CN104528735B - A kind of absorption purifying plant of purifying column output object - Google Patents
A kind of absorption purifying plant of purifying column output object Download PDFInfo
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- CN104528735B CN104528735B CN201510017547.7A CN201510017547A CN104528735B CN 104528735 B CN104528735 B CN 104528735B CN 201510017547 A CN201510017547 A CN 201510017547A CN 104528735 B CN104528735 B CN 104528735B
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Abstract
In order to overcome the problem of the effective scheme still being purified in prior art less than the silicon fluoride of output from purifying column and related impuritieses，The invention provides a kind of absorption purifying plant of purifying column output object，Described output object is the silicon fluoride and other impurities from purifying column，This absorption purifying plant includes lightness-removing column、Weight-removing column、Adsorption tower、Cooling tower、Knockout tower、Adsorption column and multiple rectifying column，It is connected by pipeline between each tower，Insert described output object to described lightness-removing column，The product of described lightness-removing column enters described adsorption tower，Described adsorption tower and weight-removing column are sequentially connected，And this weight-removing column is connected with rectifying column，This rectifying column is connected with adsorption column，Described adsorption column is connected with cooling tower，Described cooling tower is connected with knockout tower，Described knockout tower is connected with adsorption tower，Described adsorption tower is connected with another rectifying column，And described lightness-removing column and weight-removing column include catalytic combustion system and inorganic salt processing meanss respectively.Present invention saves cost, protect environment simultaneously.
Description
Technical field
The present invention relates to the purification technique field of compound, carry more particularly, to a kind of absorption of purifying column output object
Pure device.
Background technology
Polysilicon is the primary raw material manufacturing silicon polished, solaode and HIGH-PURITY SILICON product, is semi-conductor industry, electricity
Sub-information industry, main, the most basic functional material of solar-energy photo-voltaic cell industry.It is permissible that polysilicon presses purity classification
It is divided into metallurgical grade, solar level, electron level.The production method of high purity polycrystalline silicon has:Improved Siemens, silane thermal decomposition process, fluid bed
Method, metallurgy method.With large-scale developing and utilizing of green energy resource solar energy, the purposes of photovoltaic cell raw material polysilicon is more and more wider
General.The method producing polysilicon is the widest with Siemens Method, can produce during producing polysilicon raw material trichlorosilane
How substantial amounts of silicon tetrachloride as by-product, effectively utilize these by-products, be the key that polysilicon industry is capable of diverse development
Problem.
Production method with regard to Silicon fluoride. is it is known to many methods.
For example, the patent of Italian EniChem company describes a kind of H2SiF6 water making mass fraction 12%～20%
Solution is reacted in reactor with the concentrated sulphuric acid of mass fraction 96%～99% under 90～120 DEG C, 40～50kPa, Ran Houyong
The method of 96% cold sulfuric acid scrubbing is come the technique to produce Silicon fluoride..
But, in prior art, still had efficacious prescriptions less than what the silicon fluoride of output from purifying column and related impuritieses purified
Case.
Content of the invention
In order to overcome above-mentioned weak point of the prior art, the invention provides a kind of absorption of purifying column output object carries
Pure device, described output object is the silicon fluoride and other impurities from purifying column, and this absorption purifying plant includes lightness-removing column, de- weight
Tower, adsorption tower, cooling tower, knockout tower, adsorption column and multiple rectifying column, are connected by pipeline between each tower, take off to described
Described output object inserted by light tower, and the product of described lightness-removing column enters described adsorption tower, and described adsorption tower and weight-removing column are sequentially connected,
And this weight-removing column is connected with rectifying column, this rectifying column is connected with adsorption column, and described adsorption column is connected with cooling tower, described cooling tower
It is connected with knockout tower, described knockout tower is connected with adsorption tower, described adsorption tower is connected with another rectifying column, and described lightness-removing column
Include catalytic combustion system and inorganic salt processing meanss with weight-removing column respectively.
Further, the rectifying column being connected with described cooling tower is side line rectifying column.
Further, also include hydrolyzing rectifying column between described side line rectifying column and described adsorption column.
Further, also include dehydrating unit between described lightness-removing column and described adsorption tower.
Further, it is filled with one of activated alumina, silica gel, molecular sieve, activated carbon or many in described adsorption tower
Plant adsorbent.
