CN110282655A - Titanium tetrachloride rectificating method - Google Patents
Titanium tetrachloride rectificating method Download PDFInfo
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- CN110282655A CN110282655A CN201910731756.6A CN201910731756A CN110282655A CN 110282655 A CN110282655 A CN 110282655A CN 201910731756 A CN201910731756 A CN 201910731756A CN 110282655 A CN110282655 A CN 110282655A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/007—Energy recuperation; Heat pumps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
- C01G23/024—Purification of tetrachloride
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Abstract
The present invention provides a kind of titanium tetrachloride rectificating methods.This method carries out rectification process to titanium tetrachloride using first rectifying column and Second distillation column；When being handled using first rectifying column, a part in its kettle liquid is heated to reflux using the first reboiler, and its tower overhead gas is subjected to condensation process using the first condenser；When being handled using Second distillation column, a part in its kettle liquid is heated to reflux using the second reboiler, and the second refluxing opening is set so that a part in its tower overhead gas lime set to flow back in Second distillation column tower top；Wherein, the tower top pressure of Second distillation column is greater than the tower reactor pressure of first rectifying column, before the step of a part in the tower overhead gas lime set by Second distillation column flows back, the tower overhead gas of Second distillation column is passed through to the thermal medium entrance of the first reboiler, is heated to reflux to a part in the kettle liquid by first rectifying column into first rectifying column tower reactor.The present invention effectively reduces the purification energy consumption of titanium tetrachloride.
Description
Technical field
The present invention relates to titanium tetrachlorides to purify field, in particular to a kind of titanium tetrachloride rectificating method.
Background technique
Titanium tetrachloride is the important intermediate for producing Titanium and its compound, is to produce titanium sponge and Titanium Dioxide Produced by Chloride Procedure
Primary raw material, the quality of quality directly affects the quality of titanium sponge and titanium dioxide.Titanium tetrachloride impurity is complex, includes
Low-boiling point material, high boiling substance and the close substance of boiling point, predominantly SiCl4、CH2ClCOCl、POCL3、CHCl2COCl、
CCl3COCl、CH3COCl、SnCl4、VOCl3、AsCl3、VCl4、Al Cl3、Fe Cl3Deng the type and quantity of these impurity are direct
The color of titanium tetrachloride is influenced, it is very big to the performance hazards of subsequent product.
Two rectifying columns interconnected are generallyd use at present, and rectification and purification, the fortune of two rectifying columns are carried out to titanium tetrachloride
Line mode can take off gently after can also first taking off weight first to take off light rear de- weight.The tower bottom of each rectifying column is provided with tower bottom reboiler,
A part of kettle liquid for rectifying tower bottom to be discharged is heated to reflux, and another part then produces or enter next rectifying
It is carried out in tower de- light.And the tower top of each rectifying column is provided with overhead condenser, the tower overhead gas for tower top to be discharged carries out cold
Solidifying to generate tower overhead gas lime set, a part in tower overhead gas lime set is back in former rectifying column, under another part extraction or entrance
De- weight is carried out in one rectifying column.
However, because of the SnCl in impurity4、VOCl3、AsCl3、VCl4Deng with TiCl4Boiling point is very close, and high-purity four chlorination
Titanium requires the content of each impurity to control in 0.1~1ppbw, this just makes titanium tetrachloride purification difficulty bigger, each rectifying of inevitable requirement
Tower has high reflux ratio and high number of theoretical plate, so that titanium tetrachloride purification needs high heat consumption.Therefore, how to guarantee
Purification energy consumption is reduced on the basis of impurity content is up to standard, it is most important for the purification production of high-purity titanium tetrachloride.
Summary of the invention
The main purpose of the present invention is to provide a kind of titanium tetrachloride rectificating methods, to solve in the prior art high-purity four
The excessively high problem of energy consumption in titanium chloride subtractive process.
To achieve the goals above, according to an aspect of the invention, there is provided a kind of titanium tetrachloride rectificating method, uses
First rectifying column interconnected and Second distillation column carry out rectification process to titanium tetrachloride；Wherein, using first rectifying column into
When row rectification process, a part in the kettle liquid of first rectifying column is heated to reflux to first rectifying column tower using the first reboiler
In kettle, and the tower overhead gas of first rectifying column is subjected to condensation process using the first condenser；Rectifying is carried out using Second distillation column
When processing, a part in the kettle liquid of Second distillation column is heated to reflux into Second distillation column tower reactor using the second reboiler,
And the is back in a part that the tower top of Second distillation column is arranged in tower overhead gas lime set of second refluxing opening by Second distillation column
In two rectifying columns；Wherein, the tower top pressure of Second distillation column is greater than the tower reactor pressure of first rectifying column, by Second distillation column
Before the step of a part in tower overhead gas lime set is back to Second distillation column, titanium tetrachloride rectificating method further includes following step
It is rapid: the tower overhead gas of Second distillation column to be passed through to the thermal medium entrance of the first reboiler, in the kettle liquid by first rectifying column
A part is heated to reflux into first rectifying column tower reactor.
Further, the tower overhead gas of Second distillation column is passed through after the thermal medium entrance of the first reboiler, after heat exchange
It is discharged from the thermal medium outlet of the first reboiler, titanium tetrachloride rectificating method is further comprising the steps of: utilizing the second condenser pair
The tower overhead gas of Second distillation column after heat exchange carries out condensing or crossing cold treatment, obtains the tower overhead gas lime set of Second distillation column.
Further, the tower top pressure of first rectifying column be 0.02~0.1MPa of gauge pressure, tower reactor pressure be gauge pressure 0.03~
0.11MPa；The tower top pressure of Second distillation column is 0.15~0.25MPa of gauge pressure, and tower reactor pressure is 0.16~0.26MPa of gauge pressure.
