CN102795629B - Method for purification of dichlorosilane from dry method recovered material - Google Patents
Method for purification of dichlorosilane from dry method recovered material Download PDFInfo
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Abstract
The invention discloses a method for purification of dichlorosilane from dry method recovered materials, and comprises the following steps of: a) obtaining a dry-method recovered material by recovering from reduction tail gas of the polysilicon production process by a dry method, feeding the recovered material into a first dry method rectifying tower for rectification, recovering a first low-boiling-point substance from the tower top of the first dry method rectifying tower, and recovering intermediate chlorosilane from the tower bottom of the first dry method rectifying tower; b) feeding the first low-boiling-point substance into a separation column for separation, recovering boron impurity from the top of the separation column, and recovering dichlorosilane from the bottom of the separation column; c) feeding the intermediate chlorosilane into a second dry method rectifying tower for rectification, recovering a second low-boiling-point substance from the tower top of the second dry method rectifying tower, and recovering silicon tetrachloride from the tower bottom of the second dry method rectifying tower. According to the method of the invention, the second low-boiling-point substance is a mixture of dichlorosilane and trichlorosilane which can be directly fed into a reducing furnace for reduction reaction, thereby saving the process of mixing the dichlorosilane and the trichlorosilane.
Description
Technical field
The present invention relates to field of polysilicon technology, more specifically, the present invention relates to a kind of method of the dichloro-dihydro silicon of purifying from dry back rewinding.
Background technology
Its distinctive lower boiling of polysilicon by-product dichloro-dihydro silicon, inflammable and explosive characteristic has become the technical bottleneck of polysilicon enterprise expanding production, and traditional treatment process not only in safety, and has been brought problems in environmental protection; And can the purifying technique of dichloro-dihydro silicon be to determine its follow-up key that recycle.
Improveing closed Siemens Method produces in polysilicon process, one ton of polysilicon of every production can produce 1.6 tons of dichloro-dihydro silicon, the boiling point of dichloro-dihydro silicon under 101Kpa is 8.2 ℃, inflammable and explosive in air, continuous expansion along with polysilicon scope of the enterprise, current polysilicon factory passes into reduction furnace according to a certain percentage by dichloro-dihydro silicon and trichlorosilane after purifying, utilize dichloro-dihydro silicon in reduction process, to suppress trichlorosilane disproportionation, thereby reduce trichlorosilane consumption, improve utilization ratio of trichlorosilane, both reduced silicon tetrachloride generation, solved the problem of dichloro-dihydro silicon, can improve polysilicon surface form quality simultaneously.Traditional dichloro-dihydro silicon purifying technique is that the mixed solution of dichloro-dihydro silicon, trichlorosilane and the silicon tetrachloride of dry method recovery is sent into dry method rectifying tower, through the first dry method rectifying tower, remove the low-boiling-point substance impurity containing dichloro-dihydro silicon and trichlorosilane respectively, middle chlorosilane material at the bottom of tower enters the second dry method rectifying tower, at the bottom of the second dry method rectifying tower, discharge the high boiling material impurity such as silicon tetrachloride and send into hydrogenation system, and the trichlorosilane products of the second dry method rectifying tower tower top can reach the purity requirement of being sent to reduction furnace.Its idiographic flow as shown in Figure 1.
In the low-boiling-point substance of the first dry method rectifying tower tower top, the ratio of trichlorosilane and dichloro-dihydro silicon is probably 0.8～1.3:1, in order to reclaim this part trichlorosilane, and makes dichloro-dihydro silicon reach the requirement of further reduction, need to increase knockout tower and further purify.Higher directly outer the selling of low-boiling-point substance foreign matter content of knockout tower, the chlorosilane at the bottom of knockout tower tower enters separated 2 towers, and separated 2 column overhead obtain dichloro-dihydro silicon product, and the trichlorosilane at the bottom of separated 2 tower towers enters recovery tower and further reclaims.And from separated complexity, the boiling point of dichloro-dihydro silicon and low-boiling-point substance is very approaching, very difficult with knockout tower removal of impurities, need considerable number of theoretical plate and reflux ratio, this just needs a large amount of thermal loads.Through high-purity trichlorosilane products of rectifying or dry method rectifying and the dichloro-dihydro silicon product obtaining through knockout tower, send in specific proportions reduction furnace like this.
