Thermal insulation separation device and tantalum ethoxide separation method

Abstract

The invention belongs to the technical field of production, discharging and storage of chemical liquid medicaments, and particularly relates to a heat preservation separation device and a tantalum ethoxide separation method. The thermal insulation separation device provided by the invention comprises a heat transfer part and a thermal insulation part. The invention provides the tantalum ethoxide separation method, and the thermal insulation separation device is used for separating tantalum ethoxide. While heat preservation discharging of tantalum ethoxide is guaranteed, condensation heat recovery is achieved, the temperature of tantalum ethoxide is higher than the crystallization temperature of tantalum ethoxide, and tantalum ethoxide can smoothly flow out of the discharging pipe and the receiving tank. Therefore, the temperature of the discharge pipe and the receiving tank is maintained, and the tantalum ethoxide is accelerated to be condensed and flow out of the rectifying tower. The technical problem that a pipeline is blocked by crystals during discharging of tantalum ethoxide is solved. As the heat source of the heat transfer component comes from the rectified gas needing cooling, a new heat source is not needed, energy consumption of the water chilling unit in the condensation process is reduced, cost is saved, and energy conservation and environmental protection are achieved.

Description

Technical Field

[0001] The invention belongs to the technical field of production, discharging and storage of chemical liquid medicines, and in particular relates to a heat preservation separation device and a tantalum ethoxide separation method. Background Art

[0002] Tantalum ethoxide is mainly used as an ideal precursor of tantalum oxide and is widely used in high-tech fields such as IC insulating materials, electrolytic anode surface coatings, memory, catalysts, and the preparation of ultra-high purity ultra-fine tantalum pentoxide powder. In addition, tantalum ethoxide can also be used to deposit tantalum oxide coatings or metal tantalum coatings through chemical vapor deposition (CVD). This film exhibits good optical activity and has potential applications in solar cells and photocatalysts. Tantalum ethoxide can generate tantalum nitride with a high melting point and a microcrystalline structure in circuit boards. This nitride layer structure can inhibit the diffusion of copper after contact with silicon or silicon dioxide in circuit boards. In addition, tantalum nitride can withstand higher temperatures than other barrier metals without degradation.

[0003] Based on the wide application of tantalum ethoxide mentioned above, the market demand for tantalum ethoxide is growing day by day, so there is an urgent need to improve the production efficiency of tantalum ethoxide.

[0004] Tantalum ethoxide is a colorless, transparent, viscous liquid at room temperature. It dissolves in most organic solvents, has a density of 1.566 g / mL (25 / 4°C), and a melting point of 21°C. Therefore, when the temperature is below 21°C under normal pressure, tantalum ethoxide is prone to precipitate crystals, causing material retention and blocking the discharge pipeline, which will seriously affect the production efficiency of tantalum ethoxide. Summary of the invention

[0005] The purpose of the present invention is to provide a thermal insulation separation device and a tantalum ethoxide separation method. The thermal insulation separation device provided by the present invention is used to separate tantalum ethoxide, which can realize condensation heat recovery, so that the temperature of the tantalum ethoxide discharge is higher than its crystallization temperature, and the tantalum ethoxide can flow smoothly out of the discharge pipe and the receiving tank, thereby solving the technical problem of crystallization blocking the pipeline when tantalum ethoxide is discharged.

[0006] In order to achieve the above object, the present invention provides the following technical solutions:

[0007] The present invention provides a heat preservation separation device, comprising: a distillation kettle, wherein a gas outlet is arranged at the top of the distillation kettle;

[0008] A condensation tower, wherein a gas inlet and a liquid outlet are provided at the bottom of the condensation tower, and the gas inlet of the condensation tower is connected to the gas outlet of the distillation kettle through a connecting pipeline;

[0009] A liquid product receiving tank, wherein a liquid inlet is disposed at the top of the liquid product receiving tank, and the liquid inlet of the liquid product receiving tank is connected to the liquid outlet of the condensation tower through a first discharge pipe;

[0010] A liquid impurity receiving tank, wherein a liquid inlet is provided at the top of the liquid impurity receiving tank, and the liquid inlet of the liquid impurity receiving tank is connected to the liquid outlet of the condensation tower through a second discharge pipe;

[0011] A heat transfer component, wherein the heat transfer component is a metal wire, and the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe, and the outer wall of the liquid product receiving tank, or the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the second discharge pipe, and the outer wall of the liquid impurity receiving tank, or the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe, the outer wall of the second discharge pipe, the outer wall of the liquid product receiving tank, and the outer wall of the liquid impurity receiving tank;

[0012] A heat-insulating component, wherein the heat-insulating component is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a first discharge pipe wrapped with copper wire, and the outer wall of a liquid product receiving tank wrapped with copper wire, or the heat-insulating component is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a second discharge pipe wrapped with copper wire, and the outer wall of a liquid impurity receiving tank wrapped with copper wire, or the heat-insulating component is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a first discharge pipe wrapped with copper wire, the outer wall of a second discharge pipe wrapped with copper wire, the outer wall of a liquid product receiving tank wrapped with copper wire, and the outer wall of a liquid impurity receiving tank wrapped with copper wire.

