CN106379902A - Preparation method of ultra-high-purity silicon tetrachloride - Google Patents
Preparation method of ultra-high-purity silicon tetrachloride Download PDFInfo
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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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- 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
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
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Abstract
The invention discloses a preparation method of ultra-high-purity silicon tetrachloride. The preparation method comprises the following steps of S1, continuously introducing high-purity silicon tetrachloride into a photochemical reactor under the effect of nitrogen gas; S2, under the ultraviolet light illumination condition, continuously introducing chlorine gas into the photochemical reactor so that hydrogen-containing impurities in the high-purity silicon tetrachloride take photochloration reaction with the chlorine gas to obtain a primary product; S3, introducing the primary product into a stripping tower from the upper part of the stripping tower; introducing the nitrogen gas from the bottom of the stripping tower so as to remove unreacted chlorine gas in the primary product to obtain a secondary product; S4, feeding the secondary product into a silicon tetrachloride purification tower; after continuous light impurity removal and heavy impurity removal, obtaining the ultra-high-purity silicon tetrachloride. Optical fiber silicon tetrachloride prepared by the method has the advantages that the purity can reach 99.9999999 percent or higher; the relevant group infrared transmission index meets or even exceeds the Merk company high-purity silicon tetrachloride index; the quality requirements of the ultra-high-purity silicon tetrachloride are also met.
Description
Technical field
The present invention relates to technical field of electronic materials, in particular to a kind of preparation method of ultra-pure Silicon chloride..
Background technology
In polysilicon production process can the substantial amounts of Silicon chloride. of by-product, its both can be used to prepare trichlorosilane return many
Crystallographic system is united it is also possible to prepare the silicon industrial chain product of a lot of high added values, such as gas-phase silica, preform and silester
Deng wherein optical fiber level Silicon chloride. is one of important source material of optical fiber cable preparing raw material preform.
With the propulsion of the construction projects such as " light entering and copper back ", the startup of " fiber to the home " project, the integration of three networks and 3G network,
China has become global most important optical fiber cable market and the optical fiber cable manufacturing nation of whole world maximum.But it is used for preparing predispersed fiber
The high purity silicon tetrachloride heavy dependence import of system rod, this makes the development of China's optical communications industry greatly be subject to external pining down,
Realize its large-scale production to contribute to solving China's optical communication industry bottleneck problem.
Optical fiber prefabricating rod production process is divided into sedimentation in pipe external sediment method and pipe, according to the difference of production technology, optical fiber
Level Silicon chloride. can be divided into high purity silicon tetrachloride (more than purity 6N, that is, more than 99.9999%) and ultra-pure Silicon chloride. (purity
9N～13N, that is, 99.9999999%～99.99999999999%), the quality index of wherein high purity silicon tetrachloride product is easy
Reached by schemes such as rectification and purification or absorption, product can be used for pipe external sediment method and prepares preform, and ultra-pure tetrachloro
The prescription of SiClx is higher, and it separates difficult point and is micro hydrogen containing foreign, and product can be used for managing interior sedimentation prepares optical fiber
Prefabricated rods and semicon industry.Table 1 is part hydrogen containing foreign and its boiling point in Silicon chloride., it can be found that hydrogen containing foreign and four
The boiling point of silicon chloride is sufficiently close to, and is difficult to remove hydrogen containing foreign by conventional rectification process.
Table 1 Silicon chloride. and part hydrogen containing foreign boiling point table
Content of the invention
The present invention is intended to provide a kind of preparation method of ultra-pure Silicon chloride., this technique is particularly suited for polysilicon enterprise
The ultra-pure Silicon chloride. of large-scale continuous production.
To achieve these goals, according to an aspect of the invention, it is provided a kind of preparation of ultra-pure Silicon chloride.