Further, the tower top temperature of first rectifying column is 137~158 DEG C, and bottom temperature is 145~167 DEG C；Second essence
The tower top temperature for evaporating tower is 168~185 DEG C, and bottom temperature is 177~193 DEG C.
Further, the reflux entry ratio of first rectifying column is 1~20, and the reflux entry ratio of Second distillation column is 1~20.
Further, it is provided with the first packing layer in the tower of first rectifying column, is provided with second in the tower of Second distillation column
The filler of packing layer, the first packing layer and/or the second packing layer is wire packing.
Further, rectification process is carried out to titanium tetrachloride using first rectifying column interconnected and Second distillation column
In the process, de- light processing is carried out to titanium tetrachloride using first rectifying column, using Second distillation column to the kettle liquid of first rectifying column
In a part carry out it is de- handle again, and another part in the kettle liquid of first rectifying column is heated to reflux using the first reboiler
Into first rectifying column tower reactor.
Further, rectification process is carried out to titanium tetrachloride using first rectifying column interconnected and Second distillation column
In the process, titanium tetrachloride take off using first rectifying column and be handled again, the first condenser is discharged using Second distillation column
A part in tower overhead gas lime set carries out de- light processing, and the tower top of first rectifying column is additionally provided with the first refluxing opening, and utilizes the
Another part in tower overhead gas lime set that first condenser is discharged is back in first rectifying column by one refluxing opening.
Further, rectification process is carried out to titanium tetrachloride using first rectifying column interconnected and Second distillation column
In the process, de- light processing is carried out to titanium tetrachloride using Second distillation column, using first rectifying column to the kettle liquid of Second distillation column
In a part carry out it is de- handle again, and another part in the kettle liquid of Second distillation column is heated to reflux using the second reboiler
Into Second distillation column tower reactor.
Further, rectification process is carried out to titanium tetrachloride using first rectifying column interconnected and Second distillation column
In the process, titanium tetrachloride take off using Second distillation column and be handled again, using first rectifying column to the tower top of Second distillation column
A part in airsetting liquid carries out de- light processing, and utilizes another portion in the tower overhead gas lime set of the second refluxing opening Second distillation column
Divide and is back in Second distillation column.
It applies the technical scheme of the present invention, provides a kind of titanium tetrachloride rectificating method, this method is using interconnected
First rectifying column and Second distillation column carry out rectification process to titanium tetrachloride；Wherein, rectification process is carried out using first rectifying column
When, a part in the kettle liquid of first rectifying column is heated to reflux into first rectifying column tower reactor using the first reboiler, and benefit
The tower overhead gas of first rectifying column is subjected to condensation process with the first condenser；When carrying out rectification process using Second distillation column, benefit
A part in the kettle liquid of Second distillation column is heated to reflux into Second distillation column tower reactor with the second reboiler, and in the second essence
The tower top for evaporating tower is arranged the second refluxing opening and is back to Second distillation column with a part in the tower overhead gas lime set by Second distillation column
In；Wherein, the tower top pressure of Second distillation column is greater than the tower reactor pressure of first rectifying column, by the tower top airsetting of Second distillation column
Before the step of a part in liquid is back to Second distillation column, titanium tetrachloride rectificating method is further comprising the steps of: by second
The tower overhead gas of rectifying column is passed through the thermal medium entrance of the first reboiler, to a part heating in the kettle liquid by first rectifying column
It is back in first rectifying column tower reactor.
When the present invention provides above-mentioned titanium tetrachloride rectificating method to titanium tetrachloride progress rectification process, the tower of Second distillation column
Pressure on top surface is greater than the tower reactor pressure of first rectifying column, in this way, the tower overhead gas that the tower top of Second distillation column is discharged is compared to the first essence
Evaporate tower tower bottom discharge kettle liquid for have higher temperature.The higher Second distillation column tower overhead gas of temperature is passed directly into first
In the first reboiler thermal medium entrance at rectifying tower bottom, the waste heat of this part tower overhead gas can be efficiently used to first rectifying column
A part in kettle liquid is heated to reflux.In this way, the present invention steams the tower top of high-pressure tower according to differential pressure thermal coupled process principle
Heat source of the vapour as lower pressure column bottom liquid realizes the exchange of cooling and heating load inside titanium tetrachloride rectifying column group, carries out to energy
It applies, effectively reduces the purification energy consumption of high-purity titanium tetrachloride.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 shows titanium tetrachloride rectifier unit schematic diagram according to an embodiment of the present；
Fig. 2 shows the titanium tetrachloride rectifier unit schematic diagrames of another embodiment according to the present invention；
Fig. 3 shows the titanium tetrachloride rectifier unit schematic diagram of another embodiment according to the present invention；And
Fig. 4 shows the titanium tetrachloride rectifier unit schematic diagram of another embodiment according to the present invention.
Wherein, the above drawings include the following reference numerals:
10, first rectifying column；11, the first reboiler；12, the first condenser；13, the first return tank；20, the second rectifying
Tower；21, the second reboiler；22, the second condenser；23, the second return tank.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The present invention will be described in detail below with reference to the accompanying drawings and embodiments.
The application is described in further detail below in conjunction with specific embodiment, these embodiments should not be understood as limitation originally
Apply for range claimed.
As described in background technology part, there are energy consumption mistakes in the subtractive process of high-purity titanium tetrachloride in the prior art
High problem.
