CN109810132A - Use the device and method of circulation multi-effect distillation technology separation organic silicon monomer methylchlorosilane - Google Patents
Use the device and method of circulation multi-effect distillation technology separation organic silicon monomer methylchlorosilane Download PDFInfo
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Abstract
The invention discloses a kind of device and methods using circulation multi-effect distillation technology separation organosilicon mix monomer methylchlorosilane.Multitower process of this method based on cis- cutting, altogether include following core procedure: a first diformazan mixture first flows into diformazan tower, the dimethyldichlorosilane product of tower bottom output qualification, and the mixture of tower top output is sent to Yi Jiata；One first product of one first column overhead output qualification, the mixture of tower bottom output send back at diformazan tower product inlet；By adjusting each tower temperature, pressure, making de- high tower overhead vapours can be the heat supply of diformazan tower, and diformazan column overhead steam can be a first tower, take off low tower, gently divide tower heat supply.By the method, it can be achieved that the significant energy-saving and water-saving effect of organosilicon rectification process process.Meanwhile present invention also proposes the improvement device and methods based on heat pump distillation technology, further improve energy-saving effect instead of the high steam demand of the second reboiler of diformazan tower by indirect type heat pump distillation.
Description
Technical field
The present invention relates to a kind of organic silicon monomer rectifying methods, especially energy-saving and water-saving type methylchlorosilane rectificating method；
The method for recycling multi-effect distillation technology separation methylchlorosilane and the improvement based on heat pump distillation technology are used more particularly to a kind of
Method.
Background technique
Organo-silicon compound generally refer to the compound containing Si-C key, because having both the property of inorganic material and organic material
Can, polymer possesses many excellent properties, and it is each to be widely used in electric, building, chemical industry, weaving, light industry, medical treatment etc.
Industry has the title of " industrial monosodium glutamate ".And starting raw materials for production of the organic silicon monomer as Organosilicon Polymers, in organosilicon industry
In play an important role.Methylchlorosilane, mainly include Trichloromethyl silane (then claim a first), dimethyldichlorosilane (after
Claim diformazan), three kinds of tri-methyl-chlorosilane (claiming front three afterwards), as important organic silicon monomer type, the section of separating technology
It can optimize and have huge economic benefit.Currently, only being realized in industry to methylchlorosilane isolation technics common in industry
The application of conventional distillation technology.Corresponding rectifying scheme is broadly divided into cis- cutting, trans- cutting, three kinds of middle section cutting, wherein
Trans- cutting is cut with middle section because being easy to cause diformazan product not up to standard in practical operation, at present mainly using cis- in industry
Cut flow scheme.
Common cis- cutting process has eight tower processes, nine tower processes etc..Typical cis- nine towers process include de- high tower,
High boiling tower, lightness-removing column, diformazan tower, Yi Jiata, light Fen Ta, the hydrogeneous tower of a first, azeotrope column, front three tower totally nine tower, wherein a first tower
Circulation rectifying is constituted with diformazan tower.Material enters from de- high tower, and Jing Qingfen tower separates light component and a first diformazan mixture, later
Dimethyldichlorosilane is produced from diformazan tower tower bottom, a first column overhead produces Trichloromethyl silane；It is adopted from the hydrogeneous tower top of a first
Methyl hydrogen dichlorosilane out；Tri-methyl-chlorosilane is produced from front three column overhead, detailed process can refer to " domestic methylchlorosilane
Isolation technics status and improved method " (Sun Jianyang etc., 2015).Since the process is longer, rectifying column number is more, whole energy consumption
Greatly, general only from angle consideration is thermally integrated to the optimisation technique of nine tower distillation processes, such as patent CN201010132940.8, lead
Causing whole flow process economic benefit, there are still improve space.Thus, it is necessary in conjunction with a variety of new-type distillation technologies, explore energy-efficient
Method.
Circulation multi-effect distillation technology (multi-effect distillation, abbreviation MED) refers to by by entire rectifying
Process is divided into the different multiple towers of energy grade (i.e. temperature), with temperature compared with the overhead vapours of high tower boiling again to the lower tower of temperature
Device heat supply, while steam being condensed.In this way, the tower reactor of only first tower needs high steam to mention in circulation multi-effect distillation
The overhead vapours of heating load, the last one tower is condensed with cooling working medium, remaining each tower no longer needs to be supplied by the external world
Hot and cold but, thus has apparent energy-saving effect.It should be noted that in practical operation, it usually can be by inciting somebody to action single essence
The mode that tower splits into the different multiple towers of energy level is evaporated, circulation multi-effect distillation is constituted.Common circulation multi-effect distillation technology is with double
It imitates based on rectifying.
Multi-effect distillation technology (multi-effect distillation, abbreviation MED) refers to by by entire distillation process
It is divided into the different multiple towers of energy grade (i.e. temperature), is supplied compared with the overhead vapours of high tower to the reboiler of the lower tower of temperature with temperature
Heat, while steam being condensed.In this way, the tower reactor of only first tower needs high steam to provide heat in circulation multi-effect distillation
Amount, the overhead vapours of the last one tower are condensed with cooling working medium, remaining each tower no longer need to be carried out by the external world heat supply with
It is cooling, thus have apparent energy-saving effect.It should be noted that in practical operation, it usually can be by by single rectifying column
The mode of the different multiple towers of energy level is split into, circulation multi-effect distillation is constituted.Common circulation multi-effect distillation technology is with economic benefits and social benefits essence
Based on evaporating.
