CN108892143A - The method for purifying trichlorosilane - Google Patents
The method for purifying trichlorosilane Download PDFInfo
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- CN108892143A CN108892143A CN201811139932.9A CN201811139932A CN108892143A CN 108892143 A CN108892143 A CN 108892143A CN 201811139932 A CN201811139932 A CN 201811139932A CN 108892143 A CN108892143 A CN 108892143A
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- trichlorosilane
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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
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a kind of methods for purifying trichlorosilane.This approach includes the following steps：Trichlorosilane raw material containing dimethyl dichlorosilane (DMCS) is carried out disproportionated reaction with silicon tetrachloride and oxygen, obtained reaction product by S1 under the catalysis of catalyst；S2 carries out solid-liquor separation to reaction product and separates catalyst and reaction liquid product；And S3, trichlorosilane products are obtained after reaction liquid product is inputted rectifying column imurity-removal, light component and heavy constituent.Apply the technical scheme of the present invention reactive distillation process, methyl trichlorosilane is converted by carrying out anti-disproportionated reaction with silicon tetrachloride by the dimethyl dichlorosilane (DMCS) in raw material, simultaneously, it introduces micro amount of oxygen and B, P etc. and is converted into higher boiling complex compound, it is separated again by rectifying, finally obtains high-purity trichlorosilane.
Description
Technical field
The present invention relates to chemical fields, in particular to a kind of method for purifying trichlorosilane.
Background technique
High-purity trichlorosilane is the raw material of improved Siemens production electronic-grade polycrystalline silicon, and electronic-grade polycrystalline silicon is further
Be used for IC wafers, in addition, high-purity trichlorosilane is also used for epitaxial deposition silica-base material in chip manufacturing process,
Therefore, there is very high requirement to the purity of trichlorosilane and impurity.Currently, mainly to pass through metallic silicon direct with HCl for trichlorosilane
Synthesis, or silicon tetrachloride byproduct can be generated during polycrystalline reduction, it is reacted using metallic silicon with HCl and silicon tetrachloride
The impurity such as carbon, B, P can be introduced from feed end, it is necessary to remove above-mentioned impurity, otherwise during the reaction by generating trichlorosilane
It can be entered in electronic-grade polycrystalline silicon by raw material.The presence of carbon is very big on the carbon content influence in polysilicon, and carbon can be made with oxygen
With, it can also be present in silicon crystal in the form of striped in conjunction with interstitial atom and vacancy, when concentration of carbon is more than its solid solubility,
It has small carbon deposition to generate, influences the breakdown voltage and leakage current of device.During crystal-pulling, if concentration of carbon is more than
Its saturated concentration has SiC particulate and is formed, and leads to the formation of polycrystal.B, P etc. is deposited in the form of donor impurity and acceptor impurity
With HIGH-PURITY SILICON, induced crystal is easy when manufacturing wafer and generates defect, to influence the quality and yield rate of chip.
Carbon mainly exists in the form of methylchlorosilane and methyl-monosilane in trichlorosilane, such as dimethyl dichlorosilane (DMCS), first
Base trichlorosilane, dimethylsilane, monomethyl silane, trimethyl silane etc., wherein due to dimethyl dichlorosilane (DMCS) and trichlorosilane
Boiling point it is close, larger by rectification and purification difficulty, the content of carbon mainly exists in the form of dimethyl dichlorosilane (DMCS) in raw material.
B, the donor impurities such as P and acceptor impurity existence form multiplicity, may be BCl by inquiry document3、BmHn、
CH3BCl2、(CH3)3BCl2、PCl3、PmHn、(CH3)2PH、POCl3、PCl5Deng studying the method for mostly using rectifying and absorption at present
It removes, but because existence form is larger, it is partially close with trichlorosilane boiling point, in addition, system multiselect active carbon, functional resin
It cleans with silica gel etc., but because of poor selectivity, adsorbs lower limit for height, impurity is still in higher level in final products.
Summary of the invention
The present invention is intended to provide a kind of method for purifying trichlorosilane, to solve trichlorosilane impurity content in the prior art
Higher technical problem.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of method for purifying trichlorosilane.It should
Method includes the following steps：S1, by the trichlorosilane raw material containing dimethyl dichlorosilane (DMCS) with silicon tetrachloride and oxygen in catalyst
Catalysis is lower to carry out disproportionated reaction, obtained reaction product；S2 carries out solid-liquor separation for catalyst and reaction liquid to reaction product
Product separation；And S3, trichlorosilane is obtained after reaction liquid product is inputted rectifying column imurity-removal, light component and heavy constituent
Product.