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 at least provides a kind of useful business to select.
For this reason, one object of the present invention is to propose a kind of method of implementing the dichloro-dihydro silicon of purifying that convenience, good separating effect and energy consumption are low from dry back rewinding.
According to the method for the dichloro-dihydro silicon of purifying from dry back rewinding of the embodiment of the present invention, comprise the following steps: a) the reduction tail gas in production of polysilicon technique is reclaimed and obtains dry back rewinding through dry method, dry back rewinding is sent in the first dry method rectifying tower and carried out rectifying, overhead extraction the first low-boiling-point substance from described the first dry method rectifying tower, in described the first low-boiling-point substance, contain dichloro-dihydro silicon and boron-containing impurities, and discharge middle chlorosilane at the bottom of the tower of described the first dry method rectifying tower; B) described the first low-boiling-point substance is passed into knockout tower and carry out separation, with the tower top from described knockout tower, gather boron-containing impurities and gather dichloro-dihydro silicon at the bottom of tower; C) chlorosilane in the middle of described is sent in the second dry method rectifying tower and carried out rectifying, from the tower top of described the second dry method rectifying tower, gather the second low-boiling-point substance, in described the second low-boiling-point substance, contain dichloro-dihydro silicon and trichlorosilane, at the bottom of the tower of described the second dry method rectifying tower, discharge silicon tetrachloride.
According to the method for the purification dichloro-dihydro silicon of the embodiment of the present invention, in the first low-boiling-point substance that described the first dry method rectifying tower is discharged, only contain dichloro-dihydro silicon and boron-containing impurities, avoided the extraction of trichlorosilane, thereby avoided dichloro-dihydro silicon and the advanced knockout tower of trichlorosilane to isolate the trichlorosilane containing partial impurities, enter again the process that recovery tower is further purified, the operation steps that has reduced separated 2 towers and recovery tower, has reduced equipment cost; Simultaneously, because the amount of the first low-boiling-point substance reduces greatly, also just reduced the processing load of the equipment such as knockout tower and processed heat, reduce purification energy consumption and further reduced production cost, the treatment capacity of knockout tower lowers, the specification that can reduce purification tower and corresponding support equipment, has reduced equipment cost.The second low-boiling-point substance is the mixture of dichloro-dihydro silicon and trichlorosilane, can directly pass into reduction furnace and carry out reduction reaction, has saved the process of dichloro-dihydro silicon and trichlorosilane mixing.
In addition, the method for purification dichloro-dihydro silicon according to the above embodiment of the present invention, can also have following additional technical characterictic:
According to one embodiment of present invention, also comprise: d) described the second low-boiling-point substance is directly sent into reduction furnace, with the trichlorosilane reducing wherein.
According to one embodiment of present invention, also comprise: e) described silicon tetrachloride is sent into hydrogenation system and carry out hydrogenation.
According to one embodiment of present invention, content >=90% of dichloro-dihydro silicon in described the first low-boiling-point substance.
According to one embodiment of present invention, the treatment capacity of described the first dry method rectifying tower is 15m
3/ h is 0.1～0.5m in the picking rate of the first low-boiling-point substance described in described step a)
3/ h, and be 0.1～0.5m in the input speed of the first low-boiling-point substance described in described step b)
3/ h.
According to one embodiment of present invention, in described step b), the picking rate of described dichloro-dihydro silicon is 0.1～0.45m
3/ h.。
According to one embodiment of present invention, in described step b), in described the second low-boiling-point substance, contain mass percent and be 2～10% dichloro-dihydro silicon.
According to one embodiment of present invention, in described step c), the picking rate of described the second low-boiling-point substance is 5.5～7m
3/ h.
