CN206384848U - The system of heat cascade utilization during chlorosilane rectification and purification - Google Patents
The system of heat cascade utilization during chlorosilane rectification and purification Download PDFInfo
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- CN206384848U CN206384848U CN201620919654.9U CN201620919654U CN206384848U CN 206384848 U CN206384848 U CN 206384848U CN 201620919654 U CN201620919654 U CN 201620919654U CN 206384848 U CN206384848 U CN 206384848U
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Abstract
The utility model provides heat gradient utilization system during chlorosilane rectification and purification, and the system includes：High temperature rectifying column；The outlet of the high temperature rectifying column tower top is connected with the shell side inlet of the first reboiler, the tube-side inlet of first reboiler is connected with the outlet of low-temperature fractionating tower tower reactor, the tube side outlet of first reboiler is connected with low-temperature fractionating tower tower reactor entrance, the shell-side outlet of first reboiler is connected with the entrance of high temperature rectifying column aftercooler, the outlet of the high temperature rectifying column aftercooler is connected with the entrance of high temperature rectifying column reflux pump, and the outlet of the high temperature rectifying column reflux pump is connected with the entrance of the high temperature rectifying column.Herein described system is the gradient utilization system using each rectifying column tower top different brackets heat, based on heat cascade utilization between two towers, the heat cascade utilization between four towers between three towers is further increased, above-mentioned heat cascade utilization considerably reduces the consumption of distillation process heat and cold.
Description
Technical field
The utility model is related to technical field of rectification, more particularly to improved Siemens production solar-grade polysilicon process
Heat gradient utilization system during middle chlorosilane rectification and purification.
Background technology
Chlorosilane (English name：Chlorosilane), it is silane SiH4In hydrogen atom be substituted by a chlorine atom both after obtain
A series of materials, collectively referred to as chlorosilane；It is gas when chlorinty is low, is liquid when higher, colourless or yellow, formula is
HnSiCl4-n(n=0,1,2,3).Chlorosilane can carry out intense reaction with the compound containing active hydrogen, such as with water, alcohol, phenol, silicon
Alcohol, organic acid etc., release hydrogen chloride.Chlorosilane can be produced by silica flour with hydrogen chloride in 290~400 DEG C of reactions；Also can be by silicon
The mixture of powder, hydrogen and hydrogen chloride, in the presence of stannous chloride, is produced in 500 DEG C or so reactions.
Silicon source that chlorosilane is mainly used as in silicon epitaxial wafer production process and the raw material for preparing organochlorosilane.In addition, three
Chlorosilane (HSiCl3) it is the intermediate product for preparing solar level and electronic-grade polycrystalline silicon, after it is fractionated, it can obtain
The trichlorosilane of 99.9999999% (9 9) purity, then reacts with hydrogen under certain reaction condition and generates polysilicon；
Or by high-purity trichlorosilane by two-stage disproportionated reaction production high purity silane SiH4Gas, then by SiH4It is anti-that gas is passed through fluidisation
Answer and granular polysilicon (i.e. silane fluidized bed process) is cracked to form in device.
Because purity requirement of the production to raw chlorsilane of polysilicon is especially high, this is allowed in the purified of chlorosilane
Journey this step need to ask using high tray-number, big reflux ratio rectification process, it is necessary to consume substantial amounts of heat, cause polysilicon
Production cost remains high.
Utility model content
The technical problem that the utility model is solved is during providing chlorosilane rectification and purification that heat cascade utilization is
System, the system that the application is provided can reduce the consumption of heat and cold in chlorosilane distillation process.
In view of this, this application provides a kind of system of heat cascade utilization during chlorosilane rectification and purification, including：
High temperature rectifying column；The outlet of the high temperature rectifying column tower top is connected with the shell side inlet of the first reboiler, and described
The tube-side inlet of one reboiler is connected with the outlet of low-temperature fractionating tower tower reactor, the tube side outlet of first reboiler and cryogenic rectification
Tower tower reactor entrance is connected, and the shell-side outlet of first reboiler is connected with high temperature rectifying column aftercooler entrance, the high-temperature fine
The outlet for evaporating tower aftercooler is connected with high temperature rectifying column backflow pump intake, the high temperature rectifying column backflow pump discharge and the high temperature
Rectifying column inlet is connected；The high temperature rectifying column is silicon tetrachloride weight-removing column, and the low-temperature fractionating tower is trichlorosilane and dichloro
Dihydro silicon knockout tower, trichlorosilane weight-removing column or trichlorosilane lightness-removing column；The low-temperature fractionating tower and the high temperature rectifying tower
Kettle is provided with liquid outlet.
It is preferred that, described high temperature rectifying tower top is not less than 8 DEG C, the high temperature rectifying tower with low-temperature fractionating tower kettle temperature difference
Top heat is more than the 3~8% of low-temperature fractionating tower tower reactor institute calorific requirement.
It is preferred that, time high temperature rectifying column is also included in the system, the tube side of first reboiler is exported and described time
The entrance of high temperature rectifying column is connected, and the outlet of described high temperature rectifying column tower top is connected with the shell side inlet of the second reboiler, institute
The tube side outlet for stating the second reboiler is connected with the entrance of low-temperature fractionating tower, the shell-side outlet of second reboiler and described secondary
The entrance of high temperature rectifying column aftercooler is connected, the outlet of described high temperature rectifying column aftercooler and time high temperature rectifying column reflux pump
Entrance is connected, and the outlet of described high temperature rectifying column reflux pump is connected with the entrance of described high temperature rectifying column, the low temperature essence
The outlet for evaporating tower tower reactor is connected with the entrance of described high temperature rectifying column；Described high temperature rectifying be trichlorosilane weight-removing column or
Trichlorosilane lightness-removing column, the low-temperature fractionating tower tower reactor is provided with liquid outlet.
It is preferred that, described secondary high temperature rectifying column tower top is not less than 8 DEG C, described high-temperature fine with low-temperature fractionating tower kettle temperature difference
Evaporate column overhead heat is more than low-temperature fractionating tower tower reactor institute calorific requirement 3~8%.
It is preferred that, time low-temperature fractionating tower is also included in the system, the tube side of second reboiler is exported and described time
The entrance of low-temperature fractionating tower is connected, the outlet of described cryogenic rectification column overhead and the shell side inlet phase of the 3rd reboiler
Even, the tube side of the 3rd reboiler outlet is connected with the entrance of low-temperature fractionating tower, the shell-side outlet of the 3rd reboiler and
The entrance of described low-temperature fractionating tower aftercooler is connected, and the outlet of described low-temperature fractionating tower aftercooler is returned with time low-temperature fractionating tower
The entrance for flowing pump is connected, and the outlet of described low-temperature fractionating tower reflux pump is connected with the entrance of described low-temperature fractionating tower, described
The outlet of low-temperature fractionating tower tower reactor is connected with the entrance of described low-temperature fractionating tower；The outlet of described low-temperature fractionating tower tower reactor with
The entrance of described high temperature rectifying column is connected, and described cryogenic rectification is trichlorosilane lightness-removing column.