Method.This preparation method comprises the following steps：S1, high purity silicon tetrachloride is continuously passed through photochemical reactor under nitrogen effect
Interior；S2, under ultraviolet irradiation condition, is continuously passed through chlorine into photochemical reactor, makes hydrogeneous miscellaneous in high purity silicon tetrachloride
There is optical chlorinating reaction with chlorine in matter, obtain primary product；S3, primary product are passed through in stripper from the top of stripper,
Nitrogen is passed through from the bottom of stripper, obtains secondary products to remove unreacted chlorine in primary product；And S4, by secondary
Product sends into Silicon chloride. purifying column, after continuously taking off light and de- weight, obtains ultra-pure Silicon chloride..
Further, in S1 and S3, the dew point of nitrogen is not less than -90 DEG C.
Further, in S2, the purity of chlorine is not less than 99.999%.
Further, in S2, chlorine is 1～10 with the volume ratio of high purity silicon tetrachloride:1.
Further, in S3, the temperature of nitrogen is 120～200 DEG C, and nitrogen is 1～10 with the volume ratio of primary product:1.
Further, Silicon chloride. purifying column is made up of de- light purifying column and de- repurified tower, wherein, takes off light purifying column
Reflux ratio is 100～200, and the reflux ratio of de- repurified tower is 10～20.
Further, taking off light purifying column and de- repurified tower is packed tower, and the filler of packed tower includes metal gauze ripple
One or more of filler BX, corrugated wire gauze packing CY and metal mellapak packing.
Further, taking off light purifying column and de- repurified tower is 316L stainless steel, tower top operating pressure is 0.2～
0.5MPa.
Further, high purity silicon tetrachloride is polycrystalline silicon reduction exhaust and hydrogenates four chlorinations obtaining after condensation material purifies
Silicon.
Further, photochemical reactor is the microchannel reaction unit of quartz material, a diameter of micron order of reaction channel,
Reaction temperature is 20～60 DEG C, reaction pressure 0.3～1MPa.
Application technical scheme, the method being combined using Light chlorimation and rectification and purification, wherein hydrogen containing foreign are led to
Cross optical chlorinating reaction and generate high boiling chloride, then again chloride is effectively removed by rectification, carry thus reaching and separating
Pure effect.Using the optical fiber Silicon chloride. of the method preparation, up to more than 99.9999999%, related group is infrared for its purity
Meet through index and be even more than Merk company high purity silicon tetrachloride index, reached ultra-pure Silicon chloride. prescription.
Brief description
The Figure of description constituting the part of the application is used for providing a further understanding of the present invention, and the present invention shows
Meaning property embodiment and its illustrate for explaining the present invention, does not constitute inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 shows the schematic flow sheet of according to embodiments of the present invention 1 preparation method of ultra-pure Silicon chloride..
Specific embodiment
It should be noted that in the case of not conflicting, the embodiment in the application and the feature in embodiment can phases
Mutually combine.To describe the present invention below with reference to the accompanying drawings and in conjunction with the embodiments in detail.
According to a kind of typical embodiment of the present invention, provide a kind of preparation method of ultra-pure Silicon chloride..The method
Comprise the following steps：S1, high purity silicon tetrachloride is continuously passed through in photochemical reactor under nitrogen effect；S2, in ultraviolet light
According under the conditions of, continuously into photochemical reactor, be passed through chlorine, make hydrogen containing foreign in high purity silicon tetrachloride, with chlorine, light occur
Chlorination reaction, obtains primary product；S3, primary product is passed through in stripper from the top of stripper, nitrogen is from stripper
Bottom is passed through, and obtains secondary products to remove unreacted chlorine in primary product；And S4, secondary products is sent into four chlorinations
Silicon purifying column, after continuously taking off light and de- weight, obtains ultra-pure Silicon chloride..
The present invention prepares ultra-pure Silicon chloride. by way of Light chlorimation and rectification and purification combine.
