CN207596482U - A kind of rectifying device for purifying trichlorosilane - Google Patents
A kind of rectifying device for purifying trichlorosilane Download PDFInfo
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- CN207596482U CN207596482U CN201721572269.2U CN201721572269U CN207596482U CN 207596482 U CN207596482 U CN 207596482U CN 201721572269 U CN201721572269 U CN 201721572269U CN 207596482 U CN207596482 U CN 207596482U
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Abstract
The utility model discloses a kind of rectifying device for purifying trichlorosilane, including pre-tower, first rectifying column, Second distillation column and third distillation column；The tower top of pre-tower is equipped with pre-tower condenser, and the condensate outlet of pre-tower condenser is connect with the feed inlet of pre-tower return tank, and the discharge port of pre-tower return tank and the refluxing opening of pre-tower connect；The bottom of towe discharge port of pre-tower is equipped with pre- tower reboiler, and pre- tower reboiler is sequentially connected trichlorosilane feed well, trichlorosilane feed pump；The trichlorosilane feed pump and the feed inlet of first rectifying column connect, and the top of first rectifying column is equipped with rectifying column condenser one, and the condensate outlet of rectifying column condenser one and the feed inlet of Second distillation column connect；The bottom of towe discharge port of Second distillation column is equipped with rectifying tower reboiler, the feed inlet connection of rectifying tower reboiler and third distillation column, and the tower top of third distillation column is equipped with rectifying column condenser.The utility model realizes the technique effect for reducing impurities in trichlorosilane.
Description
Technical field
The utility model belongs to chemical technology field, is related to a kind of rectifying device, and in particular to a kind of purification trichlorosilane
Rectifying device.
Background technology
Trichlorosilane is also known as silicochloroform, silicon is imitated or trichlorosilane, English name：Trichlorosilane or
Silicochloroform, molecular formula SiHCl3, belong to polar substances, for the synthesis of organosilan, while be also to produce
The primary raw material of polysilicon.
With the development of the industries such as electronic device, integrated circuit, solar energy, the production scale of polysilicon constantly expands, work
Requirement of the industry production to its purity is also higher and higher.At present, most of polysilicon is obtained by hydrogen reducing trichlorosilane,
And industrial trichlorosilane typically contains 20 plurality of impurities, these impurity influence whether the purity of polysilicon.Therefore, it is right
Trichlorosilane is purified, and removal impurity is conducive to produce the polysilicon of high quality.
The method of a variety of purification trichlorosilanes is had been disclosed in the prior art.At present, common purification trichlorosilane
Method is multitower rectification method, i.e., the plurality of impurities in trichlorosilane is divided step by step using up to ten grades or more of rectifying column
From.Above-mentioned multitower rectification method can only successively be detached according to the height of impurity content, although can achieve the effect that purification, just
Secondary cost of investment is big, and production cost is high, and high energy consumption.
The prior art also discloses that the method purified using less rectifying column to trichlorosilane.Chinese patent literature
CN101249312A discloses a kind of separator and method of high precision rectification purification trichlorosilane, using double packed tower conducts
Separation equipment detaches low-boiling compound and higher-boiling compound by pressurized with hydrogen, finally reaches purity of trichlorosilane respectively
More than 99.999%, boron, phosphorus content can be down to 10ppb.But this method is higher to equipment requirement, and the boron of 10ppb, phosphorus
Content cannot still meet the requirement of electronic-grade polycrystalline silicon.
Utility model content
The purpose of this utility model is to provide a kind of rectifying device for purifying trichlorosilane, although miscellaneous in trichlorosilane
Matter type is more, but be most difficult to remove critical impurities mainly include two parts, a part is boron-containing compound, as boron chloride,
Diborane etc., another part are phosphorus-containing compounds, such as phosphorus trichloride, phosphorus pentachloride, since boron-containing compound is for trichlorine hydrogen
The relative volatility of silicon approaches, therefore considers to be divided impurity according to the volatility of the boron-containing compound and phosphorus-containing compound
Class, and rectifying column is designed to purify trichlorosilane according to the volatility of the boron-containing compound and phosphorus-containing compound, to realize
Reduce trichlorosilane in boron impurities, phosphorus content technique effect.