It is preferred that, described secondary cryogenic rectification tower top is not less than 8 DEG C, described low temperature essence with the low-temperature fractionating tower tower reactor temperature difference
Evaporate column overhead heat is more than low-temperature fractionating tower tower reactor institute calorific requirement 3~8%.
It is preferred that, the outlet of described low-temperature fractionating tower tower reactor is connected with the second reboiler tube-side inlet, and described second again
The outlet of boiling device tube side is connected with the entrance of described low-temperature fractionating tower, outlet and the 3rd reboiler of the low-temperature fractionating tower tower reactor
Tube-side inlet is connected, and the 3rd reboiler tube side outlet is connected with the entrance of the low-temperature fractionating tower.
It is preferred that, the outlet of the cryogenic rectification column overhead is connected with the entrance of low-temperature fractionating tower condenser, the low temperature
The outlet of rectifying column condenser is connected with the entrance of low-temperature fractionating tower reflux pump, the outlet of the low-temperature fractionating tower reflux pump and institute
The entrance for stating cryogenic rectification column overhead is connected；The outlet of the low-temperature fractionating tower tower reactor also with the first reboiler tube-side inlet
It is connected.
It is preferred that, the tube-side inlet exported also with the 4th reboiler of the high temperature tower bottom of rectifying tower is connected, and the described 4th
The outlet of reboiler tube side is connected with the entrance of the high temperature rectifying column.
It is preferred that, described high temperature rectifying column, secondary high temperature rectifying, secondary low-temperature fractionating tower and low-temperature fractionating tower is packed tower
Or plate column.
It is preferred that, the tube-side inlet exported also with the first reboiler bottom of described high temperature tower bottom of rectifying tower is connected, institute
The outlet of the tube side at the top of the first reboiler is stated with the entrance of described high temperature rectifying column to be connected；The low-temperature fractionating tower tower reactor goes out
Tube-side inlet of the mouth also with the second reboiler bottom is connected, tube side outlet and the cryogenic rectification at the top of second reboiler
The entrance of tower is connected.
It is preferred that, the outlet of described low-temperature fractionating tower tower reactor is connected with the tube-side inlet of the second reboiler bottom, described
Tube side outlet at the top of second reboiler is connected with the entrance of described low-temperature fractionating tower, the outlet of the low-temperature fractionating tower tower reactor
It is connected with the tube-side inlet of the 3rd reboiler bottom, tube side outlet and the low-temperature fractionating tower at the top of the 3rd reboiler
Entrance is connected.
This application provides the system of heat cascade utilization during chlorosilane rectification and purification, the system includes：High temperature
Rectifying column；The outlet of the high temperature rectifying column tower top is connected with the shell side inlet of the first reboiler, the pipe of first reboiler
Journey entrance is connected with the outlet of low-temperature fractionating tower tower reactor, tube side outlet and the low-temperature fractionating tower tower reactor entrance phase of first reboiler
Even, the shell-side outlet of first reboiler is connected with the entrance of high temperature rectifying column aftercooler, the high temperature rectifying column aftercooler
Outlet be connected with the entrance of high temperature rectifying column reflux pump, the outlet of the high temperature rectifying column reflux pump and the high temperature rectifying column
Entrance be connected；The high temperature rectifying column is silicon tetrachloride weight-removing column, and the low-temperature fractionating tower is trichlorosilane and dichloro-dihydro
Silicon knockout tower, trichlorosilane weight-removing column or trichlorosilane lightness-removing column；The low-temperature fractionating tower and the high temperature tower bottom of rectifying tower are equal
It is provided with liquid outlet.Herein described system is the gradient utilization system using different brackets heat, with the heat between two towers
Amount cascade utilization is base, further increases the heat cascade utilization between the heat cascade utilization between three towers and four towers, on
It is to be used as cryogenic rectification tower reactor reboiler thermal source, maximum limit by the use of high temperature rectifying column tower top steam to state three kinds of heat cascade utilizations
The step for realizing heat of degree is reused, and heat reuses number of times up to 3 times, greatly reduces the steam of distillation process
Consumption, steam consumption can reduce 40~75%, while the consumption of tower top recirculated water can be also greatly reduced.
Brief description of the drawings
Fig. 1 be the tower of the utility model two between rectification process system structural representation；
Fig. 2 be the tower of the utility model three between rectification process system structural representation；
Fig. 3 be the tower of the utility model four between rectification process system structural representation.
Embodiment
For a further understanding of the utility model, the utility model preferred embodiment is retouched with reference to embodiment
State, but it is to be understood that these descriptions are simply to further illustrate feature and advantage of the present utility model, rather than to this practicality
The limitation of new claim.
The system that the utility model embodiment discloses heat cascade utilization during a kind of chlorosilane rectification and purification, bag
Include：
High temperature rectifying column；The outlet of the high temperature rectifying column tower top is connected with the shell side inlet of the first reboiler, and described
The tube-side inlet of one reboiler is connected with the outlet of low-temperature fractionating tower tower reactor, the tube side outlet of first reboiler and cryogenic rectification
Tower tower reactor entrance is connected, and the shell-side outlet of first reboiler is connected with high temperature rectifying column aftercooler entrance, the high-temperature fine
The outlet for evaporating tower aftercooler is connected with high temperature rectifying column backflow pump intake, the high temperature rectifying column backflow pump discharge and the high temperature
Rectifying column inlet is connected；The high temperature rectifying column is silicon tetrachloride weight-removing column, and the low-temperature fractionating tower is trichlorosilane and dichloro
Dihydro silicon knockout tower, trichlorosilane weight-removing column or trichlorosilane lightness-removing column；The low-temperature fractionating tower and the high temperature rectifying tower
Kettle is provided with liquid outlet.
As shown in figure 1, Fig. 1 is the structural representation of the utility model chlorosilane rectifying and purifying system, wherein 1 is low temperature essence
Tower is evaporated, 2 be overhead condenser, and 3 be low-temperature fractionating tower reflux pump, and 4 be the first reboiler, and 5 be high temperature rectifying column, and 6 be high-temperature fine
Tower aftercooler is evaporated, 7 be high temperature rectifying column reflux pump, and 8 be the 4th reboiler.
According to system of the present utility model, low-temperature fractionating tower be first stage tower can be trichlorosilane/dichloro hydrogen silicon knockout tower,
Trichlorosilane lightness-removing column or trichlorosilane weight-removing column, high temperature rectifying column are that two grades of towers are silicon tetrachloride weight-removing column.
Based on heat cascade utilization of the application between low-temperature fractionating tower and high temperature rectifying column, wherein low-temperature fractionating tower
For first order tower, effect is substantial amounts of dichlorosilane in separation trichlorosilane, and high temperature rectifying column is second level tower, and effect is four
Silicon chloride weight-removing column.
