CN102701217A - Impurity removing equipment for dichlorosilane - Google Patents
Impurity removing equipment for dichlorosilane Download PDFInfo
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- CN102701217A CN102701217A CN2012102103107A CN201210210310A CN102701217A CN 102701217 A CN102701217 A CN 102701217A CN 2012102103107 A CN2012102103107 A CN 2012102103107A CN 201210210310 A CN201210210310 A CN 201210210310A CN 102701217 A CN102701217 A CN 102701217A
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- dihydro silicon
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Abstract
The invention discloses impurity removing equipment for dichlorosilane. The impurity removing equipment comprises a purifying column, wherein the purifying column comprises a filler purifying zone and an adsorption zone; the adsorption zone is arranged above the filler purifying zone and an adsorbent is arranged in the adsorption zone for finely purifying the gaseous dichlorosilane to remove the impurities in the dichlorosilane. According to the impurity removing equipment for the dichlorosilane, which is disclosed by the embodiment of the invention, firstly, the dichlorosilane with a lower boiling point is separated by rough purification; and secondly, boron, phosphor and metal impurities in the gaseous dichlorosilane are removed by an adsorbent to obtain high-purity dichlorosilane. The impurity removing equipment has the advantages of simple structure, less investment and low energy consumption; and the obtained product, namely the dichlorosilane is higher in purity and favorable in quality of products and certain economic benefits can be obtained.
Description
Technical field
The present invention relates to technical field of polysilicon production, more specifically, the present invention relates to a kind of dichloro-dihydro silicon impurity removing equipment.
Background technology
Polysilicon is that unicircuit and photovoltaic generation are used crucial starting material, is the important content of the preferential theme of National Program for Medium-to Long-term Scientific and Technological Development manufacture field basic raw material.The industrialization technology of world's production of polysilicon mainly contains two kinds of technologies, promptly improves siemens process and silane thermal decomposition process technology.
The improvement Siemens Method is produced in the process of polysilicon, can produce the dichloro-dihydro silicon of part.There are inflammable, explosive, low-boiling characteristics in this material, if mustn't go to effective recycling, then can get into the polysilicon tail gas system, causes the tail gas load big, the problem that security incident takes place frequently.To the character of dichloro-dihydro silicon, there has been part producer to adopt the disproportionation technology that dichloro-dihydro silicon is converted into trichlorosilane now both at home and abroad, return the utilization of polysilicon system again.This has alleviated the negative impact that the dichloro-dihydro silicon ribbon comes to a certain extent.
Along with further research to the improvement siemens process, find that the high-purity dichloro-dihydro silicon of quality can directly send into the reduction furnace growing polycrystalline silicon, and can greatly improve the growth velocity of polysilicon with after trichlorosilane mixes, reduce polysilicon and reduce power consumption.To this discovery; Part producer is arranged in the technical study of actively developing the dichloro-dihydro Si reduction; But find that in research process dichloro-dihydro silicon belongs to low-boiling-point substance, contain impurity such as a large amount of B, P; Cause dichloro-dihydro silicon quality product to be difficult to guarantee, cause the polysilicon product quality very big landslide to occur.In order to solve dichloro-dihydro silicon product quality problem, domesticly carried out some research work, mainly all be through changing dichloro-dihydro silicon purification form, wanting to reach the purpose that promotes quality product.And the actual effect that obtains is following:
1, adopts sieve-tray tower purification dichloro-dihydro silicon.This traditional distillation technology, its inefficiency, power consumption height, the poor product quality of belonging to.
2, adopt packing tower purification dichloro-dihydro silicon.Packing tower has been obtained very big effect in trichlorosilane purification field in recent years; So just having the researchist that this technology is applied to dichloro-dihydro silicon purifies; From refining effect; Energy consumption has significant optimization than sieve-tray tower, but the B of refined product, P, metals content impurity are still very high, can't reach that to produce high purity polycrystalline silicon required.
Summary of the invention
The present invention one of is intended to solve the problems of the technologies described above at least to a certain extent or provides a kind of useful commerce to select at least.