Further, the addition mole of silicon tetrachloride is 1~10 times of dimethyl dichlorosilane (DMCS) mole, and oxygen addition rubs
Your amount is 2~50 times of donor and acceptor's impurity mole in trichlorosilane raw material.
Further, the catalyst separated in step S2 returns to S1 and re-uses.
Further, the temperature of disproportionated reaction is 20~200 DEG C in step S1, and pressure is 0.1MPa~2.0MPa.
Further, catalyst is ion exchange resin, 100 microns of partial size <, preferably 50 microns.
Further, 50 microns of solid separation accuracy < being separated by solid-liquid separation in step S2, preferably 1 micron.
Further, the tower top pressure of rectifying column is 40KPa~200KPa, and temperature is 42~68 DEG C.
Further, step S1 is carried out in the continuous flow reactor of microchannel.
Further, it before trichlorosilane raw material enters microchannel continuous flow reactor, is mixed with catalyst.
Further, the pressure of disproportionated reaction is 1.0MPa in step S1.
Apply the technical scheme of the present invention reactive distillation process, by the dimethyl dichlorosilane (DMCS) in raw material by with silicon tetrachloride
It carries out anti-disproportionated reaction and is converted into methyl trichlorosilane, meanwhile, it introduces micro amount of oxygen and B, P etc. and is converted into higher boiling complex compound, then
It is separated by rectifying, finally obtains high-purity trichlorosilane.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings：
Fig. 1 shows the flow diagram of purification trichlorosilane according to an embodiment of the present invention；And
Fig. 2 shows the apparatus structure schematic diagrams of purification trichlorosilane according to an embodiment of the present invention.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
The application proposes to use reactive distillation process, and the dimethyl dichlorosilane (DMCS) in raw material is anti-by carrying out with silicon tetrachloride
Disproportionated reaction is converted into methyl trichlorosilane, meanwhile, it introduces micro amount of oxygen and B, P etc. and is converted into higher boiling complex compound, then pass through essence
It evaporates and is separated, finally obtain high-purity trichlorosilane.Furthermore it is also possible to carry out process intensification to reaction, guarantee that system is continuous
Operation, the essential safety of lifting system introduce continuous flow micro passage reaction.
A kind of typical embodiment according to the present invention provides a kind of method for purifying trichlorosilane.This method include with
Lower step：S1 carries out the trichlorosilane raw material containing dimethyl dichlorosilane (DMCS) with silicon tetrachloride and oxygen under the catalysis of catalyst
Disproportionated reaction, obtained reaction product；S2 carries out solid-liquor separation to reaction product and separates catalyst and reaction liquid product；
And S3, trichlorosilane products are obtained after reaction liquid product is inputted rectifying column imurity-removal, light component and heavy constituent.
In step sl, dimethyl dichlorosilane (DMCS) under the action of catalyst, by the way that anti-disproportionated reaction occurs with silicon tetrachloride, makes
It obtains chloride ion distributing between silicon tetrachloride and dimethyl dichlorosilane (DMCS), converts methyl trichlorosilane for dimethyl dichlorosilane (DMCS),
Boiling point is promoted to 66 DEG C by 41 DEG C, so that the boiling-point difference with 32 DEG C of trichlorosilane increases, to be easy to carry out by rectifying column
Separation, meanwhile, it is trichlorosilane by converting silicon tetrachloride, does not introduce other impurity, reaction equation is as follows：
CH3SiHCl2+SiCl4——CH3SiCl3+SiHCl3
Preferably, the addition mole of silicon tetrachloride is 1~10 times of dimethyl dichlorosilane (DMCS) mole.In addition, reacting
In be passed through a small amount of oxygen, in the presence of oxygen, donor and acceptor's impurity by carry out chemical reaction formed Si-O-B key or
Si-O-P key, converts donor impurity and acceptor impurity, then is separated by subsequent rectifying, the oxygen demand used into
Row purifying, the addition of oxygen need excess, it is preferred that it is donor and acceptor's impurity mole in trichlorosilane raw material that mole, which is added, in oxygen
2~50 times of amount.
