CN110282655B - Titanium tetrachloride rectification method - Google Patents
Titanium tetrachloride rectification method Download PDFInfo
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- CN110282655B CN110282655B CN201910731756.6A CN201910731756A CN110282655B CN 110282655 B CN110282655 B CN 110282655B CN 201910731756 A CN201910731756 A CN 201910731756A CN 110282655 B CN110282655 B CN 110282655B
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- 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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- C01G23/024—Purification of tetrachloride
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Abstract
The invention provides a titanium tetrachloride rectification method. The method comprises the steps of rectifying titanium tetrachloride by adopting a first rectifying tower and a second rectifying tower; when the first rectifying tower is adopted for treatment, a part of the kettle liquid is heated and refluxed by using a first reboiler, and the top gas of the tower is condensed by using a first condenser; when a second rectifying tower is adopted for treatment, a second reboiler is utilized to heat and reflux a part of the kettle liquid, and a second reflux opening is arranged at the top of the second rectifying tower so as to reflux a part of the gas condensate at the top of the second rectifying tower; and before the step of refluxing a part of the top gas condensate of the second rectifying tower, introducing the top gas of the second rectifying tower into a heat medium inlet of the first reboiler to heat and reflux a part of the bottom liquid of the first rectifying tower into the bottom of the first rectifying tower. The method effectively reduces the refining energy consumption of the titanium tetrachloride.
Description
Technical Field
The invention relates to the field of titanium tetrachloride purification, and particularly relates to a titanium tetrachloride rectification method.
Background
Titanium tetrachloride is an important intermediate for producing metal titanium and compounds thereof, is a main raw material for preparing titanium sponge and titanium dioxide by a chlorination process, and the quality of the titanium tetrachloride directly influences the quality of the titanium sponge and the titanium dioxide. Titanium tetrachloride impurities are complex and include low boiling point materials, high boiling point materials and close boiling point materials, primarily SiCl4、CH2ClCOCl、POCL3、CHCl2COCl、CCl3COCl、CH3COCl、SnCl4、VOCl3、AsCl3、VCl4、Al Cl3、Fe Cl3And the types and the amount of the impurities directly influence the color of the titanium tetrachloride, and the damage to the performance of subsequent products is great.
At present, two mutually connected rectifying towers are generally adopted to carry out rectification and purification on titanium tetrachloride, and the two rectifying towers can operate in a mode of removing light firstly and then removing heavy, and can also remove heavy firstly and then removing light. The tower bottom reboiler is arranged at the tower bottom of each rectifying tower and used for heating and refluxing one part of the kettle liquid discharged from the tower bottom of the rectifying tower, and the other part of the kettle liquid is extracted or enters the next rectifying tower for removing light. And the top of each rectifying tower is provided with a top condenser for condensing the top gas discharged from the top of the tower to generate top gas condensate, one part of the top gas condensate flows back to the original rectifying tower, and the other part of the top gas condensate is extracted or enters the next rectifying tower for de-weighting.
However, due to SnCl in the impurities4、VOCl3、AsCl3、VCl4Is equal to TiCl4The boiling points are very close, and the content of each impurity of high-purity titanium tetrachloride is required to be controlled to be 0.1-1 ppbw, so that the refining difficulty of the titanium tetrachloride is higher, and each rectifying tower is inevitably required to have a high reflux ratio and a high theoretical plate number, so that the refining of the titanium tetrachloride needs extremely high heat consumption. Therefore, how to reduce refining energy consumption on the basis of ensuring the impurity content to reach the standard is very important for the refining production of high-purity titanium tetrachloride.
Disclosure of Invention
The invention mainly aims to provide a titanium tetrachloride rectification method to solve the problem of over high energy consumption in the refining process of high-purity titanium tetrachloride in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for rectifying titanium tetrachloride, comprising subjecting titanium tetrachloride to a rectification treatment using a first rectification column and a second rectification column connected to each other; when the first rectifying tower is adopted for rectifying, a first reboiler is used for heating and refluxing a part of the kettle liquid of the first rectifying tower into the kettle of the first rectifying tower, and a first condenser is used for condensing the top gas of the first rectifying tower; when the second rectifying tower is adopted for rectification treatment, a second reboiler is utilized to heat and reflux a part of the kettle liquid of the second rectifying tower into the kettle of the second rectifying tower, and a second reflux opening is arranged at the top of the second rectifying tower to reflux a part of the top gas condensate of the second rectifying tower into the second rectifying tower; wherein the tower top pressure of the second rectifying tower is greater than the tower still pressure of the first rectifying tower, and before the step of refluxing a part of the tower top gas condensate of the second rectifying tower to the second rectifying tower, the titanium tetrachloride rectifying method further comprises the following steps: introducing the overhead gas of the second rectifying tower into the heat medium inlet of the first reboiler to heat and reflux a part of the kettle liquid of the first rectifying tower into the kettle of the first rectifying tower.
Further, after the overhead gas of the second distillation column is introduced into the heat medium inlet of the first reboiler, the overhead gas is discharged from the heat medium outlet of the first reboiler after heat exchange, and the titanium tetrachloride distillation method further comprises the following steps: and condensing or supercooling the overhead gas of the second rectifying tower after heat exchange by using a second condenser to obtain the overhead gas condensate of the second rectifying tower.
Further, the tower top pressure of the first rectifying tower is 0.02-0.1 MPa of gauge pressure, and the tower kettle pressure is 0.03-0.11 MPa of gauge pressure; the tower top pressure of the second rectifying tower is gage pressure of 0.15-0.25 MPa, and the tower kettle pressure is gage pressure of 0.16-0.26 MPa.
Further, the tower top temperature of the first rectifying tower is 137-158 ℃, and the tower kettle temperature is 145-167 ℃; the tower top temperature of the second rectifying tower is 168-185 ℃, and the tower kettle temperature is 177-193 ℃.
Furthermore, the reflux feed ratio of the first rectifying tower is 1-20, and the reflux feed ratio of the second rectifying tower is 1-20.