Further, also include low temperature dewatering tower between described cooling tower and knockout tower.
Further, described adsorption tower is adsorbing tower with molecular sieve.
Further, described adsorption column is cryogenic absorption post.
Further, described inorganic salt processing meanss include packing groove, reactor and the precipitation inserting composition metal raw material
Thing recovery room.
The invention has the beneficial effects as follows：So that rectification and absorption is combined, save in prior art to production of polysilicon institute
Need high cost, simultaneously the garbage in output object obtained effective process, protect environment.
Brief description
Fig. 1 is the composition figure of the absorption purifying plant of purifying column output object according to a preferred embodiment of the invention.
Specific embodiment
For further appreciate that the present invention, with reference to embodiment, above-mentioned technical scheme being further elaborated and saying
Bright.
The absorption purifying plant of purifying column output object, described output object is the silicon fluoride and other impurities from purifying column.
These impurity include nitrogen, oxygen, carbon monoxide, carbon dioxide, nitrous oxide, difluoro hydrazine, tetrafluorohydrazine, carbon tetrafluoride, hexafluoro
Change sulfur, Silicon fluoride., fluorine gas, fluohydric acid gas, water etc..
Silicon fluoride and above-mentioned other impurities are passed through lightness-removing column, removing nitrogen, oxygen, carbon dioxide at -150 DEG C, one
Carbonoxide, the operating pressure of lightness-removing column is 0.1MPa；The bottom liquid phases material of lightness-removing column is passed through weight-removing column, in -20 DEG C of temperature
Under degree, moisture and fluohydric acid gas are removed from bottom of towe, silicon tetrafluoride gas are discharged by tower top, the product of this discharge enters catalysis combustion
Burn device and adsorption tower.Catalytic combustion system carries out catalysis burning to fuel gas, generates non-combustible gas, subsequently into absorption
One or more of the activated alumina of filling, silica gel, molecular sieve, activated carbon adsorbent, preferably molecular sieve adsorption in tower
Various remaining air-polluting gases are adsorbed by tower.
Subsequently, product enters weight-removing column.The operating pressure of weight-removing column is 0.5MPa.Described weight-removing column includes iron salt and processes dress
Put.This iron salt processing means makes the iron ion of the waste and ionization discharged by weight-removing column carry out exchanging and in soda acid ring between matter
Carry out reaction under border to obtain inorganic salt and discharge.
Output object is pressed into side line rectifying column, and tower reactor is heated using stream mode, and gas phase is carried out through overhead condenser
Cooling, enters return tank after cooling, a part is collected to storage tank as the backflow of rectifying column, part row's light component；Tower
Heavy constituent containing Silicon fluoride. arranged by kettle；Side take-off silicon fluoride, fixed gas is discharged through return tank.Fluorine silicon from rectifying column side take-off
Alkane, enters hydrolysis rectifying column, is passed through high-purity wet nitrogen, water content controls in 800～10000ppm, wet nitrogen on feeding line
Mol ratio 1 with silicon fluoride:20～1:100, high-purity wet nitrogen and silicon fluoride are mixed in hydrolysis rectifying column, tower reactor sets
Putting steam is heating source, tower reactor re-scheduling component, and top gaseous phase is cooled down through overhead condenser, entrance return tank after cooling, one
As the backflow of rectifying column, part extraction silicon fluoride, tower top fixed gas is given off part by return tank.
Enter low temperature silicon fluoride adsorption column, the gold in absorption silicon fluoride from the silicon fluoride liquid of hydrolysis rectifying column tower top extraction
Belong to impurity and nonmetallic inclusion, the silicon fluoride adsorbing column outlet output from silicon fluoride after being purified through silicon fluoride adsorption column enters
Silicon fluoride knockout tower, bottom of towe separates discharges Silicon fluoride., and overhead reflux produces trifluoro hydrogen silicon product, from the output of silicon fluoride knockout tower
Silicon fluoride. enter rectifying column purified, tower reactor reboiler lead to steam heating vaporization, tower top discharge the silicon of hydrogen containing trifluoro light
Component, tower reactor produces Silicon fluoride. product.