Photochemically reactive principle is：Cl2Under ultraviolet light irradiates, it is dissociated into two active chlorine radicals：
Cl2→2Cl·(1)
The chlorine radical of photodissociation can make hydrogen containing foreign that dehydrochlorination reaction, process such as following formula (2), (3) occur：
(CH3)3SiCl+2Cl·+2e-→C3H8ClSiCl+HCl (2)
(CH3)3BCl2+2Cl·+2e-→C3H8ClBCl2+HCl (3)
Reacted chloride boiling point is far above Silicon chloride., can be removed by the method for rectification and purification.
Application technical scheme, the method being combined using Light chlorimation and rectification and purification, wherein hydrogen containing foreign are led to
Cross optical chlorinating reaction and generate high boiling chloride, then again chloride is effectively removed by rectification, carry thus reaching and separating
Pure effect.Using the optical fiber Silicon chloride. of the method preparation, its purity is up to more than 9N (99.9999999%), related group
Infrared transmission index meets even more than Merk company high purity silicon tetrachloride index, and having reached ultra-pure Silicon chloride. quality will
Ask.
Preferably, in S1 and S3, the dew point of nitrogen is not less than -90 DEG C, and now the oxygen content in nitrogen and water content are
Ppb rank, will not impact to Silicon chloride. product quality.
Preferably, in S2, the purity of chlorine is not less than 99.999%.
According to a kind of typical embodiment of the present invention, in S2, chlorine is 1～10 with the volume ratio of high purity silicon tetrachloride:
1, thus can ensure that the raw material in Silicon chloride. is fully contacted with chlorine.
According to a kind of typical embodiment of the present invention, in S3, the temperature of nitrogen is 120～200 DEG C, and nitrogen is produced with primary
The volume ratio of product is 1～10:1, thus can be significantly separated unreacted chlorine.
Preferably, Silicon chloride. purifying column is made up of de- light purifying column and de- repurified tower, wherein, takes off returning of light purifying column
Flow ratio is 100～200, and the reflux ratio of de- repurified tower is 10～20.Suitable reflux ratio both can ensure that product Silicon chloride.
Purity, and do not affect the disposal ability of purifying column.In other words, reflux ratio is too small, and gas-liquid mass transfer is not good, and Silicon chloride. purity reaches
Less than production requirement；Reflux ratio is excessive, and purifying column production capacity reduces, and then increases energy consumption.
According to a kind of typical embodiment of the present invention, taking off light purifying column and de- repurified tower is packed tower, and filler includes
One or more of corrugated wire gauze packing BX, corrugated wire gauze packing CY and metal mellapak packing.
Preferably, taking off light purifying column and de- repurified tower is 316L stainless steel, tower top operating pressure is 0.2～
0.5MPa, is thus remarkably improved the efficiency of purifying column.
According to a kind of typical embodiment of the present invention, high purity silicon tetrachloride is polycrystalline silicon reduction exhaust and hydrogenation condensation material
The Silicon chloride. obtaining after purification.
Preferably, photochemical reactor is the microchannel reaction unit of quartz material, a diameter of micron order of reaction channel, instead
Temperature is answered to be 20～60 DEG C, reaction pressure 0.3～1MPa, thus can dramatically speed up response speed.
Further illustrate beneficial effects of the present invention below in conjunction with embodiment.
Embodiment 1
As shown in figure 1, ultra-pure Silicon chloride. production technology of the present embodiment comprises the following steps：
S1, purity more than 99.9999% is high purity silicon tetrachloride raw material, and it contains micro trichlorosilane, methyl chloride silicon
Raw material Silicon chloride. is sent in photochemical reaction device using high pure nitrogen, described high pure nitrogen by the impurity such as alkane and boron phosphorus
Dew point be not less than -90 DEG C.