[0013] Preferably, the metal wire is a copper wire, which is composed of a plurality of copper wires, and the diameter of each copper wire is 4.4 mm.

[0014] Preferably, the liquid outlet of the condensation tower is connected to the condensation tower discharge pipe;

[0015] The liquid inlet of the liquid product receiving tank is connected to the condensation tower discharge pipe through the product discharge pipe;

[0016] The liquid inlet of the liquid impurity receiving tank is connected to the condensation tower discharge pipeline through an impurity discharge pipe.

[0017] The present invention provides the application of the heat preservation separation device described in the above technical solution in the separation of tantalum ethoxide.

[0018] The present invention provides a method for separating tantalum ethoxide, which uses the heat-insulating separation device described in the above technical solution to separate tantalum ethoxide, wherein the metal wire of the heat-insulating separation device is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe and the outer wall of the liquid product receiving tank; the heat-insulating component is wrapped on the outer wall of the connecting pipe wound with copper wire, the outer wall of the first discharge pipe wound with copper wire and the outer wall of the liquid product receiving tank wound with copper wire;

[0019] The following steps are involved:

[0020] placing a synthetic liquid in a rectification kettle for a first rectification, the synthetic liquid comprising ethanol, tantalum ethoxide and an intermediate product, obtaining ethanol gas and a first impurity-removed synthetic liquid, the ethanol gas entering the condensation tower for a first condensation, obtaining ethanol liquid, and the ethanol liquid being collected in a liquid impurity receiving tank;

[0021] The first impurity-removed synthetic liquid in the distillation kettle is subjected to a second distillation to obtain an intermediate product gas and a second impurity-removed synthetic liquid, the intermediate product gas enters the condensation tower for a second condensation to obtain an intermediate product liquid, and the intermediate product liquid is collected in a liquid impurity receiving tank;

[0022] The second impurity-removed synthetic liquid in the distillation kettle is subjected to a third distillation to obtain tantalum ethoxide gas, and the tantalum ethoxide gas enters the condensation tower for a third condensation to obtain tantalum ethoxide liquid, which is collected in a liquid product receiving tank.

[0023] Preferably, the mass concentration of tantalum ethoxide in the synthetic solution is 250-300 g / L.

[0024] Preferably, the pressure of the first distillation is normal pressure, and the temperature is 130-170°C; the temperature at which the first distillation ends is 60-90°C;

[0025] The temperature of the first condensation is 23-25°C.

[0026] Preferably, the pressure of the second distillation is 50-100 Pa, the temperature is 100-150° C., and the temperature at which the second distillation ends is 120-150° C.;

[0027] The temperature of the second condensation is 23-25°C.

[0028] Preferably, the pressure of the third distillation is 0-20 Pa, the temperature is 150-230° C., and the temperature at which the third distillation ends is 150-200° C.;

[0029] The temperature of the third condensation is 17-25°C.

[0030] Preferably, the synthetic liquid is obtained by electrolysis of a tantalum anode plate and ethanol.

