CN212594079U - Gas phase separation device for low-boiling-point impurities in titanium tetrachloride - Google Patents
Gas phase separation device for low-boiling-point impurities in titanium tetrachloride Download PDFInfo
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- CN212594079U CN212594079U CN202021812351.XU CN202021812351U CN212594079U CN 212594079 U CN212594079 U CN 212594079U CN 202021812351 U CN202021812351 U CN 202021812351U CN 212594079 U CN212594079 U CN 212594079U
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Abstract
A gas phase separation device for low-boiling point impurities in titanium tetrachloride comprises a distillation tower, a distillation tower reflux tank, a distillation tower reflux pump and a tower top byproduct tank, wherein a jacket for heating and insulating the tank is sleeved outside the tank body of the distillation tower reflux tank; the liquid outlet of the bottom of the distillation column reflux tank is connected with the inlet of the distillation column reflux pump, the outlet of the distillation column reflux pump is connected with two pipelines, the main line of the first pipeline is connected with the liquid phase inlet of the distillation column through the distillation column reflux cooler, the branch line of the first pipeline is connected with the column top by-product tank, the second pipeline is connected with the nozzle arranged at the top of the distillation column reflux tank, and the top of the distillation column reflux tank is connected with the tail gas condensing system. Utilize the utility model discloses can increase the gaseous phase partial pressure of low boiling point impurity for more low boiling point impurities get into the gaseous phase, get into tail gas condensing system again and collect, improve the separation effect of low boiling point impurity and the quality of titanium tetrachloride product.
Description
Technical Field
The utility model belongs to the technical field of chemical production technology, concretely relates to gas phase separation device of low boiling point impurity in titanium tetrachloride production process.
Background
The method comprises the steps of producing titanium tetrachloride by a boiling chlorination method, obtaining crude titanium tetrachloride after chlorination, gas-solid separation and condensation, wherein the crude titanium tetrachloride contains a large amount of unreacted titanium dioxide, carbon particles, aluminum chloride, niobium chloride, zirconium chloride and other impurities, the impurities are solid or liquid, the boiling point of the impurities is greatly different from that of the titanium tetrachloride, the impurities belong to high-boiling-point impurities, and the titanium tetrachloride can be effectively separated from a discharge hole at the top of a distillation tower through heating distillation. Meanwhile, the crude titanium tetrachloride contains a large amount of impurities such as silicon tetrachloride, tin tetrachloride, sulfur-oxygen carbon, monochloroacetic chloride, dichloroacetyl chloride and the like, the boiling points of part of the impurities are relatively close to the boiling point of the titanium tetrachloride, even the difference between the boiling points of part of the impurities and the boiling point of the titanium tetrachloride is less than 5 ℃, the impurities belong to low-boiling impurities, the separation difficulty of part of the impurities is extremely high, the requirement on a low-boiling impurity removal tower is extremely high, the impurities can be effectively separated by a large number of tower plates, or the total amount of the low-boiling impurities in the tower is reduced by increasing the discharge amount of byproducts at the top of the tower.
At present, when titanium tetrachloride is separated into low-boiling impurities, titanium tetrachloride containing the low-boiling impurities is fed from the middle upper part of a distillation tower, the heat is increased by reboiling titanium tetrachloride liquid at the bottom of the tower, and a gas phase mixture containing the low-boiling impurities and titanium tetrachloride is produced, and the gas phase mixture is condensed and enters a product reflux tank at the top of the distillation tower, and is divided into two parts by a reflux pump to be respectively fed into the distillation tower and a byproduct discharge system. In the process, in order to improve the separation effect of low-boiling-point impurities, the heat exchange area of the condenser needs to be large enough, so that the total condensation of the product can be met, and the reflux temperature of the reflux to the distillation tower can be ensured to be below 40 ℃, so that the volume and the cost of the condenser are increased. If all the products are condensed and then refluxed to the distillation tower, the discharge amount of the gas phase mixture as a byproduct must be increased, and at this time, the gas phase mixture contains a large amount of titanium tetrachloride, and if the gas phase mixture is directly discharged as a byproduct, the waste of titanium tetrachloride is caused, and the yield of titanium tetrachloride is reduced.