Furthermore, a first packing layer is arranged in the first rectifying tower, a second packing layer is arranged in the second rectifying tower, and the packing of the first packing layer and/or the second packing layer is wire mesh packing.
Further, in the process of rectifying titanium tetrachloride by adopting a first rectifying tower and a second rectifying tower which are connected with each other, the first rectifying tower is adopted to carry out lightness removal treatment on the titanium tetrachloride, the second rectifying tower is adopted to carry out weight removal treatment on one part of the kettle liquid of the first rectifying tower, and a first reboiler is adopted to heat and reflux the other part of the kettle liquid of the first rectifying tower into the kettle of the first rectifying tower.
Further, in the process of rectifying titanium tetrachloride by adopting a first rectifying tower and a second rectifying tower which are connected with each other, the first rectifying tower is adopted to carry out de-weighting treatment on the titanium tetrachloride, the second rectifying tower is adopted to carry out de-weighting treatment on one part of the top gas condensate discharged by the first condenser, the top of the first rectifying tower is also provided with a first return port, and the other part of the top gas condensate discharged by the first condenser is returned to the first rectifying tower by utilizing the first return port.
Further, in the process of rectifying titanium tetrachloride by adopting a first rectifying tower and a second rectifying tower which are connected with each other, the second rectifying tower is adopted to carry out lightness removing treatment on the titanium tetrachloride, the first rectifying tower is adopted to carry out weight removing treatment on one part of the kettle liquid of the second rectifying tower, and a second reboiler is utilized to heat and reflux the other part of the kettle liquid of the second rectifying tower into the kettle of the second rectifying tower.
Further, in the process of rectifying titanium tetrachloride by adopting a first rectifying tower and a second rectifying tower which are connected with each other, the second rectifying tower is adopted to carry out de-weighting treatment on the titanium tetrachloride, the first rectifying tower is adopted to carry out de-weighting treatment on one part of the top gas condensate of the second rectifying tower, and the other part of the top gas condensate of the second rectifying tower at a second reflux port is utilized to reflux to the second rectifying tower.
The technical scheme of the invention provides a titanium tetrachloride rectification method, which adopts a first rectification tower and a second rectification tower which are connected with each other to carry out rectification treatment on titanium tetrachloride; when the first rectifying tower is adopted for rectifying, a first reboiler is used for heating and refluxing a part of the kettle liquid of the first rectifying tower into the kettle of the first rectifying tower, and a first condenser is used for condensing the top gas of the first rectifying tower; when the second rectifying tower is adopted for rectification treatment, a second reboiler is utilized to heat and reflux a part of the kettle liquid of the second rectifying tower into the kettle of the second rectifying tower, and a second reflux opening is arranged at the top of the second rectifying tower so as to reflux a part of the top gas condensate of the second rectifying tower into the second rectifying tower; wherein the tower top pressure of the second rectifying tower is greater than the tower still pressure of the first rectifying tower, and before the step of refluxing a part of the tower top gas condensate of the second rectifying tower to the second rectifying tower, the titanium tetrachloride rectifying method further comprises the following steps: introducing the overhead gas of the second rectifying tower into the heat medium inlet of the first reboiler to heat and reflux a part of the kettle liquid of the first rectifying tower into the kettle of the first rectifying tower.
When the titanium tetrachloride is rectified by the titanium tetrachloride rectifying method, the tower top pressure of the second rectifying tower is higher than the tower kettle pressure of the first rectifying tower, so that the tower top gas discharged from the tower top of the second rectifying tower has higher temperature than the kettle liquid discharged from the tower bottom of the first rectifying tower. The second rectifying tower overhead gas with higher temperature is directly introduced into the first reboiler heat medium inlet at the bottom of the first rectifying tower, so that the waste heat of the part of the overhead gas can be effectively utilized to heat and reflux a part of the first rectifying tower bottoms. Therefore, according to the differential pressure thermal coupling technical principle, the invention enables the tower top steam of the high-pressure tower to be used as the heat source of the tower bottom liquid of the low-pressure tower, realizes the exchange of cold and hot loads in the titanium tetrachloride rectifying tower set, applies the energy mechanically and effectively reduces the refining energy consumption of the high-purity titanium tetrachloride.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a schematic view of a titanium tetrachloride rectification apparatus according to one embodiment of the invention;
FIG. 2 shows a schematic view of a titanium tetrachloride rectification apparatus according to another embodiment of the invention;
FIG. 3 shows a schematic view of a titanium tetrachloride rectification apparatus according to another embodiment of the invention; and
fig. 4 shows a schematic view of a titanium tetrachloride rectification apparatus according to yet another embodiment of the present invention.
Wherein the figures include the following reference numerals:
10. a first rectification column; 11. a first reboiler; 12. a first condenser; 13. a first reflux drum; 20. a second rectification column; 21. a second reboiler; 22. a second condenser; 23. a second reflux drum.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
As described in the background section, the prior art purification of high purity titanium tetrachloride has a problem of excessive energy consumption.
In order to solve the problem, the present invention provides a method for rectifying titanium tetrachloride, as shown in fig. 1 to 4, which comprises rectifying titanium tetrachloride by using a first rectifying tower 10 and a second rectifying tower 20 connected to each other; when the first rectifying tower 10 is adopted for rectification, a part of the kettle liquid of the first rectifying tower 10 is heated and refluxed to the kettle of the first rectifying tower 10 by using a first reboiler 11, and the top gas of the first rectifying tower 10 is condensed by using a first condenser 12; when the second rectifying tower 20 is adopted for rectification treatment, a second reboiler 21 is utilized to heat and reflux a part of the bottom liquid of the second rectifying tower 20 to the bottom of the second rectifying tower 20, and a second reflux opening is arranged at the top of the second rectifying tower 20 to reflux a part of the top gas condensate of the second rectifying tower 20 to the second rectifying tower 20; wherein the top pressure of the second rectifying tower 20 is greater than the bottom pressure of the first rectifying tower 10, and before the step of refluxing a part of the top gas condensate of the second rectifying tower 20 to the second rectifying tower 20, the titanium tetrachloride rectifying method further comprises the following steps: introducing the overhead gas of the second rectifying tower 20 into the heat medium inlet of the first reboiler 11 to heat and reflux a part of the bottoms of the first rectifying tower 10 to the bottom of the first rectifying tower 10.