[0031] The present invention provides a heat-insulating separation device, comprising: a distillation kettle, wherein a gas outlet is arranged on the top of the distillation kettle; a condensation tower, wherein a gas inlet and a liquid outlet are arranged at the bottom of the condensation tower, and the gas inlet of the condensation tower is connected with the gas outlet of the distillation kettle through a connecting pipe; a liquid product receiving tank, wherein a liquid inlet is arranged on the top of the liquid product receiving tank, and the liquid inlet of the liquid product receiving tank is connected with the liquid outlet of the condensation tower through a first discharge pipe; a liquid impurity receiving tank, wherein a liquid inlet is arranged on the top of the liquid impurity receiving tank, and the liquid inlet of the liquid impurity receiving tank is connected with the liquid outlet of the condensation tower through a second discharge pipe; a heat transfer component, wherein the heat transfer component is a metal wire, and the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe and the outer wall of the liquid product receiving tank, or the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the second discharge pipe and the outer wall of the liquid impurity receiving tank, or the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe, the outer wall of the second discharge pipe, the outer wall of the liquid product receiving tank and the outer wall of the liquid impurity receiving tank; a heat-insulating component, the heat-insulating component is wrapped on the outer wall of the connecting pipe wrapped with copper wire, the outer wall of the first discharge pipe wrapped with copper wire and the outer wall of the liquid product receiving tank wrapped with copper wire, or the heat-insulating component is wrapped on the outer wall of the connecting pipe wrapped with copper wire, the outer wall of the second discharge pipe wrapped with copper wire and the outer wall of the liquid impurity receiving tank wrapped with copper wire, or the heat-insulating component is wrapped on the outer wall of the connecting pipe wrapped with copper wire, the outer wall of the first discharge pipe wrapped with copper wire, the outer wall of the second discharge pipe wrapped with copper wire, the outer wall of the liquid product receiving tank wrapped with copper wire and the outer wall of the liquid impurity receiving tank wrapped with copper wire. In the present invention, the connecting pipe is used to transport the high-temperature gas generated by distillation in the distillation kettle to the condensation tower. Therefore, the connecting pipe conducts the heat of the high-temperature gas passing through it to the metal wire wrapped around the outer wall of the connecting pipe through heat conduction. The heat is conducted on the metal wire and transferred in turn to the metal wire wrapped around the outer wall of the first discharge pipe and / or the outer wall of the second discharge pipe and the metal wire wrapped around the outer wall of the liquid product receiving tank and / or the outer wall of the liquid impurity receiving tank, thereby providing heat for the first discharge pipe and / or the second discharge pipe and the liquid product receiving tank and / or the liquid impurity receiving tank, ensuring that the liquid in the first discharge pipe or the second discharge pipe maintains a liquid form when transporting the liquid output by the condensation tower, can smoothly flow out of the first discharge pipe or the second discharge pipe to reach the liquid product receiving tank or the liquid impurity receiving tank, and can maintain a liquid form in the liquid product receiving tank and / or the liquid impurity receiving tank, and can smoothly flow out of the liquid product receiving tank or the liquid impurity receiving tank.The thermal insulation separation device provided by the present invention not only realizes condensation heat recovery, but also can keep the liquid output from the thermal insulation condensation tower in liquid form in the discharge pipe and the receiving tank, thereby avoiding the problem of material retention and clogging of the discharge pipe due to condensation in the pipe and the receiving tank during liquid discharge; at the same time, since the heat transfer components of the discharge pipe and the receiving tank do not need to obtain a heat source from the outside, the heat source comes from the high-temperature gas obtained by distillation in the distillation kettle, and the heat of the high-temperature gas in the connecting pipe is exchanged, which not only reduces the energy consumption of the chiller of the condensation tower, but also reduces energy consumption and saves costs.

[0032] The present invention provides a method for separating tantalum ethanol, and uses the heat-insulating separation device described in the above technical solution to separate tantalum ethanol. The beneficial effect of the tantalum ethanol separation method provided by the present invention is that, while ensuring the heat-insulating discharge of tantalum ethanol, the present invention realizes condensation heat recovery, so that the temperature of tantalum ethanol is higher than its crystallization temperature, and it can flow out of the discharge pipe and the receiving tank smoothly. Therefore, the present invention not only achieves the purpose of maintaining the temperature of the discharge pipe and the receiving tank, but also accelerates the condensation of tantalum ethanol and its outflow from the distillation tower. The technical problem of crystallization blocking the pipeline when tantalum ethanol is discharged is solved. Since the heat source of the heat transfer component comes from the distillation gas that needs to be cooled, there is no need to add a new heat source, and the energy consumption of the chiller during the condensation process is reduced, saving costs, and being energy-saving and environmentally friendly. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 A schematic diagram of the crystallization of a synthetic solution containing tantalum ethoxide obtained by electrolysis of tantalum anode plate and ethanol in a pipeline;

[0034] Figure 2 This is a physical picture of the copper wire wrapped around the outer wall of the discharge pipe;

[0035] Figure 3 A schematic diagram of the structure of the heat preservation separation device provided by the present invention;

[0036] Figure 3 Middle: 1 is a distillation kettle, 2 is a condensation tower, 3 is a liquid impurity receiving tank, 4 is a liquid product receiving tank, and 5 is a first discharge pipe;

[0037] Figure 4 A schematic diagram of the partial structure of the heat preservation separation device provided by the present invention;

[0038] Figure 5 A schematic diagram of the partial structure of the heat preservation separation device provided by the present invention;

[0039] Figure 6 A schematic diagram of the partial structure of the heat preservation separation device provided by the present invention. DETAILED DESCRIPTION

[0040] The present invention provides a heat preservation separation device, comprising: a distillation kettle, wherein a gas outlet is arranged at the top of the distillation kettle;

[0041] A condensation tower, wherein a gas inlet and a liquid outlet are provided at the bottom of the condensation tower, and the gas inlet of the condensation tower is connected to the gas outlet of the distillation kettle through a connecting pipeline;

[0042] A liquid product receiving tank, wherein a liquid inlet is disposed at the top of the liquid product receiving tank, and the liquid inlet of the liquid product receiving tank is connected to the liquid outlet of the condensation tower through a first discharge pipe;