Therefore, the separation effect and the economic cost of the low-boiling-point impurities in the titanium tetrachloride are not ideal at present.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a gaseous phase separator of low boiling point impurity in titanium tetrachloride, through the temperature that improves distillation column tower top product condensate, increase the gaseous phase partial pressure of low boiling point impurity for more low boiling point impurity gets into the gaseous phase, and rethread pressure release pipeline gets into tail gas condensing system and collects, and the quality of titanium tetrachloride product is showing to improve in the top of the tower by-product output that significantly reduces like this.
In order to realize the purpose, the utility model discloses the technical scheme who adopts is: a gas phase separation device for low-boiling-point impurities in titanium tetrachloride comprises a distillation tower, a distillation tower reflux tank, a distillation tower reflux pump and a tower top byproduct tank, wherein a liquid phase inlet of the distillation tower is used for feeding mixed liquid to be separated; the gas phase outlet at the top of the distillation tower is connected with the inlet of the reflux tank of the distillation tower through a condenser; a jacket for heating and insulating the tank body is sleeved outside the tank body of the distillation tower reflux tank, and an inner cavity of the jacket is connected with a heat source through a pipeline; a liquid outlet at the bottom of the distillation tower reflux tank is connected with an inlet of a distillation tower reflux pump outside the tank body, an outlet of the distillation tower reflux pump is connected with two pipelines, a main line of the first pipeline is connected with a liquid phase inlet of the distillation tower through a distillation tower reflux cooler, a branch line of the first pipeline is connected with the tower top byproduct tank, and a second pipeline is connected with a nozzle arranged at the top inside the distillation tower reflux tank; valves for controlling the liquid flow are respectively arranged on the main line, the branch line and the second pipeline of the first pipeline; the top of the distillation tower reflux tank is also connected with a tail gas condensing system outside the tank body so as to discharge a gas phase mixture in a space above the liquid level of the distillation tower reflux tank.
The heat source is waste heat steam generated in the production of titanium tetrachloride.
The nozzle is a spiral nozzle.
The jet angle of the spiral nozzle is 170 degrees at most.
The main line of the first pipeline is also provided with a filter for intercepting solid particles, and the filter is positioned at the upstream of the reflux cooler of the distillation tower.
The filter has a titanium powder sintered filter element.
The filter had a filtration accuracy of 3 microns.
The utility model has the advantages that: when the separation device of the utility model is used for carrying out the gas phase separation of low boiling point impurities, the heating of the reflux tank of the distillation tower is carried out through the jacket, the gas phase balance partial pressure of the low boiling point impurities can be increased, the space for separating more low boiling point impurities from the liquid phase mixture to enter the top of the reflux tank is facilitated, and a part of the liquid phase mixture which is forced to circulate is atomized and sprayed out by the nozzle at the top of the reflux tank, the atomized low boiling point impurities are further enabled to enter the gas phase, so that the gas phase concentration of the low boiling point impurities at the top of the reflux tank of the distillation tower is promoted by 3-5 times, and the recovery of the low boiling point impurities; because a part of liquid phase mixture is forced to circulate and flow back to the reflux tank of the distillation column, can reduce the discharge of the by-product at the top of the distillation column, namely can reduce the loss of titanium tetrachloride, relatively raise the output of titanium tetrachloride, through testing, the by-product in the by-product tank of the top of the column can be reduced by more than 50%; the utility model discloses separation effect to low boiling point impurity has obvious improvement, through detecting, and oxygen content can fall to 0.03% in the titanium tetrachloride product after separating low boiling point impurity, and carbon content can fall to 0.005%, all is less than the level of oxygen content and carbon content among the prior art.