For this reason, one object of the present invention is to propose a kind of good impurity removing effect, efficient is high, energy consumption is low and the dichloro-dihydro silicon impurity removing equipment of good product quality.
Dichloro-dihydro silicon impurity removing equipment according to the embodiment of the invention; Comprise purification tower; Said purification tower comprises: the filler purification section; Said filler purification section is provided with the liquid phase dichloro-dihydro silicon of treating removal of impurities is delivered into the opening for feed in the said purification tower, and said filler purification section is slightly purified to the liquid phase dichloro-dihydro silicon that is provided by said opening for feed, obtains gas phase dichloro-dihydro silicon and liquid high boiling material; And adsorption zone; Said adsorption zone is located in said filler purification section top and the said adsorption zone and disposes sorbent material, removes impurity wherein said gas phase dichloro-dihydro silicon is carried out smart the purification, wherein; The below of said filler purification section is provided with inlet mouth; Through said inlet mouth the chlorosilane of gas phase is provided in said purification tower, the top of said adsorption zone is provided with the air outlet, discharging said purification tower through the gas phase dichloro-dihydro silicon that essence is purified.
According to the dichloro-dihydro silicon impurity removing equipment of the embodiment of the invention, at first separate through the dichloro-dihydro silicon vaporization that boiling point is lower of thick purification, remove boron, phosphorus and metallic impurity in the gaseous state dichloro-dihydro silicon through sorbent material again; Obtain high-purity dichloro-dihydro silicon, this impurity removing equipment is simple in structure, less investment; Energy consumption is low; And it is higher to obtain product dichloro-dihydro silicon purity, and good product quality can bring certain economic benefit.
In addition, dichloro-dihydro silicon impurity removing equipment according to the above embodiment of the present invention can also have following additional technical characterictic:
According to one embodiment of present invention, said purification tower also has: leakage fluid dram, said leakage fluid dram are located at the bottom of said purification tower so that said liquid high boiling material is discharged said purification tower.
According to one embodiment of present invention, said liquid high boiling material is the chlorosilane that is rich in impurity.
According to one embodiment of present invention, also comprise: reboiler, said reboiler links to each other with said leakage fluid dram, and wherein liquid chlorosilane is heated into the gas phase chlorosilane.
According to one embodiment of present invention, the said gas phase chlorosilane that obtains of heating sent into said purification tower through said inlet mouth so as to conduct heat with the liquid phase dichloro-dihydro silicon of said filler purification section, mass transfer.
According to one embodiment of present invention, the high boiling material water cooler, said high boiling material water cooler links to each other with cooling segment liquid chlorosilane and extraction with said leakage fluid dram.
According to one embodiment of present invention, also comprise: condensing surface, said condensing surface will be cooled to liquid phase dichloro-dihydro silicon through the gas phase dichloro-dihydro silicon that essence is purified.
According to one embodiment of present invention, the part of the liquid phase dichloro-dihydro silicon that obtains of cooling is back to said purification tower.
According to one embodiment of present invention, said filler purification section is filled with the waved plate wire mesh packing.
According to one embodiment of present invention, said sorbent material is an acticarbon.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize through practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage obviously with are easily understood becoming the description of embodiment from combining figs, wherein:
Fig. 1 is the dichloro-dihydro silicon impurity removing equipment structural representation according to the embodiment of the invention;
Fig. 2 is the impurity-removing method schematic flow sheet according to the dichloro-dihydro silicon impurity removing equipment of the embodiment of the invention.
Embodiment
Describe embodiments of the invention below in detail, the example of said embodiment is shown in the drawings, and wherein identical from start to finish or similar label is represented identical or similar elements or the element with identical or similar functions.Be exemplary through the embodiment that is described with reference to the drawings below, be intended to be used to explain the present invention, and can not be interpreted as limitation of the present invention.