[0043] A liquid impurity receiving tank, wherein a liquid inlet is provided at the top of the liquid impurity receiving tank, and the liquid inlet of the liquid impurity receiving tank is connected to the liquid outlet of the condensation tower through a second discharge pipe;

[0044] A heat transfer component, wherein the heat transfer component is a metal wire, and the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe, and the outer wall of the liquid product receiving tank, or the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the second discharge pipe, and the outer wall of the liquid impurity receiving tank, or the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe, the outer wall of the second discharge pipe, the outer wall of the liquid product receiving tank, and the outer wall of the liquid impurity receiving tank;

[0045] A heat-insulating component, wherein the heat-insulating component is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a first discharge pipe wrapped with copper wire, and the outer wall of a liquid product receiving tank wrapped with copper wire, or the heat-insulating component is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a second discharge pipe wrapped with copper wire, and the outer wall of a liquid impurity receiving tank wrapped with copper wire, or the heat-insulating component is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a first discharge pipe wrapped with copper wire, the outer wall of a second discharge pipe wrapped with copper wire, the outer wall of a liquid product receiving tank wrapped with copper wire, and the outer wall of a liquid impurity receiving tank wrapped with copper wire.

[0046] Figure 3 A schematic diagram of the structure of the heat preservation separation device provided by the present invention, Figures 4 to 6 This is a partial structural diagram of the heat preservation separation device provided by the present invention. Figures 3 to 6 The heat preservation separation device provided by the present invention is described in detail.

[0047] The heat preservation separation device provided by the present invention comprises a distillation kettle, and a gas outlet is arranged on the top of the distillation kettle. In the present invention, the distillation kettle is used to distill the mixed solution therein to separate the components in the mixed solution.

[0048] The heat preservation separation device provided by the present invention comprises a condensation tower, wherein a gas inlet and a liquid outlet are arranged at the bottom of the condensation tower, and the gas inlet of the condensation tower is connected to the gas outlet of the distillation kettle through a connecting pipe. In the present invention, the condensation tower is used to condense the gas components, so as to facilitate the collection of the separated components.

[0049] As one or more embodiments of the present invention, the liquid outlet of the condensation tower is connected to a discharge pipe of the condensation tower.

[0050] The heat preservation separation device provided by the present invention comprises a liquid product receiving tank, the top of which is provided with a liquid inlet, and the liquid inlet of the liquid product receiving tank is connected to the liquid outlet of the condensation tower through a first discharge pipe. In the present invention, the liquid product receiving tank is used to temporarily store the separated liquid product.

[0051] The heat preservation separation device provided by the present invention comprises a liquid impurity receiving tank, the top of which is provided with a liquid inlet, and the liquid inlet of the liquid impurity receiving tank is connected to the liquid outlet of the condensation tower through a second discharge pipe. In the present invention, the liquid impurity receiving tank is used to temporarily store the separated impurity components, which include solvent components and / or intermediate product components.

[0052] As one or more embodiments of the present invention, the liquid inlet of the liquid product receiving tank is connected to the condensation tower discharge pipe through a product discharge pipe.

[0053] As one or more embodiments of the present invention, the liquid inlet of the liquid impurity receiving tank is connected to the condensation tower discharge pipeline through an impurity discharge pipe.

[0054] The thermal insulation separation device provided by the present invention includes a heat transfer component, which is a metal wire. The metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe and the outer wall of the liquid product receiving tank, or the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the second discharge pipe and the outer wall of the liquid impurity receiving tank, or the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe, the outer wall of the second discharge pipe, the outer wall of the liquid product receiving tank and the outer wall of the liquid impurity receiving tank.

[0055] As one or more embodiments of the present invention, the metal wire is a copper wire, which is composed of a plurality of copper wires, and the diameter of each copper wire is 4.4 mm.

[0056] As one or more embodiments of the present invention, the copper wire consists of 100 copper wires.

[0057] As one or more embodiments of the present invention,

[0058] As one or more embodiments of the present invention, the metal wire is wound around the outer wall of the connecting pipe, the outer wall of the first discharge pipe and the outer wall of the liquid product receiving tank at the same time, one end of the metal wire is located on the outer wall of the connecting pipe, and the other end of the metal wire is located on the outer wall of the product receiving tank. The metal wire is a whole metal wire of sufficient length from the outer wall of the connecting pipe to the outer wall of the product receiving tank.

[0059] The thermal insulation separation device provided by the present invention includes a thermal insulation component, which is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a first discharge pipe wrapped with copper wire, and the outer wall of a liquid product receiving tank wrapped with copper wire, or the thermal insulation component is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a second discharge pipe wrapped with copper wire, and the outer wall of a liquid impurity receiving tank wrapped with copper wire, or the thermal insulation component is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a first discharge pipe wrapped with copper wire, the outer wall of a second discharge pipe wrapped with copper wire, the outer wall of a liquid product receiving tank wrapped with copper wire, and the outer wall of a liquid impurity receiving tank wrapped with copper wire.