Heat pump distillation technology (heat pump distillation, abbreviation HPD) is with pump or compressor, by heat from temperature
It spends in lower overhead condenser and takes out, be sent in the higher tower bottom reboiler of temperature later, thus by rectifying column and refrigeration
Circulation combines, and realizes efficient conversion of the mechanical work to thermal energy, energy-saving effect is substantially improved.According to process whether needs
Additional heat-carrying agent can be divided into indirect type and two kinds of direct-type.In practical heat pump distillation process design, takes the condenser of heat and put
The reboiler of heat can not belong to same tower.
Summary of the invention
It is organic to separate using circulation multi-effect distillation technology, especially circulation three-effect distillation technology that the present invention provides one
The device and method of silicon monomer methylchlorosilane mixture, the device include feed preheater E1, take off high tower T1, take off high tower tower
Bottom reboiler H1；High boiling tower T9, high boiling tower tower bottom reboiler H9, high boiling tower overhead condenser C9；Lightness-removing column T2, lightness-removing column tower bottom
Reboiler H2, lightness-removing column overhead condenser C2；Diformazan tower T3, diformazan tower tower bottom reboiler H3A, diformazan tower the second reboiler of tower bottom
H3B；One first tower T4, first tower tower bottom reboiler a H4, a first column overhead condenser C4；Gently divide tower T5, gently divides tower tower bottom reboiler
H5 gently divides column overhead condenser C5；The hydrogeneous tower T6 of one first, the hydrogeneous tower tower bottom reboiler H6 of a first, the hydrogeneous column overhead condensation of a first
Device C6；Azeotrope column T7, azeotrope column tower bottom reboiler H7A, azeotrope column overhead condenser C7；Front three tower T8, front three tower tower bottom are boiled again
Device H8, front three column overhead condenser C8.Wherein, high tower T1 overhead vapours pipeline and diformazan tower tower bottom the first reboiler H3A phase are taken off
Even；Diformazan tower T3 overhead vapours pipeline and a first tower tower bottom reboiler H4, lightness-removing column tower bottom reboiler H2, gently tower tower bottom is divided to boil again
Device H5 is connected；The condensed high-temperature water pipeline of high steam and feed preheater E1, azeotrope column tower bottom reboiler H7A, a first contain
Hydrogen tower tower bottom reboiler H6 is connected；Diformazan tower T3 tower bottom high-temperature product logistics is connected with azeotropic tower bottom reboiler H8.Remaining is boiled again
Device is connected with high steam pipeline, and condenser is connected with technical cooling waterpipe.
Using the method for the device, circulation distillation process is constituted first between a first tower T3 and diformazan tower T4,
On this basis by adjusting the operating pressure and temperature of de- high tower T1, diformazan tower T3, a first tower T4, it is divided into three energy grades
Different tower, to constitute circulation three-effect rectifying.In addition, the present invention proposes also according to heat pump distillation technical principle about above-mentioned
The improvement device and method of method, further improves energy-saving and water-saving effect.
The specific technical solution of the present invention is as follows:
A method of organic silicon monomer methylchlorosilane being separated using circulation multi-effect distillation technology, it is characterized in that including such as
Lower step:
(1) enter de- high tower T1 after raw material crude monomer is preheated, tower bottom output temperature is not higher than 130 DEG C of mixture, stream
Enter into high boiling tower T9；High boiling tower overhead vapours is after high boiling tower overhead condenser C9 total condensation is at liquid, refluxing portion stream
Enter high boiling tower T9, product section is flowed into de- high tower T1, and tower bottom flows out high-boiling components product；
(2) it is completely cold through the first reboiler of lightness-removing column tower bottom H2A, diformazan tower tower bottom reboiler H3 to take off high tower T1 overhead vapours
After congealing into liquid, refluxing portion flows into de- high tower T1, and product section flows into lightness-removing column T2；One first diformazan of lightness-removing column T2 tower bottom is mixed
After composition powder is mixed with a first tower T4 tower bottom product, it is flowed into diformazan tower T3；Diformazan tower T3 overhead mixture steam is through one
First tower tower bottom reboiler H4, lightness-removing column tower bottom reboiler H2, gently divide tower tower bottom reboiler H5 total condensation after, refluxing portion flow into
Diformazan tower T3, product section are flowed into a first tower T4, and the high-purity dimethyldichlorosilane product of diformazan tower T3 tower bottom high temperature is through three
After the cooling heat supply of first tower tower bottom reboiler H8, flowed out as dimethyldichlorosilane product；The one high-purity monomethyl of first tower T4 tower top
Trichlorosilane steam is after overhead condenser C4 total condensation, and refluxing portion flows into a first tower T4, and product section is as monomethyl
The outflow of trichlorosilane product；One first tower T4 tower bottom mixture is flowed into the inlet diformazan tower T3, mixed with lightness-removing column T2 bottom product
It is flowed into after conjunction in diformazan tower T3；
(3) for lightness-removing column T2 overhead vapours after lightness-removing column overhead condenser C2 total condensation, refluxing portion flows into lightness-removing column
T2, product section inflow gently divide in tower T5；Gently divide tower T5 tower top light component product steam complete through light point column overhead condenser C5
After condensation, refluxing portion, which flows into, gently divides tower T5, and for product section as discarded light component outflow, it is hydrogeneous that bottom product is flowed into a first
In tower T6；The hydrogeneous tower T6 tower top methyl hydrogen dichlorosilane product steam of one first is through the hydrogeneous column overhead condenser C6 total condensation of a first
Afterwards, refluxing portion flows into the hydrogeneous tower T6 of a first, and product section is flowed out as methyl hydrogen dichlorosilane product, and bottom product is flowed into
In azeotrope column T7；Azeotrope column T7 tower top azeotropic mixture product steam is after azeotrope column overhead condenser C7 total condensation, refluxing portion
Azeotrope column T7 is flowed into, product section is flowed out as azeotropic mixture, and bottom product is flowed into front three tower T8；Front three tower T8 tower top front three
For one chlorosilane product steam of base after front three column overhead condenser C8 total condensation, refluxing portion flows into front three tower T8, product department
It is allocated as flowing out for tri-methyl-chlorosilane product, bottom product is recycled back to head tank or sends out battery limit (BL).