When the titanium tetrachloride is rectified by the titanium tetrachloride rectifying method, the tower top pressure of the second rectifying tower 20 is higher than the tower bottom pressure of the first rectifying tower 10, so that the tower top gas discharged from the tower top of the second rectifying tower 20 has higher temperature than the kettle liquid discharged from the tower bottom of the first rectifying tower 10. The overhead gas of the second rectifying tower 20 with higher temperature is directly introduced into the heat medium inlet of the first reboiler 11 at the bottom of the first rectifying tower 10, and the residual heat of the overhead gas can be effectively utilized to heat and reflux one part of the first rectifying tower bottoms. Therefore, according to the differential pressure thermal coupling technical principle, the invention enables the tower top steam of the high-pressure tower to be used as the heat source of the tower bottom liquid of the low-pressure tower, realizes the exchange of cold and hot loads in the titanium tetrachloride rectifying tower set, applies the energy mechanically and effectively reduces the refining energy consumption of the high-purity titanium tetrachloride.
Specifically, by using the above rectification method, the cooling load required for condensing the overhead gas of the second rectification column 20 into the supercooled state can be equivalent to the heat load required for vaporizing the bottoms of the first rectification column 10, so that the first reboiler 11 does not require an external heat source, and the heat source load can be reduced by 30 to 50%.
In addition to the above advantages, the above rectification method of the present invention has the following beneficial effects: when the cooling load required for condensing the overhead gas of the second rectifying tower 20 to the supercooled state can be equivalent to the heat load required for vaporizing the bottoms of the first rectifying tower 10, the top of the second rectifying tower 20 may not be provided with a condenser, thereby reducing the number of equipment.
In the present invention, the rectification order and the light and heavy removal type of the first rectification column 10 and the second rectification column 20 are not limited, and the first rectification column 10 may be disposed upstream of the second rectification column 20, and titanium tetrachloride may be first subjected to light and heavy removal treatment by the first rectification column 10 and then subjected to heavy and light removal by the second rectification column 20, or the second rectification column 20 may be disposed upstream of the first rectification column 10, and titanium tetrachloride may be first subjected to light and heavy removal treatment by the second rectification column 20 and then subjected to heavy and light removal by the first rectification column 10. The energy consumption of the titanium tetrachloride rectifying device can be effectively reduced according to the differential pressure thermal coupling arrangement only by setting the tower top pressure of the second rectifying tower 20 to be higher than the tower bottom pressure of the first rectifying tower 10.
In the actual production process, when the overhead gas of the second rectifying tower 20 enters the heat medium outlet of the first reboiler 11 for heat jacket, the overhead gas itself can be completely condensed or even subcooled, and at this time, the top of the second rectifying tower 20 does not need to be provided with a condenser. Of course, in order to further improve the production operation stability of the apparatus, in an alternative embodiment, after the overhead gas of the second distillation column 20 is introduced into the heat medium inlet of the first reboiler 11, the overhead gas is heat-exchanged and then discharged from the heat medium outlet of the first reboiler 11, and the above titanium tetrachloride distillation method further includes the following steps: the overhead gas of the second rectification column 20 after the heat exchange is condensed or subcooled by the second condenser 22 to obtain the overhead gas condensate of the second rectification column 20. In this way, after the overhead gas of the second rectification column 20 enters the heat medium outlet of the first reboiler 11 and completes the heat exchange, the overhead gas after the heat exchange may be further condensed or subcooled by the second condenser 22 to obtain the overhead gas condensate of the second rectification column 20. It should be noted that the overhead gas of the second rectification column 20 can be completely condensed or subcooled after being condensed by the first reboiler 11, so that the flow rate of the heat sink of the second condenser 22 can be reduced to a small value or even 0 (the second condenser 22 can be eliminated when the flow rate is 0), and the load of the heat sink of the second condenser 22 can be reduced by 30-50%.
The process parameters for each step in the above-described method may be adjusted in accordance with the above teachings of the present invention. In a preferred embodiment, the tower top pressure of the first rectifying tower is 0.02-0.1 MPa gauge pressure, and the tower kettle pressure is 0.03-0.11 MPa gauge pressure; the tower top pressure of the second rectifying tower is gage pressure of 0.15-0.25 MPa, and the tower kettle pressure is gage pressure of 0.16-0.26 MPa. Therefore, the differential pressure thermal coupling effect in the two rectification treatments is better, and the titanium tetrachloride rectification effect is better. More preferably, the tower top temperature of the first rectifying tower is 137-158 ℃, and the tower kettle temperature is 145-167 ℃; the tower top temperature of the second rectifying tower is 168-185 ℃, and the tower kettle temperature is 177-193 ℃.
In a preferred embodiment, the reflux-to-feed ratio of the first rectification column 10 is 1 to 20, and the reflux-to-feed ratio of the second rectification column 20 is 1 to 20. The reflux ratio in the two times of rectification treatment is set within the range, so that the rectification effect of the titanium tetrachloride is better.
