CN103950938B - Chlorosilane purification system - Google Patents
Chlorosilane purification system Download PDFInfo
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- CN103950938B CN103950938B CN201410127032.8A CN201410127032A CN103950938B CN 103950938 B CN103950938 B CN 103950938B CN 201410127032 A CN201410127032 A CN 201410127032A CN 103950938 B CN103950938 B CN 103950938B
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Abstract
The invention discloses chlorosilane purification system, comprising: the first to the 5th rectifying tower, each rectifying tower in the first to the 5th rectifying tower all has the opening for feed be positioned on this rectifying tower, air outlet, liquid outlet, fluid inlet and inlet mouth; First to the 5th reboiler, each in the first to the 5th reboiler all has the fluid inlet be positioned on this reboiler, air outlet, steam inlet and condensate outlet; First to the 5th reflux pump; A condenser.Compared with simple coupling rectification technique, in chlorosilane purification system of the present invention, the continuous coupled energy-saving effect of five towers is more obvious, and energy consumption reduces by 80%, solves the problem of purification process high energy consumption in polysilicon system, and then reduces production cost.
Description
Technical field
The present invention relates to field polysilicon, specifically, the present invention relates to chlorosilane purification system.
Background technology
Polysilicon is a kind of ultra-pure material, for unicircuit, electron device and solar cell, is the foundation stone of information and New Energy Industry, and being the strategic material that country encourages to first develop, is also the Product and industry of state key encourage growth.2012, instead to affect by global economic crisis and European Union are two, how the continued downturn of polysilicon market, reduced production of polysilicon cost, how to enhance the core competitiveness of enterprises, and becomes the top priority of the long-term sustainable development of each polysilicon enterprise.
The main production process of current domestic polysilicon is improved Siemens, mainly comprises trichlorosilane synthesis, rectification and purification, reduction, the recovery of reduction tail gas dry process and hydrogenation five operations.Rectification and purification provides high pure raw material for reduction operation, is the important procedure of polysilicon system.The ultra-high purity of polysilicon requires that the foreign matter content of refined product reaches ppta rank (10
-12), purity reaches 9 " 9 ", and inevitable requirement high reflux ratio and high number of theoretical plate, must need relatively high heat exhaustion, the energy consumption of purification process is one of main energy consumption of polysilicon system, and the energy consumption therefore reducing purification process is one of most effective way reducing polysilicon cost.
But the system at present for chlorine purification silane need further improvement.
Summary of the invention
The present invention is intended to one of solve the problems of the technologies described above at least to a certain extent.For this reason, one object of the present invention is to propose a kind of chlorosilane purification system, this system can reach expands as 5 towers by the quantity of coupled by 2 or 3 towers, realize the continuous coupled energy-saving effect of five towers thus more obvious, energy consumption reduces by 80%, solve the problem of purification process high energy consumption in polysilicon system, reduce enterprise's production cost, enhance the core competitiveness of enterprises.
According to an aspect of the present invention, the present invention proposes a kind of chlorosilane purification system, comprising:
First to the 5th rectifying tower, each rectifying tower in the described first to the 5th rectifying tower all has the opening for feed be positioned on this rectifying tower, air outlet, liquid outlet, fluid inlet and inlet mouth;
First to the 5th reboiler, each in the described first to the 5th reboiler all has the fluid inlet be positioned on this reboiler, air outlet, steam inlet and condensate outlet,
First to the 5th reflux pump, each pump in the described first to the 5th reflux pump all has pump inlet and pump discharge;
First to the 5th return tank, each return tank in the described first to the 5th return tank all has and is positioned at tank import on this first to the 5th return tank and tank outlet;
A condenser, a described condenser has inlet mouth, liquid outlet, low-temperature receiver import and low-temperature receiver outlet;
Wherein,
The air outlet of described first rectifying tower is connected with the inlet mouth of described condenser, the liquid outlet of described condenser is connected with the tank import of described first return tank, the tank outlet of described first return tank is connected with the pump inlet of described first reflux pump, the pump discharge of described first reflux pump is connected with the fluid inlet of described first rectifying tower, a part of chlorosilane condensate liquid is back to described first rectifying tower; The fluid inlet of the described first to the 5th reboiler is connected with the liquid outlet of the described first to the 5th rectifying tower successively respectively, boils to heat a part for liquid at the bottom of chlorosilane tower again; The air outlet of the described first to the 5th reboiler is connected with the inlet mouth of the described first to the 5th rectifying tower; The air outlet of the described second to the 5th rectifying tower is connected with the steam inlet of described first to fourth reboiler successively respectively, the condensate outlet of described first to fourth reboiler is connected with the tank import of described the second to five return tank successively respectively, the tank outlet of described the second to five return tank is connected with the pump inlet of the described second to the 5th reflux pump successively respectively, the pump discharge of the described second to the 5th reflux pump is connected with the fluid inlet of the described second to the 5th rectifying tower successively respectively, a part for chlorosilane condensate liquid to be back to the described second to the 5th rectifying tower;
Wherein, the low-temperature receiver import of described condenser is connected with low-temperature receiver; The steam inlet of described 5th reboiler is connected with thermal source.
The above embodiment of the present invention chlorosilane purification system is compared with simple coupling rectification technique, the continuous coupled energy-saving effect of five towers is more obvious, and energy consumption reduces by 80%, solves the problem of purification process high energy consumption in polysilicon system, reduce enterprise's production cost, enhance the core competitiveness of enterprises.
