CN102515169A - Method for producing disilane by reaction of magnesium silicide and ammonium chloride - Google Patents
Method for producing disilane by reaction of magnesium silicide and ammonium chloride Download PDFInfo
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- CN102515169A CN102515169A CN2011104233914A CN201110423391A CN102515169A CN 102515169 A CN102515169 A CN 102515169A CN 2011104233914 A CN2011104233914 A CN 2011104233914A CN 201110423391 A CN201110423391 A CN 201110423391A CN 102515169 A CN102515169 A CN 102515169A
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- silicoethane
- silane
- valve
- silicide
- ammonium chloride
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Abstract
The invention discloses a method for producing disilane by the chemical reaction of magnesium silicide and ammonium chloride in a liquid ammonia medium. A silicide is synthesised at 600-900 DEG C and may be high-order magnesium chloride, i.e., Mg2Si2. The silicide is good for forming disilane. Once the mixed airflow of a crude silane purification device flows through a cold trap at minus 110 DEG C, the disilane is changed into liquid and condensed in a liquefaction bottle for disilane, and then the silane and hydrogen continue to enter in a working procedure of purification along a pipeline.
Description
Technical field
The invention belongs to the organic intermediate preparing technical field, relate to silicoethane the preparation method, say so more specifically adopt magnesium silicide and ammonium chloride to react to produce silicoethane method.
Background technology
Existing silicoethane production technique is mainly used gas item chromatography, and this method output small-scale production cost is very high, is difficult to the mass-producing supply, can not satisfy the growing market requirement.
Silicoethane is spontaneous combustion in air, and point of ignition is a room temperature, runs into air just burning of moment, and is decomposed into SiH
4And H
2The burning concentration wide ranges, 0.2% when above, flame is sent in burning, 0.2% when following, carries out oxidizing reaction and generates white SiO
2In chlorine, burn also explosively.React with halogen gas explosively,, then moderately carry out halogenation as at low temperature.With SF
6Contact is blast then.With tetracol phenixin and chloroform intense reaction.Generate silane and hydrogen with basic metal and mercury alloys reaction decomposes.With the Ke Xingjia effect H that dissociates
2Do not react with pure water and acid, but generate silicate and hydrogen with alkali reaction.Even from glass, dissolve the existence of the sort of degree trace alkali that, also can make the silicoethane hydrolysis.In the presence of KH or LiCl impurity, also decompose lentamente at normal temperature.
Si
2H
6—→SiH4+(SiH2)x
Silicoethane dissolves in dithiocarbonic anhydride, ethyl alcohol, benzene and ethyl silicic acid.Its corrosion rubber, butter class, lubricating oil, lead etc., but most metal is not corroded.
At present, in the prior art silicoethane the preparation method be that reduction silicoethane verivate obtains silicoethane in solvent, at normal pressure or add to depress and react, and to 10～80 ℃ reaction solution, be blown into rare gas element heating, separablely from solvent go out silicoethane.The long flow path that this kind method is produced, foreign gas is many, water-content is high, and production cost is very high, and purity is low, for next step purification causes very big difficulty.
Summary of the invention
Problem to be solved by this invention is, overcomes the deficiency of prior art, provide a kind of adopt magnesium silicide and ammonium chloride to react to produce silicoethane method.
Preparing method of the present invention is following:
A kind of adopt magnesium silicide and ammonium chloride in the liquefied ammonia medium, carry out chemical reaction produce silicoethane method, it is characterized in that silicide 600-900 ℃ of following synthesizing silane production,
2Mg
2Si?+?8NH
4Cl
?Si
2H
6?
?+?4MgCl
2?+?8NH
3?
?+?H
2 
Close 1#, 4# valve, open 2# and 3# valve; (main ingredient is H from the mixed airflow of thick silane purifying plant
2, SiH
4, Si
2H
6) ,-110 ℃ of cold-traps of flowing through, silicoethane just becomes liquid state, silicoethane in the liquefaction bottle cohesion down, silane continues to descend purification process along the pipeline entering with hydrogen; When silicoethane in liquefaction bottle, take in a great deal of after, close 2#, 3# valve, open 1#, 4# valve; 1. let production of silane proceed; 2. let liquid silicoethane vaporize again, purify, just can obtain high-purity silicoethane product silicon and magnesium through purifying plant.