S2, high purity silicon tetrachloride raw material is sent into after photochemical reaction device, under ultraviolet irradiation condition, a certain amount of high
Pure chlorine is passed through in photochemical reactor.The method is first passed through liquid material high purity silicon tetrachloride, then it is high-purity to be passed through gas material
Chlorine.Wherein, photochemical reactor is made up of micro passage reaction, ultraviolet source and heat transmission equipment, raw material high purity silicon tetrachloride
Flow in microchannel reaction unit inner laminar flow with high-purity chlorine, outside the reaction unit of microchannel, be equipped with ultraviolet source, raw material tetrachloro
Trichlorosilane in SiClx and hydrogen containing foreign are reacted with high-purity chlorine and heat release, in reaction unit under ultraviolet light
Temperature remain constant by heat transmission equipment.
S3, the primary product of photochemical reactor outlet enter from the top of stripper, the High Purity Nitrogen of a certain amount of and temperature
Gas is passed through from stripper bottom, and in photochemical reactor exported product, unreacted chlorine is laggard by high pure nitrogen stripper to be gone out
Enter exhaust treatment system to be processed.
S4, the secondary products without chlorine is discharged from stripper bottom, enters Silicon chloride. purifying column.Silicon chloride. purifies
Tower is made up of double tower, reactor product through Silicon chloride. purifying column continuously take off frivolous heavy after, chloride and boron and phosphorus matter are from high low boiling
Middle discharge, the Silicon chloride. purity after purification, up to more than 9N, meets ultra-pure Silicon chloride. prescription.
The actual conditions of the present embodiment is as follows：
Using the ultra-pure Silicon chloride. production technology according to the present invention, carried out ultra-pure using flow chart as shown in Figure 1
The production of Silicon chloride..
Raw material Silicon chloride. purity more than 99.9999%, polycrystalline silicon reduction exhaust and hydrogenation condensation material purification after
Silicon chloride. all can meet requirement.The dew point temperature of high pure nitrogen is not less than -90 DEG C, and the purity of high-purity chlorine is not less than
99.999%.
Photochemical reactor is quartz material microchannel reaction unit, a diameter of micron order of reaction channel, and reaction temperature is
30 DEG C, reaction pressure 0.4MPa, the volume ratio of high-purity chlorine and raw material Silicon chloride. is 10:1, light source can adopt high pressure ultraviolet mercury
Lamp or cold light source uviol lamp.Heat transferring medium is conduction oil, for cooling down photochemical reaction device, maintains the reaction temperature in reactor
Degree.
Contain unreacted chlorine in photochemical reactor product, need to be taken out of with high pure nitrogen after stripper.High-purity
120 DEG C of nitrogen temperature, the volume ratio with reactor product is 10:1.
Product without chlorine is passed through Silicon chloride. purifying column, and Silicon chloride. purifying column is 316L material, tower internal and
The equal electropolishing of tower internals is processed, and tower top operating pressure is 0.2MPa, and tower top employing under this operating pressure can adopt circulating water,
Tower reactor can adopt hot water heating.Described purifying column is made up of double tower, continuously discharges low-boiling-point substance and height by lightness-removing column and weight-removing column
After boiling thing, product purity can reach more than 9N.
Stripper and Silicon chloride. purifying column can adopt plate column or packed tower, preferred filler tower.Filler includes but does not limit
In one or more of corrugated wire gauze packing BX, corrugated wire gauze packing CY and metal mellapak packing.Ultra-pure
The reflux ratio that Silicon chloride. takes off light purifying column is 100, and the reflux ratio of de- repurified tower is 10.
Product after purification need to enter ultra-pure Silicon chloride. and carry out storage tank, and storage tank is 316L material, at internal electropolishing
Reason.Products pot is filled or the free time treats the used time, need to be protected to 0.1～0.2MPa with high pure nitrogen punching press.
After such stable operation 15 days, product in product storage tank is sampled analyze.
Analysis method：Analyze the infrared transmittivity of hydrogen containing foreign group using Fourier's radar stealthy materials, analysis result is shown in Table 1.
Can obtain after the standard of analysis result and German Merck company is contrasted, in storage tank, product can meet ultra-pure grade of SiCl4Matter
Amount requires.