Additional aspect of the present invention and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage accompanying drawing below combination obviously and is easily understood becoming the description of embodiment, wherein:
Fig. 1 is the schematic flow sheet of dichloro-dihydro silicon of purifying in prior art;
Fig. 2 is according to the schematic flow sheet of the purification dichloro-dihydro silicon of the embodiment of the present invention.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings.Below by the embodiment being described with reference to the drawings, be exemplary, be intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.
First with reference to figure 2, describe according to the flow process of the method for purification dichloro-dihydro silicon of the present invention below.
Particularly, according to the method for the purification dichloro-dihydro silicon of the embodiment of the present invention, comprise the following steps:
A) the reduction tail gas in production of polysilicon technique is reclaimed and obtains dry back rewinding through dry method, dry back rewinding is sent in the first dry method rectifying tower and carried out rectifying, from the tower top of described the first dry method rectifying tower, discharge the first low-boiling-point substance, in described the first low-boiling-point substance, contain dichloro-dihydro silicon and boron-containing impurities, and discharge middle chlorosilane at the bottom of the tower of described the first dry method rectifying tower;
B) described the first low-boiling-point substance is carried out to separation by knockout tower, to gather boron-containing impurities from tower top and discharge dichloro-dihydro silicon at the bottom of tower.
Thus, according to the method for the purification dichloro-dihydro silicon of the embodiment of the present invention, in the first low-boiling-point substance that described the first dry method rectifying tower is discharged, only contain dichloro-dihydro silicon and boron-containing impurities, avoided the extraction of trichlorosilane, thereby avoided dichloro-dihydro silicon and the advanced knockout tower of trichlorosilane to isolate the trichlorosilane containing partial impurities, enter again the process that recovery tower is further purified, reduced the operation steps of separated 2 towers and recovery tower, reduced equipment cost; Simultaneously, because the amount of the first low-boiling-point substance reduces greatly, the reflux ratio needing according to quality product, can reduce reflux in tower amount, reduce the tower internal loading of the first dry method rectifying tower, also reduced the processing load of the equipment such as knockout tower and processed heat, reduce purification energy consumption and further reduced production cost, the treatment capacity of knockout tower lowers, and can reduce the specification of purification tower and corresponding support equipment, has reduced equipment cost.
About described step a), it will be appreciated that, dry back rewinding in described production of polysilicon technique is the mixed solution of dichloro-dihydro silicon, trichlorosilane and the silicon tetrachloride of dry method recovery, in the first dry method rectifying tower during rectifying, in order to make a tower top discharge section of the first dry method rectifying tower containing the first low-boiling-point substance of dichloro-dihydro silicon and boron impurity, and guaranteeing content >=90% of dichloro-dihydro silicon in described the first low-boiling-point substance, the pressure that can control the first dry method rectifying tower is 0.4～0.7MPa.
In step b), described the first low-boiling-point substance is carried out to separation in knockout tower.Thus, can gather boron-containing impurities and discharge dichloro-dihydro silicon at the bottom of tower from knockout tower tower top, the boron-containing impurities of extraction can be sold outward, and dichloro-dihydro silicon can mix and reduce with the trichlorosilane of other operation.About the rectificating method of middle chlorosilane, will be described in detail below.
Rectificating method about chlorosilane in the middle of described is not particularly limited, and its concrete operations can comprise: chlorosilane in the middle of described is sent into the second dry method rectifying tower and carry out rectifying.Thus, can obtain from the tower top of described the second dry method rectifying tower the second low-boiling-point substance, at the bottom of the tower of described the second dry method rectifying tower, discharge silicon tetrachloride, in described the second low-boiling-point substance, contain dichloro-dihydro silicon and trichlorosilane, directly send into reduction furnace reduction trichlorosilane wherein, after having avoided dichloro-dihydro silicon and trichlorosilane to be mixed in holding furnace, pass into again the process that reduction furnace reduces, and accelerated the speed of growth of silicon rod in reduction process, greatly reduce power consumption, and guaranteed the quality of silicon rod; Silicon tetrachloride can make full use of, and adds hydrogenation system to carry out hydrogenation.