Preferably, for effectively save energy, outlet and the low temperature essence of herein described cryogenic rectification column overhead
The entrance for evaporating tower condenser is connected, and the low-temperature fractionating tower condensator outlet is connected with the entrance of low-temperature fractionating tower reflux pump, institute
Low-temperature fractionating tower backflow pump discharge is stated with the cryogenic rectification column overhead entrance to be connected.Equally, the low-temperature fractionating tower tower reactor
Outlet is also connected with the first reboiler tube-side inlet, so that a low-temperature fractionating tower tower reactor liquid part is through the first reboiler quilt
Low-temperature fractionating tower is returned to after two grades of overhead vapours heating vaporizations to be separated again.Equally, the high temperature tower bottom of rectifying tower goes out
Mouth is also connected with the 4th reboiler tube-side inlet, the entrance phase of the 4th reboiler tube side outlet and the high temperature rectifying column
Even.
The application has also carried out the rectification and purification of chlorosilane using said system, comprises the following steps：
Silicon tetrachloride raw material take off and handled again, the silicon tetrachloride gas after separation is used as trichlorosilane and dichloro-dihydro
The thermal source of the mixture separation of silicon, after silicon tetrachloride gas is exchanged heat again, obtains gas-liquid mixture；
The gas-liquid mixture is condensed, after condensed liquid pressing, phegma and Produced Liquid is obtained；
Raw material trichlorosilane and the mixture of dichlorosilane are subjected to rectifying separation in the presence of above-mentioned thermal source, obtained
Trichlorosilane and dichlorosilane after separation.
As shown in figure 1, the method that the system being connected using above-mentioned two tower carries out chlorosilane rectification and purification is specially：
Raw material silicon tetrachloride (9) into two grades of towers (5) take off and handled again first, and reflux ratio is 1~5, the tower after separation
Silicon tetrachloride gas (10) is pushed up as the thermal source of first stage tower (1) reboiler (4), is changed into gas-liquid mixture (11) after heat exchange, then
Liquid all is condensed into two grades of tower aftercoolers (6), tower top is used as by two grades of tower reflux pumps (7) pressurization rear portions afterwards
Phegma (13), another part is used as overhead extraction liquid (14)；Tower reactor liquid (15) part is through reboiler (8) is by steam or leads
It is changed into steam (16) after deep fat heating and returns to two grades of towers (5), another part (17) is produced as tower reactor heavy constituent；Raw material trichlorine hydrogen
Silicon and the mixed thing (18) of dichlorosilane (1~10wt% of content) are then separated into first stage tower (1), reflux ratio 10~100,
Pressurizeed after tower top dichlorosilane (22) is condensed through overhead condenser (2) after separation by first stage tower reflux pump (3), a part of conduct
Overhead reflux liquid (24), another part is used as overhead extraction liquid (25)；Tower reactor trichlorosilane liquid (19) part is through reboiler
(4) first stage tower (1) is returned to after two grades of overhead vapours (10) heating vaporizations, another part removes next stage tower as tower reactor extraction.
According to the utility model, due in process of production in order to ensure first stage tower (1) stable operation, two grades of tower (5) towers
Top steam heat needs 3~8% more than low-temperature fractionating tower reboiler institute calorific requirement, and therefore, two grades of tower aftercoolers (6) must open
Open.
In the application, the operating pressure of first stage tower (1) is 0.3~0.9MPa, the operating pressures of two grades of towers (5) for 0.2~
0.8MPa；Two grades of tower (5) tower tops need to be not less than 8 DEG C with first stage tower (1) tower reactor temperature difference.
Preferably, time high temperature rectifying column is also included in the system of herein described chlorosilane rectification and purification, it is described
Secondary high temperature rectifying is trichlorosilane weight-removing column or trichlorosilane lightness-removing column；Described high temperature rectifying column is arranged at the low temperature essence
Evaporate between tower and the high temperature rectifying column, the heat step profit that the system containing the formation of secondary high temperature rectifying tower belongs between three towers
With the system preferably includes low-temperature fractionating tower i.e. first stage tower, and effect is substantial amounts of dichlorosilane in separation trichlorosilane, secondary
High temperature rectifying column is three-level tower, and effect is trichlorosilane weight-removing column, and high temperature rectifying column is two grades of towers, and effect is the de- weight of silicon tetrachloride
Tower.Specifically, the system is in the case where also including time high temperature rectifying column, except it is above-mentioned it is stated that annexation, also have
Following location annexation：
The first reboiler tube side outlet is connected with the entrance of described high temperature rectifying column, described high temperature rectifying tower
The outlet on top is connected with the second reboiler shell side inlet, the second reboiler tube side outlet and the entrance phase of low-temperature fractionating tower
Even, the second reboiler shell-side outlet is connected with the entrance of described high temperature rectifying column aftercooler, described high temperature rectifying column
The outlet of aftercooler is connected with the entrance of secondary high temperature rectifying column reflux pump, the outlet of described high temperature rectifying column reflux pump with it is described
The entrance of secondary high temperature rectifying column is connected, and the outlet of the low-temperature fractionating tower tower reactor is connected with the entrance of described high temperature rectifying column,
Described time low-temperature fractionating tower tower reactor is provided with liquid outlet.
As shown in Fig. 2 Fig. 2 is the structural representation of the system of the rectification process between the tower of the utility model three, wherein 1 is
Low-temperature fractionating tower, 2 be overhead condenser, and 3 be low-temperature fractionating tower reflux pump, and 4 be the first reboiler, and 5 be high temperature rectifying column, and 6 are
High temperature rectifying column aftercooler, 7 be high temperature rectifying column reflux pump, and 8 be the 4th reboiler, and 9 be time high temperature rectifying column reboiler, and 10 are
Low-temperature fractionating tower tower reactor produces pump, and 11 be time high temperature rectifying column, and 12 be time high temperature rectifying column aftercooler, and 13 be time high temperature rectifying column
Reflux pump.
Equally, in such a system, the outlet of the cryogenic rectification column overhead is connected with the entrance of low-temperature fractionating tower condenser,
The low-temperature fractionating tower condensator outlet is connected with the entrance of low-temperature fractionating tower reflux pump, and the low-temperature fractionating tower reflux pump goes out
Mouth is connected with the cryogenic rectification column overhead entrance；The outlet of the low-temperature fractionating tower tower reactor also with the first reboiler tube side
Entrance is connected.The outlet of described high temperature tower bottom of rectifying tower is also connected with the first reboiler tube-side inlet, first reboiler
Tube side outlet is connected with the entrance of described high temperature rectifying column；The outlet of the low-temperature fractionating tower tower reactor also with the second reboiler pipe
Journey entrance is connected, and the second reboiler tube side outlet is connected with the entrance of the low-temperature fractionating tower.