The characteristics of program, is as follows:
(1) on the basis of common nine tower separation process (i.e. circulation process) of cis- cutting, by the behaviour for adjusting de- high tower
Make pressure, so that de- high tower T1 and diformazan tower T3, diformazan tower T3 and a first tower T4, diformazan tower T3 and lightness-removing column T2, diformazan tower T3
It is not less than 15 DEG C with the temperature difference of tower T5 is gently divided；Meanwhile the operation temperature pressure and a first tower of diformazan tower T3 is flowed by adjusting
The tower bottom circulation product flow of T4, makes the tower top material steam of diformazan tower T3 by chance be used to boil again to a first tower T4 tower bottom enough
Device H4, it takes off low tower T2 tower bottom reboiler H2, gently divide tower T5 tower bottom reboiler H5 heat supply.
(2) circulation three-effect rectifying method is used between the de- high tower T1, diformazan tower T3, a first tower T4 described in, by de- high tower
Reboiler H3A heat supply of the tower top material steam of T1 to diformazan tower T3 tower bottom, the tower top material steam of diformazan tower T3 tower top is to one
The reboiler H4 heat supply of first tower T4 tower bottom.The de- high tower T1 tower top material steam can separate some vapor, give lightness-removing column T2
Reboiler H2 and gently divide the reboiler H5 heat supply of tower T5；The de- high tower tower bottom reboiler H1 is supplied using high steam condensation
Heat.
(3) the condensed high-temperature water of high steam can be used to feed preheater E1, azeotrope column tower bottom reboiler H7A, one
The hydrogeneous tower reboiler H6 heat supply of first；The bottom product of diformazan tower T3 can be used for after front three tower tower bottom reboiler H8 heat supply as product
Outflow.
The overhead reflux ratio of the de- high tower T1 is between 5-10, and full pressure tower is between 300kPa-450kPa；
The overhead reflux ratio of the lightness-removing column T2 is between 50-90, and full pressure tower is between 110kPa-140kPa；
The overhead reflux ratio of the diformazan tower T3 is between 8-20, and between 180kPa-250kPa, tower bottom is set full pressure tower
There are two reboiler H3A and H3B, the first reboiler H3A is adopted using de- high tower tower top material steam heating, the second reboiler H3B
Heat supply is condensed with high steam；
The overhead reflux ratio of the one first tower T4 is between 50-130, and full pressure tower is between 100kPa-140kPa；
The overhead extraction light component for gently dividing tower T5, reflux ratio is between 800-1000, and full pressure tower is in 180kPa-
Between 250kPa, tower bottom is set there are two reboiler H5A and H5B, and the first reboiler H5A is using the high-temperature water heat supply after preheating, and the
Two reboiler H5B use high steam heat supply；
For the overhead reflux ratio of the hydrogeneous tower T6 of one first between 2-4, full pressure tower maintains normal pressure state；
For the overhead reflux ratio of the azeotrope column T7 between 100-160, full pressure tower maintains 150kPa-200kPa；
For the overhead reflux ratio of the front three tower T8 between 3-5, full pressure tower maintains normal pressure state.
In improved heat pump-circulation multiple-effect joint rectifier unit, following equipment is increased, with a first tower column overhead condenser
C4 together constitutes with heat pump distillation working medium closed circuit circulatory system: compressor P1, and azeotrope column tower bottom adds reboiler H7B, cooler E2,
Dropping valve P2.It is as follows that it improves the connection method that installs pipes: condenser C4 high temperature stream outlet is connected to compressor P1 import, pressure
Contracting machine P1 is exported through steam distributor, is connected to diformazan tower the second reboiler of tower bottom H3B, azeotrope column tower bottom adds reboiler H7B
High temperature substrate flow into mouth, diformazan tower the second reboiler of tower bottom H3B, azeotrope column tower bottom add the high temperature stream outlet of reboiler H7B
It is connected to cooler E2 import, the outlet cooler E2 is connected to dropping valve P2 import, and the outlet dropping valve P2 is connected to condenser C4
High temperature substrate flows into mouth, constitutes closed loop cycle circuit.