In order to further reduce the production energy consumption, in a preferred embodiment, a first packing layer is arranged in the column of the first rectification column 10, a second packing layer is arranged in the column of the second rectification column 20, and the packing of the first packing layer and/or the second packing layer is a wire mesh packing. The pressure drop of the wire mesh packing is small, after the wire mesh packing is adopted, the pressure difference between the top and the bottom of the rectifying tower can be reduced to 0.01-0.02 MPa, and the pressure difference between the top and the bottom of the sieve plate or the float valve tower under the same theoretical plate number is 0.05-0.3 MPa. After the wire mesh packing is adopted, when the pressure at the top of the first rectifying tower 10 is fixed, the pressure drop of tower equipment is reduced, the pressure and the temperature at the bottom of the first rectifying tower 10 are further reduced, and correspondingly, the pressure and the temperature at the top of the second rectifying tower 20 coupled with the pressure and the temperature at the top of the second rectifying tower 20 are reduced, so that the quality of a heat source (such as water vapor) of a second reboiler 21 at the bottom of the second rectifying tower 20 can be reduced, and the refining energy consumption of titanium tetrachloride can be further reduced.
As described above, the above method is not limited to the connection sequence and the light and heavy removal type of the first rectifying tower 10 and the second rectifying tower 20, and for example, the following processes can be adopted:
in a typical embodiment, as shown in fig. 1, in the process of rectifying titanium tetrachloride by using a first rectifying tower 10 and a second rectifying tower 20 connected to each other, titanium tetrachloride a is subjected to lightness removal by using the first rectifying tower 10, a part of the bottoms of the first rectifying tower 10 is subjected to weight removal by using the second rectifying tower 20, and another part of the bottoms of the first rectifying tower 10 is heated and refluxed to the bottom of the first rectifying tower 10 by using a first reboiler 11. In the actual production process, after titanium tetrachloride enters a first rectifying tower 10 for lightness removal treatment, the gas at the top of the first rectifying tower 10 enters a first condenser 12, one part of condensate reflows to the first rectifying tower 10, and the other part of condensate is extracted as low-boiling-point impurities; the second rectifying tower 20 is subjected to de-weighting treatment, the gas at the top of the second rectifying tower enters the first reboiler 11 for heat exchange, the gas enters the second condenser 22 for further condensation, one part of the condensate reflows to the second rectifying tower 20, the other part of the condensate is extracted as a refined titanium tetrachloride product B, the tower kettle of the second rectifying tower 20 extracts one part of the condensate, the other part of the condensate is heated by the second reboiler 21 and then returns to the tower kettle of the second rectifying tower 20, and the other part of the condensate is extracted as high-boiling-point impurities.
In another exemplary embodiment, as shown in fig. 2, in the process of rectifying titanium tetrachloride by using a first rectifying tower 10 and a second rectifying tower 20 connected to each other, the first rectifying tower 10 is used to perform de-weighting treatment on titanium tetrachloride a, the second rectifying tower 20 is used to perform de-lightening treatment on a part of the overhead gas condensate discharged from the first condenser 12, the first rectifying tower 10 is further provided with a first reflux opening at the top thereof, and another part of the overhead gas condensate discharged from the first condenser 12 is refluxed to the first rectifying tower 10 by using the first reflux opening. In the actual production process, titanium tetrachloride enters a first rectifying tower 10 for weight removal treatment, the gas at the top of the first rectifying tower 10 enters a first condenser 12, one part of condensate reflows to the first rectifying tower 10, the other part of condensate is extracted and enters a second rectifying tower 20, one part of condensate extracted from the tower kettle of the first rectifying tower 10 returns to the tower kettle of the first rectifying tower 10 after being heated by a first reboiler 11, and the other part of condensate is used as high-boiling-point impurities; and (3) performing lightness-removing treatment on the second rectifying tower 20, condensing the gas at the top of the tower in the first reboiler 11, further condensing the condensate in the second condenser 22, refluxing a part of the condensate to the second rectifying tower 20, extracting the other part of the condensate as low-boiling-point impurities, extracting a part of the condensate from the tower bottom of the second rectifying tower 20, heating the part of the condensate in the second reboiler 21, returning the heated part of the condensate to the tower bottom of the second rectifying tower, and extracting the other part of the condensate as a refined product B of titanium tetrachloride.
In still another exemplary embodiment, as shown in fig. 3, in the process of rectifying titanium tetrachloride by using a first rectifying tower 10 and a second rectifying tower 20 connected to each other, titanium tetrachloride a is subjected to lightness removal by using the second rectifying tower 20, a part of the bottom liquid of the second rectifying tower 20 is subjected to weight removal by using the first rectifying tower 10, and another part of the bottom liquid of the second rectifying tower 20 is heated and refluxed to the bottom of the second rectifying tower 20 by using a second reboiler 21. In the actual production process, titanium tetrachloride enters a second rectifying tower 20 for lightness removal treatment, the gas at the top of the second rectifying tower 20 enters a first reboiler 11 for condensation, condensate enters a second condenser 22 for further condensation, part of the condensate flows back to the second rectifying tower, the other part of the condensate is extracted as low-boiling-point impurities, part of the condensate extracted from the tower bottom of the second rectifying tower 20 returns to the tower bottom of the second rectifying tower after being heated by a second reboiler 21, and the other part of the condensate enters the first rectifying tower 10; the first rectifying tower 10 is subjected to de-weighting treatment, the gas at the top of the tower enters a first condenser 12, one part of condensate liquid flows back to the first rectifying tower, the other part of condensate liquid is extracted as a refined product B of titanium tetrachloride, one part of condensate liquid extracted from the tower bottom of the first rectifying tower is heated by a first reboiler 11 and then returns to the tower bottom of the first rectifying tower, and the other part of condensate liquid is extracted as high-boiling-point impurities.