Method of the present invention mainly is at 600-900 ℃ of following synthesizing magnesium silicide, and it is with a kind of Mg
2The form of Si exists, and what obtain is silicomethane entirely.Silicide the high-order magnesium silicide can occur, Mg at 400-500 ℃ of following synthetic
2Si
2This silicide helps forming silicoethane.
2Mg
2Si?+?8NH
4Cl
Si
2H
6?
?+?4MgCl
2?+?8NH
3?
?+?H
2 
When carrying out production of silane, close 1#, 4# valve, open 2# and 3# valve.(main ingredient is H2, SiH4, Si2H6 from the mixed airflow of thick silane purifying plant ... )-110 ℃ of cold-traps of flowing through; Silicoethane just becomes liquid state; Silicoethane in the liquefaction bottle cohesion down, silane continues to descend purification process along the pipeline entering with hydrogen.
When silicoethane in liquefaction bottle, take in a great deal of after, close 2#, 3# valve, open 1#, 4# valve.1. let production of silane proceed.2. let liquid silicoethane vaporize again, purify, just can obtain high-purity silicoethane product through purifying plant.
Subject matter is that the raw material magnesium silicide burns and makes temperature controlling in the process in preparation silicoethane process; To be lower than 600 degree scarcely; Preferably remain on about 900 degree, the silicoethane output of preparation is high like this, and the silicomethane that the magnesium silicide reaction back that other temperature are produced produces is many.
The present invention adopt magnesium silicide and ammonium chloride in the liquefied ammonia medium, carry out chemical reaction produce silicoethane method compared with prior art, have the following advantages:
(1) the present invention adopt magnesium silicide and ammonium chloride to react to produce silicoethane method, silicoethane is just produced a kind of sub product in the silane process, reduced investment, saving energy, production cost are lower.
(2) the present invention solve the scale operation silicoethane technical problem, improve to produce greatly high-purity silicoethane production efficiency reduce production costs, very high economic benefit is just arranged.
Description of drawings:
Fig. 1 is a silicoethane preparation technology schema; Wherein 1-magnesium silicide, ammonium chloride charging system; 2-liquefied ammonia storage tank; The 3-reaction kettle; The 4-condensing surface; The thick silane purifying plant of 5-; The dark purifying plant of 6-silane; 7-silicoethane liquefying plant; 8-silicoethane purifying plant.
Embodiment:
Below in conjunction with embodiment the present invention is described; The scheme of embodiment described here; Do not limit the present invention; One of skill in the art can make improvements and change according to spirit of the present invention, and described these improvement and variation all should be regarded as within the scope of the invention, and scope of the present invention and essence are limited claim.
Adopt magnesium silicide and ammonium chloride in the liquefied ammonia medium, carry out chemical reaction produce silicoethane method, it is characterized in that silicide 800 ℃ of following synthesizing silane productions,
2Mg
2Si?+?8NH
4Cl?
Si
2H
6?
?+?4MgCl
2?+?8NH
3?
?+?H
2 
Close 1#, 4# valve, open 2# and 3# valve; (main ingredient is H from the mixed airflow of thick silane purifying plant
2, SiH
4, Si
2H
6) ,-110 ℃ of cold-traps of flowing through, silicoethane just becomes liquid state, silicoethane in the liquefaction bottle cohesion down, silane continues to descend purification process along the pipeline entering with hydrogen; When silicoethane in liquefaction bottle, take in a great deal of after, close 2#, 3# valve, open 1#, 4# valve; 1. let production of silane proceed; 2. let liquid silicoethane vaporize again, purify, just can obtain high-purity silicoethane product through purifying plant.
Adopt magnesium silicide and ammonium chloride in the liquefied ammonia medium, carry out chemical reaction produce silicoethane method, it is characterized in that silicide 600 ℃ of following synthesizing silane productions,
2Mg
2Si?+?8NH
4Cl
?Si
2H
6?
?+?4MgCl
2?+?8NH
3?
?+?H
2 
Close 1#, 4# valve, open 2# and 3# valve; (main ingredient is H from the mixed airflow of thick silane purifying plant
2, SiH
4, Si
2H
6) ,-110 ℃ of cold-traps of flowing through, silicoethane just becomes liquid state, silicoethane in the liquefaction bottle cohesion down, silane continues to descend purification process along the pipeline entering with hydrogen; When silicoethane in liquefaction bottle, take in a great deal of after, close 2#, 3# valve, open 1#, 4# valve; 1. let production of silane proceed; 2. let liquid silicoethane vaporize again, purify, just can obtain high-purity silicoethane product through purifying plant.
