CN102344145B - Method for preparing silane with trichlorosilane - Google Patents
Method for preparing silane with trichlorosilane Download PDFInfo
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- CN102344145B CN102344145B CN 201010244420 CN201010244420A CN102344145B CN 102344145 B CN102344145 B CN 102344145B CN 201010244420 CN201010244420 CN 201010244420 CN 201010244420 A CN201010244420 A CN 201010244420A CN 102344145 B CN102344145 B CN 102344145B
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- catalytic bed
- gas
- trichlorosilane
- exchange resin
- hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/04—Hydrides of silicon
- C01B33/043—Monosilane
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Abstract
The invention, belonging to the technical field of silicon purification, discloses a method for preparing silane with trichlorosilane, comprising the following steps that: (1) mixed gas comprising trichlorosilane gas and hydrogen is conveyed into a rectifying tower through a 20-100 DEG C catalyst bed to separate dichlorosilane gas out; (2) mixed gas comprising the dichlorosilane gas obtained from the step (1) and hydrogen is conveyed into the rectifying tower through the 20-100 DEG C catalyst bed for separation to obtain silane gas; wherein, the catalyst bed comprises anion exchange resin. According to the invention, the conversion efficiency is greatly improved, the conversion rates of the two steps can respectively reach to 18 % and 20 %; simultaneously the amount of the byproduct SiCl4 is greatly reduced, the amount of the recycled SiCl4 is reduced, and the energy consumption of the whole process is greatly reduced.
Description
Technical field
The invention belongs to silicon purification techniques field, relate in particular to a kind of method of preparing silane with trichlorosilane.
Background technology
Silane is as electronics, semi-conductor, and the critical materials gas of photovoltaic industry, and its use range is more and more wider, and usage quantity is also increasing.
At present, existing great majority enterprise both at home and abroad utilize the method for preparing silane with trichlorosilane to be discrimination method, i.e. UCC technique.Inhomogeneous reaction occurs in trichlorosilane under catalyzer exists, disproportionation obtains dichlorosilane; Dichloro hydrogen silicon is again through inhomogeneous reaction, and disproportionation obtains silane.The reaction that this technique relates to is as follows:
2?SiHCl
3＝SiH
2Cl
2+SiCl
4
2?SiH
2Cl
2＝SiH
4+SiHCl
3
In UCC technique, the two-step reaction from the trichlorosilane to silane is all reversible disproportionation reactions, and the reaction conversion ratio of product is lower.If wish improves the product transformation efficiency, being chosen to for key factor of catalyzer, but the final transformation efficiency of general catalyzer all can only be between 6%～8%.
Existing research staff gathers sight on the new efficient new catalyst of research and development, and efficiency of conversion of the catalyzer of for example improvement of Mitsui East Asia company reaches 8%～10%.Also has the new improved catalysts of many patent documentation introductions.The highest transformation efficiency at present of improved catalysts can reach 12%.But due to the unstable in various improved catalysts preparation process, and there are the problems such as absorption loss to silane product, pollution in the carrier of catalyzer, thereby improved catalysts is used and is only limited to laboratory stage always.
Therefore, improve transformation efficiency of reaction and become problem that needing to demand at present solution urgently.
Summary of the invention
Technical problem to be solved by this invention is: the low conversion rate of preparing silane with trichlorosilane in prior art, thus the method for the high preparing silane with trichlorosilane of a kind of transformation efficiency is provided.
A kind of method of preparing silane with trichlorosilane, it comprises the steps:
(1) with the mixed gas of trichlorosilane gas and hydrogen, by the catalytic bed of 20～100 ℃, then send into rectifying tower and isolate dichloro hydrogen silicon gas;
(2) step (1) is obtained the mixed gas of dichloro hydrogen silicon gas and hydrogen, by the catalytic bed of 20～80 ℃, then send into the rectifying tower separation and obtain silane gas;
Contain anionite-exchange resin in described catalytic bed.
The method of preparing silane with trichlorosilane provided by the present invention, its transformation efficiency improves greatly, and two step transformation efficiency maximums can reach respectively 18%, 20%.While by product SiCl
4Amount greatly reduce, reduced the SiCl of recycling
4Amount, greatly reduce whole process energy consumption.And in whole reaction, the utilization ratio of silicon is high.
Description of drawings
Fig. 1 is part process flow sheet of the present invention.