To achieve the above object, the utility model provides following technical solution：
A kind of rectifying device for purifying trichlorosilane, including pre-tower, first rectifying column, Second distillation column and third rectifying
Tower；
The feed inlet of pre-tower is connect with pre-tower feed pump；The tower top of pre-tower be equipped with pre-tower condenser, pre-tower condenser it is cold
Condensate outlet is connect with the feed inlet of pre-tower return tank, and the discharge port of pre-tower return tank and the refluxing opening of pre-tower connect；Pre-tower
Bottom of towe discharge port is equipped with pre- tower reboiler, and pre- tower reboiler is sequentially connected trichlorosilane feed well, trichlorosilane feed pump；
The trichlorosilane feed pump and the feed inlet of first rectifying column connect, the bottom of towe discharge port connection of first rectifying column
There is holding vessel one；The top of first rectifying column is equipped with rectifying column condenser one, the condensate outlet of rectifying column condenser one and the
The feed inlet connection of two rectifying columns；The tower top of Second distillation column is equipped with rectifying column condenser two, the condensation of rectifying column condenser two
Liquid outlet is connected to holding vessel two, and the bottom of towe discharge port of Second distillation column is equipped with rectifying tower reboiler, rectifying tower reboiler and the
The feed inlet connection of three rectifying columns, the tower top of third distillation column are equipped with rectifying column condenser two, and the bottom of towe of third distillation column discharges
Mouth is connect with trichlorosilane holding vessel.
The pre-tower is guide sieve-plate tower, and the number of plates is 24 pieces.
The first rectifying column is guide sieve-plate tower, and the number of plates is 40 pieces.
The Second distillation column is guide sieve-plate tower, and the number of plates is 40 pieces.
The third distillation column is guide sieve-plate tower, and the number of plates is 40 pieces.
Compared with prior art, the beneficial effects of the utility model are：
1st, the utility model divides impurity with the volatility of opposite trichlorosilane, selects two kinds of critical impurities：Containing boronation
Object and phosphorus-containing compound are closed, three-level rectifying then is designed to the relative volatility of trichlorosilane according to described two critical impurities,
In first rectifying column, major part can be removed containing phosphorus impurities and be more difficult to the substance to volatilize；It is removed in second rectifying column big
Part boron-containing impurities and more volatile substance, then continue rectifying with higher reflux ratio in third rectifying column, so as to
Achieve the purpose that reduce boron impurities in trichlorosilane.Or due to other impurities volatility close to boron-containing compound volatilization
Degree or the volatility close to phosphorus-containing compound, so other impurities can also be realized in above-mentioned rectifying column and trichlorosilane
Separation.
2nd, the utility model uses three rectifying columns, can reduce production cost, reduces ability consumption, avoids secondary dirt
Dye.
3rd, the utility model employs high-efficiency guide sieve-plate tower, and a large amount of sieve pores have been opened up on the tower column plate and small part is oriented to
Hole, by the gas of sieve pore on column plate with liquid cross-flow, across liquid layer vertical ascent, by the gas of linde sieve tray, along tower
Plate level advances, and momentum is passed to the liquid of bottom horizontal flow sheet on column plate, so as to push liquid uniform and stable advance on column plate,
The liquid level drop and backmixing of liquid phase on original column plate are overcome, improves production capacity and plate efficiency, solves stifled tower, liquid flooding etc.
Problem.
Description of the drawings
Fig. 1 is a kind of structure diagram for the rectifying device for purifying trichlorosilane of the utility model；
It is indicated in figure：1- pre-tower feed pumps, 2- pre-towers, 3- pre-tower condensers, 4- pre-tower return tanks, the pre- tower reboilers of 5-,
6- trichlorosilane feed wells, 7- trichlorosilane feed pumps, 8- first rectifying columns, 9- holding vessels one, 10- rectifying columns condenser one,
11- Second distillation columns, 12- rectifying tower reboilers, 13- rectifying columns condenser two, 14- holding vessels two, 15- third distillation columns, 16-
Trichlorosilane holding vessel.