In description of the invention; It will be appreciated that; The orientation of indications such as term " " center ", " vertically ", " laterally ", " length ", " width ", " thickness ", " on ", D score, " preceding ", " back ", " left side ", " right side ", " vertically ", " level ", " top ", " end " " interior ", " outward ", " clockwise ", " counterclockwise " or position relation are for based on orientation shown in the drawings or position relation; only be to describe with simplifying for the ease of describing the present invention; rather than the device or the element of indication or hint indication must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as limitation of the present invention.
In addition, term " first ", " second " only are used to describe purpose, and can not be interpreted as indication or hint relative importance or the implicit quantity that indicates indicated technical characterictic.Thus, one or more a plurality of these characteristics can be shown or impliedly comprised to the characteristic that is limited with " first ", " second " clearly.In description of the invention, the implication of " a plurality of " is two or more, only if clear and definite concrete qualification is arranged in addition.
In the present invention, only if clear and definite regulation and qualification are arranged in addition, broad understanding should be done in terms such as term " installation ", " linking to each other ", " connection ", " fixing ", for example, can be to be fixedly connected, and also can be to removably connect, or connect integratedly; Can be mechanical connection, also can be to be electrically connected; Can be directly to link to each other, also can link to each other indirectly through intermediary, can be the connection of two element internals.For those of ordinary skill in the art, can understand above-mentioned term concrete implication in the present invention as the case may be.
In the present invention; Only if clear and definite regulation and qualification are arranged in addition; First characteristic second characteristic it " on " or D score can comprise that first and second characteristics directly contact, can comprise that also first and second characteristics are not directly contacts but through the contact of the additional features between them.And, first characteristic second characteristic " on ", " top " and " above " comprise first characteristic directly over second characteristic and oblique upper, or only represent that the first characteristic level height is higher than second characteristic.First characteristic second characteristic " under ", " below " and " below " comprise first characteristic directly over second characteristic and oblique upper, or only represent that the first characteristic level height is less than second characteristic.
At first, describe according to dichloro-dihydro silicon impurity removing equipment of the present invention in conjunction with Fig. 1.
As shown in Figure 1, said dichloro-dihydro silicon impurity removing equipment comprises purification tower 10, and purification tower 10 comprises: filler purification section 20 and adsorption zone 30.
Wherein, the below of filler purification section 20 is provided with inlet mouth 22, through inlet mouth 22 chlorosilane of gas phase is provided in purification tower 10, and the top of adsorption zone 30 is provided with air outlet 31, discharging purification tower 10 through the gas phase dichloro-dihydro silicon that essence is purified.
Thus, can realize the removal of impurities of dichloro-dihydro silicon obtaining high-purity dichloro-dihydro silicon through said dichloro-dihydro silicon impurity removing equipment, this device structure is simple, less investment, and energy consumption is low, and it is higher to obtain product dichloro-dihydro silicon purity, and good product quality is fit to promote the use of.
In one example, purification tower 10 also has leakage fluid dram 11, and leakage fluid dram 11 is located at the liquid high boiling material that the bottom of purification tower 10 produced will slightly purifying and discharges purification tower 10.
In one example, said impurity removing equipment also comprises reboiler 60, and reboiler 60 links to each other with leakage fluid dram 11 so that purification tower 10 is discharged high boiling material, and liquid chlorosilane wherein is heated into the gas phase chlorosilane.。The liquid dichloro-dihydro silicon that the gas phase chlorosilane can be delivered to purification tower 10 and filler purification section 20 carries out mass transfer, heat transfer, to increase the gas-liquid exchange efficiency, improves overall operation efficiency.
In order liquid phase chlorosilane in the high boiling material to be cooled to the liquid phase trichlorosilane that is rich in impurity of easy storage and the mixture of dichloro-dihydro silicon; In one example; Preferably; Said impurity removing equipment also comprises high boiling material water cooler 50, and high boiling material water cooler 50 links to each other with leakage fluid dram 11 high temperature trichlorosilane wherein is cooled to the low temperature trichlorosilane of easy storage.
In one example, said impurity removing equipment also comprises condensing surface 70, and condensing surface 70 can carry out condensation with said high-purity dichloro-dihydro silicon.Thus, liquid high-purity dichloro-dihydro silicon that condensation obtains can be with its part as the product extraction; Another part is back to purification tower 10 as phegma; The phegma flow that is back to purification tower 10 can suitably be adjusted, thereby increases the gas-liquid exchange efficiency, improves overall operation efficiency.