The application has also carried out the rectification and purification of chlorosilane using said system, comprises the following steps：
Silicon tetrachloride raw material take off and handled again, the silicon tetrachloride gas after separation is used as trichlorosilane to take off heavy heat
Source, after silicon tetrachloride gas is exchanged heat again, obtains the first gas-liquid mixture；
First gas-liquid mixture is condensed, after condensed liquid pressing, the first phegma and is obtained
One Produced Liquid；
The mixture of raw material trichlorosilane and dichlorosilane is separated, the trichlorosilane liquid after being separated with
Dichlorosilane；
The trichlorosilane liquid is separated in the presence of above-mentioned thermal source, obtained trichlorosilane gas is as trichlorine hydrogen
The thermal source that silicon and the mixture of dichlorosilane are separated again, after trichlorosilane gas is exchanged heat again, obtains the second gas-liquid and mixes
Compound；
Second gas-liquid mixture is condensed, after condensed liquid pressing, the second phegma and is obtained
Two Produced Liquids.
As shown in Fig. 2 the method that the system being connected using above-mentioned three tower carries out chlorosilane rectification and purification is specially：
The mixed thing (14) of raw material trichlorosilane and dichlorosilane (1~10%wt of content) enters into first stage tower (1) first
Row separation, reflux ratio 10~100 is returned after tower top dichlorosilane (15) is condensed through overhead condenser (2) after separation by first stage tower
Pump (3) pressurization is flowed, a part is as overhead reflux liquid (16), and another part is used as overhead extraction liquid (17)；Tower reactor trichlorosilane
Liquid (18) part is returned to first stage tower (1), another part warp through reboiler (9) after three-level overhead vapours (22) heating vaporization
Tower reactor pump (10) produces the charging (21) as three-level tower (11)；The trichlorosilane that act as of three-level tower (11) takes off weight, reflux ratio
For 4~12, after the trichlorosilane (21) from first stage tower (1) tower reactor is separated through three-level tower, tower top trichlorosilane gas (22) enters
Enter first stage tower (1) reboiler (9) as thermal source, be changed into gas-liquid mixture (23) after heat exchange, enter back into three-level tower aftercooler
(12) liquid all is condensed into, pressurizes rear portion as overhead reflux liquid (25) by three-level tower reflux pump (13) afterwards, separately
A part is used as overhead extraction liquid (26)；Tower reactor trichlorosilane liquid (27) part is through reboiler (4) by two grades of overhead vapours
(32) three-level tower (11) is returned to after heating vaporization, another part is produced as tower reactor heavy constituent (30)；Two grades of towers (5) are four chlorinations
Silicon weight-removing column, reflux ratio is 1~5, and raw material silicon tetrachloride (31) enters two grades of towers (5), the tower top silicon tetrachloride gas after separation
(32) as the thermal source of three-level tower (11) reboiler (4), it is changed into gas-liquid mixture (33) after heat exchange, enters back into cold after two grades of towers
Device (6) is all condensed into liquid (34), is used as overhead reflux liquid by two grades of tower reflux pumps (7) pressurization rear portions afterwards
(35), another part is used as overhead extraction liquid (36)；Tower reactor liquid (37) part is added through reboiler (8) by steam or conduction oil
It is changed into steam (39) after heat and returns to two grades of towers (5), another part (40) is produced as tower reactor heavy constituent.
Required according to of the present utility model, due in process of production in order to ensure that first stage tower (1) and three-level tower (11) are grasped
Stablize, two grades of tower (10) overhead vapours heats need 3~8% more than low-temperature fractionating tower reboiler institute calorific requirement, therefore,
2nd, three-level tower aftercooler (6) and (12) must be turned on.
According to regulation of the present utility model, the operating pressure of first stage tower (1) is 0.3~0.9MPa, the behaviour of three-level tower (11)
Make pressure for 0.4~1MPa, two grades of tower (6) operating pressures are 0.3~0.8MPa；Two grades of tower (5) tower tops and three-level tower (11) tower
Kettle temperature difference need to be not less than 8 DEG C, and three-level tower (11) tower top is not less than 8 DEG C with first stage tower (1) tower reactor temperature difference.
Preferably, go out in the system of herein described chlorosilane rectification and purification outside including secondary high temperature rectifying column, also
Including secondary low-temperature fractionating tower, described cryogenic rectification is trichlorosilane lightness-removing column, described low-temperature fractionating tower and time high temperature rectifying
Tower is set in turn between the low-temperature fractionating tower and the high temperature rectifying column, contains secondary low-temperature fractionating tower and time high temperature rectifying column
The heat cascade utilization that the system of formation belongs between four towers, the system includes：Low-temperature fractionating tower is first stage tower, and effect is point
From substantial amounts of dichlorosilane in trichlorosilane, secondary low-temperature fractionating tower is level Four tower, and effect is trichlorosilane lightness-removing column, secondary high temperature
Rectifying column is three-level tower, and effect is trichlorosilicane weight-removing column, and high temperature rectifying column is two grades of towers, and effect is silicon tetrachloride weight-removing column.
Specifically, the system is in the case where also including time low-temperature fractionating tower and time high temperature rectifying column, except it is above-mentioned it is stated that connection
Outside relation, also with following location annexation：
The second reboiler tube side outlet is connected with the entrance of described low-temperature fractionating tower, described low-temperature fractionating tower tower
The outlet on top is connected with the 3rd reboiler shell side inlet, the 3rd reboiler tube side outlet and the entrance of low-temperature fractionating tower
It is connected, the 3rd reboiler shell-side outlet is connected with the entrance of described low-temperature fractionating tower aftercooler, described cryogenic rectification
The outlet of tower aftercooler is connected with the entrance of secondary low-temperature fractionating tower reflux pump, the outlet of described low-temperature fractionating tower reflux pump and institute
The entrance for stating time low-temperature fractionating tower is connected, the outlet of the low-temperature fractionating tower tower reactor and the entrance phase of described low-temperature fractionating tower
Even, the outlet of described low-temperature fractionating tower tower reactor is connected with the entrance of described high temperature rectifying column.
As shown in figure 3, Fig. 3 is the structural representation of the system of the rectification process between the tower of the utility model four, wherein 1 is
Low-temperature fractionating tower, 2 be overhead condenser, and 3 be low-temperature fractionating tower reflux pump, and 4 be the first reboiler, and 5 be high temperature rectifying column, and 6 are
High temperature rectifying column aftercooler, 7 be high temperature rectifying column reflux pump, and 8 be the 4th reboiler, and 9 be time high temperature rectifying column reboiler, and 10 are
Low-temperature fractionating tower tower reactor produces pump, and 11 be time high temperature rectifying column, and 12 be time high temperature rectifying column aftercooler, and 13 be time high temperature rectifying column
Reflux pump, 14 be time low-temperature fractionating tower, and 15 be time low-temperature fractionating tower aftercooler, and 16 be time low-temperature fractionating tower reflux pump, and 17 be secondary
Low-temperature fractionating tower reboiler, 18 be time low-temperature fractionating tower tower reactor extraction pump.