Drawings
Fig. 1 is a schematic structural view of the present invention;
the labels in the figure are: 1. a distillation column reflux tank 2, a distillation column reflux pump 3, a nozzle 4, a jacket 5, a column top product storage tank 6, a tail gas condensing system 7, a filter 8, a distillation column reflux cooler 9 and a distillation column.
Detailed Description
The following detailed description of the present invention is provided with reference to the accompanying drawings and examples, but not to be construed as limiting the present invention in any way.
Referring to the attached drawing, the gas phase separation device for low-boiling point impurities in titanium tetrachloride comprises a distillation tower reflux tank 1, a distillation tower reflux pump 2, a tower top byproduct tank 5, a tail gas condensation system 6, a filter 7, a distillation tower reflux cooler 8 and a distillation tower 9.
A liquid phase inlet is arranged at the middle upper part of the distillation tower 9 and used for feeding mixed liquid to be separated, a gas phase outlet is arranged at the top of the distillation tower 9 and is connected with an inlet of a condenser through a pipeline, an outlet of the condenser is connected with an inlet of the distillation tower reflux tank 1, a gas phase mixture which is generated by heating and boiling of mixed liquid in the distillation tower 9 and contains low-boiling-point impurities and titanium tetrachloride enters the condenser through the gas phase outlet to be condensed into liquid, and then the liquid flows into the distillation tower reflux tank 1, as shown in fig. 1, a vertical arrow at the top of the distillation tower reflux tank 1 is the direction in which the condensed liquid enters the distillation tower reflux tank 1. The condensation of the gaseous mixture in the distillation column 9 into the distillation column reflux drum 1 belongs to the prior art in the field, and for the sake of simplicity of illustration and also to highlight the improvements of the present invention, the condenser is not shown in fig. 1.
The tank body of the distillation tower reflux tank 1 is externally sleeved with a jacket 4, a cavity is formed in the jacket 4, the two ends of the jacket 4 are respectively an inlet and an outlet of a heat source (shown by arrows at the jacket in fig. 1), the heat source is hot steam or hot water, preferably residual heat steam in the titanium tetrachloride production process, so that extra steam preparation is not needed, the residual heat can be recycled, and the effects of energy conservation and consumption reduction are achieved. After waste heat steam is introduced into the jacket 4, the distillation tower reflux tank 1 can be heated, the temperature in the tank body is generally heated to 120 ℃, so that the vapor equilibrium partial pressure of low-boiling-point impurities in the mixed liquid in the tank can be improved (the vapor equilibrium partial pressure of titanium tetrachloride changes less than the low-boiling-point impurities), more low-boiling-point impurities are separated from the mixed liquid in a vapor form, the content of the low-boiling-point impurities in vapor substances in the upper space of the liquid level of the distillation tower reflux tank 1 is improved, and the content of the low-boiling-point impurities in the mixed liquid is reduced.
The tank bottom of distillation column reflux tank 1 is equipped with the liquid outlet, the liquid outlet pass through the pipeline with 2 access connections of distillation column reflux pump, with 2 export lug connection's of distillation column reflux pump pipeline again through tee bend and two different tube coupling: the first pipeline comprises a main line and a branch line, a filter 7 and a distillation tower reflux cooler 8 are arranged on the main line along the liquid flowing direction, the mixed liquid entering the main line is filtered by the filter 7 to remove the particulate matters of the mixed liquid, then enters the distillation tower reflux cooler 8 to be cooled to below 40 ℃, and then enters the distillation tower 9 through a liquid phase inlet of the distillation tower 9 to be boiled and gasified again; the branch line is connected with the tower top byproduct tank 5, and the mixed liquid entering the branch line enters the tower top byproduct tank 5 to be collected as a byproduct; the second pipeline is connected with a nozzle 3 arranged at the top of the distillation tower reflux tank 1, namely, the mixed liquid entering the second pipeline is forcibly circulated back to the distillation tower reflux tank 1 by a distillation tower reflux pump 2 and is atomized and sprayed out by the nozzle 3, and after the mixed liquid is atomized and sprayed out, the mixed liquid can be gasified at high temperature in the tank at an accelerated speed, so that low-boiling-point impurities in the mixed liquid enter the gas phase, the content of the low-boiling-point impurities in the gas phase is improved, and the content of the low-boiling-point impurities in the mixed liquid in the tank is. And valves for controlling the liquid flow are respectively arranged on the main line, the branch line and the second pipeline of the first pipeline.