In order to solve this problem, the present invention provides a kind of titanium tetrachloride rectificating methods, as shown in Figures 1 to 4, this method
Rectification process is carried out to titanium tetrachloride using first rectifying column 10 interconnected and Second distillation column 20；Wherein, using first
When rectifying column 10 carries out rectification process, a part in the kettle liquid of first rectifying column 10 is heated to reflux using the first reboiler 11
The tower overhead gas of first rectifying column 10 is subjected to condensation process into 10 tower reactor of first rectifying column, and using the first condenser 12；It adopts
When carrying out rectification process with Second distillation column 20, a part in the kettle liquid of Second distillation column 20 is added using the second reboiler 21
Heat is back in 20 tower reactor of Second distillation column, and the second refluxing opening is arranged with by Second distillation column in the tower top of Second distillation column 20
A part in 20 tower overhead gas lime set is back in Second distillation column 20；Wherein, the tower top pressure of Second distillation column 20 is greater than
The tower reactor pressure of first rectifying column 10, a part in the tower overhead gas lime set by Second distillation column 20 are back to Second distillation column
Before 20 the step of, titanium tetrachloride rectificating method is further comprising the steps of: the tower overhead gas of Second distillation column 20 is passed through first again
The thermal medium entrance for boiling device 11, being heated to reflux a part in the kettle liquid of first rectifying column 10 to 10 tower of first rectifying column
In kettle.
When the present invention provides above-mentioned titanium tetrachloride rectificating method to titanium tetrachloride progress rectification process, Second distillation column 20
Tower top pressure is greater than the tower reactor pressure of first rectifying column 10, in this way, the tower overhead gas that is discharged of the tower top of Second distillation column 20 compared to
There is higher temperature for the kettle liquid of 10 tower bottom of first rectifying column discharge.Higher 20 tower overhead gas of Second distillation column of temperature is straight
It connects in the 11 thermal medium entrance of the first reboiler of 10 tower bottom of first rectifying column, the remaining of this part tower overhead gas can be efficiently used
Heat is heated to reflux a part in first rectifying column kettle liquid.In this way, the present invention makes according to differential pressure thermal coupled process principle
Heat source of the overhead vapours of high-pressure tower as lower pressure column bottom liquid realizes the friendship of cooling and heating load inside titanium tetrachloride rectifying column group
It changes, energy is applied, effectively reduce the purification energy consumption of high-purity titanium tetrachloride.
Specifically, using above-mentioned rectificating method, the tower overhead gas of Second distillation column 20 is condensed to cold negative needed for supercooled state
Thermic load needed for lotus can vaporize with 10 kettle liquid of first rectifying column is suitable, and such first reboiler 11 is not necessarily to external heat source, heat
Source load can reduce 30~50%.
Other than the above advantage, the above-mentioned rectificating method of the present invention also has the advantages that Second distillation column 20
Tower overhead gas condense to refrigeration duty needed for supercooled state can with 10 kettle liquid of first rectifying column vaporize needed for thermic load it is suitable when,
The tower top of Second distillation column 20 can be not provided with condenser, reduce number of devices.
It should be noted that the present invention for first rectifying column 10 and Second distillation column 20 rectifying sequence and take off it is frivolous heavy
Type does not limit, and first rectifying column 10 can be arranged in the upstream of Second distillation column 20, titanium tetrachloride is made to first pass through first
Rectifying column 10 take off gently or be taken off and handles again, is carried out de- weight using Second distillation column 20 or is taken off gently, can also be by the second rectifying
The upstream of first rectifying column 10 is arranged in tower 20, make titanium tetrachloride first pass through Second distillation column 20 carry out it is de- light or it is de- handle again,
De- weight is carried out using first rectifying column 10 or is taken off light.The tower top pressure by Second distillation column 20 is only needed to be set above first
The tower reactor pressure of rectifying column 10 can be provided with effect according to above-mentioned differential pressure thermal coupling reduces the energy consumption of titanium tetrachloride rectifier unit.
In the actual production process, the thermal medium outlet that the tower overhead gas of Second distillation column 20 enters the first reboiler 11 carries out
When heat is applied, tower overhead gas itself can total condensation be even subcooled, that just no setting is required is cold for the tower top of Second distillation column 20 at this time
Condenser.Certainly, in order to further increase the production run stability of equipment, in a kind of optional embodiment, the second rectifying
The tower overhead gas of tower 20 is passed through after the thermal medium entrance of the first reboiler 11, from the thermal medium of the first reboiler 11 after heat exchange
Outlet discharge, above-mentioned titanium tetrachloride rectificating method is further comprising the steps of: using 22 pairs of the second condenser after heat exchange the
The tower overhead gas of two rectifying columns 20 carries out condensing or crossing cold treatment, obtains the tower overhead gas lime set of Second distillation column 20.In this way, second
After the tower overhead gas of rectifying column 20 enters the thermal medium outlet of the first reboiler 11 and completes heat exchange, second can be further utilized
22 pairs of the condenser tower overhead gases Jing Guo heat exchange are further condensed or cross cold treatment, to obtain the tower top of Second distillation column 20
Airsetting liquid.It should be noted that the tower overhead gas of Second distillation column 20 through the first reboiler 11 condensation after can total condensation or supercooling,
The cold source flow of such second condenser 22 can reduce the numerical value for very little or even (the second condenser 22 when being 0 that is reduced to 0
Cancel), therefore the cold source load of the second condenser 22 can reduce 30~50%.
Above-mentioned introduction according to the present invention can be adjusted the technological parameter of step each in the above method.In one kind
In preferred embodiment, the tower top pressure of first rectifying column is 0.02~0.1MPa of gauge pressure, tower reactor pressure be gauge pressure 0.03~
0.11MPa；The tower top pressure of Second distillation column is 0.15~0.25MPa of gauge pressure, and tower reactor pressure is 0.16~0.26MPa of gauge pressure.
In this way, the better effect of the differential pressure thermal coupling in rectification process twice, while titanium tetrachloride rectification effect is more preferably.It is highly preferred that
The tower top temperature of first rectifying column is 137~158 DEG C, and bottom temperature is 145~167 DEG C；The tower top temperature of Second distillation column is
168~185 DEG C, bottom temperature is 177~193 DEG C.
In a preferred embodiment, the reflux entry ratio of first rectifying column 10 is 1~20, Second distillation column 20
Reflux entry ratio is 1~20.Within the above range by the reflux ratio setting in rectification process twice, the rectification effect of titanium tetrachloride
More preferably.