A kind of typical embodiment according to the present invention, the catalyst separated in step S2 return to S1 and re-use,
Catalyst utilization is improved, production cost is saved.Preferably, the temperature of disproportionated reaction is 20~200 DEG C in step S1, and pressure is
0.1MPa~2.0MPa, preferably 1.0MPa.Under this reaction temperature and pressure, be conducive to the abundant progress of disproportionated reaction.
Preferably, step S1 is carried out in the continuous flow reactor of microchannel.Reaction mass realizes that high speed is touched in microchannel
Mixing is hit, moment reaches uniform reaction environment, and reaction efficiency is high, and reaction time is short, avoids the decomposition of reactant and product
With the generation of other by-products, to improve reaction efficiency.
Preferably, it before trichlorosilane raw material enters microchannel continuous flow reactor, is mixed with catalyst.Catalyst is
Ion exchange resin loads amido, and Form Sphere guarantees that it has a preferable mobility, 100 microns of partial size <, preferably 50 microns,
So that catalyst continuously flows in microreactor channel, do not block.
A kind of typical embodiment according to the present invention, is arranged liquid-solid separator after reactor, will be in reaction product
Catalyst is continuously separated with reaction liquid product, and catalyst Returning reactor is reused, the liquid material after separation into
Enter subsequent rectifying column to be refined.Liquid-solid separator is internally provided with seperation film, 50 microns of solid separation accuracy <, and is less than and urges
The minimum grain size of agent, preferably 1 micron continuously carry out two-phase laminated flow in flowing, and process is one-way process, no air-teturning mixed phenomenon,
It avoids interval to separate, guarantees the stable operation of system.
Those skilled in the art can be calculated according to simulation and tower diameter, tower height, the tower of purification operating experience setting rectifying column
The parameters such as disk quantity and internals and filler, tower internals are plate column or sieve-plate tower, and wherein filler is metal or nonmetallic regular
Or random packing, preferably rectifying column is packed tower, and the filler in more preferable packed tower is dumped packing.Tower top pressure is 40KPa
~200KPa, in 42~68 DEG C of ranges, tower top is cooled down control temperature using recirculated water, tower reactor using hot water or conduction oil into
Row heating.
A kind of typical embodiment according to the present invention, as shown in Figure 1, the trichlorosilane raw material containing dimethyl dichlorosilane (DMCS) with
Silicon tetrachloride and oxygen carry out disproportionated reaction under the catalysis of catalyst, obtained reaction product；Using solid-liquid separator to anti-
It answers product to carry out solid-liquor separation, catalyst and reaction liquid product is separated；By reaction liquid product sequentially input lightness-removing column and
Trichlorosilane products are obtained after weight-removing column.
A kind of typical embodiment according to the present invention provides a kind of device for purifying trichlorosilane.The device mainly wraps
Include three parts, reactor, solid-liquid separator and rectifying column, wherein reactor is used for the trichlorosilane containing dimethyl dichlorosilane (DMCS)
Raw material and silicon tetrachloride and oxygen carry out being disproportionated under the catalysis of catalyst instead, and solid-liquid separator from reactor for that will be discharged
Reaction product be separated by solid-liquid separation and rectifying column for will the reaction liquid product removal that be discharged from solid-liquid separator it is miscellaneous
Matter, light component and heavy constituent.
Liquid-solid separator is set after reactor, and reactor is provided with catalyst and mouth is added, and solid-liquid separator is provided with solid
Body outlet, and the solids outlet port of solid-liquid separator is added mouth with the catalyst of reactor and is connected.It will be in reaction product
Catalyst is continuously separated with reaction liquid product, and catalyst Returning reactor is reused, the liquid material after separation into
Enter subsequent rectifying column to be refined.Liquid-solid separator is internally provided with seperation film, 50 microns of solid separation accuracy <, and is less than and urges
The minimum grain size of agent, preferably 1 micron continuously carry out two-phase laminated flow in flowing, and process is one-way process, and no back-mixing is existing
As avoiding interval and separating, guarantee the stable operation of system.
Preferably, reactor is microchannel continuous flow reactor, the channel diameter of microchannel continuous flow reactor is 100~
200 microns.Reaction mass realizes that high velocity impact mixes in microchannel, and moment reaches uniform reaction environment, and reaction efficiency is high,
Reaction time is short, the decomposition of reactant and product and the generation of other by-products is avoided, to improve reaction efficiency.