[0060] As one or more embodiments of the present invention, the heat-insulating component is formed of a heat-insulating material. The present invention has no special requirements on the material of the heat-insulating material.

[0061] The present invention provides the application of the heat preservation separation device described in the above technical solution in the separation of tantalum ethoxide.

[0062] The present invention provides a method for separating tantalum ethoxide, which uses the heat-insulating separation device described in the above technical solution to separate tantalum ethoxide, wherein the metal wire of the heat-insulating separation device is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe and the outer wall of the liquid product receiving tank; the heat-insulating component is wrapped on the outer wall of the connecting pipe wound with copper wire, the outer wall of the first discharge pipe wound with copper wire and the outer wall of the liquid product receiving tank wound with copper wire;

[0063] The following steps are involved:

[0064] placing a synthetic liquid in a rectification kettle for a first rectification, the synthetic liquid comprising ethanol, tantalum ethoxide and an intermediate product, obtaining ethanol gas and a first impurity-removed synthetic liquid, the ethanol gas entering the condensation tower for a first condensation, obtaining ethanol liquid, and the ethanol liquid being collected in a liquid impurity receiving tank;

[0065] The first impurity-removed synthetic liquid in the distillation kettle is subjected to a second distillation to obtain an intermediate product gas and a second impurity-removed synthetic liquid, the intermediate product gas enters the condensation tower for a second condensation to obtain an intermediate product liquid, and the intermediate product liquid is collected in a liquid impurity receiving tank;

[0066] The second impurity-removed synthetic liquid in the distillation kettle is subjected to a third distillation to obtain tantalum ethoxide gas, and the tantalum ethoxide gas enters the condensation tower for a third condensation to obtain tantalum ethoxide liquid, which is collected in a liquid product receiving tank.

[0067] In the present invention, unless otherwise specified, all preparation raw materials / components are commercially available products well known to those skilled in the art.

[0068] In the present invention, a synthetic liquid is placed in a distillation kettle for a first distillation. The synthetic liquid includes ethanol, tantalum ethoxide and an intermediate product to obtain ethanol gas and a first impurity-removed synthetic liquid. The ethanol gas enters the condensation tower for a first condensation to obtain ethanol liquid, which is collected in a liquid impurity receiving tank. In the present invention, the synthetic liquid is obtained by electrolysis of anode tantalum plates and ethanol, and the present invention has no special requirements for the specific implementation process of the electrolysis. The mass concentration of tantalum ethoxide in the synthetic liquid is preferably 250-300 g / L, and is specifically 275 g / L, 300 g / L or 260 g / L in the embodiment. The first distillation is to remove ethanol from the synthetic liquid. The pressure of the first distillation is preferably normal pressure, and the temperature of the first distillation is preferably 130-170°C, and is specifically 135°C, 155°C or 165°C in the embodiment. The temperature at which the first distillation ends is preferably 60-90°C, and is specifically 70°C in the embodiment. In the present invention, during the first distillation, as the first distillation proceeds, the liquid temperature in the distillation kettle drops to the temperature at which the first distillation ends, and the first distillation ends. The temperature of the first condensation is preferably 23-25°C, and specifically 25°C or 24°C in the embodiment.

[0069] After the first distillation is completed, the present invention performs a second distillation on the first impurity-removed synthetic liquid in the distillation kettle to obtain an intermediate product gas and a second impurity-removed synthetic liquid. The intermediate product gas enters the condensation tower for a second condensation to obtain an intermediate product liquid, and the intermediate product liquid is collected in a liquid impurity receiving tank. In the present invention, the second distillation is to remove the intermediate product in the synthetic liquid. The pressure of the second distillation is preferably 50-100 Pa. The temperature of the second distillation is preferably 100-150°C, and in the embodiment, it is specifically 175°C or 170°C. The temperature at which the second distillation ends is 120-150°C, and in the embodiment, it is specifically 120°C or 125°C. In the present invention, during the second distillation, as the second distillation proceeds, the liquid temperature in the distillation kettle drops to the temperature at which the second distillation ends, and the second distillation ends. The temperature of the second condensation is preferably 23-25°C, and in the embodiment, it is specifically 24°C, 23°C or 25°C.