Equally, in such a system, the outlet of the cryogenic rectification column overhead is connected with the entrance of low-temperature fractionating tower condenser,
The low-temperature fractionating tower condensator outlet is connected with the entrance of low-temperature fractionating tower reflux pump, and the low-temperature fractionating tower reflux pump goes out
Mouth is connected with the cryogenic rectification column overhead entrance；The outlet of the low-temperature fractionating tower tower reactor also with the first reboiler tube side
Entrance is connected.The outlet of the high temperature tower bottom of rectifying tower also spreads to entrance with the 4th reboiler and is connected, the 4th reboiler pipe
Journey outlet is connected with the entrance of the high temperature rectifying column.The outlet of described low-temperature fractionating tower tower reactor enters with the second reboiler tube side
Mouth is connected, and the second reboiler tube side outlet is connected with the entrance of described low-temperature fractionating tower, the low-temperature fractionating tower tower reactor
Outlet be connected with the 3rd reboiler tube-side inlet, the entrance phase of the 3rd reboiler tube side outlet and the low-temperature fractionating tower
Even.
The system that the application is also connected using above-mentioned four tower has carried out the rectification and purification of chlorosilane, comprises the following steps：
Silicon tetrachloride raw material take off and handled again, the silicon tetrachloride gas after separation is used as trichlorosilicane to take off heavy heat
Source, after silicon tetrachloride gas is exchanged heat again, obtains the first gas-liquid mixture；
First gas-liquid mixture is condensed, after condensed liquid pressing, the first phegma and is obtained
One Produced Liquid；
The mixture of raw material trichlorosilane and dichlorosilane is separated, the trichlorosilane liquid after being separated with
Dichlorosilane；
The trichlorosilane liquid is subjected to de- light processing, trichlorosilane gas and the first trichlorosilane liquid, institute is obtained
State the thermal source that trichlorosilane gas is separated again as the mixture of trichlorosilane and dichlorosilane, the trichlorosilane gas
After being exchanged heat again, the second gas-liquid mixture is obtained；
Second gas-liquid mixture is condensed, after condensed liquid pressing, the second phegma and is obtained
Two Produced Liquids；
First trichlorosilane liquid in the presence of thermal source take off and handled again, the first trichlorosilane gas is obtained
With the second trichlorosilane liquid, the first trichlorosilane gas is used as the de- thermal source gently handled of trichlorosilane, the described 1st
After chlorine hydrogen silicon gas is exchanged heat again, the 3rd gas-liquid mixture is obtained；The thermal source is the step of obtaining the first gas-liquid mixture
In thermal source；
3rd gas-liquid mixture is condensed, after condensed liquid pressing, the 3rd phegma and is obtained
Three Produced Liquids.
As shown in figure 3, the method that the system being connected using above-mentioned four tower carries out chlorosilane rectification and purification is specially：
The mixed thing (19) of raw material trichlorosilane and dichlorosilane (1~10%wt of content) then enters first stage tower (1) first
Separated, reflux ratio 10~100, by first stage tower after tower top dichlorosilane (20) is condensed through overhead condenser (2) after separation
Reflux pump (3) pressurizes, and a part is as overhead reflux liquid (22), and another part is used as overhead extraction liquid (23)；Tower reactor trichlorine hydrogen
Silicon liquid body (24) part is returned to first stage tower (1), another portion through reboiler (17) after level Four overhead vapours (29) heating vaporization
Lease making tower reactor pump (5) produces the charging (28) as level Four tower (14)；The trichlorosilane that act as of level Four tower (14) takes off light, backflow
Than for 80~250, after the trichlorosilane (28) from first stage tower (1) tower reactor is separated through level Four tower, tower top trichlorosilane gas
(29) enter first stage tower (1) reboiler (17) as thermal source, be changed into gas-liquid mixture (30) after heat exchange, enter back into after level Four tower
Cooler (15) is all condensed into liquid, is used as overhead reflux liquid by level Four tower reflux pump (16) pressurization rear portion afterwards
(32), another part is produced as tower top light component (33)；Tower reactor trichlorosilane liquid (34) part is through reboiler (9) by three
Level Four tower (14) is returned to after level overhead vapours (38) heating vaporization, another part is used as three-level tower (11) through tower reactor pump (18) extraction
Charging (37)；The trichlorosilane that act as of three-level tower (11) takes off weight, and reflux ratio is 4~12, from level Four tower (14) tower reactor
After trichlorosilane (37) is separated through three-level tower, tower top trichlorosilane gas (38) enters level Four tower (14) reboiler (9) as heat
Source, is changed into gas-liquid mixture (39) after heat exchange, enter back into three-level tower aftercooler (12) all be condensed into liquid (40), after pass through
Cross three-level tower reflux pump (13) and pressurize rear portion as overhead reflux liquid (41), another part is used as overhead extraction liquid (42)；
Tower reactor trichlorosilane liquid (43) part is returned to three-level tower through reboiler (4) after two grades of overhead vapours (47) heating vaporizations
(11), another part recombinates (46) point extraction as tower reactor；Two grades of towers (5) are silicon tetrachloride weight-removing column, and reflux ratio is 1~5, former
Expect that silicon tetrachloride (56) enters two grades of towers (5), tower top silicon tetrachloride gas (47) is used as three-level tower (11) reboiler after separation
(4) thermal source, is changed into gas-liquid mixture (48) after heat exchange, enters back into two grades of tower aftercoolers (6) and is all condensed into liquid (49),
Rear portion is pressurizeed as overhead reflux liquid (50) by two grades of tower reflux pumps (7) afterwards, and another part is used as overhead extraction liquid
(51)；Tower reactor liquid (52) part is changed into steam (54) through reboiler (8) and returns to two grades of towers after steam or heat-conducting oil heating
(15), another part (55) is produced as tower reactor heavy constituent.
Required according to of the present utility model, due in process of production in order to ensure the stability of operation, from level Four tower
(14) start, 3~8% more than previous stage low-temperature fractionating tower reboiler institute calorific requirement are needed per one-level overhead vapours heat, because
This, four, three, two grades of tower aftercoolers (15), (12) and (6) must be turned on.
According to regulation of the present utility model, the operating pressure of first stage tower (1) is 0.3~0.9MPa, the behaviour of level Four tower (14)
Make pressure for 0.4~0.8MPa, three-level tower (11) operating pressure is 0.4~1MPa, two grades of tower (5) operating pressures are 0.3~
0.8MPa；Between high temperature rectifying column (4,3,2) tower top temperature and low-temperature fractionating tower (3,2,1) bottom temperature should at least 8 DEG C with
On the temperature difference.
As described above, this application provides a kind of system of heat cascade utilization, the above-mentioned heat described between two towers
The heat cascade utilization between heat cascade utilization and four towers between cascade utilization, three towers, for the purposes of production the need for,
The number of rectifying column can be further added by according to the principle of heat cascade utilization, this application is had no particular limits.
Meanwhile, above-mentioned rectifying column, including high temperature rectifying column, secondary high temperature rectifying, secondary low-temperature fractionating tower and low-temperature fractionating tower are equal
Can be packed tower or plate column.
The utility model takes full advantage of the steam of high temperature rectifying tower top to heat the liquid of cryogenic rectification tower reactor, maximum limit
The step for realizing heat of degree is reused, and heat reuses number of times up to 3 times, greatly reduces the steam of distillation process
Consumption, steam consumption can reduce 40%~75%；The consumption of tower top recirculated water is also drastically reduce the area simultaneously.Due to the application
The system of offer can be realized in the recycling of heat, distillation operation to greatest extent, in the certain situation of the number of plates, Ke Yitong
Cross increasing reflux ratio to obtain the rectifying product that purity is higher, so as to produce the polysilicon close to electron level.