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become obvious and easy understand from accompanying drawing below combining to the description of embodiment, wherein:
Fig. 1 is the structural representation of chlorosilane purification system according to an embodiment of the invention.
Fig. 2 is the structural representation of chlorosilane purification system in accordance with another embodiment of the present invention.
Fig. 3 is the structural representation of the chlorosilane purification system according to another embodiment of the present invention.
Fig. 4 is the structural representation of the chlorosilane purification system according to another embodiment of the present invention.
Embodiment
Be described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the present invention, and can not limitation of the present invention be interpreted as.
In describing the invention, it will be appreciated that, term " " center ", " longitudinal direction ", " transverse direction ", " length ", " width ", " thickness ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end " " interior ", " outward ", " clockwise ", orientation or the position relationship of the instruction such as " counterclockwise " are based on orientation shown in the drawings or position relationship, only the present invention for convenience of description and simplified characterization, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore limitation of the present invention can not be interpreted as.
In addition, term " first ", " second " only for describing object, and can not be interpreted as instruction or hint relative importance or imply the quantity indicating indicated technical characteristic.Thus, be limited with " first ", the feature of " second " can express or impliedly comprise one or more these features.In describing the invention, the implication of " multiple " is two or more, unless otherwise expressly limited specifically.
In the present invention, unless otherwise clearly defined and limited, the term such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or connect integratedly; Can be mechanical connection, also can be electrical connection; Can be directly be connected, also indirectly can be connected by intermediary, can be the connection of two element internals.For the ordinary skill in the art, above-mentioned term concrete meaning in the present invention can be understood as the case may be.
In the present invention, unless otherwise clearly defined and limited, fisrt feature second feature it " on " or D score can comprise the first and second features and directly contact, also can comprise the first and second features and not be directly contact but by the other characterisation contact between them.And, fisrt feature second feature " on ", " top " and " above " comprise fisrt feature directly over second feature and oblique upper, or only represent that fisrt feature level height is higher than second feature.Fisrt feature second feature " under ", " below " and " below " comprise fisrt feature immediately below second feature and tiltedly below, or only represent that fisrt feature level height is less than second feature.
Though some tower group of current rectification and purification has adopted differential pressure heat to be coupled, reduce energy consumption, all adopt two towers or three-tower differential pressure thermal coupling, coupled limited amount.When designing, for ensureing that tower also can normally be produced when fluctuation appears in the fluctuation of tower pressure or heat exchange inventory, two material temperature difference of coupled and heat-exchange are generally 15 ~ 30 DEG C in the past; In tower, tower top tower base pressure difference is comparatively large simultaneously, and get 0.05 ~ 0.3MPa during design, this all limits differential pressure heat coupled quantity, therefore farthest can not reduce energy consumption.
For this reason, the present invention proposes a kind of chlorosilane purification system, five tower differential pressure heat couplings can be realized.The chlorosilane purification system of one embodiment of the invention is described in detail below with reference to Fig. 1-2.
Chlorosilane purification system as shown in Figure 1-2, comprising: the first rectifying tower is to the 5th rectifying tower (T1-T5); First to the 5th reboiler (E2-E6); First to the 5th reflux pump (P1-P5); A condenser E1.
Wherein, first to the 5th rectifying tower (T1-T5) has and is positioned at opening for feed (T11-T51) in the middle part of this rectifying tower, the air outlet (T12-T52), the liquid outlet (T13-T53) being positioned at this rectifier bottoms that are positioned at this rectifying tower top, is positioned at this rectifier fluid inlet (T14-T54), is positioned at this rectifying tower bottom inlet mouth (T15-T55).
First to the 5th reboiler (E2-E6), each in first to the 5th reboiler (E2-E6) all has and is positioned at fluid inlet (E21-E61) bottom this reboiler, the air outlet (E22-E62) that is positioned at this reboiler top, is positioned at the steam inlet (E23-E63) on this reboiler top and is positioned at the condensate outlet (E24-E64) of this reboiler bottom
First to the 5th reflux pump (P1-P5), each pump in the described first to the 5th reflux pump (P1-P5) all has pump inlet (P11-P51) and pump discharge (P12-P52);
First to the 5th return tank (V1-V5), each return tank in the described first to the 5th return tank (V1-V5) all has and is positioned at tank import (V11-V51) on this first to the 5th return tank and tank outlet (V12-V52);
A condenser E1, a described condenser E1 have inlet mouth E11, liquid outlet E12, low-temperature receiver import (not shown) and low-temperature receiver outlet (not shown).
According to a particular embodiment of the invention, as shown in Figure 1-2, the annexation of above-mentioned parts is:
The air outlet T12 of (1) first rectifying tower T1 is connected with the inlet mouth E11 of described condenser E1, the liquid outlet E12 of condenser E1 is connected with the import V11 of return tank V1, the outlet V12 of return tank V1 is connected with the pump inlet P11 of reflux pump P1, the pump discharge P12 of the first reflux pump P1 is connected with the fluid inlet T14 of the first rectifying tower T1, a part of chlorosilane condensate liquid is back to the first rectifying tower T1, another chlorosilane condensate liquid is as light constituent extraction.