[0070] After the second distillation is completed, the present invention performs a third distillation on the second impurity-removing synthetic liquid in the distillation kettle to obtain tantalum ethoxide gas, and the tantalum ethoxide gas enters the condensation tower for a third condensation to obtain tantalum ethoxide liquid, and the tantalum ethoxide liquid is collected in a liquid product receiving tank. In the present invention, the third distillation is used to separate tantalum ethoxide from the nucleating liquid. The pressure of the third distillation is preferably 0-20 Pa. The temperature of the third distillation is preferably 150-230°C, and specifically 170°C, 200°C or 220°C in the embodiment. The temperature at which the third distillation ends is preferably 150-200°C, and specifically 155°C or 180°C in the embodiment. In the present invention, during the third distillation process, as the third distillation proceeds, the temperature of the liquid in the distillation kettle drops to the temperature at which the third distillation ends, and the third distillation ends. The temperature of the third condensation is preferably 17-25°C, and specifically 22°C, 23°C or 19°C in the embodiment.

[0071] In order to further illustrate the present invention, the technical solutions provided by the present invention are described in detail below in conjunction with embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0072] Example 1

[0073] (1) adding a synthetic liquid containing tantalum ethoxide at a concentration of 260 g / L obtained by electrolysis of an anode tantalum plate and ethanol into a distillation kettle 1, wherein the synthetic liquid contains tantalum ethoxide, an intermediate product and ethanol;

[0074] The synthetic liquid is heated to a set temperature of 135° C. in a distillation reactor 1 under normal pressure;

[0075] evaporating ethanol in a synthetic liquid heated at a set temperature into ethanol gas;

[0076] The evaporated ethanol gas is condensed into ethanol liquid through a condensation tower 2 at 25°C, and the condensed ethanol liquid flows out from the outlet of the condensation tower and enters the ethanol receiving tank 3 through a discharge pipe connecting the outlet of the condensation tower and the inlet of the ethanol receiving tank 3 and a valve on the pipe;

[0077] When the liquid temperature in the distillation kettle 1 drops to 70°C, the ethanol distillation is finished and the discharge valve of the condensing tower is closed;

[0078] (2) When the liquid temperature in the distillation kettle 1 reaches 170° C., the distillation kettle 1 is slowly evacuated to a certain pressure, and the discharge valve of the distillation kettle 1 is slowly opened;

[0079] The intermediate product in the synthetic liquid heated at a set temperature of 170°C and a pressure of 50Pa is evaporated into an intermediate gas;

[0080] The evaporated intermediate gas is condensed into an intermediate liquid through a condensation tower 2 at 24° C. The condensed intermediate liquid flows out from the outlet of the condensation tower and enters the intermediate product receiving tank through a discharge pipe connecting the outlet of the condensation tower and the inlet of the intermediate product receiving tank and a valve on the pipe. In this embodiment, since the intermediate product accounts for a very small proportion of the mass of the synthetic liquid, before slowly evacuating the distillation kettle 1 to a certain pressure (10 Pa) in step (2), the ethanol received in the ethanol receiving tank in step (1) is emptied in this embodiment. During the process of slowly evacuating the distillation kettle 1 to a certain pressure in step (2), the intermediate product flows to the ethanol receiving tank 3. At this time, the ethanol receiving tank 3 serves as the intermediate product receiving tank.

[0081] When the liquid temperature in the distillation reactor 1 drops to 120°C, close the discharge valve of the condensing tower;

[0082] (3) adjusting the heating temperature of the distillation kettle 1 to 170° C. and the pressure to negative pressure;

[0083] The tantalum ethoxide in the synthetic liquid at a set temperature (170° C.) and pressure (0 Pa) is evaporated into tantalum ethoxide gas;

[0084] The evaporated tantalum ethoxide gas is condensed into tantalum ethoxide liquid via a condensation tower 2 at 22°C;

[0085] The condensed tantalum ethoxide liquid flows out from the outlet of the condensation tower 2, and enters the tantalum ethoxide receiving tank 4 through the discharge pipe connecting the condensation tower outlet and the tantalum ethoxide receiving tank 4 and the valve on the pipe;

[0086] When no tantalum ethoxide flows out of the discharge pipe, the temperature in the distillation kettle 1 rises to 155° C. and does not change, and no liquid flows out of the discharge pipe, the distillation of tantalum ethoxide is completed.

[0087] In this embodiment, the gas outlet of the distillation kettle 1 and the gas inlet of the condensation tower are connected by

[0088] Copper wire is wound around the outer wall of the connecting pipe between the distillation kettle 1 and the condensation tower 2, the outer wall of the tantalum ethanol discharge pipe from the liquid outlet of the condensation tower 2 to the feed port of the tantalum ethanol receiving tank, and the outer wall of the tantalum ethanol receiving tank at the same time; then, the outer wall of the copper wire is wrapped with insulation material, one end of the copper wire is connected to the outer wall of the connecting pipe, and the other end is connected to the outer wall of the bottom of the tantalum ethanol receiving tank, and the copper wire conducts the heat of the connecting pipe to the tantalum ethanol discharge pipe and the tantalum ethanol receiving tank.