Using the method as described above for improving device, the biggish organic matter pure material of specific heat capacity or mixing are chosen first
Object is as heating working medium (in the case select azeotrope column T7 tower top azeotropic mixture product), by indirect type pump rectification method,
Under normal pressure at a first column overhead condenser C4 heat exchange diformazan tower tower bottom the is sent into after compressor P1 pressurization to being gasified totally
Two reboiler H3B, azeotrope column tower bottom add reboiler H7B, after after cooler E2 is cooled to 48 DEG C of liquid, through dropping valve P2
It is down to after normal pressure and exchanges heat again at a first column overhead condenser C4.
The heating working medium need to keep the state that is gasified totally in compressor P1 pressure process, while drop in dropping valve P2
Complete liquefaction is kept during pressure；The compressor P1 outlet pressure is 300kPa-600kPa, dropping valve P2 outlet pressure
For 60kPa-100kPa.
The beneficial effects of the present invention are embodied in:
1. by circulation multi-effect distillation technology, the heat for making full use of high steam that can provide；In combination with being thermally integrated
Technology, significantly reduces the demand of whole flow process mesohigh steam, and energy-saving and water-saving effect is obvious.
2. this method is while playing obvious energy saving effect, to equipment compared with the common cis- cutting process of industry
Instrument control requirement is almost the same, and operation controllability is strong, highly-safe, has stronger industrial practice feasibility.
3. in improved method, distillation technology is combined based on heat pump-circulation multiple-effect, is recycled using indirect type heat pump distillation,
High steam demand is further decreased, more preferably energy-saving and water-saving effect, remarkable in economical benefits are obtained.
Detailed description of the invention:
Fig. 1 is the organic silicon monomer circulation three-effect rectifying separation process schematic diagram based on circulation multi-effect distillation technology；
Fig. 2 is the organic silicon monomer circulation three-effect rectifying separation improvement stream for combining distillation technology based on heat pump-circulation multiple-effect
Journey schematic diagram；
Wherein: E1-feed preheater, T1-take off high tower, and H1-takes off high tower tower bottom reboiler, T9-high boiling tower, H9-height
Tower tower bottom reboiler is boiled, C9-high boiling tower overhead condenser, T2-lightness-removing column, H2-lightness-removing column tower bottom reboiler, C2-are de- light
Column overhead condenser, T3-diformazan tower, H3A-diformazan tower the first reboiler of tower bottom, H3B-diformazan tower the second reboiler of tower bottom,
T4-Yi Jiata, H4-a first tower tower bottom reboiler, a C4-first column overhead condenser, T5-gently divide tower, and H5-gently divides tower tower
Bottom reboiler, C5-gently divide column overhead condenser；The hydrogeneous tower of a T6-first, the hydrogeneous tower tower bottom reboiler of a H6-first, C6-mono-
The hydrogeneous column overhead condenser of first；T7-azeotrope column, H7A-azeotrope column tower bottom reboiler, C7-azeotrope column overhead condenser；T8—
Front three tower, H8-front three tower tower bottom reboiler, P1-compressor, H7B-azeotrope column tower bottom add reboiler, E2-cooler,
P2-dropping valve.
Specific embodiment:
The present invention is described in further detail in the following with reference to the drawings and specific embodiments:
[embodiment 1]
As shown in Figure 1, a kind of method based on circulation multi-effect distillation technology separation organic silicon monomer methylchlorosilane, dress
It is as follows to set connection type: de- high tower T1 overhead vapours pipeline is connected with diformazan tower the first reboiler of tower bottom H3A；Diformazan tower T3 tower top
Jet chimney and a first tower tower bottom reboiler H4, lightness-removing column tower bottom reboiler H2, gently tower tower bottom reboiler H5 is divided to be connected；High pressure is steamed
The condensed high-temperature water pipeline of vapour and feed preheater E1, the hydrogeneous tower tower bottom reboiler H6 of azeotrope column tower bottom reboiler H7A, a first
It is connected；Diformazan tower T3 tower bottom high-temperature product logistics is connected with azeotropic tower bottom reboiler H8.Remaining reboiler and high-pressure steam pipe
Road is connected, and condenser is connected with technical cooling waterpipe.
The present invention uses circulation three-effect distillation technology, and process flow includes the following steps: that 1) raw material crude monomer is preheated
Enter de- high tower T1 afterwards；2) it takes off high tower T1 bottom product and enters high boiling tower T9, high boiling tower T9 overhead fraction returns raw material crude monomer
Tank field is recycled, tower bottom output high-boiling components product；3) high tower T1 tower top output material is taken off into low tower T2 is taken off, and takes off low tower for stream
Journey bifurcation point, tower base stream are large first diformazan product line, and overhead stream is a variety of shallow bid product lines；4) low tower T2 tower bottom is taken off
It after logistics is mixed with T4 tower base stream, is flowed into diformazan tower T3, tower bottom output dimethyldichlorosilane high-temperature product, tower top produces
A first diformazan mixture out is flowed into a first tower C104；One first tower C104 tower top output Trichloromethyl silane product, tower bottom
One first diformazan mixture of output is returned at diformazan tower C103 entrance logistics through pump circulation and is mixed with T2 tower base stream, and described one
Methyl trichlorosilane and dimethyldichlorosilane product are cooled to 40 DEG C of feeding storage tanks.5) it takes off low tower T2 tower top material and enters light point
Tower T5, overhead product are the component mixture that boiling point is higher than methyl hydrogen dichlorosilane or more, and bottom product is to contain methyl hydrogen two
The mixture of chlorosilane, silicon tetrachloride and tri-methyl-chlorosilane successively passes through hydrogeneous tower T6 (the overhead product methyl hydrogen two of a first
Chlorosilane), azeotrope column T7 (overhead product silicon tetrachloride and tri-methyl-chlorosilane azeotropic mixture ensure front three tower product purity) and
Front three tower T8 (tower top output tri-methyl-chlorosilane, tower bottom go out a small amount of impurity, are recycled back to crude monomer tank field or out battery limit (BL)).