The gas phase at the upper part of the distillation tower reflux tank 1 can enter a tail gas condensing system 6 outside the tank body through pipeline pressure relief, condensable gas is collected by a corresponding container after being condensed, and non-condensable gas is collected by a negative pumping system.
The filter element of the filter 7 is a titanium powder sintered filter element, the filtering precision of the filter element is 3 microns, and a sewage discharge outlet is formed in the bottom of the filter 7, namely the arrow at the bottom of the filter 7 in figure 1.
The nozzle 3 is a spiral nozzle, preferably a large-angle spiral nozzle with a maximum spraying angle of 170 degrees; other types of atomizing nozzles can also be used for the nozzle 3.
Cooler 8 adopts recirculated cooling water to carry out the heat exchange, and on the cooler, the bottom is equipped with the import of recirculated cooling water, and the top is equipped with the export of recirculated cooling water to import and export adopt the heteropleural setting, are located the both ends of cooler 8 respectively, and the arrow of horizontal direction on cooler 8 in the flow direction of recirculated cooling water refers to figure 1.
When the separation device is used for separating the gas phase of the low-boiling-point impurities in the titanium tetrachloride, the distillation tower 9 is a secondary distillation tower, a primary distillation tower is arranged in front of the secondary distillation tower and is mainly used for separating the high-boiling-point impurities in the titanium tetrachloride, the high-boiling-point impurities are remained in the primary distillation tower after separation, and the titanium tetrachloride gas phase mixture containing the low-boiling-point impurities flows into the secondary distillation tower through condensation. Therefore, what the distillation column liquid phase import got into can be the mixed liquid after the high boiling impurity of one-level distillation column separation, can also be mixed liquid in the distillation column reflux tank, in the following description of the gaseous phase separation method, the unified description is the liquid phase mixture who contains low boiling impurity and titanium tetrachloride.
The method for carrying out gas phase separation on low-boiling-point impurities in titanium tetrachloride by using the device comprises the following steps:
firstly, a liquid phase mixture containing low boiling point impurities and titanium tetrachloride enters a distillation tower 9 from a liquid phase inlet of the distillation tower 9, and is heated and boiled to generate a gas phase mixture containing the low boiling point impurities and the titanium tetrachloride;
secondly, the gas phase mixture containing the low boiling point impurities and the titanium tetrachloride generated by heating and boiling enters a condenser through a gas phase outlet at the top of a distillation tower 9 to be condensed into a liquid phase mixture, the content of the low boiling point impurities in the liquid phase mixture is higher than that of the low boiling point impurities in the liquid phase mixture in the previous step, and then the liquid phase mixture flows out of the condenser and enters a distillation tower reflux tank 1;
thirdly, the reflux tank 1 of the distillation tower is heated by the jacket 4, so that the temperature in the reflux tank is 120 ℃, under the temperature, the gas phase equilibrium partial pressure of low-boiling-point impurities in a liquid phase mixture in the reflux tank 1 of the distillation tower is increased, more low-boiling-point impurities enter a gas phase and fill the space above the liquid level of the reflux tank 1 of the distillation tower, the content of the low-boiling-point impurities in the liquid phase mixture is reduced, and the low-boiling-point impurities are pumped out by the reflux pump 2 of the distillation tower along with the liquid phase mixture;
and fourthly, in the previous step, the gas phase low boiling point impurities and other gas phase substances in the space above the liquid level of the distillation tower reflux tank 1 enter a tail gas condensation system 6 through a pressure relief pipeline connected with the top of the distillation tower reflux tank 1, and the liquid phase mixture containing the low boiling point impurities and pumped out by the distillation reflux pump 2 is distributed according to the following three paths: (1) enters the main line of the first line and, after being filtered and cooled, is refluxed to the distillation column 9; (2) after entering a branch line of the first pipeline, the mixture is sent to a byproduct tank 5 at the top of the tower for collection; (3) enters a second pipeline, flows back to the distillation tower reflux tank 1, and is atomized and sprayed out through the nozzle 3;
and fifthly, in the previous step, the liquid phase mixture refluxed to the distillation tower 9 repeats the processes from the first step to the fourth step, and the liquid phase mixture refluxed to the distillation tower reflux tank 1 repeats the processes from the third step and the fourth step, so that the separation of the low-boiling-point impurities from the titanium tetrachloride is finally completed.