[0089] Example 2

[0090] (1) adding a synthetic liquid containing tantalum ethoxide at a concentration of 300 g / L obtained by electrolysis of an anode tantalum plate and ethanol into a distillation kettle 1, wherein the synthetic liquid contains tantalum ethoxide, an intermediate product and ethanol;

[0091] The synthetic liquid is heated to a set temperature of 155° C. in a distillation reactor 1 under normal pressure;

[0092] evaporating ethanol in a synthetic liquid heated at a set temperature into ethanol gas;

[0093] The evaporated ethanol gas is condensed into ethanol liquid through a condensation tower 2 at 24°C, and the condensed ethanol liquid flows out from the outlet of the condensation tower and enters the ethanol receiving tank 3 through a discharge pipe connecting the outlet of the condensation tower and the inlet of the ethanol receiving tank 3 and a valve on the pipe;

[0094] When the liquid temperature in the distillation kettle 1 drops to 70°C, the ethanol distillation is finished and the discharge valve of the condensing tower is closed;

[0095] (2) When the liquid temperature in the distillation kettle 1 reaches 175°C, the distillation kettle 1 is slowly evacuated to a certain pressure, and the discharge valve of the distillation kettle 1 is slowly opened;

[0096] The intermediate product in the synthetic liquid heated at a set temperature of 175°C and a pressure of 50Pa is evaporated into an intermediate gas;

[0097] The evaporated intermediate gas is condensed into an intermediate liquid through a condensation tower 2 at 23° C. The condensed intermediate liquid flows out from the outlet of the condensation tower and enters the intermediate product receiving tank through a discharge pipe connecting the outlet of the condensation tower and the inlet of the intermediate product receiving tank and a valve on the pipe. In this embodiment, since the mass proportion of the intermediate product in the synthetic liquid is very small, before the distillation kettle 1 is slowly evacuated to a certain pressure (10 Pa) in step (2), the ethanol received in the ethanol receiving tank in step (1) is emptied in this embodiment. During the process of slowly evacuating the distillation kettle 1 to a certain pressure in step (2), the intermediate product flows to the ethanol receiving tank 3, and at this time, the ethanol receiving tank 3 serves as the intermediate product receiving tank;

[0098] When the liquid temperature in the distillation kettle drops to 120°C, close the discharge valve of the condensing tower;

[0099] (3) adjusting the heating temperature of the distillation kettle 1 to 200° C. and the pressure to negative pressure;

[0100] The tantalum ethoxide in the synthetic liquid at a set temperature (170° C.) and pressure (0 Pa) is evaporated into tantalum ethoxide gas;

[0101] The evaporated tantalum ethoxide gas is condensed into tantalum ethoxide liquid via a condensation tower 2 at 23°C;

[0102] The condensed tantalum ethoxide liquid flows out from the outlet of the condensation tower 2, passes through the constant temperature pipe 5 of the condensation discharge pipe of the distillation kettle and enters the tantalum ethoxide receiving tank 4;

[0103] When no tantalum ethoxide flows out of the discharge pipe, the temperature in the distillation kettle 1 rises to 180° C. and does not change, and no liquid flows out of the discharge pipe, the distillation of tantalum ethoxide is completed.

[0104] Copper wire is wound around the outer wall of the connecting pipe between the distillation kettle 1 and the condensation tower 2, the outer wall of the tantalum ethanol discharge pipe from the liquid outlet of the condensation tower 2 to the feed port of the tantalum ethanol receiving tank, and the outer wall of the tantalum ethanol receiving tank at the same time; then, the outer wall of the copper wire is wrapped with insulation material, one end of the copper wire is connected to the outer wall of the connecting pipe, and the other end is connected to the outer wall of the bottom of the tantalum ethanol receiving tank, and the copper wire conducts the heat of the connecting pipe to the tantalum ethanol discharge pipe and the tantalum ethanol receiving tank.

[0105] Example 3

[0106] (1) adding a synthetic liquid containing tantalum ethoxide at a concentration of 275 g / L obtained by electrolysis of an anode tantalum plate and ethanol into a distillation kettle 1, wherein the synthetic liquid contains tantalum ethoxide, an intermediate product and ethanol;

[0107] The synthetic liquid is heated to a set temperature of 165° C. in a distillation reactor 1 under normal pressure;

[0108] evaporating ethanol in a synthetic liquid heated at a set temperature into ethanol gas;

[0109] The evaporated ethanol gas is condensed into ethanol liquid through a condensation tower 2 at 24°C, and the condensed ethanol liquid flows out from the outlet of the condensation tower and enters the ethanol receiving tank 3 through a discharge pipe connecting the outlet of the condensation tower and the inlet of the ethanol receiving tank 3 and a valve on the pipe;