The fluid inlet (E21-E61) of (2) first to the 5th reboilers (E2-E6) is connected with the liquid outlet of the first to the 5th rectifying tower (T13-T53), boil to heat a part for liquid at the bottom of chlorosilane tower, another portion can as the feeding liquid of other rectifying tower or as heavy component extraction again; The air outlet (E22-E62) of the first to the 5th reboiler is connected with the inlet mouth (T15-T55) of the first to the 5th rectifying tower.
The air outlet (T22-T52) of (3) second to the 5th rectifying tower (T2-T5) is connected with the steam inlet (E23-E53) of first to fourth reboiler (E2-E5), the condensate outlet (E24-E54) of first to fourth reboiler (E2-E5) be connected with the tank import (V21-V51) of the second to five return tank (V2-V5) respectively successively, tank outlet (V22-V52) of the second to five return tank is connected with the pump inlet (P21-P51) of the second to the 5th reflux pump (P2-P5) successively respectively; The pump discharge of the second to the 5th reflux pump (P2-P5) is connected with the fluid inlet (T24-T54) of the second to the 5th rectifying tower (T2-T5), a part for chlorosilane condensate liquid to be back to the second to the 5th rectifying tower, another part chlorosilane condensate liquid can be delivered to the 3rd to the 5th rectifying tower (T3-T5) as feeding liquid or as light constituent extraction.
According to a particular embodiment of the invention, the low-temperature receiver import (not shown) of condenser E1 is connected with low-temperature receiver; The steam inlet E63 of the 5th reboiler E6 is connected with thermal source.
The chlorosilane purification system of the above embodiment of the present invention is compared with simple coupling rectification technique, the continuous coupled energy-saving effect of five towers is more obvious, and energy consumption reduces by 80%, solves the problem of purification process high energy consumption in polysilicon system, reduce enterprise's production cost, enhance the core competitiveness of enterprises.
According to a particular embodiment of the invention, the temperature of the low-temperature receiver be connected with the low-temperature receiver import (not shown) of condenser E1 can be 32 ~ 42 degrees Celsius.Low-temperature receiver particular type is also not particularly limited, such as, can be the recirculated water of 32 ~ 42 degrees Celsius.The temperature of the thermal source be connected with the steam inlet E63 of the 5th reboiler E6 can be 150 degrees Celsius.The chlorosilane purification system of the above embodiment of the present invention only needs for condenser E1 and the 5th reboiler E6 two devices provide low-temperature receiver and thermal source thus, and is mutually made full use of by internal system cold and heat.Chlorosilane purification system according to the abovementioned embodiments of the present invention, can make full use of heat coupling, save the auxiliary condenser of the second to the 5th rectifying tower, and then save considerably energy consumption.
According to a particular embodiment of the invention, first to the 5th rectifying tower (T1-T5) and condenser (E1), the first to the 5th reboiler (E2-E6), the first to five return tank (V1-V5), the first to the 5th reflux pump (P2-P5) adopt the mode of connection of above-described embodiment, and it is 8 degrees Celsius that the tower reactor of rectifying tower at different levels can be made to be down to minimum with the mean temperature difference of the next stage rectifying tower tower top be coupled with it.Be specially, the tower reactor of the first rectifying tower and the tower top temperature difference of Second distillation column are 8-12 degree Celsius, the tower reactor of described Second distillation column and the tower top temperature difference of the 3rd rectifying tower are 8-12 degree Celsius, the tower reactor of described 3rd rectifying tower and the tower top temperature difference of the 4th rectifying tower are 8-12 degree Celsius, and the tower reactor of described 4th rectifying tower and the tower top temperature difference of the 5th rectifying tower are 8-12 degree Celsius.Thus by adopting the mode of connection of the above embodiment of the present invention, the temperature difference can be reduced to the quantitative limitation of pressure reduction thermal coupling tower number.Only the first rectifying tower and the 5th rectifying tower need be adopted respectively the high-temperature water of low-temperature receiver-recirculated water and thermal source-150 degrees Celsius simultaneously, pressure reduction thermal coupling tower quantity can be expanded to 5 towers by traditional 2 or 3 towers.Therefore, five towers only need have a tower to need low-temperature receiver, and a tower needs thermal source, low-temperature receiver, thermal source energy consumption can be reduced to 80% thus.
According to a particular embodiment of the invention, by adopting above-mentioned annexation, the tower top of same tower and tower base pressure difference minimumly can also be reduced to 0.01MPa, be specially, the tower top of first to the 5th and the pressure reduction at the bottom of tower can be 0.01 ~ 0.06MPa.According to a particular embodiment of the invention, the pressure in the first to the 5th rectifying tower can raise successively or reduce successively.
According to a particular embodiment of the invention, the annexation between the first to the 5th rectifying tower (T1-T5) divide into the first to the 5th opening for feed be connected in series, be connected in parallel or onrelevant connect.
Be specially, be connected in series and refer to that each rectifying tower connects according to following mode of connection:
The opening for feed of the first rectifying tower passes into the pending raw material of chlorosilane, the opening for feed of the second to the 5th rectifying tower is connected with the liquid outlet of first to fourth rectifying tower or the pump discharge of first to fourth reflux pump successively respectively, so that at least one of the de-light constituent of the pump discharge discharge of the de-heavy constituent of being discharged by the liquid outlet of first to fourth rectifying tower and first to fourth reflux pump is delivered to the second to the 5th rectifying tower.When adopting series system and tower pressure from low to high, except last step rectifying tower, the tower tower reactor extraction of de-function light arranges a column bottoms pump to during the charging of next stage rectifying tower.