The present invention uses circulation three-effect distillation technology, by adjusting the operating pressure and temperature and a first tower tower of each tower
Bottoming cycle uninterrupted, so that de- high tower T1 overhead vapours can be used to give diformazan tower T3 tower bottom reboiler H3 heat supply, diformazan tower T3
Overhead vapours just can to a first tower T4 tower bottom reboiler H4, lightness-removing column T2 tower bottom reboiler H2, gently divide tower H5 tower bottom again
Boil device H5 heat supply.The condensed high-temperature water of high steam, in preheater E1 to the preheating of raw material crude monomer, the hydrogeneous tower T6 tower bottom of a first
Reboiler H6 and the H7A heat supply of azeotrope column T7 tower bottom reboiler；The tower bottom high-temperature product of diformazan tower T3 boils again to front three tower T8 tower bottom
Device H8 heat supply.
The full tower average operating pressure of de- high tower T1 is 300kPa, and overhead reflux ratio is 5, and bottom temperature control exists
130℃；The full pressure tower average operation of the lightness-removing column T2 is 140kPa, and overhead reflux ratio is 90；The diformazan tower T3 is complete
Tower average operating pressure is 180kPa, and overhead reflux ratio is 8, in tower bottom setting there are two reboiler, with different working medium come into
Row heating；The one full tower average operating pressure of first tower T4 is 100kPa, and overhead reflux ratio is 50；Described gently divides tower T5 complete
Tower average operating pressure is 250kPa, and overhead reflux ratio is 1000；The overhead reflux ratio of the hydrogeneous tower T6 of one first is 3, full tower
Pressure is 110kPa；The overhead reflux ratio of the azeotrope column T7 is 160, and full pressure tower is 200kPa；The front three tower T8 is complete
Tower average operating pressure is 100kPa, and overhead reflux ratio is 3.
Compared with existing industrial flow, the steam consumption of the unit monomers product of this flow scheme is 1.21, the index
Lower than the device (unit consumption 2.7) about 55% or so being currently in operation.
[embodiment 2]
As shown in Figure 1, a kind of method based on circulation multi-effect distillation technology separation organic silicon monomer methylchlorosilane, work
Skill process and example example 1 are consistent, wherein the full tower average operating pressure of de- high tower T1 is 400kPa, overhead reflux ratio is
7.6, bottom temperature is controlled at 130 DEG C；The full pressure tower average operation of the lightness-removing column T2 is 110kPa, and overhead reflux ratio is
50；The full tower average operating pressure of diformazan tower T3 is 215kPa, and overhead reflux ratio is 14；The one first tower T4 Quan Taping
Equal operating pressure is 125kPa, and overhead reflux ratio is 90；Described gently divides the full tower average operating pressure of tower T5 to be 285kPa, tower top
Reflux ratio is 910；The overhead reflux ratio of the hydrogeneous tower T6 of one first is 2, and full pressure tower is 100kPa；The tower of the azeotrope column T7
Pushing up reflux ratio is 130, and full pressure tower is 175Pa；The full tower average operating pressure of front three tower T8 is 100kPa, overhead reflux
Than being 3.8.Lightness-removing column T2, gently divide tower T5, there are two reboilers in tower bottom setting by front three tower T8, are carried out with different working medium
Heating.
Compared with existing industrial flow, the steam consumption of the unit monomers product of this flow scheme is 1.26, the index
Lower than the device (unit consumption 2.7) about 54% or so being currently in operation.
[embodiment 3]
As shown in Figure 1, a kind of method based on circulation multi-effect distillation technology separation organic silicon monomer methylchlorosilane, work
Skill process and example example 1 are consistent, wherein the full tower average operating pressure of de- high tower T1 is 450kPa, overhead reflux ratio is
10, bottom temperature is controlled at 130 DEG C；The full pressure tower average operation of the lightness-removing column T2 is 125kPa, and overhead reflux ratio is 75；
The full tower average operating pressure of diformazan tower T3 is 250kPa, and overhead reflux ratio is 20；The one full tower of first tower T4 is average
Operating pressure is 140kPa, and overhead reflux ratio is 130；Described gently divides the full tower average operating pressure of tower T5 to be 250kPa, tower top
Reflux ratio is 800；The overhead reflux ratio of the hydrogeneous tower T6 of one first is 4, and full pressure tower is 120kPa；The tower of the azeotrope column T7
Pushing up reflux ratio is 100, and full pressure tower is 150kPa；The full tower average operating pressure of front three tower T8 is 110kPa, and tower top returns
Stream is than being 5.Lightness-removing column T2, gently divide tower T5, there are two reboilers in tower bottom setting by front three tower T8, are carried out with different working medium
Heating.