The velocity of discharge about described the first low-boiling-point substance, it will be appreciated that, the rate of yield of described the first low-boiling-point substance need to guarantee that purification system can normally move, and the produced quantity of the first low-boiling-point substance is as far as possible little, and wherein foreign matter content is many as far as possible.Because the rate of yield of described the first low-boiling-point substance is affected by the treatment capacity of the first dry method rectifying tower, preferably, the treatment capacity of described the first dry method rectifying tower is 15m
3/ h.The concrete of its velocity of discharge determines that method can be: the pressure of controlling the first dry method rectifying tower is 0.4～0.7MPa, in the situation that other conditions are constant, gradually reduce the produced quantity of the first low-boiling-point substance, each first low-boiling-point substance produced quantity that reduces all guarantees the normal operation regular hour of tower system, the content of boron and phosphorus matter content and dichloro-dihydro silicon in the second low-boiling-point substance of repeated detection second dry method rectifying tower in this period, records the parameters of the normal operation of the first and second dry method rectifying tower simultaneously; Along with gradually reducing of the first low-boiling-point substance produced quantity, in the second low-boiling-point substance, dichloro-dihydro silicone content increases gradually, when the first low-boiling-point substance produced quantity is reduced to a certain degree, the second low-boiling-point substance in the second dry method rectifying tower can not meet purity and the impurity requirement of reduction, or in the second low-boiling-point substance, the mass percent of dichloro-dihydro silicon is greater than 2～10%.
Through test of many times, can show that the best velocity of discharge of the first low-boiling-point substance is 0.1～0.5m
3/ h, the first low-boiling-point substance velocity of discharge is as shown in table 1.
Table 1 the first low-boiling-point substance picking rate table
Rate of yield according to the first low-boiling-point substance from the first dry method rectifying tower, can regulate the first low-boiling-point substance to pass into knockout tower and carry out separated input speed, and preferably, the input speed of described the first low-boiling-point substance is 0.1～0.5m
3/ h, the first low-boiling-point substance gathers dichloro-dihydro silicon after separation at the bottom of knockout tower tower, and for assurance system can normally be moved, the rate of yield of dichloro-dihydro silicon is 0.1～0.45m
3/ h.From the chlorosilane of discharging at the bottom of the first dry method rectifying tower, through the second dry method rectifying tower, carry out rectifying, and from overhead extraction second low-boiling-point substance of the second dry method rectifying tower, preferably, the picking rate of the second low-boiling-point substance is 5.5～7m
3/ h.
Below with reference to specific embodiment, describe according to the method for purification dichloro-dihydro silicon of the present invention.
Embodiment 1
Employing is stated according to the method for purification dichloro-dihydro silicon of the present invention, utilizes schema as shown in Figure 2 to carry out the purification of dichloro-dihydro silicon.
Dry back rewinding in production of polysilicon technique is sent into the first dry method rectifying tower and carry out rectifying, the treatment capacity of controlling the first dry method rectifying tower is 15m
3/ h.
With 0.1～0.5m
3the rate of yield of/h is passed through the first low-boiling-point substance of rectifying from the overhead extraction of the first dry method rectifying tower, and discharges middle chlorosilane at the bottom of tower.In the first low-boiling-point substance, contain dichloro-dihydro silicon and boron-containing impurities.
By the first low-boiling-point substance with 0.1～0.5m
3the speed of/h passes into knockout tower and carries out separation, and with 0.1～0.45m
3the speed of/h is from extraction dichloro-dihydro silicon at the bottom of knockout tower tower, from the boron-containing impurities of overhead extraction trace.Boron-containing impurities can be sold outward, and dichloro-dihydro silicon can pass into reduction furnace reduction trichlorosilane.
With 14.5～14.9m
3the speed of/h passes into the second dry method rectifying tower by middle chlorosilane and carries out rectifying, from the second dry method rectifying tower tower top with 5.5～7m
3speed acquisition the second low-boiling-point substance of/h is discharged silicon tetrachloride at the bottom of tower.In the second low-boiling-point substance, contain dichloro-dihydro silicon and trichlorosilane, can directly send into reduction furnace reduction trichlorosilane wherein, silicon tetrachloride can make full use of, and adds hydrogenation system to carry out hydrogenation.In each step, material transferring speed is shown in Table 2.