For a further understanding of the utility model, the chlorosilane rectifying that the utility model is provided is carried with reference to embodiment
Pure System and method for is described in detail, and protection domain of the present utility model is not limited by the following examples.
Embodiment 1
Heat cascade utilization technological process a between two towers, process operation is as follows：
As shown in figure 1, raw material silicon tetrachloride (9) is handled into two grades of towers (5) progress are de- first again, reflux ratio is 1~5,
Tower top silicon tetrachloride gas (10) is changed into gas-liquid mixed as the thermal source of first stage tower (1) reboiler (4) after heat exchange after separation
Thing (11), enters back into two grades of tower aftercoolers (6) and is all condensed into liquid, afterwards by two grades of latter portions of tower reflux pumps (7) pressurization
It is allocated as overhead reflux liquid (13), another part is used as overhead extraction liquid (14)；Tower reactor liquid (15) part is through reboiler (8)
It is changed into steam (16) after steam or heat-conducting oil heating and returns to two grades of towers (5), another part (17) is produced as tower reactor heavy constituent；
Raw material trichlorosilane and the mixed thing (18) of dichlorosilane (1~10wt% of content) are then separated into first stage tower (1), backflow
Than 10~100, pressurizeed after tower top dichlorosilane (22) is condensed through overhead condenser (2) after separation by first stage tower reflux pump (3),
A part is as overhead reflux liquid (24), and another part is used as overhead extraction liquid (25)；Tower reactor trichlorosilane liquid (19) one
Lease making reboiler (4) is returned to first stage tower (1) after two grades of overhead vapours (10) heating vaporizations, and another part is gone as tower reactor extraction
Next stage tower.
Required according to of the present utility model, due in process of production in order to ensure first stage tower (1) stable operation, two grades of towers
(5) overhead vapours heat needs 3~8% more than low-temperature fractionating tower reboiler institute calorific requirement, therefore, two grades of tower aftercoolers (6)
It must be turned on.
Application example 1：Produce the rectification and purification of chlorosilane in 10000 tons of polysilicon production process per year, specific process parameter is such as
Under：First stage tower (1) inlet amount 24m3/ h, feed composition：Trichlorosilane content 96.4%, dichloro-dihydro silicone content 3.5%, tetrachloro
SiClx content 0.1%, the impurity such as B, P, Fe, Al, Ca is micro；Two grades of tower (5) inlet amount 59m3/ h, feed composition：Trichlorosilane
0.1%, silicon tetrachloride 99.9%, the impurity such as B, P, Fe, Al, Ca is micro；First stage tower (1) operating pressure 0.4MPa, tower top temperature
52.3 DEG C, reflux ratio 100, number of theoretical plate 100；Two grades of tower (5) operating pressure 0.3MPa, 95.2 DEG C of tower top temperature, reflux ratio
1.4, number of theoretical plate 60.
Calculated by simulating, as shown in table 1, the data in bracket are conventional to each tower thermic load of two tower heat cascade utilizations
The thermic load of rectificating method.
Each tower thermic load tables of data of the present embodiment of table 1
| Reboiler (Gcal/h) | Condenser duty (Gcal/h) | Amount to (Gcal/h) | |
| First stage tower | 0(6.41) | 6.117 | 6.117(12.527) |
| Two grades of towers | 6.692 | 0.211(6.621) | 6.903(13.313) |
| Amount to | 6.692(13.102) | 6.328(12.739) | 13.02(25.841) |
As can be seen from the above table, reboiler heat duty total after two tower heat cascade utilizations is used for 6.692Gcal/h, phase
Than in conventional method (total thermic load is 13.106Gcal/h) energy-conservation 49.3%；Condenser heat load energy-conservation 50.32%；It is overall
Energy-conservation 49.81%.
Embodiment 2
Heat cascade utilization technological process b between three towers, process operation is as follows：
As shown in Fig. 2 the mixed thing (14) of raw material trichlorosilane and dichlorosilane (1~10%wt of content) first enters one
Level tower (1) separated, reflux ratio 10~100, after separation tower top dichlorosilane (15) through overhead condenser (2) condensation after by
First stage tower reflux pump (3) pressurizes, and a part is as overhead reflux liquid (16), and another part is used as overhead extraction liquid (17)；Tower reactor
Trichlorosilane liquid (18) part is returned to first stage tower (1) through reboiler (9) after three-level overhead vapours (22) heating vaporization, separately
A part produces the charging (21) as three-level tower (11) through tower reactor pump (10)；The trichlorosilane that act as of three-level tower (11) takes off
Weight, reflux ratio is 4~12, after the trichlorosilane (21) from first stage tower (1) tower reactor is separated through three-level tower, tower top trichlorosilane gas
Body (22) enters first stage tower (1) reboiler (9) as thermal source, is changed into gas-liquid mixture (23) after heat exchange, enters back into three-level tower
Aftercooler (12) is all condensed into liquid, is used as overhead reflux liquid by three-level tower reflux pump (13) pressurization rear portion afterwards
(25), another part is used as overhead extraction liquid (26)；Tower reactor trichlorosilane liquid (27) part is through reboiler (4) by two grades of towers
Three-level tower (11) is returned to after pushing up steam (32) heating vaporization, another part is produced as tower reactor heavy constituent (30)；Two grades of towers (5) are
Silicon tetrachloride weight-removing column, reflux ratio is 1~5, and raw material silicon tetrachloride (31) enters two grades of towers (5), the chlorination of tower top four after separation
Silicon gas (32) is changed into gas-liquid mixture (33) after heat exchange, enters back into two grades as the thermal source of three-level tower (11) reboiler (4)
Tower aftercooler (6) is all condensed into liquid (34), is used as overhead reflux by two grades of tower reflux pumps (7) pressurization rear portions afterwards
Liquid (35), another part is used as overhead extraction liquid (36)；Tower reactor liquid (37) part is through reboiler (8) by steam or conduction oil
It is changed into steam (39) after heating and returns to two grades of towers (5), another part (40) is produced as tower reactor heavy constituent.
Required according to of the present utility model, due in process of production in order to ensure that first stage tower (1) and three-level tower (11) are grasped
Stablize, two grades of tower (5) overhead vapours heats need 3~8% more than low-temperature fractionating tower reboiler institute calorific requirement, therefore, two,
Three-level tower aftercooler (6) and (12) must be turned on.