Embodiment
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
A kind of method of preparing silane with trichlorosilane, it comprises the steps:
(1) with the mixed gas of trichlorosilane gas and hydrogen, by the catalytic bed of 20～100 ℃, then send into rectifying tower and isolate dichloro hydrogen silicon gas;
(2) step (1) is obtained the mixed gas of dichloro hydrogen silicon gas and hydrogen, by the catalytic bed of 20～80 ℃, then send into the rectifying tower separation and obtain silane gas;
Contain anionite-exchange resin in described catalytic bed.
Reaction of the present invention is carried out under anhydrous and oxygen free condition, and this is known in those skilled in the art.Therefore before the reaction beginning, must remove whole reactive system moisture and oxygen.
Clear operation of the present invention specifically is preferably: first use nitrogen purging catalytic bed 10～60min, then be evacuated to pressure less than 100Pa; More preferably repeat aforesaid operations 5～10 times.
Wherein, trichlorosilane gas and hydrogen can be purchased, and also can oneself prepare.
For the purity that makes final product of the present invention is higher, for the requirement of material purity be: the purity of trichlorosilane gas is preferably greater than 99.99wt%.The purity of hydrogen gas is preferably 99.999wt%.
At first trichlorosilane gas is mixed with hydrogen, in mixed gas the mol ratio of trichlorosilane gas and hydrogen be preferably 4: 1～1: 6, more preferably 2: 1～1: 4.Be conducive to like this make the transformation efficiency of reaction more excellent.
Under preferable case, carried out processed before by catalytic bed, more preferably mixed gas is dewatered by dehydration column.
Then, by catalytic bed, keep the temperature of catalytic bed to remain on 20～100 ℃, more preferably 60～100 ℃ mixed gas.
Under preferable case, mixed gas refers to by catalytic bed: mixed gas passes into from the bottom of catalytic bed, flows out from the top of catalytic bed.
Mixed gas can be had an effect with anionite-exchange resin in catalytic bed by catalytic bed the time, and anionite-exchange resin can promote mixed gas to be converted into dichloro hydrogen silicon and hydrogenchloride.
Main reaction is as follows: SiHCl
3+ H
2=SiH
2Cl
2+ HCl
Also can follow main side reaction: 2SiHCl
3=SiH
2Cl
2+ SiCl
4
Also may follow other side reactions.
Wherein, anionite-exchange resin is known in those skilled in the art, and in anionite-exchange resin, the catalytic activity group can be had an effect with chlorosilane gas, changes the chlorosilane reaction intermediate, reduce reaction activity, thereby accelerate the reaction of chlorosilane and hydrogen.
The catalytic activity group of anionite-exchange resin of the present invention is preferably tertiary ammonium salt group or quaternary ammonium salt group.
The preferred macroporous type anionite-exchange resin of anionite-exchange resin of the present invention is conducive to passing through of mixed gas like this, and the larger Pressure Drop of unlikely generation.
Under preferable case, the median size of anionite-exchange resin is 0.2～1.0mm, more preferably 0.6mm.
The packing height of anionite-exchange resin in catalytic bed is preferably 400～1000mm.
When in step (1), mixed gas was by catalytic bed, be 2～5s the duration of contact of controlling mixed gas and anionite-exchange resin.
Under preferable case, in the maintenance catalytic bed, pressure is 1～12bar, more preferably 4～10bar.
From the catalytic bed effluent air, both contained dichloro hydrogen silicon, hydrogenchloride that main reaction changes into, also contain unreacted trichlorosilane, hydrogen, and tetrachloro silicane and other materials of side reaction generation.
To send into rectifying tower from the catalytic bed effluent air and carry out rectifying, then isolate dichloro hydrogen silicon gas.
Each cut outlet at rectifying tower is collected each cut and recycles.
Step (2), same step (1), first catalytic bed is carried out moisture and oxygen cleaning, preferred operations is: first use nitrogen purging whole system 10～60min, then be evacuated to pressure less than 100Pa; More preferably repeat aforesaid operations 5～10 times.
The dichloro hydrogen silicon gas that step (1) is obtained and hydrogen mix, in mixed gas the mol ratio of dichloro hydrogen silicon gas and hydrogen be preferably 3: 1～1: 5, more preferably 1: 1～1: 3.Be conducive to like this raising of transformation efficiency.
Then, by catalytic bed, keep the temperature of catalytic bed to remain on 20～80 ℃, more preferably 40～80 ℃ mixed gas.
Same step (1) also preferred mixed gas passes into from the bottom of catalytic bed, flows out from the top of catalytic bed.