Embodiment 3
Adopt magnesium silicide and ammonium chloride in the liquefied ammonia medium, carry out chemical reaction produce silicoethane method, it is characterized in that silicide 900 ℃ of following synthesizing silane productions,
2Mg
2Si?+?8NH
4Cl?
Si
2H
6?
+?4MgCl
2?+?8NH
3?
?+?H
2 
Close 1#, 4# valve, open 2# and 3# valve; (main ingredient is H from the mixed airflow of thick silane purifying plant
2, SiH
4, Si
2H
6) ,-110 ℃ of cold-traps of flowing through, silicoethane just becomes liquid state, silicoethane in the liquefaction bottle cohesion down, silane continues to descend purification process along the pipeline entering with hydrogen; When silicoethane in liquefaction bottle, take in a great deal of after, close 2#, 3# valve, open 1#, 4# valve; 1. let production of silane proceed; 2. let liquid silicoethane vaporize again, purify, just can obtain high-purity silicoethane product through purifying plant.
Embodiment 4
Adopt magnesium silicide and ammonium chloride in the liquefied ammonia medium, carry out chemical reaction produce silicoethane method, it is characterized in that silicide 750 ℃ of following synthesizing silane productions,
2Mg
2Si?+?8NH
4Cl?
Si
2H
6?
?+?4MgCl
2?+?8NH
3 
+?H
2 
Close 1#, 4# valve, open 2# and 3# valve; (main ingredient is H from the mixed airflow of thick silane purifying plant
2, SiH
4, Si
2H
6) ,-110 ℃ of cold-traps of flowing through, silicoethane just becomes liquid state, silicoethane in the liquefaction bottle cohesion down, silane continues to descend purification process along the pipeline entering with hydrogen; When silicoethane in liquefaction bottle, take in a great deal of after, close 2#, 3# valve, open 1#, 4# valve; 1. let production of silane proceed; 2. let liquid silicoethane vaporize again, purify, just can obtain high-purity silicoethane product through purifying plant.
Comparison test:
The silicoethane of ordinary method preparation:
Silicoethane the preparation method be that reduction silicoethane verivate obtains silicoethane in solvent, at normal pressure or add to depress and react, and to 10～80 ℃ reaction solution, be blown into rare gas element heating, separablely from solvent go out silicoethane.The long flow path that this kind method is produced, foreign gas is many, water-content is high, and production cost is very high, and purity is low, for next step purification causes very big difficulty;
The silicoethane quality examination situation of the present invention's preparation:
| NO. | Item | Specification | |
| 1 | Purity? | Silicoethane | 99.999% |
| 2 | Oxyen& Argon | O 2+AR | 1ppm |
| 3 | Hydrogen | H2 | 12 ppm |
| 4 | Nitrogen | N2 | 0. 5 |
| 5 | Carbon Dioxide | C02 | 0.11? ppm |
| 6 | Carbon Monoxide | C0 | 0.18 ppm |
| 7 | Water | H2O | 0.1 ppm |
| 8 | Particle | ? | 10 pcs/cu.ft>;0.1 μm |
The silicoethane method steps of the present invention's preparation:
The first step: silica flour and magnesium powder are placed in the synthetic furnace, at 1000 ℃ of following synthesizing magnesium silicides.
Second step: adopt magnesium silicide and ammonium chloride in the liquefied ammonia medium, carry out chemical reaction produce silicoethane method,
2Mg
2Si?+?8NH
4Cl
?Si
2H
6?
?+?4MgCl
2?+?8NH
3?
?+?H
2 
Close 1#, 4# valve, open 2# and 3# valve; (main ingredient is H from the mixed airflow of thick silane purifying plant
2, SiH
4, Si
2H
6) ,-110 ℃ of cold-traps of flowing through.
The 3rd step: silicoethane just becomes liquid state, silicoethane in the liquefaction bottle cohesion down, silane continues purification process under the pipeline entering with hydrogen; When silicoethane in liquefaction bottle, take in a great deal of after, close 2#, 3# valve, open 1#, 4# valve; 1. let production of silane proceed; 2. let liquid silicoethane vaporize again, purify, just can obtain high-purity silicoethane product through purifying plant.