In still another exemplary embodiment, as shown in fig. 4, in the process of rectifying titanium tetrachloride using a first rectifying tower 10 and a second rectifying tower 20 connected to each other, titanium tetrachloride a is subjected to a de-weighting treatment using the second rectifying tower 20, a part of the top gas condensate of the second rectifying tower 20 is subjected to a de-lightening treatment using the first rectifying tower 10, and another part of the top gas condensate of the second rectifying tower 20 is refluxed to the second rectifying tower 20 using a second reflux port. In the actual production process, titanium tetrachloride enters a second rectifying tower 20 for weight removal treatment, the gas at the top of the second rectifying tower 20 enters a first reboiler 11 for condensation, condensate enters a second condenser 22 for further condensation, one part of the condensate flows back to the second rectifying tower 20, and the other part of the condensate is extracted into a first rectifying tower 10; one part of the distillate from the tower bottom of the second rectifying tower 20 is heated by a second reboiler 21 and then returns to the tower bottom of the second rectifying tower 20, and the other part of the distillate is used as high-boiling-point impurities; the first rectifying tower 10 is subjected to lightness removing treatment, the gas at the top of the tower enters a first condenser 12, one part of condensate liquid reflows to the first rectifying tower, the other part of condensate liquid is extracted as low-boiling-point impurities, one part of condensate liquid extracted from the tower bottom of the first rectifying tower 10 is heated by a first reboiler 11 and then returns to the tower bottom of the first rectifying tower 10, and the other part of condensate liquid is extracted as a refined product B of titanium tetrachloride.
According to another aspect of the present invention, there is provided a titanium tetrachloride rectifying apparatus, as shown in fig. 1 to 4, comprising a first rectifying tower 10 and a second rectifying tower 20 connected to each other for rectifying titanium tetrachloride; the tower bottom of the first rectifying tower 10 is provided with a first reboiler 11 connected with the tower kettle of the first rectifying tower 10, and the tower top is provided with a first condenser 12 connected with a gas outlet at the tower top of the first rectifying tower 10; the tower bottom of the second rectifying tower 20 is provided with a second reboiler 21 connected with the tower kettle of the second rectifying tower 20, and the tower top is provided with a second reflux port; wherein, the top gas outlet of the second rectifying tower 20 is communicated with the heat medium inlet of the first reboiler 11 through a heat medium pipeline, the heat medium outlet of the first reboiler 11 is communicated with the second reflux port of the second rectifying tower 20 through a reflux pipeline, and the top pressure of the second rectifying tower 20 is greater than the bottom pressure of the first rectifying tower 10.
When the titanium tetrachloride rectifying device provided by the invention is used for rectifying titanium tetrachloride, the tower top pressure of the second rectifying tower 20 is higher than the tower bottom pressure of the first rectifying tower 10, so that the tower top gas discharged from the tower top of the second rectifying tower 20 has higher temperature than the kettle liquid discharged from the tower bottom of the first rectifying tower 10. The overhead gas of the second rectifying tower 20 with higher temperature is directly introduced into the heat medium inlet of the first reboiler 11 at the bottom of the first rectifying tower 10, and the residual heat of the overhead gas can be effectively utilized to heat and reflux one part of the first rectifying tower bottoms. Therefore, according to the differential pressure thermal coupling technical principle, the invention enables the tower top steam of the high-pressure tower to be used as the heat source of the tower bottom liquid of the low-pressure tower, realizes the exchange of cold and hot loads in the titanium tetrachloride rectifying tower set, applies the energy mechanically and effectively reduces the refining energy consumption of the high-purity titanium tetrachloride.
Specifically, with the above-described rectification apparatus, the cooling load required for condensing the overhead gas of the second rectification column 20 into a supercooled state can be equivalent to the heating load required for vaporizing the bottoms of the first rectification column 10, so that the first reboiler 11 does not require an external heating source, and the heat source load can be reduced by 30 to 50%.
In addition to the above advantages, the above rectification apparatus of the present invention has the following beneficial effects: when the cooling load required for condensing the overhead gas of the second rectifying tower 20 into the supercooled state can be equivalent to the heat load required for vaporizing the bottoms of the first rectifying tower 10, the second condenser 22 may not be provided at the top of the second rectifying tower 20.
In the present invention, the connection order and the light and heavy removal type of the first rectifying tower 10 and the second rectifying tower 20 are not limited, and the first rectifying tower 10 may be disposed upstream of the second rectifying tower 20, and titanium tetrachloride may be first subjected to light and heavy removal treatment by the first rectifying tower 10 and then subjected to heavy and light removal by the second rectifying tower 20, or the second rectifying tower 20 may be disposed upstream of the first rectifying tower 10, and titanium tetrachloride may be first subjected to light and heavy removal treatment by the second rectifying tower 20 and then subjected to heavy and light removal by the first rectifying tower 10. The energy consumption of the titanium tetrachloride rectifying device can be effectively reduced according to the differential pressure thermal coupling arrangement only by setting the tower top pressure of the second rectifying tower 20 to be higher than the tower bottom pressure of the first rectifying tower 10.
In the actual production process, when the overhead gas of the second rectifying tower 20 enters the heat medium outlet of the first reboiler 11 for heat jacket, the overhead gas itself can be completely condensed or even subcooled, and at this time, the top of the second rectifying tower 20 does not need to be provided with a condenser. Of course, in order to further improve the production operation stability of the apparatus, in an alternative embodiment, the titanium tetrachloride rectification apparatus further includes a second condenser 22, the second condenser 22 is disposed on the return line, an inlet of the second condenser 22 is connected to the outlet of the heating medium of the first reboiler 11, and an outlet of the second condenser 22 is connected to the second return port. With this arrangement, after the overhead gas of the second rectification column 20 enters the heat medium outlet of the first reboiler 11 and completes the heat exchange, the overhead gas after the heat exchange may be further condensed or subcooled by the second condenser 22 to obtain the overhead gas condensate of the second rectification column 20. It should be noted that the overhead gas of the second rectification column 20 can be completely condensed or subcooled after being condensed by the first reboiler 11, so that the flow rate of the heat sink of the second condenser 22 can be reduced to a small value or even 0 (the second condenser 22 can be eliminated when the flow rate is 0), and the load of the heat sink of the second condenser 22 can be reduced by 30-50%.