Specific embodiment
A kind of rectifying device for purifying trichlorosilane, referring to Fig. 1, including pre-tower 2, first rectifying column 8, Second distillation column 11
With third distillation column 15；
The pre-tower 2 is guide sieve-plate tower, and the number of plates is 24 pieces；The feed inlet of pre-tower 2 is connect with pre-tower feed pump 1；In advance
The tower top of tower 2 is equipped with pre-tower condenser 3, and the condensate outlet of pre-tower condenser 3 is connect with the feed inlet of pre-tower return tank 4, in advance
The discharge port of tower return tank 4 is connect with the refluxing opening of pre-tower 2；The bottom of towe discharge port of pre-tower 2 is equipped with pre- tower reboiler 5, and pre-tower is again
Boiling device 5 is sequentially connected trichlorosilane feed well 6, trichlorosilane feed pump 7；
The trichlorosilane feed pump 7 is connect with the feed inlet of first rectifying column 8, the bottom of towe discharge port of first rectifying column 8
It is connected with holding vessel 1；The top of first rectifying column 8 is equipped with rectifying column condenser 1, the condensation of rectifying column condenser 1
Liquid outlet is connect with the feed inlet of Second distillation column 11；The tower top of Second distillation column 11 is equipped with rectifying column condenser 2 13, rectifying
The condensate outlet of tower condenser 2 13 is connected to holding vessel 2 14, and the bottom of towe discharge port of Second distillation column 11 is equipped with rectifying column again
Device 12 is boiled, rectifying tower reboiler 12 is connect with the feed inlet of third distillation column 15, and the tower top of third distillation column 15 is equipped with rectifying column
Condenser 2 13, the bottom of towe discharge port of third distillation column 15 are connect with trichlorosilane holding vessel 16；
The first rectifying column 8 be guide sieve-plate tower, the number of plates be 40 pieces, Second distillation column 11 be guide sieve-plate tower, tower
Plate number is 40 pieces, and third distillation column 15 is guide sieve-plate tower, and the number of plates is 40 pieces；
The operation principle of the utility model is as follows：
The thick Synthesis liquid of trichlorosilane a concentration of 85% or so sent from synthesizing section is thrown into pre- by pre-tower feed pump 1
2 upper feed inlet of tower, the pre-tower 2 are guide sieve-plate tower, and the number of plates is 24 pieces, and tower top pressure is 65KPa, and tower top temperature is
45 DEG C, reflux ratio 0.15-0.2,2 lower part reboiler 5 of pre-tower uses 500Kpa saturated vapor indirectly heat liquid crude trichlorine hydrogen
Silicon, 2 tower top of pre-tower are equipped with pre-tower condenser 3, and it is 5 DEG C that 3 tube side of pre-tower condenser, which is passed through temperature, and pressure is the freezing salt of 450Kpa
Water, from the liquid that pre-tower condenser 3 condenses out into pre-tower return tank 4, using the potential difference of pre-tower return tank 4, liquid enters pre-
Dichloro-dihydro is entered by pipeline under 2 overhead condensation of pre-tower as phegma, low-boiling dichlorosilane in 2 tower of tower
Silicon product storage tank；
Through pre-tower 2 except the liquid after dichlorosilane passes sequentially through trichlorosilane tower feed well 6, trichlorosilane tower in bottom of towe
Feed pump 7 enters 8 middle part feed inlet of first rectifying column, and first rectifying column 8 carries out rectifying, separation first part impurity, mainly into
It is divided into phosphorus-containing compound, trichlorosilane is 1.6-2.5 for the relative volatility of first part's impurity；The operation of first rectifying column
Condition is：Operating pressure P1 is 0.25MPa, and tower top temperature is 70 DEG C, and column bottom temperature is 110 DEG C, reflux ratio 8；
Material liquid containing trichlorosilane enters first rectifying column 8, upflowing vapor in tower from bottom to top, it is contained therein
Heavy constituent, such as silicon tetrachloride, phosphorus-containing compound step by step tray are transmitted to liquid phase；And phegma in tower from top to bottom, it is therein light
Component, such as trichlorosilane, boron-containing compound step by step tray are transmitted to gas phase.By the mass exchange, trichlorine hydrogen is obtained in tower top
The volatile substance such as silicon, boron-containing compound discharges first part's impurity of more difficult volatilization in bottom of towe, realizes first step separation；
Rectifying column condenser 1 is equipped in 8 tower top of first rectifying column, it is 5 that one 10 tube side of rectifying column condenser, which is passed through temperature,
~7 DEG C, pressure is the chilled brine of 400~500Kpa, and the liquid of the condensate outlet of rectifying column condenser 1 utilizes potential difference
Into Second distillation column 11, second part impurity is detached from 11 overhead fraction of Second distillation column, main component is boracic chemical combination
Object, second part impurity are 1.4-1.7 for the relative volatility of trichlorosilane；The operating condition of Second distillation column 11 is：Behaviour
Make pressure P2 as 0.20MPa, column bottom temperature is 80 DEG C, reflux ratio 6000；
Material liquid containing trichlorosilane enters Second distillation column 11, upflowing vapor in tower from bottom to top, it is contained therein
Heavy constituent (mainly trichlorosilane) step by step tray transmitted to liquid phase, and phegma in tower from top to bottom, light component therein, such as
The steps by step tray such as boron-containing compound are transmitted to gas phase, by the mass exchange, in volatile objects such as tower top discharge boron-containing compounds
Matter obtains the higher trichlorosilane of purity in bottom of towe；
The tower bottom distillate of Second distillation column 11 enters third distillation column 15, and the effect of third distillation column 15 is further to detach
Second part impurity in Second distillation column tower bottom distillate.Increase the reflux ratio of rectifying column in favor of improving overhead fraction and bottom of towe
The purity of fraction can make separation more thorough.Therefore, it is proposed, according to the invention, the reflux ratio of the third distillation column is higher than described
The reflux ratio of Second distillation column, the reflux ratio of third distillation column is 8000, the operation item of other operating conditions and Second distillation column
Part is identical；
In third distillation column 15, contained heavy constituent, mainly trichlorosilane in upflowing vapor are transmitted to liquid phase, and
Light component in dropping liq is transmitted to gas phase；Meanwhile exchanged by above-mentioned substance, obtain boron-containing compound and ratio in tower top
The light components such as the more volatile impurity of boron-containing compound, can be handled according to method well-known to those skilled in the art,
It utilizes, the present invention is not particularly limited；The trichlorosilane of high-purity is obtained in bottom of towe.After third distillation column, trichlorosilane
Middle boracic, phosphorus amount are down to 0.01ppba, 0.1ppba respectively.