In order to further decrease production energy consumption, in a preferred embodiment, setting in the tower of first rectifying column 10
There is the first packing layer, be provided with the second packing layer in the tower of Second distillation column 20, the first packing layer and/or the second packing layer are filled out
Material is wire packing.The pressure drop of wire packing is small, and after wire packing, the tower top and tower bottom pressure difference of rectifying column can be reduced to
0.01~0.02MPa, and the tower top and tower bottom pressure difference of sieve plate or valve tower under same theory plate number are 0.05~0.3MPa.It adopts
After wire packing, when fixing 10 tower top pressure of first rectifying column, tower pressure drop is reduced, the tower reactor pressure of first rectifying column 10
It is further decreased with temperature, the tower top pressure and temperature of corresponding Second distillation column 20 coupled thereto reduce, this just can reduce
The quality of 21 heat source of the second reboiler (such as vapor) of 20 tower bottom of Second distillation column, so as to further decrease four chlorinations
The purification energy consumption of titanium.
As it was noted above, the above method for first rectifying column 10 and Second distillation column 20 the order of connection and take off it is frivolous heavy
Type does not limit, for example can use following several processing modes:
In a kind of typical embodiment, as shown in Figure 1, using first rectifying column 10 interconnected and the second rectifying
During tower 20 carries out rectification process to titanium tetrachloride, de- light processing is carried out to titanium tetrachloride A using first rectifying column 10, is adopted
A part in the kettle liquid of first rectifying column 10 take off with Second distillation column 20 and is handled again, and will using the first reboiler 11
Another part in the kettle liquid of first rectifying column 10 is heated to reflux into 10 tower reactor of first rectifying column.In the actual production process,
After titanium tetrachloride carries out de- light processing into first rectifying column 10, the tower overhead gas of first rectifying column 10 is condensed into the first condenser 12
Liquid a part is back to first rectifying column 10, and another part is produced to be produced as the tower reactor of low boiling impurity first rectifying column 10
A part returns to the tower reactor of first rectifying column 10 after heating into the first reboiler 11, another part is into Second distillation column 20；Second
Rectifying column 20 take off and is handled again, after tower overhead gas carries out heat exchange into the first reboiler 11, further into the second condenser 22
Condensation, condensate liquid a part are back to Second distillation column 20, and another part extraction is used as titanium tetrachloride purified product B, the second essence
Evaporate tower reactor of the tower reactor extraction a part of tower 20 into return Second distillation column 20 after the heating of the second reboiler 21, another part extraction
As high-boiling-point impurity.
In another typical embodiment, as shown in Fig. 2, using first rectifying column 10 interconnected and the second essence
Evaporate during tower 20 carries out rectification process to titanium tetrachloride, using first rectifying column 10 to titanium tetrachloride A carry out it is de- handle again,
A part in tower overhead gas lime set that first condenser 12 is discharged using Second distillation column 20 carries out de- light processing, the first rectifying
The tower top of tower 10 is additionally provided with the first refluxing opening, and in the tower overhead gas lime set the first condenser 12 being discharged using the first refluxing opening
Another part be back in first rectifying column 10.In the actual production process, titanium tetrachloride is taken off into first rectifying column 10
It handles again, for the tower overhead gas of first rectifying column 10 into the first condenser 12, condensate liquid a part is back to first rectifying column 10, another
Part is produced into Second distillation column 20, and tower reactor extraction a part of first rectifying column 10 is into returning to the after the heating of the first reboiler 11
The tower reactor of one rectifying column 10, another part is as high-boiling-point impurity；Second distillation column 20 carries out de- light processing, and tower overhead gas is into first
Reboiler 11 condenses, and into the second condenser 22, further condensation, condensate liquid a part are back to Second distillation column 20 to condensate liquid, separately
A part extraction is used as low boiling impurity, and 20 tower reactor of Second distillation column extraction a part is into returning to the after the heating of the second reboiler 21
Two tower bottom of rectifying tower, another part extraction are used as titanium tetrachloride purified product B.
In another typical embodiment, as shown in figure 3, using first rectifying column 10 interconnected and the second essence
During evaporating tower 20 to titanium tetrachloride progress rectification process, de- light processing is carried out to titanium tetrachloride A using Second distillation column 20,
A part in the kettle liquid of Second distillation column 20 take off using first rectifying column 10 and is handled again, and utilizes the second reboiler 21
Another part in the kettle liquid of Second distillation column 20 is heated to reflux into 20 tower reactor of Second distillation column.In actual production process
In, titanium tetrachloride carries out de- light processing into Second distillation column 20, and the tower overhead gas of Second distillation column 20 is condensed into the first reboiler 11,
Condensate liquid is back to Second distillation column into the second further condensation of condenser 22, condensate liquid a part, and another part produces conduct
Low boiling impurity, 20 tower reactor of Second distillation column extraction a part return to Second distillation column tower reactor after heating into the second reboiler 21,
Another part is into first rectifying column 10；First rectifying column 10 carry out it is de- handle again, tower overhead gas is into the first condenser 12, condensate liquid one
It is partly refluxed to first rectifying column, another part extraction is used as titanium tetrachloride purified product B, and first rectifying column tower reactor produces one
First rectifying column tower reactor is returned to after dividing into the heating of the first reboiler 11, another part extraction is used as high-boiling-point impurity.