The main reaction of step (2) is as follows: SiH
2Cl
2+ 2H
2=SiH
4+ 2HCl
And main side reaction: 2SiH
2Cl
2=SiH
4+ SiHCl
3
Also may follow other side reactions.
Catalytic bed is identical with principle and the purpose of the catalytic bed of step (1).According to the practical situation of reaction, the type of anionite-exchange resin can be the same, also can be different.The median size of anionite-exchange resin and packing height are also can be the same, also can be different.
When in step (2), mixed gas was by catalytic bed, be 2～5s the duration of contact of controlling mixed gas and anionite-exchange resin.
Under preferable case, in the middle maintenance of step (2) catalytic bed, pressure is 1～10bar, more preferably 4～8bar.
Step (2) had both contained from the catalytic bed effluent air silane, hydrogenchloride that main reaction changes into, also contained unreacted dichloro hydrogen silicon, hydrogen, and trichlorosilane and other materials of side reaction generation.
To send into rectifying tower from the catalytic bed effluent air and carry out rectifying, then isolate dichloro hydrogen silicon gas.
Each cut outlet at rectifying tower is collected each cut and recycles.
As shown in Figure 1, in Fig. 1, A1 represents that dehydration column, A2 represent that catalytic bed, A3 represent that chromatographic instrument, K represent that valve, 1 expression chlorosilane gas, 2 expressions connect vacuum pump, 3 expressions connect rectifying tower.
Below in conjunction with Fig. 1, as an example of step (1) example, technical process is described.At first valve-off K2, K3, K7, K8, K9, all the other valve opens; Utilize nitrogen purging pipeline 10～60min, then valve-off K1, K5, open valve K8, K9, and system is vacuumized, and pressure reaches 1～100Pa; Repeat aforesaid operations 5～10 times, in order to drain oxygen and the moisture in system.
Then valve-off K1, K8, K9, open valve K2, K3, K5, trichlorosilane gas and hydrogen are mixed after together with through dehydration column A1 dehydration, after enter in catalytic bed A2, enter rectifying tower through 3 together.Open valve K7 after question response is stable, make portion gas enter chromatographic instrument A3, analyze its composition.
The present inventor is unexpected to be found, with the mixed gas of trichlorosilane and the hydrogen catalytic bed by anionite-exchange resin, its transformation efficiency and twice transformation efficient have all had significantly raising.The present inventor is by the analysis that studies for a long period of time, and its reason of inferring is: the utilization of existing UCC method be disproportionation reaction, and the transformation efficiency of disproportionation reaction when reaching molecular balance itself is lower.And the reaction that the present invention occurs under the hydrogen effect is:
SiHCl
3+H
2＝SiH
2Cl
2+HCl
SiH
2Cl
2+2H
2＝SiH
4+2HCl
The present invention has fundamentally changed the reaction scheme of UCC technique, obtains in essence lifting from the transformation efficiency of reaction.
The invention will be further elaborated below in conjunction with specific embodiment.
Embodiment 1-5 is used for the explanation first set reaction, and embodiment 6-10 is used for explanation reaction for the second time.
First use the whole catalytic bed of nitrogen purging and each gas passage 40min, then be evacuated to pressure to 90Pa; Repeat aforesaid operations 10 times.
Trichlorosilane gas, hydrogen are mixed as 1: 2 take mol ratio, then be passed into catalytic bed with the flow of the 1.5L/min bottom inflow hole from catalytic bed.
Fill the high anionite-exchange resin of 800mm in catalytic bed, this anionite-exchange resin is macroporous type anionite-exchange resin, contains tertiary amine groups active group (Amberlyst A-21).The median size of anionite-exchange resin is 0.59mm.
In reaction process, keeping the temperature of reaction of catalytic bed is 80 ℃, and pressure is 10bar.
To introduce rectifying tower and carry out rectifying separation from catalytic bed top effluent air, obtain dichloro hydrogen silicon gas.And other each cuts are recycled.
Embodiment 2
With embodiment 1 difference be: trichlorosilane and hydrogen mix as 4: 1 take mol ratio.Other parts are with embodiment 1.
With embodiment 1 difference be: trichlorosilane and hydrogen mix as 1: 6 take mol ratio.Other parts are with embodiment 1.
Embodiment 4
With embodiment 1 difference be: the packing height of anionite-exchange resin in catalytic bed is 400mm, and other parts are with embodiment 1.