A kind of typical embodiment according to the present invention, reactor include conversion zone and are arranged around conversion zone
Heat exchanging interlayer, control the temperature of reaction.Microchannel continuous flow reactor liquid holdup is small, may be implemented continuously to manufacture, material without
Back-mixing, while enlarge-effect can be effectively eliminated, reactor is the materials such as glass, silicon carbide, ceramics, stainless steel or alloy,
Reactor setting there are three feed inlet and a discharge port, trichlorosilane, silicon tetrachloride and oxygen pass through respectively trichlorosilane into
Material mouth, silicon tetrachloride feeding mouth and oxygen feeding mouth enter reactor.
Preferably, rectifying column is made of two towers, respectively lightness-removing column and weight-removing column, and material is introduced into after reaction and filtering
Lightness-removing column separates the light component in raw material, and lightness-removing column tower reactor extraction intermediate material enters weight-removing column, removes therein heavy
Component obtains high-purity trichlorosilane products from tower top.
A kind of typical embodiment according to the present invention, as shown in Fig. 2, the mixture of trichlorosilane raw material and catalyst,
Silicon tetrachloride and oxygen pass through trichlorosilane feed inlet 11, silicon tetrachloride feeding mouth 12 and oxygen feeding mouth 13 respectively and enter instead
Device 10 is answered, the reaction product in reactor 10 inputs solid-liquid separator 20 by discharge port and carries out catalyst and reaction liquid product
Separation, mouth is added by the catalyst of the solids outlet port input reactor of solid-liquid separator in isolated catalyst, real
Existing catalyst recycles.Reaction liquid product sequentially inputs lightness-removing column 31 and weight-removing column 32 and carries out impurity, light component and again
The removing of component, wherein 31 removed overhead low-boiling-point substance of lightness-removing column, 32 tower bottom of weight-removing column remove high-boiling components, the product (trichlorine of purification
Hydrogen silicon) it is discharged from the tower top of weight-removing column 32.
Beneficial effects of the present invention are further illustrated below in conjunction with embodiment.
Embodiment 1
Using process shown in FIG. 1, using device shown in Fig. 2, wherein reactor is microchannel continuous flow reactor,
Specific test parameters such as table 1.
Table 1
In the present embodiment, trichlorosilane raw material dimethyl dichlorosilane (DMCS) content 20ppm, B content 0.5ppb, P content 1.0ppb,
Under the above conditions, dimethyl dichlorosilane (DMCS) content 2ppm, B impurity content 0.23ppb, P impurity contains in product trichlorosilane products
Measure 0.35ppb.
Embodiment 2
Using process shown in FIG. 1, using device shown in Fig. 2, wherein reactor is microchannel continuous flow reactor,
Specific test parameters such as table 2.
Table 2
In the present embodiment, trichlorosilane raw material dimethyl dichlorosilane (DMCS) content 20ppm, B content 0.5ppb, P content 1.0ppb,
Under the above conditions, dimethyl dichlorosilane (DMCS) content 1.2ppm, B impurity content 0.1ppb, P impurity contains in product trichlorosilane products
Measure 0.21ppb.
Embodiment 3
Using process shown in FIG. 1, using device shown in Fig. 2, wherein reactor is microchannel continuous flow reactor,
Specific test parameters such as table 3.
Table 3
In the present embodiment, trichlorosilane raw material dimethyl dichlorosilane (DMCS) content 20ppm, B content 0.5ppb, P content 1.0ppb,
Under the above conditions, dimethyl dichlorosilane (DMCS) content 0.2ppm, B impurity content 0.15ppb, P impurity in product trichlorosilane products
Content 0.17ppb.
Embodiment 4
Using process shown in FIG. 1, using device shown in Fig. 2, wherein reactor is microchannel continuous flow reactor,
Specific test parameters such as table 4.
Table 4
In the present embodiment, trichlorosilane raw material dimethyl dichlorosilane (DMCS) content 20ppm, B content 0.5ppb, P content 1.0ppb,
Under the above conditions, dimethyl dichlorosilane (DMCS) content 0.03ppm, B impurity content 0.02ppb, P impurity in product trichlorosilane products
Content 0.07ppb.
Embodiment 5
Using process shown in FIG. 1, using device shown in Fig. 2, wherein reactor is microchannel continuous flow reactor,
Specific test parameters such as table 5.