Compared with existing industrial flow, the steam consumption of the unit monomers product of this flow scheme is 1.29, the index
Lower than the device (unit consumption 2.7) about 56% or so being currently in operation.
[embodiment 4]
As shown in Fig. 2, a kind of based on heat pump-circulation multiple-effect joint distillation technology separation organic silicon monomer methylchlorosilane
Improved method, technical process and the circulation multi-effect distillation process in Fig. 1 are almost the same, but increase the indirect type of closed loop
Heat pump cycle is realized the efficient utilization of energy using the mechanical work of compressor P2 and the heat of a first tower T4 overhead vapours, is increased
Add economic benefit.
The connection method of this improvement device is as follows: condenser C4 high temperature stream outlet is connected to compressor P1 import, compression
Machine P1 is exported through steam distributor, is connected to diformazan tower the second reboiler of tower bottom H3B, azeotrope column tower bottom adds reboiler H7B's
High temperature substrate flows into mouth, and the high temperature stream outlet that diformazan tower the second reboiler of tower bottom H3B, azeotrope column tower bottom add reboiler H7B connects
It is connected to cooler E2 import, the outlet cooler E2 is connected to dropping valve P2 import, and the outlet dropping valve P2 is connected to condenser C4 high
Warm logistics import constitutes closed loop circulating system.
In addition to the main process flow described in the example 1 of this improved method, additional heat pump distillation closed loop cycle technique stream is constructed
Journey, process are as follows: selected heating working medium exchanges heat at condenser C4 to being gasified totally, through pressing with a first tower T4 overhead vapours
Be sent into the second reboiler of diformazan tower T3 H3B, azeotrope column T7 after contracting machine P1 pressurization and add reboiler H7B heat supply, after through cooler
After B2 is cooled to 48 DEG C, exchange heat again with a first tower T4 overhead vapours after dropping valve P2 is down to normal pressure.Under the improved method, except de-
Other than high tower T1 and high boiling tower T9, remaining tower is not required to additional high steam, thus can be further reduced high pressure significantly
Steam flow demand.
The heating working medium selects silicon tetrachloride/tri-methyl-chlorosilane azeotropic under azeotropic state in present case
Object；In addition, organic matter simple substance/mixture of the boiling point at 50 DEG C or so under the normal pressures such as furans also can be selected；Its compressor outlet pressure
Power is 300kPa, and decompression valve outlet pressure is 60kPa.Remaining each rectifying column operating condition and case 1 are consistent.
Compared with existing industrial flow, the steam consumption of the unit monomers product of this flow scheme is 0.77, the index
Lower than the device (unit consumption 2.7) about 71% or so being currently in operation.
[embodiment 5]
As shown in Fig. 2, a kind of based on heat pump-circulation multiple-effect joint distillation technology separation organic silicon monomer methylchlorosilane
Method, process flow and example example 4 are consistent, wherein the heating working medium selects the tetrachloro under azeotropic state in present case
SiClx/tri-methyl-chlorosilane azeotropic mixture；Its compressor delivery pressure is 600kPa, and decompression valve outlet pressure is 80kPa.Remaining
Each rectifying column operating condition and case 2 are consistent.
Compared with existing industrial flow, the steam consumption of the unit monomers product of this flow scheme is 0.78, the index
Lower than the device (unit consumption 2.7) about 71% or so being currently in operation.
[embodiment 6]
As shown in Fig. 2, a kind of based on heat pump-circulation multiple-effect joint distillation technology separation organic silicon monomer methylchlorosilane
Method, process flow and example example 4 are consistent, wherein the heating working medium selects the tetrachloro under azeotropic state in present case
SiClx/tri-methyl-chlorosilane azeotropic mixture；Its compressor delivery pressure is 450kPa, and decompression valve outlet pressure is 100kPa.Its
Remaining each rectifying column operating condition and case 3 are consistent.
Compared with existing industrial flow, the steam consumption of the unit monomers product of this flow scheme is 0.79, the index
Lower than the device (unit consumption 2.7) about 71% or so being currently in operation.
In conclusion this method separates work using circulation multi-effect distillation technical principle, to organic silicon monomer methylchlorosilane
Skill process realizes the energy-saving effect compared to existing process 55% or so, and cooling water and steam consumption is greatly reduced, has aobvious
Write economic benefit；Its enforcement difficulty is low, and operation possibility is strong with controllability.In improved method, joined using heat pump-circulation multiple-effect
Energy saving amplitude is improved to 71% or so, energy-saving effect is significant with distillation technology by indirect type heat pump cycle.