The opening for feed being connected in parallel at least one rectifying tower referred in the first to the 5th rectifying tower is separately connected with same chlorosilane feedway.First to the 5th rectifying tower provides material by same chlorosilane feedway.
The opening for feed that onrelevant connects at least one rectifying tower referred in the first to the 5th rectifying tower is separately connected from different chlorosilane feedwaies, also can be understood as the chlorosilane source having two rectifying tower in five rectifying tower at least different, namely have at least two rectifying tower opening for feeds to be connected from different chlorosilane feedwaies.
Wherein, chlorosilane type can for be selected from the hydrogenation condensation material of hydrogenation process in polysilicon system, Dry recovery operation dry back rewinding, process the rectifying tower raw material of recovery tower raw material, further process hydrogenation condensation material and the recovery tower product of each group of low impurity that boils of tower height.
Below with reference to Fig. 3, chlorosilane purification system is according to an embodiment of the invention described, this chlorosilane purification system is with five tower continuous pressure difference thermal couplings, five tower tower pressures raise successively, five towers adopt series system, the function of tower be respectively de-light, de-light, de-heavy, de-heavy, de-be heavily example, the reflux entry ratio of 5 towers is 1 ~ 10.
Its particularly the structural representation of chlorosilane purification system and schema see Fig. 3.Operating process is: raw material S01 enters the first rectifying tower T1, overhead vapours S02 is through condenser E1 condensation, phlegma S03 enters return tank V1, phlegma S04 enters reflux pump P1, after pump, liquid is according to certain reflux ratio, a part returns the first rectifying tower T1 as phegma S05, and a part is as light constituent extraction S06; Produced Liquid S07 at the bottom of tower, according to certain ratio, a part enters reboiler E2, and after condensation reboiler is heat vaporized, gas S08 returns the first rectifying tower T1, and a part of Produced Liquid S09 enters Second distillation column T2 through column bottoms pump P6; The overhead vapours S11 of Second distillation column T2 enters the shell side heating medium inlet of reboiler E2, return tank V2 is entered through the condensed material S12 of reboiler, phlegma S13 enters reflux pump P2, after pump, liquid is according to certain reflux ratio, a part returns Second distillation column tower T2 as phegma S14, a part is as light constituent extraction S15, Produced Liquid S16 at the bottom of tower, according to certain ratio, a part enters reboiler E3, after reboiler is heat vaporized, gas S17 returns Second distillation column T2, and a part of Produced Liquid S18 enters the 3rd rectifying tower T3 through column bottoms pump P7; The overhead vapours S20 of the 3rd rectifying tower T3 enters the shell side heating medium inlet of reboiler E3, return tank V3 is entered through the condensed material S21 of reboiler, phlegma S22 enters reflux pump P3, after pump, liquid is according to certain reflux ratio, a part returns the 3rd rectifying tower T3 as phegma S23, a part enters the 4th rectifying tower T4 as extraction S24, Produced Liquid S25 at the bottom of tower, according to certain ratio, a part enters reboiler E4, after reboiler is heat vaporized, gas S26 returns the 3rd rectifying tower T3, and a part is as heavy constituent S27 extraction; The overhead vapours S28 of the 4th rectifying tower T4 enters the shell side heating medium inlet of reboiler E4, return tank V4 is entered through the condensed material S29 of condensation reboiler, phlegma S30 enters reflux pump P4, after pump, liquid is according to certain reflux ratio, a part returns the 4th rectifying tower T4 as phegma S31, a part enters the 5th rectifying tower T5 as product S32 extraction, Produced Liquid S33 at the bottom of tower, according to certain ratio, a part enters reboiler E5, after reboiler is heat vaporized, gas S34 returns the 4th rectifying tower T4, and a part is as heavy constituent S35 extraction; The overhead vapours S36 of the 5th rectifying tower T5 enters the shell side heating medium inlet of condensation reboiler E5, return tank V5 is entered through the condensed material S37 of condensation reboiler, phlegma S38 enters reflux pump P5, after pump, liquid is according to certain reflux ratio, a part returns the 5th rectifying tower T5 as phegma S39, a part is as product S40 extraction, Produced Liquid S41 at the bottom of tower, according to certain ratio, a part enters reboiler E6, after reboiler is heat vaporized, gas S42 returns the 5th rectifying tower T5, and a part is as heavy constituent S43 extraction.
Below with reference to Fig. 4, chlorosilane purification system is in accordance with another embodiment of the present invention described, this chlorosilane purification system is with five tower continuous pressure difference thermal couplings, five tower tower pressures reduce successively (be first rectifying tower with the tower that pressure is minimum), five towers adopt series system, the function of tower be respectively de-light, de-light, de-heavy, de-heavy, de-be heavily example, the reflux entry ratio of 5 towers is 1 ~ 10.
The difference of Fig. 4 and Fig. 3: for the tower of de-function light, when tower reactor extraction is to the charging of next stage rectifying tower, when five tower tower pressures raise successively, needs column bottoms pump; When five tower tower pressures reduce successively, pressure reduction charging can be utilized, without the need to arranging column bottoms pump, reduce facility investment and power consumption, simultaneously because materials at bottom of tower mostly is saturated liquid, easily causing pump cavitation or damage, increase the stability of system.