In order to further reduce the quality of the heat source of the second reboiler 21 and further reduce the energy consumption, in a preferred embodiment, a first packing layer is disposed in the first rectifying tower 10, a second packing layer is disposed in the second rectifying tower 20, and the packing of the first packing layer and/or the second packing layer is a wire mesh packing. The pressure drop of the wire mesh packing is small, after the wire mesh packing is adopted, the pressure difference between the top and the bottom of the rectifying tower can be reduced to 0.01-0.02 MPa, and the pressure difference between the top and the bottom of the sieve plate or the float valve tower under the same theoretical plate number is 0.05-0.3 MPa. After the wire mesh packing is adopted, when the pressure at the top of the first rectifying tower 10 is fixed, the pressure drop of tower equipment is reduced, the pressure and the temperature at the bottom of the first rectifying tower 10 are further reduced, and correspondingly, the pressure and the temperature at the top of the second rectifying tower 20 coupled with the pressure and the temperature at the top of the second rectifying tower 20 are reduced, so that the quality of a heat source (such as water vapor) of a second reboiler 21 at the bottom of the second rectifying tower 20 can be reduced, and the refining energy consumption of titanium tetrachloride can be further reduced.
As described above, the present invention is not limited to the connection order and the light and heavy removal type of the first rectifying tower 10 and the second rectifying tower 20, and for example, the following arrangements may be adopted:
in a typical embodiment, as shown in fig. 1, a first distillation column 10 is provided with a titanium tetrachloride inlet to perform a lightness-removing treatment on titanium tetrachloride a, a second distillation column 20 and the first distillation column 10 are connected to each other to perform a weight-removing treatment on a part of the bottoms of the first distillation column 10, and a first reboiler 11 is connected to the bottom of the first distillation column 10 to heat and reflux another part of the bottoms of the first distillation column 10 to the bottom of the first distillation column 10. In the actual production process, after titanium tetrachloride enters a first rectifying tower 10 for lightness removal treatment, the gas at the top of the first rectifying tower 10 enters a first condenser 12, one part of condensate reflows to the first rectifying tower 10, and the other part of condensate is extracted as low-boiling-point impurities; the second rectifying tower 20 is subjected to de-weighting treatment, the gas at the top of the second rectifying tower enters the first reboiler 11 for heat exchange, the gas enters the second condenser 22 for further condensation, one part of the condensate reflows to the second rectifying tower 20, the other part of the condensate is extracted as a refined titanium tetrachloride product B, the tower kettle of the second rectifying tower 20 extracts one part of the condensate, the other part of the condensate is heated by the second reboiler 21 and then returns to the tower kettle of the second rectifying tower 20, and the other part of the condensate is extracted as high-boiling-point impurities.
In another exemplary embodiment, as shown in fig. 2, a first distillation column 10 is provided with a titanium tetrachloride inlet for de-weighting titanium tetrachloride a, a second distillation column 20 and the first distillation column 10 are connected to each other for de-lightening a part of the overhead gas condensate discharged from the first condenser 12, and the first distillation column 10 is further provided at the top thereof with a first reflux port connected to the first condenser 12 for refluxing another part of the overhead gas condensate discharged from the first condenser 12 into the first distillation column 10. In the actual production process, titanium tetrachloride enters a first rectifying tower 10 for weight removal treatment, the gas at the top of the first rectifying tower 10 enters a first condenser 12, one part of condensate reflows to the first rectifying tower 10, the other part of condensate is extracted and enters a second rectifying tower 20, one part of condensate extracted from the tower kettle of the first rectifying tower 10 returns to the tower kettle of the first rectifying tower 10 after being heated by a first reboiler 11, and the other part of condensate is used as high-boiling-point impurities; and (3) performing lightness-removing treatment on the second rectifying tower 20, condensing the gas at the top of the tower in the first reboiler 11, further condensing the condensate in the second condenser 22, refluxing a part of the condensate to the second rectifying tower 20, extracting the other part of the condensate as low-boiling-point impurities, extracting a part of the condensate from the tower bottom of the second rectifying tower 20, heating the part of the condensate in the second reboiler 21, returning the heated part of the condensate to the tower bottom of the second rectifying tower, and extracting the other part of the condensate as a refined product B of titanium tetrachloride.
In still another exemplary embodiment, as shown in fig. 3, the second distillation column 20 is provided with a titanium tetrachloride inlet for lightness-removing treatment of titanium tetrachloride a, the first distillation column 10 and the second distillation column 20 are connected to each other for weight-removing treatment of a part of the bottom liquid of the second distillation column 20, and a second reboiler 21 is connected to the bottom of the second distillation column 20 for heating and refluxing another part of the bottom liquid of the second distillation column 20 to the second distillation column 20. In the actual production process, titanium tetrachloride enters a second rectifying tower 20 for lightness removal treatment, the gas at the top of the second rectifying tower 20 enters a first reboiler 11 for condensation, condensate enters a second condenser 22 for further condensation, part of the condensate flows back to the second rectifying tower, the other part of the condensate is extracted as low-boiling-point impurities, part of the condensate extracted from the tower bottom of the second rectifying tower 20 returns to the tower bottom of the second rectifying tower after being heated by a second reboiler 21, and the other part of the condensate enters the first rectifying tower 10; the first rectifying tower 10 is subjected to de-weighting treatment, the gas at the top of the tower enters a first condenser 12, one part of condensate liquid flows back to the first rectifying tower, the other part of condensate liquid is extracted as a refined product B of titanium tetrachloride, one part of condensate liquid extracted from the tower bottom of the first rectifying tower is heated by a first reboiler 11 and then returns to the tower bottom of the first rectifying tower, and the other part of condensate liquid is extracted as high-boiling-point impurities.