Claims (9)
1. a kind of device using circulation multi-effect distillation technology separation organosilicon mix monomer methylchlorosilane, it is characterized in that including
Following equipment: feed preheater (E1) takes off high tower (T1), takes off high tower tower bottom reboiler (H1)；High boiling tower (T9), high boiling tower tower bottom
Reboiler (H9), high boiling tower overhead condenser (C9)；Lightness-removing column (T2), lightness-removing column tower bottom reboiler (H2), lightness-removing column tower top are cold
Condenser (C2)；Diformazan tower (T3), diformazan tower the first reboiler of tower bottom (H3A), diformazan tower the second reboiler of tower bottom (H3B)；One first
Tower (T4), a first tower tower bottom reboiler (H4), a first column overhead condenser (C4)；Gently divide tower (T5), gently divides tower tower bottom reboiler
(H5), gently divide column overhead condenser (C5)；The hydrogeneous tower of one first (T6), the hydrogeneous tower tower bottom reboiler (H6) of a first, the hydrogeneous tower of a first
Overhead condenser (C6)；Azeotrope column (T7), azeotrope column tower bottom reboiler (H7A), azeotrope column overhead condenser (C7)；Front three tower
(T8), front three tower tower bottom reboiler (H8), front three column overhead condenser (C8)；De- high tower (T1) overhead vapours outlet is connected to two
First tower the first reboiler of tower bottom (H3A) high temperature fluid import, diformazan tower tower bottom the first reboiler (H3A) high temperature fluid outlet connection
Overhead condensation liquid to de- high tower (T1) exports；Diformazan tower (T3) overhead vapours is exported through steam distributor, is connected to Yi Jiata
Tower bottom reboiler (H4), lightness-removing column tower bottom reboiler (H2), the high temperature fluid import for gently dividing tower tower bottom reboiler (H5), Yi Jiata
Tower bottom reboiler (H4), gently divides the high temperature fluid outlet of tower tower bottom reboiler (H5) to be connected at lightness-removing column tower bottom reboiler (H2)
The overhead condensation liquid of diformazan tower (T3) exports；The condensed high-temperature water pipeline of high steam is connected to feed preheater (E1) high temperature
Fluid inlet, the outlet of feed preheater (E1) high temperature fluid are connected to azeotrope column tower bottom reboiler (H7A) high temperature fluid import, altogether
The outlet of boiling tower tower bottom reboiler (H7A) high temperature fluid is connected to hydrogeneous tower tower bottom reboiler (H6) the high temperature fluid import of a first；Two
First tower (T3) tower bottom high-temperature product logistics stream outlet is connected to azeotropic tower bottom reboiler (H8) high temperature fluid import.
2. device described in claim 1 is applied, it is characterized in that based on normal pressure binary column overhead condenser (C4) building heat pump essence
Evaporate working medium closed circuit circulatory system；Closed circuit circulatory system includes a first tower column overhead condenser (C4), compressor (P1), diformazan tower tower
The second reboiler of bottom (H3B), azeotrope column tower bottom are added reboiler (H7B), cooler (E2), dropping valve (P2)；It improves device
Pipe connecting method is as follows: condenser (C4) high temperature stream outlet is connected to compressor (P1) import, compressor (P1) outlet warp
Steam distributor is connected to diformazan tower the second reboiler of tower bottom (H3B), azeotrope column tower bottom adds the high temperature substrate of reboiler (H7B)
Mouth is flowed into, diformazan tower the second reboiler of tower bottom (H3B), azeotrope column tower bottom add the high temperature stream outlet connection of reboiler (H7B)
To cooler (E2) import, cooler (E2) outlet is connected to dropping valve (P2) import, and dropping valve (P2) outlet is connected to condensation
Device (C4) high temperature substrate flows into mouth, constitutes closed loop cycle circuit.
3. carrying out the side of circulation multi-effect distillation technology separation organosilicon mix monomer methylchlorosilane using claim 1 device
Method, it is characterized in that circulation distillation process is constituted between the Yi Jiata (T3) and diformazan tower (T4), on this basis, to de- height
Tower (T1), diformazan tower (T3) use three-effect rectification method between Yi Jiata (T4), by the tower top material steam of de- high tower (T1) to
Reboiler (H3A) heat supply of diformazan tower (T3) tower bottom, tower top material steam Xiang Yijia tower (T4) tower bottom of diformazan tower (T3) tower top
Reboiler (H4) heat supply；De- high tower (T1) the tower top material steam can separate some vapor, again to lightness-removing column (T2)
Boil reboiler (H5) heat supply of device (H2) He Qingfen tower (T5)；The de- high tower tower bottom reboiler (H1) is cold using high steam
Solidifying heat supply.
4. method as claimed in claim 3, it is characterized in that the condensed high-temperature water of high steam is used to feed preheater
(E1), azeotrope column tower bottom reboiler (H7A), the hydrogeneous tower reboiler of a first (H6) heat supply；The bottom product of diformazan tower (T3) is used for
Front three tower tower bottom reboiler (H8) heat supply is flowed out as product later.
5. method as claimed in claim 3, it is characterized in that de- high tower (T1) and diformazan tower (T3), diformazan tower (T3) and a first tower
(T4), diformazan tower (T3) and lightness-removing column (T2), diformazan tower (T3) and the light temperature difference for dividing tower (T5) are not less than 15 DEG C；Meanwhile it is logical
The tower bottom circulation product flow for overregulating the operation temperature pressure and a first tower (T4) that flow into diformazan tower (T3), makes diformazan tower
(T3) tower top material steam is by chance used to first tower (T4) tower bottom reboiler (H4) enough, takes off low tower (T2) tower bottom reboiler
(H2), gently divide tower (T5) tower bottom reboiler (H5) heat supply.