In one example, filler purification section 20 is filled with wire mesh packing.Thus, said wire mesh packing can be the waved plate wire mesh packing, and this filler purification tower can effectively be removed partial impurities, and impurity gets in the high boiling material and discharges.
In one example, said sorbent material is an acticarbon.Thus, boron, phosphorus and metallic impurity in can active adsorption dichloro-dihydro silicon obtain the higher dichloro-dihydro silicon of purity.
The flow process of describing according to the impurity-removing method of dichloro-dihydro silicon impurity removing equipment of the present invention with reference to figure 2 below.
Particularly, the impurity-removing method according to the dichloro-dihydro silicon impurity removing equipment of the embodiment of the invention may further comprise the steps:
A) the liquid dichloro-dihydro silicon of treating removal of impurities is slightly purified through wire mesh packing, obtains gaseous state dichloro-dihydro silicon and the liquid high boiling material that is rich in impurity; With
B) remove boron, phosphorus and metallic impurity in the said gaseous state dichloro-dihydro silicon through adsorbents adsorb, obtain high-purity dichloro-dihydro silicon.
Thus, according to the dichloro-dihydro silicon impurity-removing method of the embodiment of the invention, at first separate through the dichloro-dihydro silicon vaporization that boiling point is lower of the method for thick purification; Remove boron, phosphorus and metallic impurity in the gaseous state dichloro-dihydro silicon through sorbent material again, obtain high-purity dichloro-dihydro silicon, this method is simple to operate; The equipment used less investment, energy consumption is low, and it is higher to obtain product dichloro-dihydro silicon purity; Good product quality can bring certain economic benefit.
Wherein, said step a) specifically can comprise: the filler purification section that said liquid dichloro-dihydro silicon is sent in the purification tower is slightly purified, wherein, be provided with wire mesh packing in the said filler purification section.
The filler purification section that the dichloro-dihydro silicon of liquid state is sent in the purification tower is slightly purified, can obtain gaseous state dichloro-dihydro silicon and the liquid high boiling material that is rich in impurity.About thick purification; Can be employed in the method that wire mesh packing is set in the said filler purification section; The dichloro-dihydro silicon of liquid state is fed the filler purification section, under the purification of wire mesh packing, obtain and isolate gaseous state dichloro-dihydro silicon and the liquid high boiling material that is rich in impurity.In order further to improve thick effect of purifying, said wire mesh packing can be the waved plate wire mesh packing, and this filler can effectively be removed the partial impurities in the dichloro-dihydro silicon.
About step b); It will be appreciated that; The method of removing boron, phosphorus and metallic impurity in the said gaseous state dichloro-dihydro silicon through adsorbents adsorb does not have particular restriction; For example can gasiform dichloro-dihydro silicon be carried out smart the purification to remove boron, phosphorus and the metallic impurity in the said dichloro-dihydro silicon through the adsorption zone in the purification tower, obtain high-purity dichloro-dihydro silicon.About the selection of adsorption zone internal adsorption agent, can adopt can active adsorption boron, the sorbent material of phosphorus and metallic impurity, and preferably, the present invention adopts the sorbent material of sp act charcoal as adsorption zone.
In order to obtain liquid high-purity dichloro-dihydro silicon, can said high-purity gas phase dichloro-dihydro silicon be carried out condensation.Method and device about condensation do not have particular restriction, for example can adopt condensing surface with its condensation.
The liquid high-purity dichloro-dihydro silicon that obtains about condensation; Can be with its part as the product extraction, another part is back to said purification tower as phegma, and the phegma flow that is back to purification tower can suitably be adjusted; Thereby increase the gas-liquid exchange efficiency, improve overall operation efficiency.
About said liquid high boiling material, it will be appreciated that said liquid high boiling material is the liquid phase chlorosilane that is rich in impurity, said liquid phase chlorosilane is mainly liquid trichlorosilane, and contains a spot of liquid dichloro-dihydro silicon.
