ｃｍの石英管に
充填した。触媒の充填されている部分を５００℃に加熱
し、線速度１ ｃｍ／ｓｅｅで四塩化珪素を流し、生成
物を冷却してガスクロマトグラフ法により分析した。結
果は第１表に示す。Example 1 Activated alumina (5% of composite oxide containing Li and Mg in a ratio of 1:2 in terms of oxides) was supported by an impregnation method.
4.6g of lithium nitrate and 12.8g of magnesium nitrate
200 ml of water dissolved in activated alumina (diameter 2~
The activated alumina was impregnated with spherical particles (3+am), and the activated alumina was roasted in an oxygen atmosphere for 5 hours. ) was filled into a 20 cm long quartz tube. The part filled with catalyst was heated to 500° C., silicon tetrachloride was passed through it at a linear velocity of 1 cm/see, and the product was cooled and analyzed by gas chromatography. The results are shown in Table 1.
第１表
実施例２〜４、比較例１〜２
触媒の加熱温度を変えた他は実施例１と同様の実験を行
った。結果は第２表に示す。Table 1 Examples 2 to 4, Comparative Examples 1 to 2 The same experiment as in Example 1 was conducted except that the heating temperature of the catalyst was changed. The results are shown in Table 2.
実施例５〜８
触媒層の長さを変えた他は実施例１と同様の実験を行っ
た。結果は第３表に示す。Examples 5 to 8 The same experiments as in Example 1 were conducted except that the length of the catalyst layer was changed. The results are shown in Table 3.
実施例９〜ｌＯ
活性アルミナに担持させる複合酸化物の割合を変化させ
た他は実施例１と同様の実験を行った。Example 9 - IO An experiment similar to Example 1 was conducted except that the proportion of the composite oxide supported on activated alumina was changed.
結果は第４表に示す。The results are shown in Table 4.
実施例１１〜１３
触媒であるＬｉとＭｇの比を変えた他は実施例１と同様
の実験を行った。結果は第５表に示す。Examples 11 to 13 The same experiment as in Example 1 was conducted except that the ratio of Li and Mg as catalysts was changed. The results are shown in Table 5.
比較例３〜４
触媒として酸化リチウム、又は酸化マグネシウムを用い
た他は実施例１と同様の実験を行った。Comparative Examples 3 to 4 The same experiment as in Example 1 was conducted except that lithium oxide or magnesium oxide was used as a catalyst.
結果は第６表に示す。The results are shown in Table 6.
第２表 第３表 陣量％］ 第４表 ［重都−％］Table 2 Table 3 Quantity%] Table 4 [Juto -%]
Claims (1)
、２００℃〜７００℃の温度でクロロモノシランを重合
させることを特徴とするクロロポリシランの製造方法。 ２、特許請求の範囲第１項記載の方法であって、生成系
の蒸留によって目的クロロポリシランを分別採取する方
法。[Claims] 1. A method for producing chloropolysilane, which comprises polymerizing chloromonosilane at a temperature of 200°C to 700°C using a composite oxide of lithium and magnesium as a catalyst. 2. The method according to claim 1, in which the target chloropolysilane is fractionally collected by distillation of the product system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21026485A JPS6270425A (en) | 1985-09-25 | 1985-09-25 | Manufacturing method of chloropolysilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21026485A JPS6270425A (en) | 1985-09-25 | 1985-09-25 | Manufacturing method of chloropolysilane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6270425A true JPS6270425A (en) | 1987-03-31 |
| JPH0417892B2 JPH0417892B2 (en) | 1992-03-26 |
Family
ID=16586505
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21026485A Granted JPS6270425A (en) | 1985-09-25 | 1985-09-25 | Manufacturing method of chloropolysilane |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6270425A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011523926A (en) * | 2008-05-27 | 2011-08-25 | シュパウント プライベート ソシエテ ア レスポンサビリテ リミテ | Halogenated polysilane and heat treatment for its production |
-
1985
- 1985-09-25 JP JP21026485A patent/JPS6270425A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011523926A (en) * | 2008-05-27 | 2011-08-25 | シュパウント プライベート ソシエテ ア レスポンサビリテ リミテ | Halogenated polysilane and heat treatment for its production |
| US9617391B2 (en) | 2008-05-27 | 2017-04-11 | Nagarjuna Fertilizers And Chemicals Limited | Halogenated polysilane and thermal process for producing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0417892B2 (en) | 1992-03-26 |
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