Embodiment 5
With embodiment 1 difference be: the packing height of anionite-exchange resin in catalytic bed is that other parts of 1000mm are with embodiment 1.
Embodiment 6
Obtain dichloro hydrogen silicon gas from embodiment 1-5.
Dichloro hydrogen silicon gas, hydrogen are mixed as 1: 3 take mol ratio, then be passed into catalytic bed with the flow of the 1.5L/min bottom inflow hole from catalytic bed.
Fill the high anionite-exchange resin of 800mm in catalytic bed, this this anionite-exchange resin is macroporous type anionite-exchange resin, contains the active ingredient (Dowex MWA-1) of tertiary amine groups.The median size of anionite-exchange resin is 0.68mm.
In reaction process, keeping the temperature of reaction of catalytic bed is 80 ℃, and pressure is 6bar.
Will be from catalytic bed gas out, introduce rectifying tower and carry out rectifying separation.And each cut is recycled.
Embodiment 7
With embodiment 6 differences be: dichloro hydrogen silicon and hydrogen mix as 3: 1 take mol ratio.Other parts are with embodiment 6.
Embodiment 8
With embodiment 6 differences be: dichloro hydrogen silicon and hydrogen mix as 1: 5 take mol ratio.Other parts are with embodiment 6.
Embodiment 9
With embodiment 6 differences be: the catalytic bed packing height of anionite-exchange resin is 400mm, and other parts are with embodiment 6.
Embodiment 10
With embodiment 6 differences be: the catalytic bed packing height of anionite-exchange resin is 1000mm, and other parts are with embodiment 6.
Comparative Examples 1
First use the whole catalytic bed of nitrogen purging and each gas passage 40min, then be evacuated to pressure to 90Pa; Repeat aforesaid operations 10 times.
Trichlorosilane gas is passed into catalytic bed with the flow of the 1.5L/min bottom inflow hole from catalytic bed.
Fill the high anionite-exchange resin of 800mm in catalytic bed, this this anionite-exchange resin is macroporous type anionite-exchange resin, contains tertiary ammonium salt group (Amberlyst A-21).The median size of anionite-exchange resin is 0.59mm.
In reaction process, keeping the temperature of reaction of catalytic bed is 80 ℃, and pressure is 5bar.
Will be from catalytic bed gas out, introduce rectifying tower and carry out rectifying separation, obtain dichloro hydrogen silicon gas.And other each cuts are recycled.
Comparative Examples 2
Dichloro hydrogen silicon gas is passed into catalytic bed with the flow of the 1.5L/min bottom inflow hole from catalytic bed.
Fill the high anionite-exchange resin of 800mm in catalytic bed, this this anionite-exchange resin is macroporous type anionite-exchange resin, contains tertiary ammonium salt group (Dowex MWA-1).The median size of anionite-exchange resin is 0.68mm.
In reaction process, keeping the temperature of reaction of catalytic bed is 80 ℃, and pressure is 5bar.
Will be from catalytic bed gas out, introduce rectifying tower and carry out rectifying separation.And each cut is recycled.
Performance Detection:
For out gas from catalytic bed, pass into chromatographic instrument (GC-2014) and detect, the results are shown in Table 1 and table 2.In table 1 and table 2 for the record such as other gases such as hydrogenchloride.
The transformation efficiency calculation formula of target substance:
Table 1 step (2) catalytic bed eluting gas detects
Table 2 step (2) catalytic bed eluting gas detects
As can be seen from Table 1, the relative Comparative Examples 1 of the transformation efficiency of embodiment 1-5 has had significantly raising, and the content of silicon tetrachloride reduces greatly simultaneously.This illustrates method of the present invention, can effectively improve transformation efficiency, reduces the content of silicon tetrachloride as by-product.In like manner, as can be seen from Table 2, transformation efficiency also significantly improves.Associative list 1 and table 2 illustrate that method of the present invention can improve the transformation efficiency of the finished product silane greatly.
The above is only preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. the method for a preparing silane with trichlorosilane, it comprises the steps:
(1) with the mixed gas of trichlorosilane gas and hydrogen, by catalytic bed, then send into rectifying tower and isolate dichloro hydrogen silicon gas;
(2) step (1) is obtained the mixed gas of dichloro hydrogen silicon gas and hydrogen, by catalytic bed, then send into the rectifying tower separation and obtain silane gas;
In step (1), the temperature of catalytic bed is 20～100 ℃, and in step (2), the temperature of catalytic bed is 20～80 ℃; Contain anionite-exchange resin in described catalytic bed,
Wherein, also comprised before by catalytic bed: first use nitrogen purging catalytic bed 10～60min, then be evacuated to pressure less than 100Pa, mixed gas carried out processed before by catalytic bed.