At least a portion of said liquid phase chlorosilane is heated into the gas phase chlorosilane and carries out mass transfer, heat transfer with trim the top of column liquid.
Said gas phase chlorosilane mainly comprises gas phase dichloro-dihydro silicon and trichlorosilane; Gas phase dichloro-dihydro silicon and trichlorosilane delivered in the said purification tower carry out mass transfer, heat transfer with liquid dichloro-dihydro silicon with said filler purification section; Can increase the gas-liquid exchange efficiency, improve overall operation efficiency.
In order to make full use of the liquid high boiling material that is rich in impurity that the removal of impurities process produces, reduce pollution to environment, can said high boiling material further be handled.Its treatment process specifically can comprise:
Preferably, can the part of said liquid chlorosilane be cooled off the back as the high boiling material extraction.Be mainly the liquid phase trichlorosilane that is rich in impurity and the mixture of dichloro-dihydro silicon in the high boiling material.Method of cooling and equipment do not have particular restriction yet, for example can liquid chlorosilane be fed the high boiling material water cooler and obtain the cryogenic liquid phase trichlorosilane of impurity and the mixture of dichloro-dihydro silicon of being rich in.The mixture of cryogenic liquid phase trichlorosilane and dichloro-dihydro silicon can get into and carry out the secondary purification in the trichlorosilane purification tower, to obtain high-quality trichlorosilane, is used to produce polysilicon.
Thus, can make full use of, not only reduce environmental pollution, also improve overall operation efficiency the liquid high boiling material that is rich in impurity that produces of purifying.
Below in conjunction with specific embodiment and experimental example the impurity-removing method according to dichloro-dihydro silicon impurity removing equipment of the present invention is described.
Embodiment 1
Said dichloro-dihydro silicon removal of impurities equipment used is as shown in Figure 2, and said dichloro-dihydro silicon impurity removing equipment comprises purification tower 10, and purification tower 10 comprises: filler purification section 20, adsorption zone 30, high boiling material water cooler 50, reboiler 60 and condensing surface 70.
Said impurity removing equipment also comprises high boiling material water cooler 50, and high boiling material water cooler 50 low temperature that is cooled to easy storage with liquid phase chlorosilane that will be wherein that links to each other with leakage fluid dram 11 is rich in the liquid phase trichlorosilane of impurity and the mixture of dichloro-dihydro silicon.
Adopt dichloro-dihydro silicon impurity removing equipment as shown in Figure 2 to carry out removal of impurities; The filler purification section 20 that liquid dichloro-dihydro silicon is sent in the purification tower 10 is slightly purified; Be provided with wire mesh packing in the filler purification section 20 and purify, obtain gaseous state dichloro-dihydro silicon and the liquid phase high boiling material that is rich in impurity.
Gasiform dichloro-dihydro silicon is carried out smart the purification to remove boron, phosphorus and the metallic impurity in the dichloro-dihydro silicon through the adsorption zone 30 in the purification tower 10, obtain high-purity dichloro-dihydro silicon; High-purity dichloro-dihydro silicon through condensing surface 70 condensations, is obtained liquid high-purity dichloro-dihydro silicon, and with the part of the high-purity dichloro-dihydro silicon of liquid state as the product extraction, another part is back to purification tower 10 as phegma.
At least a portion of liquid phase chlorosilane is heated into the gas phase chlorosilane and is back to purification tower 10 so that carry out mass transfer, heat transfer with the liquid dichloro-dihydro silicon of filler purification section 20; Another part of liquid phase chlorosilane can cool off the back as the high boiling material extraction.
The removal of impurities that thus, can realize dichloro-dihydro silicon is purified.
Experimental example 1
Adopt embodiment 1 said method and apparatus that sample 1, sample 2 and sample 3 are carried out removal of impurities and purify, purification is the result see shown in table 1, table 2, the table 3.