In another typical embodiment, as shown in figure 4, using first rectifying column 10 interconnected and the second essence
Evaporate during tower 20 carries out rectification process to titanium tetrachloride, using Second distillation column 20 to titanium tetrachloride A carry out it is de- handle again,
De- light processing is carried out to a part in the tower overhead gas lime set of Second distillation column 20 using first rectifying column 10, and is utilized second time
Another part in the tower overhead gas lime set of Second distillation column 20 is back in Second distillation column 20 by head piece.In actual production process
In, titanium tetrachloride take off into Second distillation column 20 and be handled again, and 20 tower overhead gas of Second distillation column is condensed into the first reboiler 11, cold
For lime set into the further condensation of the second condenser 22, condensate liquid a part is back to Second distillation column 20, and another part is produced into the
One rectifying column 10；20 tower reactor of Second distillation column extraction a part returns to 20 tower of Second distillation column after heating into the second reboiler 21
Kettle, another part is as high-boiling-point impurity；First rectifying column 10 carries out de- light processing, and tower overhead gas is condensed into the first condenser 12
Liquid a part is back to first rectifying column, and another part extraction is used as low boiling impurity, and 10 tower reactor of first rectifying column produces one
10 tower reactor of first rectifying column is returned to after dividing into the heating of the first reboiler 11, another part extraction is used as titanium tetrachloride purified product B.
According to another aspect of the present invention, the present invention also provides a kind of titanium tetrachloride rectifier units, as shown in Figures 1 to 4,
It includes first rectifying column 10 interconnected and Second distillation column 20, for carrying out rectification process to titanium tetrachloride；First essence
The tower bottom for evaporating tower 10 is provided with the first reboiler 11 being connected with the tower reactor of first rectifying column 10, and tower top is provided with and the first rectifying
The first connected condenser 12 of 10 tower overhead gas of tower outlet；The tower bottom of Second distillation column 20 is provided with the tower reactor with Second distillation column 20
The second connected reboiler 21, tower top are provided with the second refluxing opening；Wherein, the tower overhead gas of Second distillation column 20 is exported with first again
The thermal medium entrance of boiling device 11 is connected by thermal medium pipeline, the thermal medium outlet and Second distillation column 20 of the first reboiler 11
The second refluxing opening be connected by reflux pipeline, and the tower top pressure of Second distillation column 20 be greater than first rectifying column 10 tower reactor
Pressure.
When the present invention provides above-mentioned titanium tetrachloride rectifier unit to titanium tetrachloride progress rectification process, Second distillation column 20
Tower top pressure is greater than the tower reactor pressure of first rectifying column 10, in this way, the tower overhead gas that is discharged of the tower top of Second distillation column 20 compared to
There is higher temperature for the kettle liquid of 10 tower bottom of first rectifying column discharge.Higher 20 tower overhead gas of Second distillation column of temperature is straight
It connects in the 11 thermal medium entrance of the first reboiler of 10 tower bottom of first rectifying column, the remaining of this part tower overhead gas can be efficiently used
Heat is heated to reflux a part in first rectifying column kettle liquid.In this way, the present invention makes according to differential pressure thermal coupled process principle
Heat source of the overhead vapours of high-pressure tower as lower pressure column bottom liquid realizes the friendship of cooling and heating load inside titanium tetrachloride rectifying column group
It changes, energy is applied, effectively reduce the purification energy consumption of high-purity titanium tetrachloride.
Specifically, using above-mentioned rectifier unit, the tower overhead gas of Second distillation column 20 is condensed to cold negative needed for supercooled state
Thermic load needed for lotus can vaporize with 10 kettle liquid of first rectifying column is suitable, and such first reboiler 11 is not necessarily to external heat source, heat
Source load can reduce 30~50%.
Other than the above advantage, the above-mentioned rectifier unit of the present invention also has the advantages that Second distillation column 20
Tower overhead gas condense to refrigeration duty needed for supercooled state can with 10 kettle liquid of first rectifying column vaporize needed for thermic load it is suitable when,
The tower top of Second distillation column 20 can be not provided with the second condenser 22.
It should be noted that the present invention for first rectifying column 10 and Second distillation column 20 the order of connection and take off it is frivolous heavy
Type does not limit, and first rectifying column 10 can be arranged in the upstream of Second distillation column 20, titanium tetrachloride is made to first pass through first
Rectifying column 10 take off gently or be taken off and handles again, is carried out de- weight using Second distillation column 20 or is taken off gently, can also be by the second rectifying
The upstream of first rectifying column 10 is arranged in tower 20, make titanium tetrachloride first pass through Second distillation column 20 carry out it is de- light or it is de- handle again,
De- weight is carried out using first rectifying column 10 or is taken off light.The tower top pressure by Second distillation column 20 is only needed to be set above first
The tower reactor pressure of rectifying column 10 can be provided with effect according to above-mentioned differential pressure thermal coupling reduces the energy consumption of titanium tetrachloride rectifier unit.
In the actual production process, the thermal medium outlet that the tower overhead gas of Second distillation column 20 enters the first reboiler 11 carries out
When heat is applied, tower overhead gas itself can total condensation be even subcooled, that just no setting is required is cold for the tower top of Second distillation column 20 at this time
Condenser.Certainly, in order to further increase the production run stability of equipment, in a kind of optional embodiment, titanium tetrachloride
Rectifier unit further includes the second condenser 22, and the second condenser 22 is arranged on reflux pipeline, the import of the second condenser 22 with
The thermal medium outlet of first reboiler 11 is connected, and the outlet of the second condenser 22 is connected with the second refluxing opening.In this way,
The tower overhead gas of two rectifying columns 20 enters the thermal medium outlet of the first reboiler 11 and after completing heat exchange, can further utilize the
Tower overhead gas of two 22 pairs of the condensers Jing Guo heat exchange is further condensed or crosses cold treatment, to obtain the tower of Second distillation column 20
Top gas lime set.It should be noted that the tower overhead gas of Second distillation column 20 being capable of total condensation or mistake after the condensation of the first reboiler 11
Cold, the cold source flow of such second condenser 22 can reduce the numerical value for very little or even (the second condenser 22 when being 0 that is reduced to 0
Can cancel), therefore the cold source load of the second condenser 22 can reduce 30~50%.