6. method as claimed in claim 3, it is characterized in that the raw material rectifying separation process includes the following steps；
(1) enter after raw material crude monomer is preheated de- high tower (T1), tower bottom output temperature is not higher than 130 DEG C of mixture, flows into
To in high boiling tower (T9)；High boiling tower overhead vapours is after high boiling tower overhead condenser C9 total condensation is at liquid, refluxing portion stream
Enter high boiling tower (T9), product section is flowed into de- high tower (T1), and tower bottom flows out high-boiling components product；
(2) it is complete through the first reboiler of lightness-removing column tower bottom (H2A), diformazan tower tower bottom reboiler (H3) to take off high tower (T1) overhead vapours
After being condensed into liquid, refluxing portion is flowed into de- high tower (T1), and product section flows into lightness-removing column (T2)；Lightness-removing column (T2) tower bottom one
After first diformazan mix product is mixed with first tower (T4) tower bottom product, it is flowed into diformazan tower (T3)；Diformazan tower (T3) tower top
Mixture steam through a first tower tower bottom reboiler (H4), lightness-removing column tower bottom reboiler (H2), gently divide tower tower bottom reboiler (H5) complete
After full condensation, refluxing portion flows into diformazan tower (T3), and product section is flowed into Yi Jiata (T4), diformazan tower (T3) tower bottom high temperature
High-purity dimethyldichlorosilane product is after the cooling heat supply of front three tower tower bottom reboiler (H8), as dimethyldichlorosilane product
Outflow；The one high-purity Trichloromethyl silane steam of first tower (T4) tower top is after overhead condenser (C4) total condensation, refluxing portion
A first tower (T4) is flowed into, product section is flowed out as Trichloromethyl silane product；One first tower (T4) tower bottom mixture is flowed into
The inlet diformazan tower (T3) is flowed into diformazan tower (T3) after mixing with lightness-removing column (T2) bottom product；
(3) for lightness-removing column (T2) overhead vapours after lightness-removing column overhead condenser (C2) total condensation, refluxing portion flows into lightness-removing column
(T2), product section inflow gently divides in tower (T5)；Gently divide tower (T5) tower top light component product steam through light point column overhead condenser
(C5) after total condensation, refluxing portion inflow gently divides tower (T5), and product section is flowed into as discarded light component outflow, bottom product
Into the hydrogeneous tower of a first (T6)；The hydrogeneous tower of one first (T6) tower top methyl hydrogen dichlorosilane product steam is cold through the hydrogeneous column overhead of a first
After condenser (C6) total condensation, refluxing portion flows into the hydrogeneous tower of a first (T6), and product section is as methyl hydrogen dichlorosilane product
Outflow, bottom product are flowed into azeotrope column (T7)；Azeotrope column (T7) tower top azeotropic mixture product steam is through azeotrope column overhead condensation
After device (C7) total condensation, refluxing portion flows into azeotrope column (T7), and product section is flowed out as azeotropic mixture, and bottom product is flowed into
In front three tower (T8)；Front three tower (T8) tower top tri-methyl-chlorosilane product steam is completely cold through front three column overhead condenser (C8)
After solidifying, refluxing portion flows into front three tower (T8), and product section is flowed out as tri-methyl-chlorosilane product, and bottom product is recycled back to
Head tank sends out battery limit (BL).
7. method as claimed in claim 3, it is characterized in that the overhead reflux ratio of the de- high tower (T1) is 5-10, full pressure tower
For 300kPa-450kPa；The overhead reflux ratio of the lightness-removing column (T2) is 50-90, and full pressure tower is 110kPa-140kPa；Institute
The overhead reflux ratio for stating diformazan tower (T3) is 8-20, and full pressure tower is being 180kPa-250kPa, and tower bottom is equipped with the first reboiler
(H3A) and the second reboiler (H3B), the first reboiler (H3A) use de- high tower tower top material steam heating, the second reboiler
(H3B) heat supply is condensed using high steam；For 50-130, full pressure tower is the overhead reflux ratio of the one first tower (T4)
100kPa-140kPa；The overhead extraction light component for gently dividing tower (T5), reflux ratio 800-1000, full pressure tower are
180kPa-250kP, tower bottom are equipped with the first reboiler (H5A) and the second reboiler (H5B), and the first reboiler (H5A) is using preheating
High-temperature water heat supply afterwards, the second reboiler (H5B) use high steam heat supply；The overhead reflux ratio of the hydrogeneous tower of one first (T6)
For 2-, full pressure tower maintains normal pressure state；The overhead reflux ratio of the azeotrope column (T7) is 100-160, and full pressure tower maintains
For 150kPa-200kPa；For the overhead reflux ratio of the front three tower (T8) for 3-5, full pressure tower maintains normal pressure state.
8. the side that the device of application claim 2 carries out circulation multi-effect distillation technology separation organosilicon mix monomer methylchlorosilane
Method, it is characterized in that choose suitable heating working medium, by indirect type pump rectification method, under normal pressure with it is cold in a first column overhead
It is exchanged heat at condenser (C4) to being gasified totally, is sent into the second reboiler of diformazan tower tower bottom (H3B), azeotropic after compressor (P1) pressurization
Tower tower bottom adds reboiler (H7B), after after cooler (E2) is cooled to 48 DEG C of liquid, after dropping valve (P2) is down to normal pressure
It exchanges heat again at a first column overhead condenser (C4).
9. improved method as claimed in claim 8, it is characterized in that the heating working medium need to be protected in compressor pressure process
The state of being gasified totally is held, while keeping complete liquefaction in dropping valve pressure reduction；The compressor delivery pressure is
300kPa-600kPa, decompression valve outlet pressure are 60kPa-100kPa.
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