Impurity change list before and after table 1 sample 1 is purified
Impurity change list before and after table 2 sample 2 is purified
Impurity change list before and after table 3 sample 3 is purified
Can find out by the foregoing description and experimental example,, can effectively remove boron, phosphorus and metallic impurity in the gaseous state dichloro-dihydro silicon according to dichloro-dihydro silicon impurity removing equipment of the present invention; Obtain high-purity dichloro-dihydro silicon, this device structure is simple, less investment; Energy consumption is low; And it is higher to obtain product dichloro-dihydro silicon purity, and good product quality can bring certain economic benefit.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means the concrete characteristic, structure, material or the characteristics that combine this embodiment or example to describe and is contained at least one embodiment of the present invention or the example.In this manual, the schematic statement to above-mentioned term not necessarily refers to identical embodiment or example.And concrete characteristic, structure, material or the characteristics of description can combine with suitable manner in any one or more embodiment or example.
Although illustrated and described embodiments of the invention; Those having ordinary skill in the art will appreciate that: under the situation that does not break away from principle of the present invention and aim, can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited claim and equivalent thereof.
Claims (10)
1. a dichloro-dihydro silicon impurity removing equipment is characterized in that, comprise purification tower, said purification tower comprises:
The filler purification section; Said filler purification section is provided with the liquid phase dichloro-dihydro silicon of treating removal of impurities is delivered into the opening for feed in the said purification tower; Said filler purification section is slightly purified to the liquid phase dichloro-dihydro silicon that is provided by said opening for feed, obtains gas phase dichloro-dihydro silicon and liquid high boiling material; With
Adsorption zone, said adsorption zone are located in said filler purification section top and the said adsorption zone and dispose sorbent material, remove impurity wherein said gas phase dichloro-dihydro silicon is carried out smart the purification, wherein,
The below of said filler purification section is provided with inlet mouth, through said inlet mouth the dichloro-dihydro silicon of gas phase is provided in said purification tower,
The top of said adsorption zone is provided with the air outlet, discharging said purification tower through the gas phase dichloro-dihydro silicon that essence is purified.
2. dichloro-dihydro silicon impurity removing equipment according to claim 1 is characterized in that said purification tower also has:
Leakage fluid dram, said leakage fluid dram are located at the bottom of said purification tower so that said liquid high boiling material is discharged said purification tower.
3. dichloro-dihydro silicon impurity removing equipment according to claim 2 is characterized in that said liquid high boiling material is the chlorosilane that is rich in impurity.
4. according to claim 2 or 3 described dichloro-dihydro silicon impurity removing equipments, it is characterized in that, also comprise:
Reboiler, said reboiler links to each other with said leakage fluid dram, and wherein liquid high boiling material is heated into the gas phase chlorosilane that is rich in impurity.
5. dichloro-dihydro silicon impurity removing equipment according to claim 4 is characterized in that, the said gas phase chlorosilane that heating obtains sent into said purification tower through said inlet mouth so as to conduct heat with the liquid phase dichloro-dihydro silicon of said filler purification section, mass transfer.
6. according to claim 2 or 3 described dichloro-dihydro silicon impurity removing equipments, it is characterized in that, also comprise:
The high boiling material water cooler, said high boiling material water cooler links to each other with cooling segment liquid chlorosilane and extraction with said leakage fluid dram.
7. dichloro-dihydro silicon impurity removing equipment according to claim 1 is characterized in that, also comprises:
Condensing surface, said condensing surface will be cooled to liquid phase dichloro-dihydro silicon through the gas phase dichloro-dihydro silicon that essence is purified.
8. dichloro-dihydro silicon impurity removing equipment according to claim 7 is characterized in that, the part of the liquid phase dichloro-dihydro silicon that cooling obtains is back to said purification tower.
9. dichloro-dihydro silicon impurity removing equipment according to claim 1 is characterized in that said filler purification section is filled with the waved plate wire mesh packing.
10. dichloro-dihydro silicon impurity removing equipment according to claim 1 is characterized in that said sorbent material is an acticarbon.
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| CN2012102103107A CN102701217A (en) | 2012-06-19 | 2012-06-19 | Impurity removing equipment for dichlorosilane |
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Application publication date: 20121003 |