In order to further decrease the heat source quality of the second reboiler 21, and then energy consumption is further decreased, a kind of preferred
In embodiment, it is provided with the first packing layer in the tower of first rectifying column 10, second is provided in the tower of Second distillation column 20 and is filled out
The filler of the bed of material, the first packing layer and/or the second packing layer is wire packing.The pressure drop of wire packing is small, using wire packing
Afterwards, the tower top of rectifying column and tower bottom pressure difference can be reduced to 0.01~0.02MPa, and sieve plate or valve tower under same theory plate number
Tower top and tower bottom pressure difference be 0.05~0.3MPa.After wire packing, when fixing 10 tower top pressure of first rectifying column, tower is set
Standby pressure drop reduces, and the tower reactor pressure and temperature of first rectifying column 10 further decreases, corresponding Second distillation column 20 coupled thereto
Tower top pressure and temperature reduce, this just can reduce 20 tower bottom of Second distillation column 21 heat source of the second reboiler (such as water steam
Gas) quality, so as to further decrease the purification energy consumption of titanium tetrachloride.
As it was noted above, the present invention for first rectifying column 10 and Second distillation column 20 the order of connection and take off frivolous heavy class
Type does not limit, for example can use following several set-up modes:
In a kind of typical embodiment, as shown in Figure 1, first rectifying column 10 is provided with titanium tetrachloride import to four
Titanium chloride A carries out de- light processing, and Second distillation column 20 and first rectifying column 10 are connected with each other with the kettle liquid to first rectifying column 10
In a part carry out it is de- handle again, the first reboiler 11 is connected with by first rectifying column 10 with the tower reactor of first rectifying column 10
Another part in kettle liquid is heated and refluxed for into the tower reactor of first rectifying column 10.In the actual production process, titanium tetrachloride into
After first rectifying column 10 carries out de- light processing, the tower overhead gas of first rectifying column 10 into the first condenser 12, return by condensate liquid a part
It flow to first rectifying column 10, another part extraction is a part of into the as the tower reactor extraction of low boiling impurity first rectifying column 10
The tower reactor of first rectifying column 10 is returned to after the heating of one reboiler 11, another part is into Second distillation column 20；Second distillation column 20 into
Row is de- to be handled again, after tower overhead gas carries out heat exchange into the first reboiler 11, into the second further condensation of condenser 22, condensate liquid
A part is back to Second distillation column 20, and another part extraction is used as titanium tetrachloride purified product B, the tower reactor of Second distillation column 20
Into the tower reactor of return Second distillation column 20 after the heating of the second reboiler 21, another part produces miscellaneous as higher boiling extraction a part
Matter.
In another typical embodiment, as shown in Fig. 2, first rectifying column 10 is provided with titanium tetrachloride import with right
Titanium tetrachloride A take off and is handled again, and Second distillation column 20 and first rectifying column 10 are connected with each other so that the first condenser 12 to be discharged
Tower overhead gas lime set in a part carry out de- light processing, the tower top of first rectifying column 10 is additionally provided with the first refluxing opening, first
Refluxing opening is connected with the first condenser 12 is back to another part in tower overhead gas lime set that the first condenser 12 is discharged
In one rectifying column 10.In the actual production process, titanium tetrachloride take off into first rectifying column 10 and be handled again, first rectifying column 10
Tower overhead gas into the first condenser 12, condensate liquid a part is back to first rectifying column 10, and another part is produced into the second rectifying
Tower 20, tower reactor extraction a part of first rectifying column 10 return to the tower reactor of first rectifying column 10 after heating into the first reboiler 11,
Another part is as high-boiling-point impurity；Second distillation column 20 carries out de- light processing, and tower overhead gas is condensed into the first reboiler 11, condensed
Liquid is back to Second distillation column 20 into the second further condensation of condenser 22, condensate liquid a part, and another part extraction is as low
Boiling contaminants, 20 tower reactor of Second distillation column extraction a part is into return Second distillation column tower reactor after the heating of the second reboiler 21, separately
A part extraction is used as titanium tetrachloride purified product B.
In another typical embodiment, as shown in figure 3, Second distillation column 20 is provided with titanium tetrachloride import with right
Titanium tetrachloride A carries out de- light processing, and first rectifying column 10 and Second distillation column 20 are connected with each other with the kettle to Second distillation column 20
A part in liquid carry out it is de- handle again, the second reboiler 21 is connected with by Second distillation column 20 with the tower reactor of Second distillation column 20
Kettle liquid in another part be heated to reflux into Second distillation column 20.In the actual production process, titanium tetrachloride is smart into second
It evaporates tower 20 and carries out de- light processing, the tower overhead gas of Second distillation column 20 is condensed into the first reboiler 11, and condensate liquid is into the second condenser
22 further condensations, condensate liquid a part are back to Second distillation column, and another part extraction is used as low boiling impurity, the second rectifying
20 tower reactor of tower extraction a part is into Second distillation column tower reactor is returned after the heating of the second reboiler 21, and another part is into first rectifying column
10；First rectifying column 10 take off and is handled again, and tower overhead gas is back to the first rectifying into the first condenser 12, condensate liquid a part
Tower, another part extraction are used as titanium tetrachloride purified product B, and first rectifying column tower reactor extraction a part adds into the first reboiler 11
First rectifying column tower reactor is returned to after heat, another part extraction is used as high-boiling-point impurity.