The judgment standard for completing the separation of the low-boiling point impurities is as follows: after several times of circulation, sampling from a liquid discharge port at the bottom of the distillation tower 9 for detection, and completing the separation of low-boiling-point impurities when the oxygen content in the titanium tetrachloride sample is 0.03% and the carbon content is 0.005%. In the prior art, after the separation of low boiling point impurities in titanium tetrachloride, the oxygen content is 0.04%, and the carbon content is 0.005%, so that after the utility model is adopted, the quality of carbon tetrachloride is obviously improved.
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and it should be understood by those of ordinary skill in the art that the embodiments of the present invention can be modified or replaced with equivalents with reference to the above embodiments, and any modifications or equivalent substitutions that do not depart from the spirit and scope of the present invention are all within the scope of the claims of the present application.
Claims (6)
1. A gas phase separation device for low-boiling-point impurities in titanium tetrachloride comprises a distillation tower, a distillation tower reflux tank, a distillation tower reflux pump and a tower top byproduct tank, wherein a liquid phase inlet of the distillation tower is used for feeding mixed liquid to be separated; the gas phase outlet at the top of the distillation tower is connected with the inlet of the reflux tank of the distillation tower through a condenser, and the distillation tower is characterized in that: a jacket for heating and insulating the tank body is sleeved outside the tank body of the distillation tower reflux tank, and an inner cavity of the jacket is connected with a heat source through a pipeline; a liquid outlet at the bottom of the distillation tower reflux tank is connected with an inlet of a distillation tower reflux pump outside the tank body, an outlet of the distillation tower reflux pump is connected with two pipelines, a main line of the first pipeline is connected with a liquid phase inlet of the distillation tower through a distillation tower reflux cooler, a branch line of the first pipeline is connected with the tower top byproduct tank, and a second pipeline is connected with a nozzle arranged at the top inside the distillation tower reflux tank; valves for controlling the liquid flow are respectively arranged on the main line, the branch line and the second pipeline of the first pipeline; the top of the distillation tower reflux tank is also connected with a tail gas condensing system outside the tank body so as to discharge a gas phase mixture in a space above the liquid level of the distillation tower reflux tank.
2. The apparatus for the vapor phase separation of low boiling impurities in titanium tetrachloride according to claim 1, wherein: the nozzle is a spiral nozzle.
3. The apparatus for the vapor phase separation of low boiling impurities in titanium tetrachloride according to claim 2, wherein: the jet angle of the spiral nozzle is 170 degrees at most.
4. The apparatus for the vapor phase separation of low boiling impurities in titanium tetrachloride according to claim 1, wherein: and a filter for intercepting solid particles is arranged on the main line of the first pipeline, and the filter is positioned at the upstream of the reflux cooler of the distillation tower.
5. The apparatus for the vapor phase separation of low boiling impurities in titanium tetrachloride according to claim 4, wherein: the filter has a titanium powder sintered filter element.
6. The apparatus for the vapor phase separation of low boiling impurities in titanium tetrachloride according to claim 5, wherein: the filter had a filtration accuracy of 3 microns.
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