2. the method for preparing silane with trichlorosilane according to claim 1, it is characterized in that: in step (1), in described mixed gas, the mol ratio of trichlorosilane gas and hydrogen is 4: 1～1: 6.
3. the method for preparing silane with trichlorosilane according to claim 1, it is characterized in that: in step (2), in described mixed gas, the mol ratio of dichloro hydrogen silicon gas and hydrogen is 3: 1～1: 5.
4. the method for preparing silane with trichlorosilane according to claim 1, it is characterized in that: the median size of described anionite-exchange resin is 0.2～1.0mm.
5. the method for preparing silane with trichlorosilane according to claim 1, it is characterized in that: the packing height of described anionite-exchange resin is 400～1000mm.
6. the method for preparing silane with trichlorosilane according to claim 1, it is characterized in that: described anionite-exchange resin contains tertiary ammonium salt group or quaternary ammonium salt group; Described anionite-exchange resin is macroporous type anionite-exchange resin.
7. the method for preparing silane with trichlorosilane according to claim 1 is characterized in that: the pressure in step (1) in catalytic bed is 1～12bar.
8. the method for preparing silane with trichlorosilane according to claim 1 is characterized in that: the pressure in step (2) in catalytic bed is 1～10bar.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010244420 CN102344145B (en) | 2010-07-29 | 2010-07-29 | Method for preparing silane with trichlorosilane |
| PCT/CN2011/077336 WO2012013123A1 (en) | 2010-07-29 | 2011-07-19 | Process and system for preparing silane from trichlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010244420 CN102344145B (en) | 2010-07-29 | 2010-07-29 | Method for preparing silane with trichlorosilane |
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|---|---|
| CN102344145A CN102344145A (en) | 2012-02-08 |
| CN102344145B true CN102344145B (en) | 2013-05-08 |
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| CN 201010244420 Expired - Fee Related CN102344145B (en) | 2010-07-29 | 2010-07-29 | Method for preparing silane with trichlorosilane |
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|---|---|
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| WO (1) | WO2012013123A1 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102951646A (en) * | 2012-11-22 | 2013-03-06 | 覃攀 | Production method of silane |
| CN103112860B (en) * | 2013-02-26 | 2015-09-02 | 天津大学 | The method of high purity silane is prepared in improved Siemens coproduction |
| CN103253676B (en) * | 2013-05-10 | 2015-04-08 | 河北工业大学 | Preparation method of trichlorosilane |
| US9352971B2 (en) | 2013-06-14 | 2016-05-31 | Rec Silicon Inc | Method and apparatus for production of silane and hydrohalosilanes |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85101821A (en) * | 1984-03-13 | 1987-01-10 | 斯瓦罗夫斯基公司 | The method for preparing silane |
| CN101391774A (en) * | 2008-10-24 | 2009-03-25 | 王少志 | Method for producing silane gas |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE784818A (en) * | 1971-06-14 | 1972-12-13 | Westinghouse Electric Corp | CALIBRATION OF THE MOVEMENT PROFILE OF THE POSITION OF A DRIVE BY MOTOR |
| US3968199A (en) * | 1974-02-25 | 1976-07-06 | Union Carbide Corporation | Process for making silane |
| JP2519080B2 (en) * | 1988-03-07 | 1996-07-31 | 高純度シリコン株式会社 | Method for producing dichlorosilane |
| DE10044794A1 (en) * | 2000-09-11 | 2002-04-04 | Bayer Ag | Process for the preparation of trichlorosilane |
| DE102004045245B4 (en) * | 2004-09-17 | 2007-11-15 | Degussa Gmbh | Apparatus and process for the production of silanes |
-
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- 2010-07-29 CN CN 201010244420 patent/CN102344145B/en not_active Expired - Fee Related
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2011
- 2011-07-19 WO PCT/CN2011/077336 patent/WO2012013123A1/en active Application Filing
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85101821A (en) * | 1984-03-13 | 1987-01-10 | 斯瓦罗夫斯基公司 | The method for preparing silane |
| CN101391774A (en) * | 2008-10-24 | 2009-03-25 | 王少志 | Method for producing silane gas |
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|---|---|
| CN102344145A (en) | 2012-02-08 |
| WO2012013123A1 (en) | 2012-02-02 |
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