According to embodiments of the invention, it is suitable with the thermal load needed for the first tower bottom of rectifying tower vaporizing liquid that Second distillation column overhead vapours is condensed to the refrigeration duty needed for supercooled state; Refrigeration duty needed for 3rd rectifying tower tower top vapor condensation to supercooled state is suitable with the thermal load needed for Second distillation column tower reactor vaporizing liquid; Refrigeration duty needed for 4th rectifying tower tower top vapor condensation to supercooled state is suitable with the thermal load needed for the 3rd tower bottom of rectifying tower vaporizing liquid; Refrigeration duty needed for 5th rectifying tower tower top vapor condensation to supercooled state is suitable with the thermal load needed for the 4th tower bottom of rectifying tower vaporizing liquid.First rectifying tower, Second distillation column, the 3rd rectifying tower, the 4th tower bottom of rectifying tower are without the need to external heat source, and thermal source load reduces by 80%.Second distillation column, the 3rd rectifying tower, the 4th rectifying tower and the 5th rectifying tower overhead vapours total condensation or excessively cold after the condensation of condensation reboiler.Second distillation column, the 3rd rectifying tower, the 4th rectifying tower, the 5th rectifying tower tower top vapor condensation are without the need to additional low-temperature receiver, and cold source load reduces by 80%.
According to embodiments of the invention, Second distillation column, the 3rd rectifying tower, the 4th rectifying tower and the 5th rectifying tower overhead vapours total condensation or excessively cold after the condensation of condensation reboiler, without the need to auxiliary condenser, reduce facility investment, reduce Equipments Setting and pipeline flowing difficulty, expand the use range of differential pressure heat coupled, especially for the tower group of transformation project.
First rectifying tower and the 5th Rectification column pressure and temperature setting, the first rectifying tower tower top temperature is greater than 50 DEG C, ensures that the first rectifying tower is using the recirculated water of cheapness (32 ~ 42 DEG C) as condenser low-temperature receiver; When with high-temperature water (130 ~ 150 DEG C) for reboiler thermal source time, the 5th tower bottom of rectifying tower temperature is less than 120 DEG C; Ensure the thermal source of heat-eliminating medium high-temperature water as rectifying tower of polycrystalline reduction operation, realize the exchange of purification process and reduction operation cooling and heating load, farthest reduce energy consumption.For certain component, the temperature of saturation of material and pressure one_to_one corresponding, then, after the first rectifying tower tower top temperature and the 5th tower bottom of rectifying tower temperature are determined, pressure is determined thereupon.The tower top tower bottom pressure difference range of rectifying tower at different levels is 0.01 ~ 0.06MPa, and the tower reactor of rectifying tower at different levels, the mean temperature difference of both next stage rectifying tower tower tops be coupled with it are 8 ~ 12 DEG C.The tower top tower reactor pressure and temperature of each tower is determined all thus.
The Trichlorosilane purification system of the above embodiment of the present invention reduces the temperature difference of coupled and heat-exchange two material, thus the quantity of differential pressure heat coupled is expanded as 5 towers by 2 or 3 towers, realizes five tower continuous pressure difference thermal couplings.Five tower continuous pressure difference thermal couplings comprise the first rectifying tower, Second distillation column, the 3rd rectifying tower, the 4th rectifying tower and the 5th rectifying tower, the pressure of five towers from low to high or from high to low, can series, parallel or onrelevant tower between tower, at the first rectifying tower tower top, condenser is set, and a condensation reboiler is respectively set between the first rectifying tower and Second distillation column, between Second distillation column and the 3rd rectifying tower, between the 3rd rectifying tower and the 4th rectifying tower, between the 4th rectifying tower and the 5th rectifying tower, the 5th rectifying tower arranges conventional reboiler.According to material feature and product requirement, each tower has dual-use function, and can take off and gently can take off again heavily, production process can adjust the function of each tower in real time.Because in chlorosilane purification, foreign matter content is less, are all trichlorosilanes of more than 95%, the changing function of Gu Ta is tower-coupled substantially without impact on five.Compared with simple coupling rectification technique, the continuous coupled energy-saving effect of five tower of the present invention is more obvious, and energy consumption reduces by 80%, solves the problem of purification process high energy consumption in polysilicon system, reduces enterprise's production cost, enhances the core competitiveness of enterprises.
According to a particular embodiment of the invention, the chlorosilane purification system of the embodiment of the present invention, its low-temperature receiver adopts cheap recirculated water (temperature is 32 degree ~ 42 degree).Thermal source adopts high-temperature-hot-water (150 ~ 130 degree), and this high-temperature-hot-water is reduce the low-temperature receiver of operation in polysilicon system.High-temperature water reduces in operation as low-temperature receiver in polysilicon system, after reduction operation, high-temperature water is elevated to 150 degree by 130 degree, and rectifying tower of the present invention just in time adopts reduction operation 150 degree of high-temperature water out as thermal source, after purifying, high-temperature water reduces to again 130 degree, and former operation of returning again is as low-temperature receiver.Thus, heat Appropriate application is accomplished to whole polysilicon system.
The chlorosilane purification system of the above embodiment of the present invention achieves 5 tower continuous pressure difference thermal couplings, wherein, only has the first rectifying tower to need low-temperature receiver and the 5th rectifying tower to need thermal source, thus can energy-conservation 80%.