Table 1
| Wave number (cm-1) | Group | Merck company standard (%) | Embodiment 1 (%) |
| 3666 | SiCl3OH | ＞ 90 | 99.54 |
| 3100～3020 | -CH | ＞ 99 | 99.91 |
| 2970～2925 | -CH | ＞ 95 | 99.86 |
| 2860～2830 | HCl | ＞ 95 | 99.93 |
| 2338 | CO2 | ＞ 95 | ＞ 99 |
| 2295 | Si(NCO)4 | ＞ 97 | ＞ 99.02 |
| 2257 | SiHCl3 | ＞ 99 | ＞ 99 |
| 2023 | Si(CH3)Cl3 | ＞ 99 | ＞ 99 |
| 1540 | Si2OCl6 | ＞ 99 | ＞ 99 |
Embodiment 2
, with embodiment 1, actual conditions is as follows for processing step：
Raw material Silicon chloride. purity more than 99.9999%, polycrystalline silicon reduction exhaust and hydrogenation condensation material purification after
Silicon chloride. all can meet requirement.The dew point temperature of high pure nitrogen is not less than -90 DEG C, and the purity of high-purity chlorine is not less than
99.999%.
Photochemical reactor is quartz material microchannel reaction unit, a diameter of micron order of reaction channel, and reaction temperature is
20 DEG C, reaction pressure 0.3MPa, the volume ratio of high-purity chlorine and raw material Silicon chloride. is 1:1, light source can adopt high pressure ultraviolet mercury
Lamp or cold light source uviol lamp.Heat transferring medium is conduction oil, for cooling down photochemical reaction device, maintains the reaction temperature in reactor
Degree.
Contain unreacted chlorine in photochemical reactor product, need to be taken out of with high pure nitrogen after stripper.High-purity
120 DEG C of nitrogen temperature, the volume ratio with reactor product is 1:1.
Product without chlorine is passed through Silicon chloride. purifying column, and Silicon chloride. purifying column is 316L material, tower internal and
The equal electropolishing of tower internals is processed, and tower top operating pressure is 0.2MPa, and tower top employing under this operating pressure can adopt circulating water,
Tower reactor can adopt hot water heating.Described purifying column is made up of double tower, continuously discharges low-boiling-point substance and height by lightness-removing column and weight-removing column
After boiling thing, product purity can reach more than 9N.
Stripper and Silicon chloride. purifying column can adopt packed tower, and filler includes but is not limited to corrugated wire gauze packing
One or more of BX, corrugated wire gauze packing CY and metal mellapak packing.Ultra-pure Silicon chloride. takes off light purifying column
Reflux ratio be 100, the reflux ratio of de- repurified tower is 10.
Product after purification need to enter ultra-pure Silicon chloride. and carry out storage tank, and storage tank is 316L material, at internal electropolishing
Reason.Products pot is filled or the free time treats the used time, need to be protected to 0.1～0.2MPa with high pure nitrogen punching press.
After such stable operation 15 days, product in product storage tank is sampled analyze.
Analysis method：Analyze the infrared transmittivity of hydrogen containing foreign group using Fourier's radar stealthy materials, analysis result is shown in Table 2.
Can obtain after the standard of analysis result and German Merck company is contrasted, in storage tank, product can meet ultra-pure grade of SiCl4Matter
Amount requires.