According to another embodiment of the invention, dehydrating unit, cooling tower are also included between lightness-removing column and described adsorption tower
Also include low temperature dewatering tower and knockout tower between, so that the absorption of raising adsorption tower and knockout tower and separation efficiency.
The structure of some specific embodiments of the present invention is illustrated above in the way of word and brief description, and non-exhaustive
Nothing left or be limited to concrete form described above.It should be pointed out that for those skilled in the art, do not taking off
On the premise of the principle of the invention, some improvements and modifications can also be made, these improvements and modifications also should be regarded as the present invention's
Protection domain.
Claims (7)
1. a kind of absorption purifying plant of purifying column output object, described output object is from the silicon fluoride of purifying column and other are miscellaneous
Matter, this absorption purifying plant includes lightness-removing column, weight-removing column, adsorption tower, condenser, knockout tower, adsorption column, cooling tower and side line
Rectifying column and hydrolysis rectifying column it is characterised in that inserting described output object to described lightness-removing column, the product of described lightness-removing column via
Weight-removing column enters described adsorption tower, and described cooling tower is located between described adsorption column and described knockout tower, described adsorption tower and side
Line rectifying column connects, and this side line rectifying column is connected with adsorption column via condenser, and described adsorption column is connected with knockout tower, described point
It is connected with hydrolysis rectifying column from tower, and described lightness-removing column and weight-removing column include catalytic combustion system and inorganic salt treatment dress respectively
Put.
2. absorption purifying plant according to claim 1 is it is characterised in that go back between described lightness-removing column and described adsorption tower
Including dehydrating unit.
3. absorption purifying plant according to claim 1 is it is characterised in that be filled with active oxidation in described adsorption tower
One or more of aluminum, silica gel, molecular sieve, activated carbon adsorbent.
4. absorption purifying plant according to claim 1 is it is characterised in that also include between described cooling tower and knockout tower
Low temperature dewatering tower.
5. absorption purifying plant according to claim 1 is it is characterised in that described adsorption tower is adsorbing tower with molecular sieve.
6. absorption purifying plant according to claim 1 is it is characterised in that described adsorption column is cryogenic absorption post.
7. absorption purifying plant according to claim 1 is it is characterised in that described inorganic salt processing meanss include inserting again
Close packing groove, reactor and the precipitate recovery room of raw metal.
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| CN201510017547.7A CN104528735B (en) | 2015-01-14 | 2015-01-14 | A kind of absorption purifying plant of purifying column output object |
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| CN201510017547.7A CN104528735B (en) | 2015-01-14 | 2015-01-14 | A kind of absorption purifying plant of purifying column output object |
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| CN104528735A CN104528735A (en) | 2015-04-22 |
| CN104528735B true CN104528735B (en) | 2017-03-08 |
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| CN111233191B (en) * | 2018-11-29 | 2021-06-29 | 中国科学院大连化学物理研究所 | Method for treating wastewater generated in process of preparing epoxy chloropropane by epoxidation of chloropropene |
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| SG174814A1 (en) * | 2007-09-21 | 2011-10-28 | Memc Electronic Materials | Processes for purification of silicon tetrafluoride |
| CN101774588B (en) * | 2010-02-11 | 2012-01-25 | 浙江中宁硅业有限公司 | Purification method of silicon tetrafluoride prepared by using fluoride and silicon source power as raw materials |
| CN201942524U (en) * | 2011-01-14 | 2011-08-24 | 浙江中宁硅业有限公司 | Simple efficient silicon tetrafluoride refinement system |
| KR101134230B1 (en) * | 2011-06-24 | 2012-04-09 | 웅진폴리실리콘주식회사 | Purification method and system of chlorosilane, and purifying material for filtering metal impurities |
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Effective date of registration: 20201211 Address after: 611130 Building 29, No. 1919 Shuangyan Road, Chengdu cross strait science and Technology Industry Development Park, Wenjiang District, Chengdu City, Sichuan Province Patentee after: Chengdu rifenstedan Biotechnology Co.,Ltd. Address before: 713, building 12, Tianfu Life Science Park, No. 88, Keyuan South Road, high tech Zone, Chengdu, Sichuan Province 610041 Patentee before: CHENGDU HERBPURIFY Co.,Ltd. |
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Granted publication date: 20170308 Termination date: 20210114 |