In yet another exemplary embodiment, as shown in fig. 4, the second distillation column 20 is provided with a titanium tetrachloride inlet for the de-weighting treatment of titanium tetrachloride a; the first rectifying tower 10 and the second rectifying tower 20 are connected with each other to perform lightness removing treatment on one part of the top gas condensate of the second rectifying tower 20, and the second reflux port is used for refluxing the other part of the top gas condensate of the second rectifying tower 20 to the second rectifying tower 20. In the actual production process, titanium tetrachloride enters a second rectifying tower 20 for weight removal treatment, the gas at the top of the second rectifying tower 20 enters a first reboiler 11 for condensation, condensate enters a second condenser 22 for further condensation, one part of the condensate flows back to the second rectifying tower 20, and the other part of the condensate is extracted into a first rectifying tower 10; one part of the distillate from the tower bottom of the second rectifying tower 20 is heated by a second reboiler 21 and then returns to the tower bottom of the second rectifying tower 20, and the other part of the distillate is used as high-boiling-point impurities; the first rectifying tower 10 is subjected to lightness removing treatment, the gas at the top of the tower enters a first condenser 12, one part of condensate liquid reflows to the first rectifying tower, the other part of condensate liquid is extracted as low-boiling-point impurities, one part of condensate liquid extracted from the tower bottom of the first rectifying tower 10 is heated by a first reboiler 11 and then returns to the tower bottom of the first rectifying tower 10, and the other part of condensate liquid is extracted as a refined product B of titanium tetrachloride.
When the first rectifying tower 10 is provided with a titanium tetrachloride inlet for the lightness-removing treatment of titanium tetrachloride, the overhead pressure in the second rectifying tower 20 located downstream is relatively high. In order to make the feeding of the second rectifying tower 20 smoother, in a preferred embodiment, a booster pump is further disposed on the feeding pipeline of the second rectifying tower 20.
In a preferred embodiment, as shown in fig. 1, 3 and 4, the titanium tetrachloride rectification apparatus further includes a first reflux tank 13, the top of the first rectification column 10 is further provided with a first reflux port, an inlet of the first reflux tank 13 is connected to an outlet of the first condenser 12, an outlet of the first reflux tank 13 is connected to the first reflux port, and a pipeline between the outlet of the first reflux tank 13 and the first reflux port is provided with a tapping branch of the top gas condensate of the first rectification column 10. Preferably, as shown in fig. 2, the titanium tetrachloride rectification apparatus further comprises a first reflux tank 13, an inlet of the first reflux tank 13 is connected to an outlet of the first condenser 12, and an outlet of the first reflux tank 13 is connected to a first reflux port and an inlet of the second rectification column 20, respectively.
In a preferred embodiment, as shown in fig. 1, 2 and 3, the titanium tetrachloride rectification apparatus further comprises a second reflux tank 23, an inlet of the second reflux tank 23 is connected to an outlet of the second condenser 22, an outlet of the second reflux tank 23 is connected to the second reflux port, and a pipeline between the outlet of the second reflux tank 23 and the second reflux port is further provided with a tapping branch of the top gas condensate of the second rectification column 20. Preferably, as shown in fig. 4, the titanium tetrachloride rectification apparatus further comprises a second reflux tank 23, an inlet of the second reflux tank 23 is connected to an outlet of the second condenser 22, and an outlet of the second reflux tank 23 is connected to the second reflux port and the inlet of the first rectification column 10, respectively.
The beneficial effects of the present invention are further illustrated by the following examples:
example 1
The treatment capacity of crude titanium tetrachloride liquid with the titanium tetrachloride mass content of 99.8 percent is 5000kg/h, and the product is required to reach the index of high-purity titanium tetrachloride: the content of each impurity is controlled to be 0.1-1 ppbw.
The refining apparatus used in this example is shown in fig. 1, the packings in both rectification columns are wire mesh packings, and the process parameters of the apparatus are as follows:
example 2
In example 2, the temperature and pressure of the rectifying column were increased compared with those in example 1, and the steam of the second reboiler heat source was changed from 1.3mpa (a) to 1.9mpa (a), resulting in a slight decrease in product quality.
Example 3
Example 3 compared with example 1, the reflux-feed ratio of the column is increased, the product quality is improved, the quality of each impurity can be basically controlled to be 0.1ppbw, but the energy consumption is increased.
Example 4
The treatment capacity of crude titanium tetrachloride liquid with the titanium tetrachloride mass content of 99.8 percent is 5000kg/h, and the product is required to reach the index of high-purity titanium tetrachloride: the content of each impurity is controlled to be 0.1-1 ppbw.
The refining device adopted in the embodiment is shown in figure 1, two rectifying tower internals are sieve plates, the process parameters of the device are shown in the following table, when the embodiment 1 is adopted, the tower internals are wire mesh packing, the pressure difference between the top of the tower and the bottom of the tower is 0.01MPa, the temperature of the bottom of the second rectifying tower is 177 ℃, the heat source can adopt saturated steam of 1.2MPa and 191.5 ℃, in the embodiment, the tower internals are sieve plates, the pressure difference between the top of the tower and the bottom of the tower is 0.05MPa, the temperature of the bottom of the second rectifying tower is 195 ℃, the heat source can adopt saturated steam of 1.8MPa and 209.8 ℃, and the quality of the heat source is greatly improved.
Comparative example 1
The treatment capacity of crude titanium tetrachloride liquid with the titanium tetrachloride mass content of 99.8 percent is 5000kg/h, and the product is required to reach the index of high-purity titanium tetrachloride: the content of each impurity is controlled to be 0.1-1 ppbw.