The relative volatility refers to the ratio between volatility of two components in mixed liquor.
Claims (5)
1. a kind of rectifying device for purifying trichlorosilane, it is characterised in that：Including pre-tower (2), first rectifying column (8), the second essence
Evaporate tower (11) and third distillation column (15)；
The feed inlet of pre-tower (2) is connect with pre-tower feed pump (1)；The tower top of pre-tower (2) is equipped with pre-tower condenser (3), and pre-tower is cold
The condensate outlet of condenser (3) is connect with the feed inlet of pre-tower return tank (4), discharge port and the pre-tower (2) of pre-tower return tank (4)
Refluxing opening connection；The bottom of towe discharge port of pre-tower (2) is equipped with pre- tower reboiler (5), and pre- tower reboiler (5) is sequentially connected trichlorine hydrogen
Silicon feed well (6), trichlorosilane feed pump (7)；
The trichlorosilane feed pump (7) connect with the feed inlet of first rectifying column (8), the bottom of towe discharging of first rectifying column (8)
Mouth is connected with holding vessel one (9)；The top of first rectifying column (8) is equipped with rectifying column condenser one (10), rectifying column condenser one
(10) condensate outlet is connect with the feed inlet of Second distillation column (11)；It is cold that the tower top of Second distillation column (11) is equipped with rectifying column
Condenser two (13), the condensate outlet of rectifying column condenser two (13) are connected to holding vessel two (14), Second distillation column (11)
Bottom of towe discharge port is equipped with rectifying tower reboiler (12), and rectifying tower reboiler (12) is connect with the feed inlet of third distillation column (15),
The tower top of third distillation column (15) is equipped with rectifying column condenser two (13), bottom of towe discharge port and the trichlorine hydrogen of third distillation column (15)
Silicon holding vessel (16) connects.
2. a kind of rectifying device for purifying trichlorosilane according to claim 1, it is characterised in that：The pre-tower (2) is
Guide sieve-plate tower, the number of plates are 24 pieces.
3. a kind of rectifying device for purifying trichlorosilane according to claim 1, it is characterised in that：The first rectifying column
(8) it is guide sieve-plate tower, the number of plates is 40 pieces.
4. a kind of rectifying device for purifying trichlorosilane according to claim 1, it is characterised in that：The Second distillation column
(11) it is guide sieve-plate tower, the number of plates is 40 pieces.
5. a kind of rectifying device for purifying trichlorosilane according to claim 1, it is characterised in that：The third distillation column
(15) it is guide sieve-plate tower, the number of plates is 40 pieces.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721572269.2U CN207596482U (en) | 2017-11-22 | 2017-11-22 | A kind of rectifying device for purifying trichlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721572269.2U CN207596482U (en) | 2017-11-22 | 2017-11-22 | A kind of rectifying device for purifying trichlorosilane |
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| Publication Number | Publication Date |
|---|---|
| CN207596482U true CN207596482U (en) | 2018-07-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201721572269.2U Active CN207596482U (en) | 2017-11-22 | 2017-11-22 | A kind of rectifying device for purifying trichlorosilane |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113144655A (en) * | 2021-04-28 | 2021-07-23 | 安徽金轩科技有限公司 | Jiale musk rectification unit and rectification process thereof |
| CN116407861A (en) * | 2023-03-16 | 2023-07-11 | 清电光伏科技有限公司 | Fixed bed-based electronic grade polysilicon rectification carbon removal device and method |
-
2017
- 2017-11-22 CN CN201721572269.2U patent/CN207596482U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113144655A (en) * | 2021-04-28 | 2021-07-23 | 安徽金轩科技有限公司 | Jiale musk rectification unit and rectification process thereof |
| CN116407861A (en) * | 2023-03-16 | 2023-07-11 | 清电光伏科技有限公司 | Fixed bed-based electronic grade polysilicon rectification carbon removal device and method |
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