Application example 2：Produce the rectification and purification of chlorosilane in 12000 tons of polysilicon production process per year, specific process parameter is such as
Under：First stage tower (1) inlet amount 29m3/ h, feed composition：Trichlorosilane content 96.2%, dichloro-dihydro silicone content 3.7%, tetrachloro
SiClx content 0.1%, the impurity such as B, P, Fe, Al, Ca is micro；Three-level tower (11) inlet amount 77m3/ h, feed composition：Trichlorosilane
0.1%, silicon tetrachloride 99.9%, the impurity such as B, P, Fe, Al, Ca is micro；First stage tower (1) operating pressure 0.4MPa, tower top temperature
52.3 DEG C, reflux ratio 80, number of theoretical plate 120；Two grades of tower (5) operating pressure 0.56MPa, 91.9 DEG C of tower top temperature, reflux ratio 4,
Number of theoretical plate 160；Three-level tower (11) operating pressure 0.4MPa, 107 DEG C of tower top temperature, reflux ratio 1.2, number of theoretical plate 60.
Calculated by simulating, as shown in table 2, the data in bracket are conventional to each tower thermic load of two tower heat cascade utilizations
The thermic load of rectificating method.
The thermic load tables of data of each tower of the present embodiment of table 2
As can be seen from the above table, reboiler heat duty total after three tower heat cascade utilizations is used for 7.619Gcal/h, phase
Than saving 64.42%, condenser heat load energy-conservation 66.13% in conventional method (thermic load is 21.412Gcal/h)；Total body segment
Energy 65.26%.
Embodiment 3
Heat cascade utilization technological process c between four towers, process operation is as follows：
As shown in figure 3, the mixed thing (19) of raw material trichlorosilane and dichlorosilane (1~10%wt of content) first then enters
First stage tower (1) is separated, reflux ratio 10~100, after tower top dichlorosilane (20) is condensed through overhead condenser (2) after separation
Pressurizeed by first stage tower reflux pump (3), a part is as overhead reflux liquid (22), and another part is used as overhead extraction liquid (23)；Tower
Kettle trichlorosilane liquid (24) part is returned to first stage tower through reboiler (17) after level Four overhead vapours (29) heating vaporization
(1), another part produces the charging (28) as level Four tower (14) through tower reactor pump (5)；Level Four tower (14) act as trichlorine hydrogen
Silicon is de- light, and reflux ratio is 80~250, after the trichlorosilane (28) from first stage tower (1) tower reactor is separated through level Four tower, tower top trichlorine
Hydrogen silicon gas (29) enters first stage tower (1) reboiler (17) as thermal source, is changed into gas-liquid mixture (30) after heat exchange, enters back into
Level Four tower aftercooler (15) is all condensed into liquid, pressurizes rear portion as tower top time by level Four tower reflux pump (16) afterwards
Flow liquid (32), another part is produced as tower top light component (33)；Tower reactor trichlorosilane liquid (34) part is through reboiler (9)
Level Four tower (14) is returned to after three-level overhead vapours (38) heating vaporization, another part is used as three-level tower through tower reactor pump (18) extraction
(11) charging (37)；The trichlorosilane that act as of three-level tower (11) takes off weight, and reflux ratio is 4~12, from level Four tower (14) tower
After the trichlorosilane (37) of kettle is separated through three-level tower, tower top trichlorosilane gas (38) enters level Four tower (14) reboiler (9) and made
For thermal source, it is changed into gas-liquid mixture (39) after heat exchange, enters back into three-level tower aftercooler (12) and be all condensed into liquid (40), it
Rear portion is pressurizeed as overhead reflux liquid (41) by three-level tower reflux pump (13) afterwards, and another part is used as overhead extraction liquid
(42)；Tower reactor trichlorosilane liquid (43) part is returned to three through reboiler (4) after two grades of overhead vapours (47) heating vaporizations
Level tower (11), another part recombinates (46) point extraction as tower reactor；Two grades of towers (5) are silicon tetrachloride weight-removing column, reflux ratio is 1~
5, raw material silicon tetrachloride (56) enters two grades of towers (5), after separation tower top silicon tetrachloride gas (47) as three-level tower (11) again
The thermal source of device (4) is boiled, is changed into gas-liquid mixture (48) after heat exchange, two grades of tower aftercoolers (6) is entered back into and is all condensed into liquid
(49) rear portion, is pressurizeed as overhead reflux liquid (50) by two grades of tower reflux pumps (7) afterwards, and another part is adopted as tower top
Go out liquid (51)；Tower reactor liquid (52) part is changed into steam (54) through reboiler (8) and returns to two after steam or heat-conducting oil heating
Level tower (15), another part (55) is produced as tower reactor heavy constituent.
Required according to of the present utility model, due in process of production in order to ensure the stability of operation, from level Four tower
(14) start, 3~8% more than previous stage low-temperature fractionating tower reboiler institute calorific requirement are needed per one-level overhead vapours heat, because
This, four, three, two grades of tower aftercoolers (15), (12) and (6) must be turned on.
Application example 3：Produce the rectification and purification of chlorosilane in 15000 tons of polysilicon production process per year, specific process parameter is such as
Under：First stage tower (1) inlet amount 36.4m3/ h, feed composition：Trichlorosilane content 96.1%, dichloro-dihydro silicone content 3.8%, four
Chlorination silicone content 0.1%, the impurity such as B, P, Fe, Al, Ca is micro；Level Four tower (15) inlet amount 96m3/ h, feed composition：Trichlorine hydrogen
Silicon 0.1%, silicon tetrachloride 99.9%, the impurity such as B, P, Fe, Al, Ca is micro；First stage tower (1) operating pressure 0.35MPa, tower top temperature
48 DEG C of degree, reflux ratio 80, number of theoretical plate 80；Two grades of tower (5) operating pressure 0.5MPa, 87.1 DEG C of tower top temperature, reflux ratio 230,
Number of theoretical plate 100；Three-level tower (10) operating pressure 0.72MPa, 103 DEG C of tower top temperature, reflux ratio 5, number of theoretical plate 100；Level Four
Tower (15) operating pressure 0.52MPa, 118.6 DEG C of tower top temperature, reflux ratio 1.5, number of theoretical plate 60.
Calculated by simulating, as shown in table 3, the data in bracket are conventional to each tower thermic load of two tower heat cascade utilizations
The thermic load of rectificating method.
Each tower thermic load tables of data of the present embodiment of table 3
As can be seen from the above table, reboiler heat duty total after four tower heat cascade utilizations is used for 10.56Gcal/h, phase
Than in conventional method (total thermic load is 38.892Gcal/h) energy-conservation 72.85%, condenser heat load is compared to conventional method
Reduction by 74.64%；Total energy-saving 73.72%.
The explanation of above example is only intended to help and understands method of the present utility model and its core concept.It should refer to
Go out, for those skilled in the art, can also be to this on the premise of the utility model principle is not departed from
Utility model carries out some improvement and modification, and these are improved and modification also falls into the utility model scope of the claims
It is interior.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or new using this practicality
Type.A variety of modifications to these embodiments will be apparent for those skilled in the art, determine herein
The General Principle of justice can in other embodiments be realized in the case where not departing from spirit or scope of the present utility model.Cause
This, the utility model is not intended to be limited to the embodiments shown herein, and is to fit to and principles disclosed herein
The most wide scope consistent with features of novelty.