Table 2
| Wave number (cm-1) | Group | Merck company standard (%) | Embodiment 2 (%) |
| 3666 | SiCl3OH | ＞ 90 | 99.68 |
| 3100～3020 | -CH | ＞ 99 | 99.59 |
| 2970～2925 | -CH | ＞ 95 | 97.71 |
| 2860～2830 | HCl | ＞ 95 | 97.91 |
| 2338 | CO2 | ＞ 95 | 96.86 |
| 2295 | Si(NCO)4 | ＞ 97 | ＞ 99 |
| 2257 | SiHCl3 | ＞ 99 | ＞ 99 |
| 2023 | Si(CH3)Cl3 | ＞ 99 | ＞ 99 |
| 1540 | Si2OCl6 | ＞ 99 | ＞ 99 |
Embodiment 3
, with embodiment 1, actual conditions is as follows for processing step：
Raw material Silicon chloride. purity more than 99.9999%, polycrystalline silicon reduction exhaust and hydrogenation condensation material purification after
Silicon chloride. all can meet requirement.The dew point temperature of high pure nitrogen is not less than -90 DEG C, and the purity of high-purity chlorine is not less than
99.999%.
Photochemical reactor is quartz material microchannel reaction unit, a diameter of micron order of reaction channel, and reaction temperature is
60 DEG C, reaction pressure 1MPa, the volume ratio of high-purity chlorine and raw material Silicon chloride. is 10:1, light source can adopt high-voltage ultraviolet mercury lamp
Or cold light source uviol lamp.Heat transferring medium is conduction oil, for cooling down photochemical reaction device, maintains the reaction temperature in reactor
Degree.
Contain unreacted chlorine in photochemical reactor product, need to be taken out of with high pure nitrogen after stripper.High-purity
200 DEG C of nitrogen temperature, the volume ratio with reactor product is 10:1.
Product without chlorine is passed through Silicon chloride. purifying column, and Silicon chloride. purifying column is 316L material, tower internal and
The equal electropolishing of tower internals is processed, and tower top operating pressure is 0.5MPa, and tower top employing under this operating pressure can adopt circulating water,
Tower reactor can adopt hot water heating.Described purifying column is made up of double tower, continuously discharges low-boiling-point substance and height by lightness-removing column and weight-removing column
After boiling thing, product purity can reach more than 9N.
Stripper and Silicon chloride. purifying column can adopt packed tower, and filler includes but is not limited to corrugated wire gauze packing
One or more of BX, corrugated wire gauze packing CY and metal mellapak packing.Ultra-pure Silicon chloride. takes off light purifying column
Reflux ratio be 200, the reflux ratio of de- repurified tower is 20.
Product after purification need to enter ultra-pure Silicon chloride. and carry out storage tank, and storage tank is 316L material, at internal electropolishing
Reason.Products pot is filled or the free time treats the used time, need to be protected to 0.1～0.2MPa with high pure nitrogen punching press.
After such stable operation 15 days, product in product storage tank is sampled analyze.
Analysis method：Analyze the infrared transmittivity of hydrogen containing foreign group using Fourier's radar stealthy materials, analysis result is shown in Table 3.
Can obtain after the standard of analysis result and German Merck company is contrasted, in storage tank, product can meet ultra-pure grade of SiCl4Matter
Amount requires.
Table 3
As can be seen from the above description, the above embodiments of the present invention achieve following technique effect：
1) ultra-pure Silicon chloride. prescription can be met according to the Silicon chloride. of embodiment preparation.
2) the method range of application that the present invention provides is more broad, can get qualified products under the conditions of low-temp low-pressure.
3) in above-described embodiment, the product quality of embodiment 1 is optimum, illustrates that the method has optimum technological parameter.
According to ultra-pure Silicon chloride. production technology of the present embodiment have output Silicon chloride. purity is high and energy consumption is low,
The advantages of emission-free pollution.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of ultra-pure Silicon chloride. is it is characterised in that comprise the following steps：
S1, high purity silicon tetrachloride is continuously passed through in photochemical reactor under nitrogen effect；
S2, under ultraviolet irradiation condition, is continuously passed through chlorine into described photochemical reactor, makes in described high purity silicon tetrachloride
Hydrogen containing foreign and chlorine there is optical chlorinating reaction, obtain primary product；
S3, described primary product are passed through in described stripper from the top of stripper, and nitrogen leads to from the bottom of described stripper
Enter, obtain secondary products to remove unreacted chlorine in described primary product；And
S4, described secondary products is sent into Silicon chloride. purifying column, after continuously taking off light and de- weight, obtains described ultra-pure four
Silicon chloride.