Table 5
In the present embodiment, trichlorosilane raw material dimethyl dichlorosilane (DMCS) content 20ppm, B content 0.5ppb, P content 1.0ppb,
Under the above conditions, dimethyl dichlorosilane (DMCS) content 0.10ppm, B impurity content 0.06ppb, P impurity in product trichlorosilane products
Content 0.11ppb.
Embodiment 6
Using process shown in FIG. 1, using device shown in Fig. 2, wherein reactor is microchannel continuous flow reactor,
Specific test parameters such as table 6.
Table 6
In the present embodiment, trichlorosilane raw material dimethyl dichlorosilane (DMCS) content 20ppm, B content 0.5ppb, P content 1.0ppb,
Under the above conditions, dimethyl dichlorosilane (DMCS) content 0.12ppm, B impurity content 0.09ppb, P impurity in product trichlorosilane products
Content 0.18ppb.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method for purifying trichlorosilane, which is characterized in that include the following steps：
Trichlorosilane raw material containing dimethyl dichlorosilane (DMCS) is disproportionated by S1 under the catalysis of catalyst with silicon tetrachloride and oxygen
Reaction, obtained reaction product；
S2 carries out solid-liquor separation to the reaction product and separates the catalyst and reaction liquid product；And
S3 obtains trichlorosilane products after the reaction liquid product is inputted rectifying column imurity-removal, light component and heavy constituent.
2. the method according to claim 1, wherein the addition mole of the silicon tetrachloride is the methyl two
1~10 times of chlorosilane mol, it is that donor and acceptor's impurity rubs in the trichlorosilane raw material that mole, which is added, in the oxygen
2~50 times of that amount.
3. the method according to claim 1, wherein described in the catalyst return separated in the S2
S1 is re-used.
4. being pressed the method according to claim 1, wherein the temperature of disproportionated reaction is 20~200 DEG C in the S1
Power is 0.1MPa~2.0MPa.
5. partial size < 100 is micro- the method according to claim 1, wherein the catalyst is ion exchange resin
Rice, preferably 50 microns.
6. the method according to claim 1, wherein the solid separation accuracy < 50 being separated by solid-liquid separation in the S2 is micro-
Rice, preferably 1 micron.
7. the method according to claim 1, wherein the tower top pressure of the rectifying column be 40KPa~200KPa,
Temperature is 42~68 DEG C.
8. the method according to claim 1, wherein the S1 is carried out in the continuous flow reactor of microchannel.
9. according to the method described in claim 8, it is characterized in that, the trichlorosilane raw material enters the microchannel continuous flow
Before reactor, mixed with catalyst.
10. according to the method described in claim 4, it is characterized in that, the pressure of disproportionated reaction is 1.0MPa in the S1.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109704345A (en) * | 2019-02-21 | 2019-05-03 | 浙江中宁硅业有限公司 | A kind of ocratation rectifier unit and its production method |
| CN111453736A (en) * | 2020-04-27 | 2020-07-28 | 江苏鑫华半导体材料科技有限公司 | Trichlorosilane purification system and method |
| CN113444121A (en) * | 2021-06-08 | 2021-09-28 | 天津大学 | Method for removing ethyl dichlorosilane impurities in dimethyl dichlorosilane |
| CN114956092A (en) * | 2022-04-21 | 2022-08-30 | 新疆大全新能源股份有限公司 | Method for separating monomethyldichlorosilane impurities from trichlorosilane |
| CN115023407A (en) * | 2020-11-05 | 2022-09-06 | 瓦克化学股份公司 | Process for removing impurities from chlorosilane mixtures |
| CN115650242A (en) * | 2022-11-21 | 2023-01-31 | 青海黄河上游水电开发有限责任公司新能源分公司 | Trichlorosilane decarbonization device and trichlorosilane decarbonization method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109704345A (en) * | 2019-02-21 | 2019-05-03 | 浙江中宁硅业有限公司 | A kind of ocratation rectifier unit and its production method |
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| CN113444121A (en) * | 2021-06-08 | 2021-09-28 | 天津大学 | Method for removing ethyl dichlorosilane impurities in dimethyl dichlorosilane |
| CN114956092A (en) * | 2022-04-21 | 2022-08-30 | 新疆大全新能源股份有限公司 | Method for separating monomethyldichlorosilane impurities from trichlorosilane |
| CN115650242A (en) * | 2022-11-21 | 2023-01-31 | 青海黄河上游水电开发有限责任公司新能源分公司 | Trichlorosilane decarbonization device and trichlorosilane decarbonization method |
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