Comparative example
Adopt the method for purification of traditional dichloro-dihydro silicon, utilize flow process as shown in Figure 1 to carry out the purification of dichloro-dihydro silicon.
Dry back rewinding in crystal silicon production technique is sent into the first dry method rectifying tower and carry out rectifying, the treatment capacity of controlling the first dry method rectifying tower is 15m
3/ h.
With 1～1.5m
3the low-boiling-point substance that the rate of yield of/h contains dichloro-dihydro silicon and trichlorosilane mixture from the overhead extraction of the first dry method rectifying tower, from chlorosilane in the middle of extraction at the bottom of tower.
At the same rate by contain the low-boiling-point substance of dichloro-dihydro silicon with trichlorosilane mixture pass into knockout tower carry out separated, from knockout tower tower top with 0.1～0.3m
3the impure low-boiling-point substance of speed extraction of/h.This low-boiling-point substance is impure higher, can sell outward.From at the bottom of tower with 0.9～1.3m
3the speed extraction chlorosilane of/h, and with identical speed, pass into separated 2 towers and carry out further separation.From separated 2 column overhead with 0.45～0.62m
3the speed extraction dichloro-dihydro silicon of/h, from the bottom of tower with 0.45～0.65m
3the speed extraction trichlorosilane of/h, and with identical speed, trichlorosilane is sent into recovery tower and further purify.
By middle chlorosilane with 13.5～14.5m
3the speed of/h passes into the second dry method rectifying tower and carries out rectifying, from the second dry method rectifying tower tower top with 5～6m
3the speed of/h is discharged trichlorosilane, and reduces after the dichloro-dihydro silicon mixing of discharging with tower top in separated 2 towers.From at the bottom of the second dry method rectifying tower with 5～7m
3the speed of/h is discharged silicon tetrachloride, and silicon tetrachloride can make full use of, and adds hydrogenation system to carry out hydrogenation.In each step, material transferring speed is shown in Table 2.
Each step material transferring speed in table 2 embodiment 1 and comparative example
By above-described embodiment and comparative example, associative list 1 can be found out, according to the method for the purification dichloro-dihydro silicon of the embodiment of the present invention, in the low-boiling-point substance that the first dry method rectifying tower is discharged, only contain dichloro-dihydro silicon and boron-containing impurities, avoided the extraction of trichlorosilane, thereby avoided dichloro-dihydro silicon and the advanced knockout tower of trichlorosilane to isolate the trichlorosilane containing partial impurities, enter again the process that recovery tower is further purified, the operation steps that has reduced separated 2 towers and recovery tower, has reduced equipment cost; Meanwhile, also reduced the processing load of the equipment such as knockout tower and processed heat, having reduced purification energy consumption and further reduced production cost, the treatment capacity of knockout tower lowers, and can reduce the specification of purification tower and corresponding support equipment, has reduced equipment cost.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present invention or example in conjunction with specific features, structure, material or the feature of this embodiment or example description.In this manual, the schematic statement of above-mentioned term is not necessarily referred to identical embodiment or example.And the specific features of description, structure, material or feature can be with suitable mode combinations in any one or more embodiment or example.
Although illustrated and described embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention in the situation that not departing from principle of the present invention and aim, modification, replacement and modification.