In addition, in existing more chlorosilane purification system, do not mate with liquid heat at the bottom of the tower of upper level to prevent next stage overhead gas, prevent overhead gas from can not total condensation be liquid after condensation reboiler, therefore add auxiliary condenser, further condensation overhead gas, and the present invention finds rectifying tower overhead vapours total condensation or excessively cold after the condensation of condensation reboiler, auxiliary condenser can be cancelled, reduce Equipments Setting and pipeline flowing difficulty, expand the use range of differential pressure heat coupled.
Compared with prior art, the chlorosilane purification system of the embodiment of the present invention has the following advantages:
(1) only have the first rectifying tower to arrange a conventional condenser and need low-temperature receiver, only having the 5th rectifying tower to arrange a conventional reboiler needs thermal source, and all the other rectifying tower all do not need low-temperature receiver and thermal source.
(2) tower reactor of rectifying tower at different levels, the mean temperature difference of both next stage rectifying tower tower tops that is coupled with it are reduced to 8 ~ 12 DEG C, the tower top of same tower and tower base pressure difference are minimumly reduced to 0.01 ~ 0.06MPa, reduce the temperature difference to the quantitative limitation of differential pressure heat coupled number.When guarantee first rectifying tower and last step rectifying tower are Cooling and Heat Source with recirculated water, high-temperature water respectively, the quantity of differential pressure heat coupled is expanded as 5 towers by 2 or 3 towers.
(3) except the first rectifying tower, the refrigeration duty needed for rectifying tower tower top vapor condensation to supercooled state at different levels is suitable with the thermal load needed for previous stage tower bottom of rectifying tower vaporizing liquid, realizes five tower continuous pressure difference thermal couplings, coupling heat exchange.The cooling and heating load of five tower continuous pressure difference thermal couplings reduces by 80%, and recirculated water, high-temperature water consumption reduce by 80%, realize the lowest energy consumption of whole rectifying and purifying system.The thermal source of the 5th rectifying tower adopts the heat-eliminating medium high-temperature water of reduction operation, realizes the exchange of purification process and reduction operation cooling and heating load, at utmost reduces polysilicon cost.
(4) each tower has dual-use function, and can take off and gently can take off again heavily, production process can adjust the function of each tower in real time.
(5) five tower relations can be columns in seriess, also can be towers in parallel, also can be the differential pressure heat couplings between uncorrelated tower, eliminate the restriction of classical tandem tower differential pressure heat coupling, expand the use range of differential pressure heat coupling.
(6) rectifying tower overhead vapours total condensation or excessively cold after the condensation of condensation reboiler, auxiliary condenser can be cancelled, and reduces Equipments Setting and pipeline flowing difficulty, expands the use range of differential pressure heat coupled, especially for the tower group of transformation project.
When (7) five towers adopt series systems and pressure to reduce gradually, the tower tower reactor extraction of de-function light can utilize pressure reduction charging to during the charging of next stage rectifying tower, without the need to arranging column bottoms pump, reduce facility investment and power consumption, simultaneously because materials at bottom of tower mostly is saturated liquid, easily cause pump cavitation or damage, increase the stability of system.
The purification system of the chlorosilane of the embodiment of the present invention has five tower structures of continuous pressure reduction coupling, the pressure that can control five towers from low to high or from high to low, and according to material feature and product requirement, each tower has dual-use function, can take off and gently can take off again heavily, production process can adjust the function of each tower in real time.Utilize the chlorosilane purification system chlorine purification silane of the embodiment of the present invention thus compared with simple coupling rectification technique, energy-saving effect is more obvious, and energy consumption can reduce by 80%, solves the high energy consumption problem of chlorine purification silane process, reduce enterprise's production cost thus, enhance the core competitiveness of enterprises.
According to a particular embodiment of the invention, usual polysilicon system has following tower group: the hydrogenation topping still of process hydrogenation process hydrogenation condensation material, the dry method rectifying tower processing the rewinding of dry method dry back, the recovery tower processing the low impurity that boils of all types of tower height, process hydrogenation slightly heat up in a steamer the rectifying tower of product and recovery tower product, and chlorosilane can be some tower chargings of any one tower group.
According to a particular embodiment of the invention, the source of above-mentioned chlorosilane to be purified and type are also not particularly limited, such as can for be selected from above-described embodiment polysilicon system in the hydrogenation condensation material of hydrogenation process, Dry recovery operation dry back rewinding, process the rectifying tower raw material of recovery tower raw material, further process hydrogenation condensation material and the recovery tower product of each group of low impurity that boils of tower height.The purification system suitability widely of chlorosilane can be improved thus further.
Below with reference to specific embodiment, present invention is described, it should be noted that, these embodiments are only descriptive, and do not limit the present invention in any way.
Embodiment 1
The same Fig. 3 of technical process, tower inlet amount is 20m
3/ h, feed composition is: trichlorosilane mass content is 98%, and silicon tetrachloride and dichlorosilane are the metallic impurity such as 1%, B, P, Fe trace.
First raw material enters the first rectifying tower T1, and material flow is from the first rectifying tower T1 to the 5th rectifying tower T5, and wherein the first rectifying tower T1 raises successively to the 5th rectifying tower T5 pressure.