In another typical embodiment, as shown in figure 4, Second distillation column 20 is provided with titanium tetrachloride import with right
Titanium tetrachloride A take off and is handled again；First rectifying column 10 and Second distillation column 20 are connected with each other with the tower to Second distillation column 20
A part in top gas lime set carries out de- light processing, and the second refluxing opening is used for will be another in the tower overhead gas lime set of Second distillation column 20
A part is back in Second distillation column 20.In the actual production process, titanium tetrachloride take off into Second distillation column 20 and locate again
Reason, 20 tower overhead gas of Second distillation column are condensed into the first reboiler 11, and condensate liquid is further condensed into the second condenser 22, condensate liquid
A part is back to Second distillation column 20, and another part is produced into first rectifying column 10；20 tower reactor of Second distillation column produces one
20 tower reactor of Second distillation column is returned to after dividing into the heating of the second reboiler 21, another part is as high-boiling-point impurity；First rectifying column
10 carry out de- light processing, and for tower overhead gas into the first condenser 12, condensate liquid a part is back to first rectifying column, another part extraction
As low boiling impurity, 10 tower reactor of first rectifying column extraction a part returns to first rectifying column 10 after heating into the first reboiler 11
Tower reactor, another part extraction are used as titanium tetrachloride purified product B.
When first rectifying column 10 is provided with titanium tetrachloride import to carry out de- light processing to titanium tetrachloride, positioned at downstream
Tower top pressure in Second distillation column 20 is relatively high.In order to keep the charging of Second distillation column 20 more smooth, a kind of preferred
Embodiment in, be additionally provided with booster pump on the feeding pipe of Second distillation column 20.
In a preferred embodiment, as shown in Fig. 1,3,4, titanium tetrachloride rectifier unit further includes the first return tank
13, the tower top of first rectifying column 10 is additionally provided with the first refluxing opening, and the import of the first return tank 13 goes out with the first condenser 12
Mouthful be connected, the outlet of the first return tank 13 is connected with the first refluxing opening, and the outlet of the first return tank 13 and the first refluxing opening it
Between pipeline on be provided with first rectifying column 10 tower overhead gas lime set extraction branch.Preferably, as shown in Fig. 2, titanium tetrachloride
Rectifier unit further includes the first return tank 13, and the import of the first return tank 13 is connected with the outlet of the first condenser 12, and first time
The outlet of stream tank 13 is connected with the import of the first refluxing opening and Second distillation column 20 respectively.
In a preferred embodiment, as shown in Figure 1, 2, 3, titanium tetrachloride rectifier unit further includes the second return tank
23, the import of the second return tank 23 is connected with the outlet of the second condenser 22, the outlet of the second return tank 23 and the second refluxing opening
It is connected, and is additionally provided with the tower overhead gas of Second distillation column 20 on the pipeline between the outlet and the second refluxing opening of the second return tank 23
The extraction branch of lime set.Preferably, as shown in figure 4, titanium tetrachloride rectifier unit further includes the second return tank 23, the second return tank
23 import is connected with the outlet of the second condenser 22, and the outlet of the second return tank 23 is respectively at the second refluxing opening and the first rectifying
The import of tower 10 is connected.
Beneficial effects of the present invention are further illustrated by the following examples:
Embodiment 1
The crude titanic chloride liquid treating capacity that titanium tetrachloride mass content is 99.8% is 5000kg/h, and product requirement reaches high
Pure titanium tetrachloride index: the content of each impurity is controlled in 0.1~1ppbw.
The refining plant used in the present embodiment is as shown in Figure 1, the filler in two rectifying columns is wire packing, device
Technological parameter is as follows:
Embodiment 2
Embodiment 2 compared with Example 1, improves the temperature and pressure of rectifying column, the second reboiler heat source vapor by
1.3MPa (A) becomes 1.9MPa (A), and product quality is declined slightly.
Embodiment 3
Embodiment 3 compared with Example 1, improves the reflux entry ratio of tower, and product quality improves, and each impurity quality substantially may be used
Control is in 0.1ppbw, but energy consumption increases.
Embodiment 4
The crude titanic chloride liquid treating capacity that titanium tetrachloride mass content is 99.8% is 5000kg/h, and product requirement reaches high
Pure titanium tetrachloride index: the content of each impurity is controlled in 0.1~1ppbw.
The refining plant used in the present embodiment is as shown in Figure 1, two rectifying tower internals is sieve plates, and device technique parameter is such as
Following table, when using embodiment 1, tower internals is wire packing, and tower top and tower reactor pressure difference are 0.01MPa, Second distillation column tower reactor
Temperature is 177 DEG C, and 1.2MPa and 191.5 DEG C of saturated vapor can be used in heat source, and the present embodiment, tower internals are sieve plate, tower top
It is 0.05MPa with tower reactor pressure difference, Second distillation column bottom temperature is 195 DEG C, and 1.8MPa and 209.8 DEG C of saturation can be used in heat source
Steam, heat source quality greatly improve.
Comparative example 1
The crude titanic chloride liquid treating capacity that titanium tetrachloride mass content is 99.8% is 5000kg/h, and product requirement reaches high
Pure titanium tetrachloride index: the content of each impurity is controlled in 0.1~1ppbw.