Claims (12)
1. the system of heat cascade utilization during a kind of chlorosilane rectification and purification, including：
High temperature rectifying column；The outlet of the high temperature rectifying column tower top is connected with the shell side inlet of the first reboiler, and described first again
The tube-side inlet for boiling device is connected with the outlet of low-temperature fractionating tower tower reactor, tube side outlet and the low-temperature fractionating tower tower of first reboiler
Kettle entrance is connected, and the shell-side outlet of first reboiler is connected with high temperature rectifying column aftercooler entrance, the high temperature rectifying column
The outlet of aftercooler is connected with high temperature rectifying column backflow pump intake, the high temperature rectifying column backflow pump discharge and the high temperature rectifying
Tower entrance is connected；The high temperature rectifying column is silicon tetrachloride weight-removing column, and the low-temperature fractionating tower is trichlorosilane and dichloro-dihydro
Silicon knockout tower, trichlorosilane weight-removing column or trichlorosilane lightness-removing column；The low-temperature fractionating tower and the high temperature tower bottom of rectifying tower are equal
It is provided with liquid outlet.
2. system according to claim 1, it is characterised in that described high temperature rectifying tower top and low-temperature fractionating tower kettle temperature are poor
Not less than 8 DEG C, the high temperature rectifying column tower top heat is more than the 3~8% of low-temperature fractionating tower tower reactor institute calorific requirement.
3. system according to claim 1, it is characterised in that also include time high temperature rectifying column in the system, described the
The tube side outlet of one reboiler is connected with the entrance of described high temperature rectifying column, the outlet of described high temperature rectifying column tower top and the
The shell side inlets of two reboilers is connected, and the tube side outlet of second reboiler is connected with the entrance of low-temperature fractionating tower, and described the
The shell-side outlet of two reboilers is connected with the entrance of described high temperature rectifying column aftercooler, described high temperature rectifying column aftercooler
Export and be connected with time entrance of high temperature rectifying column reflux pump, the outlet of described high temperature rectifying column reflux pump and described high-temperature fine
The entrance for evaporating tower is connected, and the outlet of the low-temperature fractionating tower tower reactor is connected with the entrance of described high temperature rectifying column；It is high described time
Warm rectifying is trichlorosilane weight-removing column or trichlorosilane lightness-removing column, and the low-temperature fractionating tower tower reactor is provided with liquid outlet.
4. system according to claim 3, it is characterised in that described secondary high temperature rectifying column tower top and cryogenic rectification tower reactor
The temperature difference is not less than 8 DEG C, and described time high temperature rectifying column tower top heat is more than the 3~8% of low-temperature fractionating tower tower reactor institute calorific requirement.
5. system according to claim 3, it is characterised in that also include time low-temperature fractionating tower in the system, described the
The tube side outlet of two reboilers is connected with the entrance of described low-temperature fractionating tower, the outlet of described cryogenic rectification column overhead and the
The shell side inlets of three reboilers is connected, and the tube side outlet of the 3rd reboiler is connected with the entrance of low-temperature fractionating tower, and described the
The shell-side outlet of three reboilers is connected with the entrance of described low-temperature fractionating tower aftercooler, described low-temperature fractionating tower aftercooler
Export and be connected with time entrance of low-temperature fractionating tower reflux pump, the outlet of described low-temperature fractionating tower reflux pump and described low temperature essence
The entrance for evaporating tower is connected, and the outlet of the low-temperature fractionating tower tower reactor is connected with the entrance of described low-temperature fractionating tower；It is low described time
The outlet of warm tower bottom of rectifying tower is connected with the entrance of described high temperature rectifying column, and described cryogenic rectification is that trichlorosilane is de- light
Tower.
6. system according to claim 5, it is characterised in that described secondary cryogenic rectification tower top and low-temperature fractionating tower tower reactor
The temperature difference is not less than 8 DEG C, and described time cryogenic rectification column overhead heat is more than the 3~8% of low-temperature fractionating tower tower reactor institute calorific requirement.
7. system according to claim 5, it is characterised in that boiled again with second outlet of described low-temperature fractionating tower tower reactor
Device tube-side inlet is connected, and the second reboiler tube side outlet is connected with the entrance of described low-temperature fractionating tower, the low temperature essence
The outlet for evaporating tower tower reactor is connected with the 3rd reboiler tube-side inlet, the 3rd reboiler tube side outlet and the low-temperature fractionating tower
Entrance be connected.
8. the system according to any one of claim 1~7, it is characterised in that the outlet of the cryogenic rectification column overhead with
The entrance of low-temperature fractionating tower condenser is connected, the outlet of the low-temperature fractionating tower condenser and the entrance of low-temperature fractionating tower reflux pump
It is connected, the outlet of the low-temperature fractionating tower reflux pump is connected with the entrance of the cryogenic rectification column overhead；The low-temperature fractionating tower
The outlet of tower reactor is also connected with the first reboiler tube-side inlet.
9. the system according to any one of claim 1~7, it is characterised in that the outlet of the high temperature tower bottom of rectifying tower is also
It is connected with the tube-side inlet of the 4th reboiler, the 4th reboiler tube side outlet is connected with the entrance of the high temperature rectifying column.
10. the system according to any one of claim 1~7, it is characterised in that described high temperature rectifying column, secondary high-temperature fine
Evaporate, secondary low-temperature fractionating tower and low-temperature fractionating tower are packed tower or plate column.
11. system according to claim 3, it is characterised in that the outlet of described high temperature tower bottom of rectifying tower is also with first
The tube-side inlet of reboiler bottom is connected, tube side outlet and the entrance of described high temperature rectifying column at the top of first reboiler
It is connected；Tube-side inlet of the outlet of the low-temperature fractionating tower tower reactor also with the second reboiler bottom is connected, second reboiler
The tube side outlet at top is connected with the entrance of the low-temperature fractionating tower.
12. system according to claim 5, it is characterised in that the outlet of described low-temperature fractionating tower tower reactor and second is again
The tube-side inlet for boiling device bottom is connected, tube side outlet and the entrance phase of described low-temperature fractionating tower at the top of second reboiler
Even, the outlet of the low-temperature fractionating tower tower reactor is connected with the tube-side inlet of the 3rd reboiler bottom, at the top of the 3rd reboiler
Tube side outlet be connected with the entrance of the low-temperature fractionating tower.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115719A (en) * | 2016-08-22 | 2016-11-16 | 四川永祥多晶硅有限公司 | The system and method for heat cascade utilization during chlorosilane rectification and purification |
| CN109704345A (en) * | 2019-02-21 | 2019-05-03 | 浙江中宁硅业有限公司 | A kind of ocratation rectifier unit and its production method |
-
2016
- 2016-08-22 CN CN201620919654.9U patent/CN206384848U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115719A (en) * | 2016-08-22 | 2016-11-16 | 四川永祥多晶硅有限公司 | The system and method for heat cascade utilization during chlorosilane rectification and purification |
| CN109704345A (en) * | 2019-02-21 | 2019-05-03 | 浙江中宁硅业有限公司 | A kind of ocratation rectifier unit and its production method |
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