Claims (5)
1. purify from the dry back rewinding method of dichloro-dihydro silicon, is characterized in that, comprises the following steps:
A) the reduction tail gas in production of polysilicon technique is reclaimed and obtains dry back rewinding through dry method, dry back rewinding is sent in the first dry method rectifying tower and carried out rectifying, overhead extraction the first low-boiling-point substance from described the first dry method rectifying tower, in described the first low-boiling-point substance, contain dichloro-dihydro silicon and boron-containing impurities, and discharge middle chlorosilane at the bottom of the tower of described the first dry method rectifying tower;
B) described the first low-boiling-point substance is passed into knockout tower and carry out separation, with the tower top from described knockout tower, gather boron-containing impurities and gather dichloro-dihydro silicon at the bottom of tower;
C) chlorosilane in the middle of described is sent in the second dry method rectifying tower and carried out rectifying, from the tower top of described the second dry method rectifying tower, gather the second low-boiling-point substance, in described the second low-boiling-point substance, contain dichloro-dihydro silicon and trichlorosilane, at the bottom of the tower of described the second dry method rectifying tower, discharge silicon tetrachloride
The treatment capacity of described the first dry method rectifying tower is 15m
3/ h is 0.1～0.5m in the picking rate of the first low-boiling-point substance described in described step a)
3/ h, and be 0.1～0.5m in the input speed of the first low-boiling-point substance described in described step b)
3/ h,
In described step b), the picking rate of described dichloro-dihydro silicon is 0.1～0.45m
3/ h,
In described step c), the picking rate of described the second low-boiling-point substance is 5.5～7m
3/ h.
2. the method for the dichloro-dihydro silicon of purifying from dry back rewinding according to claim 1, is characterized in that, also comprises:
D) described the second low-boiling-point substance is directly sent into reduction furnace, with the trichlorosilane reducing wherein.
3. the method for the dichloro-dihydro silicon of purifying from dry back rewinding according to claim 2, is characterized in that, also comprises:
E) described silicon tetrachloride is sent into hydrogenation system and carry out hydrogenation.
4. the method for the dichloro-dihydro silicon of purifying from dry back rewinding according to claim 1, is characterized in that, content >=90% of dichloro-dihydro silicon in described the first low-boiling-point substance.
5. the method for the dichloro-dihydro silicon of purifying from dry back rewinding according to claim 1, is characterized in that, in described step b), contains mass percent and be 2～10% dichloro-dihydro silicon in described the second low-boiling-point substance.
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| CN104928761B (en) * | 2014-03-19 | 2018-02-23 | 新特能源股份有限公司 | A kind of preparation method of silicon chip foundry alloy |
| CN106276912B (en) * | 2015-05-27 | 2018-11-06 | 内蒙古盾安光伏科技有限公司 | polysilicon production process |
| CN113247908B (en) * | 2021-06-21 | 2023-05-05 | 北京泽华化学工程有限公司 | Separation method and separation device for chlorosilane in polysilicon production |
| CN116495741B (en) * | 2023-05-31 | 2024-06-18 | 宁夏润阳硅材料科技有限公司 | Method and system for recycling polysilicon production associated disilicide raw materials |
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| CN101357286A (en) * | 2007-07-31 | 2009-02-04 | 中国恩菲工程技术有限公司 | Method for recovering dichloro-dihydro silicon from off-gas generated from the production of polycrystalline silicon |
| US20090057129A1 (en) * | 2007-09-05 | 2009-03-05 | Shin-Etsu Chemical Co., Ltd. | Method for producing trichlorosilane and method for producing polycrystalline silicon |
| CN102107876A (en) * | 2011-03-23 | 2011-06-29 | 重庆大全新能源有限公司 | Method for rectifying trichlorosilane, silicon tetrachloride and dichlorosilane and device thereof |
| CN202246098U (en) * | 2011-08-23 | 2012-05-30 | 内蒙古盾安光伏科技有限公司 | Trichlorosilane synthesizing equipment |
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| US20120082609A1 (en) * | 2010-10-01 | 2012-04-05 | Mitsubishi Materials Corporation | Method for producing trichlorosilane with reduced boron compound impurities |
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|---|---|---|---|---|
| CN101357286A (en) * | 2007-07-31 | 2009-02-04 | 中国恩菲工程技术有限公司 | Method for recovering dichloro-dihydro silicon from off-gas generated from the production of polycrystalline silicon |
| US20090057129A1 (en) * | 2007-09-05 | 2009-03-05 | Shin-Etsu Chemical Co., Ltd. | Method for producing trichlorosilane and method for producing polycrystalline silicon |
| CN102107876A (en) * | 2011-03-23 | 2011-06-29 | 重庆大全新能源有限公司 | Method for rectifying trichlorosilane, silicon tetrachloride and dichlorosilane and device thereof |
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