Refining plant that the comparative example uses as shown in Figure 1, the difference is that, do not use differential pressure heat coupling technique, the
The tower overhead gas of two rectifying columns does not enter the first reboiler thermal medium entrance, but directly condenses through the second condenser, condensed
Lime set a part is back in Second distillation column, another part extraction.Filler in two rectifying columns is wire packing, device
Technological parameter is as follows:
It can be seen from the above description that the above embodiments of the present invention realized the following chievements:
Using after differential pressure thermal coupled process in embodiment 1, refrigeration duty and thermic load compared to comparative example 1 reduce respectively
52.6% and 50%
In short, when the present invention provides above-mentioned titanium tetrachloride rectifier unit to titanium tetrachloride progress rectification process, the second rectifying
The tower top pressure of tower is greater than the tower reactor pressure of first rectifying column, in this way, the tower overhead gas that is discharged of the tower top of Second distillation column compared to
There is higher temperature for the kettle liquid of first rectifying column tower bottom discharge.The higher Second distillation column tower overhead gas of temperature is directly logical
Enter in the first reboiler thermal medium entrance of first rectifying column tower bottom, the waste heat of this part tower overhead gas can be efficiently used to first
A part in rectifying column kettle liquid is heated to reflux.In this way, the present invention makes high-pressure tower according to differential pressure thermal coupled process principle
Heat source of the overhead vapours as lower pressure column bottom liquid realizes the exchange of cooling and heating load inside titanium tetrachloride rectifying column group, to energy
Amount is applied, and the purification energy consumption of high-purity titanium tetrachloride is effectively reduced.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of titanium tetrachloride rectificating method, using first rectifying column interconnected (10) and Second distillation column (20) to tetrachloro
Change titanium and carries out rectification process；Wherein, it when carrying out rectification process using the first rectifying column (10), utilizes the first reboiler (11)
A part in the kettle liquid of the first rectifying column (10) is heated to reflux into the first rectifying column (10) tower reactor, and is utilized
The tower overhead gas of the first rectifying column (10) is carried out condensation process by the first condenser (12)；Using the Second distillation column (20)
When carrying out rectification process, a part in the kettle liquid of the Second distillation column (20) is heated to reflux using the second reboiler (21)
The second refluxing opening is set by described the in the Second distillation column (20) tower reactor, and in the tower top of the Second distillation column (20)
A part in the tower overhead gas lime set of two rectifying columns (20) is back in the Second distillation column (20)；
It is characterized in that, the tower top pressure of the Second distillation column (20) is greater than the tower reactor pressure of the first rectifying column (10),
The step of a part in the tower overhead gas lime set of the Second distillation column (20) is back to the Second distillation column (20) it
Before, the titanium tetrachloride rectificating method is further comprising the steps of: the tower overhead gas of the Second distillation column (20) is passed through described
The thermal medium entrance of one reboiler (11), being heated to reflux a part in the kettle liquid of the first rectifying column (10) to institute
It states in first rectifying column (10) tower reactor.
2. titanium tetrachloride rectificating method according to claim 1, which is characterized in that the tower top of the Second distillation column (20)
Gas is passed through after the thermal medium entrance of first reboiler (11), is situated between after heat exchange from the heat of first reboiler (11)
Matter outlet discharge, the titanium tetrachloride rectificating method are further comprising the steps of: using the second condenser (22) to after heat exchange
The Second distillation column (20) tower overhead gas carry out condense or cross cold treatment, obtain the tower overhead gas of the Second distillation column (20)
Lime set.
3. titanium tetrachloride rectificating method according to claim 1 or 2, which is characterized in that the first rectifying column (10)
Tower top pressure is 0.02~0.1MPa of gauge pressure, and tower reactor pressure is 0.03~0.11MPa of gauge pressure；The tower of the Second distillation column (20)
Pressure on top surface is 0.15~0.25MPa of gauge pressure, and tower reactor pressure is 0.16~0.26MPa of gauge pressure.
4. titanium tetrachloride rectificating method according to claim 3, which is characterized in that the tower top of the first rectifying column (10)
Temperature is 137~158 DEG C, and bottom temperature is 145~167 DEG C；The tower top temperature of the Second distillation column (20) is 168~185
DEG C, bottom temperature is 177~193 DEG C.
5. titanium tetrachloride rectificating method according to claim 4, which is characterized in that the reflux of the first rectifying column (10)
Charge ratio is 1~20, and the reflux entry ratio of the Second distillation column (20) is 1~20.
6. titanium tetrachloride rectificating method according to any one of claim 1 to 5, which is characterized in that first rectifying
It is provided with the first packing layer in the tower of tower (10), is provided with the second packing layer in the tower of the Second distillation column (20), described
The filler of one packing layer and/or second packing layer is wire packing.
7. titanium tetrachloride rectificating method according to any one of claim 1 to 6, which is characterized in that using interconnection
The first rectifying column (10) and the Second distillation column (20) to titanium tetrachloride carry out rectification process during, using institute
It states first rectifying column (10) and de- light processing is carried out to the titanium tetrachloride, using the Second distillation column (20) to first essence
Evaporate a part in the kettle liquid of tower (10) carry out it is de- handle again, and using first reboiler (11) by the first rectifying column
(10) another part in kettle liquid is heated to reflux into the first rectifying column (10) tower reactor.
8. titanium tetrachloride rectificating method according to any one of claim 1 to 6, which is characterized in that using interconnection
The first rectifying column (10) and the Second distillation column (20) to titanium tetrachloride carry out rectification process during, using institute
State first rectifying column (10) to the titanium tetrachloride carry out it is de- handle again, it is cold to described first using the Second distillation column (20)
A part in the tower overhead gas lime set of condenser (12) discharge carries out de- light processing, and the tower top of the first rectifying column (10) is also set up
There is the first refluxing opening, and another in the tower overhead gas lime set for utilizing first refluxing opening that first condenser (12) is discharged
It is partly refluxed in the first rectifying column (10).
9. titanium tetrachloride rectificating method according to any one of claim 1 to 6, which is characterized in that using interconnection
The first rectifying column (10) and the Second distillation column (20) to titanium tetrachloride carry out rectification process during, using institute
It states Second distillation column (20) and de- light processing is carried out to the titanium tetrachloride, using the first rectifying column (10) to second essence
Evaporate a part in the kettle liquid of tower (20) carry out it is de- handle again, and using second reboiler (21) by the Second distillation column
(20) another part in kettle liquid is heated to reflux into the Second distillation column (20) tower reactor.
10. titanium tetrachloride rectificating method according to any one of claim 1 to 6, which is characterized in that using interconnection
The first rectifying column (10) and the Second distillation column (20) to titanium tetrachloride carry out rectification process during, using institute
State Second distillation column (20) to the titanium tetrachloride carry out it is de- handle again, using the first rectifying column (10) to second essence
It evaporates a part in the tower overhead gas lime set of tower (20) and carries out de- light processing, and utilize Second distillation column described in second refluxing opening
(20) another part in tower overhead gas lime set is back in the Second distillation column (20).
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