Claims (1)
- One kind adopt magnesium silicide and ammonium chloride in the liquefied ammonia medium, carry out chemical reaction produce silicoethane method, it is characterized in that silicide 600-900 ℃ of following synthesizing silane production, closes 1#, 4# valve, open 2# and 3# valve; From the mixed airflow of thick silane purifying plant ,-110 ℃ of cold-traps of flowing through, silicoethane just becomes liquid state, silicoethane in the liquefaction bottle cohesion down, silane continues to descend purification process along the pipeline entering with hydrogen; When silicoethane in liquefaction bottle, take in a great deal of after, close 2#, 3# valve, open 1#, 4# valve; 1. let production of silane proceed; 2. let liquid silicoethane vaporize again, purify, just can obtain high-purity silicoethane product through purifying plant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104233914A CN102515169A (en) | 2011-12-16 | 2011-12-16 | Method for producing disilane by reaction of magnesium silicide and ammonium chloride |
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|---|---|---|---|
| CN2011104233914A CN102515169A (en) | 2011-12-16 | 2011-12-16 | Method for producing disilane by reaction of magnesium silicide and ammonium chloride |
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| CN102515169A true CN102515169A (en) | 2012-06-27 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936014A (en) * | 2012-10-22 | 2013-02-20 | 贺孝鸣 | Method and device for producing disilane through reaction of alloyed composition and ammonium chloride in liquid ammonia |
| CN104724711A (en) * | 2015-02-02 | 2015-06-24 | 上海万寅安全环保科技有限公司 | Manufacturing method for silane type product |
| CN106185949A (en) * | 2016-08-02 | 2016-12-07 | 浙江迅鼎半导体材料科技有限公司 | A kind of manufacture method of Disilicoethane |
| CN107531491A (en) * | 2016-02-16 | 2018-01-02 | 昭和电工株式会社 | The manufacture method of oligomeric silane |
| CN109803921A (en) * | 2016-09-23 | 2019-05-24 | 昭和电工株式会社 | The manufacturing method of oligomeric silane |
| CN112661161A (en) * | 2020-12-28 | 2021-04-16 | 烟台万华电子材料有限公司 | Method for continuously producing high-order silane |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102205968A (en) * | 2010-03-31 | 2011-10-05 | 天津市泰亨气体有限公司 | Process technology of method for preparing silane by using magnesium silicide |
-
2011
- 2011-12-16 CN CN2011104233914A patent/CN102515169A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102205968A (en) * | 2010-03-31 | 2011-10-05 | 天津市泰亨气体有限公司 | Process technology of method for preparing silane by using magnesium silicide |
Non-Patent Citations (1)
| Title |
|---|
| 中国工业气体工业协会: "《中国工业气体大全第四册》", 31 May 2008 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936014A (en) * | 2012-10-22 | 2013-02-20 | 贺孝鸣 | Method and device for producing disilane through reaction of alloyed composition and ammonium chloride in liquid ammonia |
| CN102936014B (en) * | 2012-10-22 | 2015-05-27 | 贺孝鸣 | Method and device for producing disilane through reaction of alloyed composition and ammonium chloride in liquid ammonia |
| CN104724711A (en) * | 2015-02-02 | 2015-06-24 | 上海万寅安全环保科技有限公司 | Manufacturing method for silane type product |
| CN107531491A (en) * | 2016-02-16 | 2018-01-02 | 昭和电工株式会社 | The manufacture method of oligomeric silane |
| CN107531491B (en) * | 2016-02-16 | 2020-12-18 | 昭和电工株式会社 | Method for producing oligomeric silane |
| CN106185949A (en) * | 2016-08-02 | 2016-12-07 | 浙江迅鼎半导体材料科技有限公司 | A kind of manufacture method of Disilicoethane |
| CN106185949B (en) * | 2016-08-02 | 2018-03-09 | 浙江迅鼎半导体材料科技有限公司 | A kind of manufacture method of disilane |
| CN109803921A (en) * | 2016-09-23 | 2019-05-24 | 昭和电工株式会社 | The manufacturing method of oligomeric silane |
| CN109803921B (en) * | 2016-09-23 | 2022-03-11 | 昭和电工株式会社 | Method for producing oligomeric silane |
| CN112661161A (en) * | 2020-12-28 | 2021-04-16 | 烟台万华电子材料有限公司 | Method for continuously producing high-order silane |
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Application publication date: 20120627 |
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