The refining device adopted in the comparative example is shown in fig. 1, and is different in that a differential pressure thermal coupling process is not adopted, the overhead gas of the second rectifying tower does not enter the heat medium inlet of the first reboiler, but is directly condensed by the second condenser, one part of condensed condensate flows back to the second rectifying tower, and the other part of condensed condensate is extracted. The fillers in the two rectifying towers are wire mesh fillers, and the technological parameters of the device are as follows:
from the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
after the differential pressure thermal coupling technology is adopted in example 1, the cold load and the heat load are respectively reduced by 52.6 percent and 50 percent compared with those of comparative example 1
In summary, when the titanium tetrachloride rectifying apparatus provided by the present invention is used for rectifying titanium tetrachloride, the pressure at the top of the second rectifying tower is higher than the pressure at the bottom of the first rectifying tower, so that the top gas discharged from the top of the second rectifying tower has a higher temperature than the bottom liquid discharged from the bottom of the first rectifying tower. The second rectifying tower overhead gas with higher temperature is directly introduced into the first reboiler heat medium inlet at the bottom of the first rectifying tower, so that the waste heat of the part of the overhead gas can be effectively utilized to heat and reflux a part of the first rectifying tower bottoms. Therefore, according to the differential pressure thermal coupling technical principle, the invention enables the tower top steam of the high-pressure tower to be used as the heat source of the tower bottom liquid of the low-pressure tower, realizes the exchange of cold and hot loads in the titanium tetrachloride rectifying tower set, applies the energy mechanically and effectively reduces the refining energy consumption of the high-purity titanium tetrachloride.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for rectifying titanium tetrachloride comprises the steps of rectifying titanium tetrachloride by adopting a first rectifying tower (10) and a second rectifying tower (20) which are connected with each other; when the first rectifying tower (10) is adopted for rectification, a first reboiler (11) is used for heating and refluxing a part of the kettle liquid of the first rectifying tower (10) to the kettle of the first rectifying tower (10), and a first condenser (12) is used for condensing the overhead gas of the first rectifying tower (10); when the second rectifying tower (20) is adopted for rectification treatment, a second reboiler (21) is utilized to heat and reflux a part of the kettle liquid of the second rectifying tower (20) to the kettle of the second rectifying tower (20), and a second reflux opening is arranged at the top of the second rectifying tower (20) to reflux a part of the top gas condensate of the second rectifying tower (20) to the second rectifying tower (20);
characterized in that the top pressure of the second rectifying tower (20) is higher than the bottom pressure of the first rectifying tower (10), and before the step of refluxing a part of the top gas condensate of the second rectifying tower (20) to the second rectifying tower (20), the titanium tetrachloride rectifying method further comprises the following steps: introducing the overhead gas of the second rectifying tower (20) into a heat medium inlet of the first reboiler (11) to heat and reflux a part of the kettle liquid of the first rectifying tower (10) into the kettle of the first rectifying tower (10);
wherein the tower top pressure of the first rectifying tower (10) is 0.02-0.1 MPa gauge pressure, and the tower kettle pressure is 0.03-0.11 MPa gauge pressure; the tower top pressure of the second rectifying tower (20) is 0.15-0.25 MPa gauge pressure, and the tower kettle pressure is 0.16-0.26 MPa gauge pressure; the tower top temperature of the first rectifying tower (10) is 137-158 ℃, and the tower kettle temperature is 145-167 ℃; the tower top temperature of the second rectifying tower (20) is 168-185 ℃, and the tower kettle temperature is 177-193 ℃.
2. The method for rectifying titanium tetrachloride according to claim 1, wherein the overhead gas of the second rectification column (20) is discharged from the heat medium outlet of the first reboiler (11) after passing through the heat medium inlet of the first reboiler (11) after heat exchange, and the method for rectifying titanium tetrachloride further comprises the steps of: and condensing or supercooling the overhead gas of the second rectifying tower (20) after heat exchange by using a second condenser (22) to obtain the overhead gas condensate of the second rectifying tower (20).
3. The method for rectifying titanium tetrachloride according to claim 1, wherein the reflux-to-feed ratio of the first rectifying tower (10) is 1 to 20, and the reflux-to-feed ratio of the second rectifying tower (20) is 1 to 20.
4. The method for rectifying titanium tetrachloride according to any one of claims 1 to 3, characterized in that a first packing layer is provided in the column of the first rectification column (10), a second packing layer is provided in the column of the second rectification column (20), and the packing of the first packing layer and/or the second packing layer is a wire mesh packing.
5. The method for rectifying titanium tetrachloride according to any one of claims 1 to 3, wherein in the rectifying process of titanium tetrachloride using the first rectifying tower (10) and the second rectifying tower (20) connected to each other, the titanium tetrachloride is subjected to a lightness removal process using the first rectifying tower (10), a part of the bottoms of the first rectifying tower (10) is subjected to a weight removal process using the second rectifying tower (20), and another part of the bottoms of the first rectifying tower (10) is heated and refluxed into the bottom of the first rectifying tower (10) using the first reboiler (11).
6. The method for rectifying titanium tetrachloride according to any one of claims 1 to 3, wherein in the process of rectifying titanium tetrachloride by using the first rectifying tower (10) and the second rectifying tower (20) which are connected to each other, the titanium tetrachloride is subjected to a de-weighting treatment by using the first rectifying tower (10), a part of the overhead vapor condensate discharged from the first condenser (12) is subjected to a de-lightening treatment by using the second rectifying tower (20), the top of the first rectifying tower (10) is further provided with a first reflux port, and another part of the overhead vapor condensate discharged from the first condenser (12) is refluxed into the first rectifying tower (10) by using the first reflux port.
7. The method for rectifying titanium tetrachloride according to any one of claims 1 to 3, wherein in the rectifying process of titanium tetrachloride using the first rectifying tower (10) and the second rectifying tower (20) connected to each other, the titanium tetrachloride is subjected to a lightness removal process using the second rectifying tower (20), a part of the bottoms of the second rectifying tower (20) is subjected to a weight removal process using the first rectifying tower (10), and another part of the bottoms of the second rectifying tower (20) is heated and refluxed into the bottom of the second rectifying tower (20) using the second reboiler (21).
8. The method for rectifying titanium tetrachloride according to any one of claims 1 to 3, wherein in the rectifying process of titanium tetrachloride using the first rectifying tower (10) and the second rectifying tower (20) connected to each other, the titanium tetrachloride is subjected to a de-weighting process using the second rectifying tower (20), a part of the overhead condensate of the second rectifying tower (20) is subjected to a de-lightening process using the first rectifying tower (10), and another part of the overhead condensate of the second rectifying tower (20) is refluxed into the second rectifying tower (20) using the second reflux port.
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