The tower top pressure of the first rectifying tower and temperature are respectively 0.25MPa(absolute pressure) and 54.9 DEG C, ensure that the tower top low-temperature receiver of the first rectifying tower (tower that namely pressure is minimum) is recirculated water; The bottom temperature of the 5th rectifying tower should lower than 120 DEG C, and ensure that the tower reactor thermal source of the 5th rectifying tower is high-temperature water, the tower top tower base pressure difference of each tower is according to 0.02MPa simultaneously, and the coupling temperature difference is according to 10 DEG C, and the tower top tower sill strip part of each tower is in table 1.
The tower top tower bottom pressure temperature of each rectifying tower of table 1.
| Title | Tower top pressure MPa | Tower top temperature DEG C | Tower reactor pressure MPa | Bottom temperature DEG C |
| First rectifying tower | 0.25 | 54.9 | 0.27 | 63.6 |
| Second distillation column | 0.35 | 73 | 0.37 | 76.4 |
| 3rd rectifying tower | 0.5 | 87.3 | 0.52 | 88.9 |
| 4th rectifying tower | 0.65 | 98.5 | 0.67 | 99.9 |
| 5th rectifying tower | 0.85 | 110.9 | 0.87 | 112 |
Ensure that the refrigeration duty needed for rectifying tower tower top vapor condensation to supercooled state at different levels is suitable with the thermal load needed for previous stage tower bottom of rectifying tower vaporizing liquid by adjustment reflux ratio, the first rectifying tower overhead condenser is only had to need low-temperature receiver, the tower reactor reboiler of the 5th rectifying tower needs thermal source, between first rectifying tower and Second distillation column, between Second distillation column and the 3rd rectifying tower, between 3rd rectifying tower and the 4th rectifying tower, a condensation reboiler is respectively set between the 4th rectifying tower and the 5th rectifying tower, do not need thermal source, and Second distillation column, 3rd rectifying tower, 4th rectifying tower, the auxiliary condenser of the 5th rectifying tower can be cancelled according to research above, therefore also do not need low-temperature receiver, therefore five towers only have a tower to need low-temperature receiver, a tower needs thermal source, low-temperature receiver and thermal source energy consumption reduce by 80%.
After said process, refined product meets the requirement that electronic-grade polycrystalline silicon is produced.
Embodiment 2
The same Fig. 4 of technical process, tower inlet amount is 20m
3/ h, feed composition is: trichlorosilane mass content is 98%, and silicon tetrachloride and dichlorosilane are the metallic impurity such as 0.1%, B, P, Fe trace.
First raw material enters the 5th rectifying tower T5, and material flow is from the 5th rectifying tower T5 to the first rectifying tower T1, and wherein the 5th rectifying tower T5 to the first rectifying tower T1 pressure reduces successively.
The tower top pressure of the first rectifying tower and temperature are respectively 0.25MPa(absolute pressure) and 54.9 DEG C, ensure that the tower top low-temperature receiver of the first rectifying tower (tower that namely pressure is minimum) is recirculated water; The bottom temperature of the 5th rectifying tower should lower than 120 DEG C, and ensure that the tower reactor thermal source of the 5th rectifying tower is high-temperature water, the tower top tower base pressure difference of each tower is according to 0.02MPa simultaneously, and the coupling temperature difference is according to 10 DEG C, and the tower top tower sill strip part of each tower is in table 2.
The tower top tower bottom pressure temperature of each rectifying tower of table 2.
| Title | Tower top pressure MPa | Tower top temperature DEG C | Tower reactor pressure MPa | Bottom temperature DEG C |
| 5th rectifying tower | 0.85 | 110.9 | 0.87 | 112 |
| 4th rectifying tower | 0.65 | 98.5 | 0.67 | 99.9 |
| 3rd rectifying tower | 0.5 | 87.3 | 0.52 | 88.9 |
| Second distillation column | 0.35 | 73 | 0.37 | 76.4 |
| First rectifying tower | 0.25 | 54.9 | 0.27 | 63.6 |
Ensure that the refrigeration duty needed for rectifying tower tower top vapor condensation to supercooled state at different levels is suitable with the thermal load needed for previous stage tower bottom of rectifying tower vaporizing liquid by adjustment reflux ratio, the first rectifying tower overhead condenser is only had to need low-temperature receiver, the tower reactor reboiler of the 5th rectifying tower needs thermal source, between first rectifying tower and Second distillation column, between Second distillation column and the 3rd rectifying tower, between 3rd rectifying tower and the 4th rectifying tower, a condensation reboiler is respectively set between the 4th rectifying tower and the 5th rectifying tower, do not need thermal source, and Second distillation column, 3rd rectifying tower, 4th rectifying tower, the auxiliary condenser of the 5th rectifying tower can be cancelled according to research above, therefore also do not need low-temperature receiver, therefore five towers only have a tower to need low-temperature receiver, a tower needs thermal source, low-temperature receiver and thermal source energy consumption reduce by 80%.
After said process, refined product meets the requirement that electronic-grade polycrystalline silicon is produced.
In the description of this specification sheets, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present invention or example.In this manual, identical embodiment or example are not necessarily referred to the schematic representation of above-mentioned term.And the specific features of description, structure, material or feature can combine in an appropriate manner in any one or more embodiment or example.
Although illustrate and describe 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 when not departing from principle of the present invention and aim, revising, replacing and modification.