2. preparation method according to claim 1 is not it is characterised in that in described S1 and S3, the dew point of described nitrogen is low
In -90 DEG C.
3. preparation method according to claim 1 is it is characterised in that in described S2, the purity of described chlorine is not less than
99.999%.
4. preparation method according to claim 1 is it is characterised in that in described S2, described chlorine and described high-purity tetrachloro
The volume ratio of SiClx is 1～10:1.
5. preparation method according to claim 1 is it is characterised in that in described S3, and the temperature of described nitrogen is 120～
200 DEG C, described nitrogen is 1～10 with the volume ratio of described primary product:1.
6. preparation method according to claim 1 it is characterised in that described Silicon chloride. purifying column by de- light purifying column and
De- repurified tower composition, wherein, the described reflux ratio taking off light purifying column is 100～200, and the reflux ratio of described de- repurified tower is
10～20.
7. preparation method according to claim 6 is it is characterised in that described de- light purifying column and described de- repurified tower are
Packed tower, the filler of described filler tower includes corrugated wire gauze packing BX, corrugated wire gauze packing CY and metallic plate ripple
One or more of filler.
8. preparation method according to claim 6 is it is characterised in that described de- light purifying column and described de- repurified tower are
316L stainless steel, tower top operating pressure is 0.2～0.5MPa.
9. preparation method according to claim 1 is it is characterised in that described high purity silicon tetrachloride is polycrystalline silicon reduction exhaust
And the Silicon chloride. obtaining after hydrogenation condensation material purification.
10. preparation method according to claim 1 is it is characterised in that described photochemical reactor is the micro- of quartz material
Pathway reaction device, a diameter of micron order of reaction channel, reaction temperature is 20～60 DEG C, reaction pressure 0.3～1MPa.
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Cited By (6)
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|---|---|---|---|---|
| CN107055552A (en) * | 2017-06-27 | 2017-08-18 | 亚洲硅业（青海）有限公司 | A kind of purification method of silicon tetrachloride and application |
| CN108946743A (en) * | 2018-09-28 | 2018-12-07 | 洛阳中硅高科技有限公司 | The method for purifying trichlorosilane |
| CN109179425A (en) * | 2018-09-28 | 2019-01-11 | 洛阳中硅高科技有限公司 | Purify the device of trichlorosilane |
| CN109678161A (en) * | 2019-01-24 | 2019-04-26 | 唐山三孚硅业股份有限公司 | Produce the processing method of the raw material of optical fiber grade silicon tetrachloride |
| CN110357150A (en) * | 2019-08-08 | 2019-10-22 | 中国恩菲工程技术有限公司 | Titanium tetrachloride rectificating method |
| CN114247180A (en) * | 2021-12-24 | 2022-03-29 | 亚洲硅业(青海)股份有限公司 | Application of active carbon containing oxygen groups in removal of impurities in silicon tetrachloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107055552B (en) * | 2017-06-27 | 2018-08-07 | 亚洲硅业（青海）有限公司 | A kind of purification method of silicon tetrachloride and application |
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| CN109179425A (en) * | 2018-09-28 | 2019-01-11 | 洛阳中硅高科技有限公司 | Purify the device of trichlorosilane |
| CN109678161A (en) * | 2019-01-24 | 2019-04-26 | 唐山三孚硅业股份有限公司 | Produce the processing method of the raw material of optical fiber grade silicon tetrachloride |
| CN110357150A (en) * | 2019-08-08 | 2019-10-22 | 中国恩菲工程技术有限公司 | Titanium tetrachloride rectificating method |
| CN114247180A (en) * | 2021-12-24 | 2022-03-29 | 亚洲硅业(青海)股份有限公司 | Application of active carbon containing oxygen groups in removal of impurities in silicon tetrachloride |
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