Claims (9)
1. a chlorosilane purification system, is characterized in that, comprising:
First to the 5th rectifying tower, each rectifying tower in the described first to the 5th rectifying tower all has the opening for feed be positioned on this rectifying tower, air outlet, liquid outlet, fluid inlet and inlet mouth;
First to the 5th reboiler, each in the described first to the 5th reboiler all has the fluid inlet be positioned on this reboiler, air outlet, steam inlet and condensate outlet;
First to the 5th reflux pump, each pump in the described first to the 5th reflux pump all has pump inlet and pump discharge;
First to the 5th return tank, each return tank in the described first to the 5th return tank all has and is positioned at tank import on this first to the 5th return tank and tank outlet;
A condenser, a described condenser has inlet mouth, liquid outlet, low-temperature receiver import and low-temperature receiver outlet;
Wherein,
The air outlet of described first rectifying tower is connected with the inlet mouth of described condenser, the liquid outlet of described condenser is connected with the tank import of described first return tank, the tank outlet of described first return tank is connected with the pump inlet of described first reflux pump, the pump discharge of described first reflux pump is connected with the fluid inlet of described first rectifying tower, a part of chlorosilane condensate liquid is back to described first rectifying tower;
The fluid inlet of the described first to the 5th reboiler is connected with the liquid outlet of the described first to the 5th rectifying tower successively respectively, boils to heat a part for liquid at the bottom of chlorosilane tower again; The air outlet of the described first to the 5th reboiler is connected with the inlet mouth of the described first to the 5th rectifying tower;
The air outlet of the described second to the 5th rectifying tower is connected with the steam inlet of described first to fourth reboiler successively respectively, the condensate outlet of described first to fourth reboiler is connected with the tank import of described the second to five return tank successively respectively, the tank outlet of described the second to five return tank is connected with the pump inlet of the described second to the 5th reflux pump successively respectively, the pump discharge of the described second to the 5th reflux pump is connected with the fluid inlet of the described second to the 5th rectifying tower successively respectively, a part for chlorosilane condensate liquid to be back to the described second to the 5th rectifying tower;
Wherein,
The low-temperature receiver import of described condenser is connected with low-temperature receiver;
The steam inlet of described 5th reboiler is connected with thermal source.
2. chlorosilane purification system according to claim 1, is characterized in that, the temperature of described low-temperature receiver is 32 ~ 42 degrees Celsius.
3. chlorosilane purification system according to claim 1, is characterized in that, described thermal source is the high-temperature water of 150 degrees Celsius, and described high-temperature water is utilize the waste heat of polycrystalline reduction operation to produce.
4. chlorosilane purification system according to claim 1, it is characterized in that, the tower reactor of described first rectifying tower and the tower top temperature difference of Second distillation column are 8-12 degree Celsius, the tower reactor of described Second distillation column and the tower top temperature difference of the 3rd rectifying tower are 8-12 degree Celsius, the tower reactor of described 3rd rectifying tower and the tower top temperature difference of the 4th rectifying tower are 8-12 degree Celsius, and the tower reactor of described 4th rectifying tower and the tower top temperature difference of the 5th rectifying tower are 8-12 degree Celsius.
5. chlorosilane purification system according to claim 1, is characterized in that, in the described first to the 5th rectifying tower, the tower top of each rectifying tower and the pressure reduction at the bottom of tower are 0.01 ~ 0.06MPa.
6. chlorosilane purification system according to claim 1, is characterized in that, the annexation between the described first to the 5th rectifying tower divide into the described first to the 5th opening for feed be connected in series, be connected in parallel or onrelevant connect.
7. chlorosilane purification system according to claim 1, it is characterized in that, the opening for feed of described first rectifying tower passes into the pending raw material of chlorosilane, and the opening for feed of the described second to the 5th rectifying tower is connected with the liquid outlet of first to fourth rectifying tower or the pump discharge of first to fourth reflux pump successively respectively.
8. chlorosilane purification system according to claim 7, is characterized in that, the mean pressure in the described first to the 5th rectifying tower raises successively.
9. chlorosilane purification system according to claim 1, is characterized in that, the opening for feed of at least one rectifying tower in the described first to the 5th rectifying tower is separately connected with chlorosilane feedway.
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| US5499506A (en) * | 1992-12-01 | 1996-03-19 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Ultra-high purity monosilane producing process and unit |
| CN203048612U (en) * | 2013-01-15 | 2013-07-10 | 昆明理工大学 | Trichlorosilane purifying device |
| CN103449448A (en) * | 2013-08-23 | 2013-12-18 | 中国恩菲工程技术有限公司 | Equipment for purifying trichlorosilane |
| CN203820469U (en) * | 2014-03-31 | 2014-09-10 | 中国恩菲工程技术有限公司 | Chlorosilane purification system |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5499506A (en) * | 1992-12-01 | 1996-03-19 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Ultra-high purity monosilane producing process and unit |
| CN203048612U (en) * | 2013-01-15 | 2013-07-10 | 昆明理工大学 | Trichlorosilane purifying device |
| CN103449448A (en) * | 2013-08-23 | 2013-12-18 | 中国恩菲工程技术有限公司 | Equipment for purifying trichlorosilane |
| CN203820469U (en) * | 2014-03-31 | 2014-09-10 | 中国恩菲工程技术有限公司 | Chlorosilane purification system |
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