[0110] When the liquid temperature in the distillation kettle 1 drops to 70°C, the ethanol distillation is finished and the discharge valve of the condensing tower is closed;

[0111] (2) When the liquid temperature in the distillation kettle 1 reaches 175°C, the distillation kettle 1 is slowly evacuated to a certain pressure, and the discharge valve of the distillation kettle 1 is slowly opened;

[0112] The intermediate product in the synthetic liquid heated at a set temperature of 175°C and a pressure of 50Pa is evaporated into an intermediate gas;

[0113] The evaporated intermediate gas is condensed into an intermediate liquid through a condensation tower 2 at 23° C. The condensed intermediate liquid flows out from the outlet of the condensation tower and enters the intermediate product receiving tank through a discharge pipe connecting the outlet of the condensation tower and the inlet of the intermediate product receiving tank and a valve on the pipe. In this embodiment, since the mass proportion of the intermediate product in the synthetic liquid is very small, before the distillation kettle 1 is slowly evacuated to a certain pressure (10 Pa) in step (2), the ethanol received in the ethanol receiving tank in step (1) is emptied in this embodiment. During the process of slowly evacuating the distillation kettle 1 to a certain pressure in step (2), the intermediate product flows to the ethanol receiving tank 3, and at this time, the ethanol receiving tank 3 serves as the intermediate product receiving tank;

[0114] When the liquid temperature in the distillation kettle drops to 125°C, close the discharge valve of the condensing tower;

[0115] (3) adjusting the heating temperature of the distillation kettle 1 to 220° C. and the pressure to negative pressure;

[0116] The tantalum ethoxide in the synthetic liquid at a set temperature (170° C.) and pressure (0 Pa) is evaporated into tantalum ethoxide gas;

[0117] The evaporated tantalum ethoxide gas is condensed into tantalum ethoxide liquid via a condensation tower 2 at 19°C;

[0118] The condensed tantalum ethoxide liquid flows out from the outlet of the condensation tower 2, passes through the constant temperature pipe 5 of the condensation discharge pipe of the distillation kettle and enters the tantalum ethoxide receiving tank 4;

[0119] When no tantalum ethoxide flows out of the discharge pipe, the temperature in the distillation kettle 1 rises to 150° C. and does not change, and no liquid flows out of the discharge pipe, the distillation of tantalum ethoxide is completed.

[0120] Copper wire is wound around the outer wall of the connecting pipe between the distillation kettle 1 and the condensation tower 2, the outer wall of the tantalum ethanol discharge pipe from the liquid outlet of the condensation tower 2 to the feed port of the tantalum ethanol receiving tank, and the outer wall of the tantalum ethanol receiving tank at the same time; then, the outer wall of the copper wire is wrapped with insulation material, one end of the copper wire is connected to the outer wall of the connecting pipe, and the other end is connected to the outer wall of the bottom of the tantalum ethanol receiving tank, and the copper wire conducts the heat of the connecting pipe to the tantalum ethanol discharge pipe and the tantalum ethanol receiving tank.

[0121] From the above embodiments, it can be seen that the present invention realizes condensation heat recovery while ensuring the thermal insulation of tantalum ethanol discharge, so that the temperature of tantalum ethanol is higher than its crystallization temperature, and it can flow out of the discharge pipe and the receiving tank smoothly. Therefore, the present invention not only achieves the purpose of maintaining the temperature of the discharge pipe and the receiving tank, but also accelerates the condensation of tantalum ethanol and its outflow from the distillation tower. The technical problem of crystallization blocking the pipeline when tantalum ethanol is discharged is solved. Since the heat transfer component does not need to obtain a heat source from the outside, the heat source comes from the distillation gas that needs to be cooled, which reduces the energy consumption of the chiller during the condensation process, reduces energy consumption, saves costs, and is energy-saving and environmentally friendly.

[0122] Although the above embodiment describes the present invention in detail, it is only a part of the embodiments of the present invention, not all of the embodiments. Other embodiments can be obtained based on this embodiment without creativity, and these embodiments all fall within the protection scope of the present invention.

Claims

1. A heat preservation separation device, characterized in that: include: A distillation kettle, wherein a gas outlet is provided at the top of the distillation kettle; A condensation tower, wherein a gas inlet and a liquid outlet are provided at the bottom of the condensation tower, and the gas inlet of the condensation tower is connected to the gas outlet of the distillation kettle through a connecting pipeline; A liquid product receiving tank, wherein a liquid inlet is disposed at the top of the liquid product receiving tank, and the liquid inlet of the liquid product receiving tank is connected to the liquid outlet of the condensation tower through a first discharge pipe; A liquid impurity receiving tank, wherein a liquid inlet is provided at the top of the liquid impurity receiving tank, and the liquid inlet of the liquid impurity receiving tank is connected to the liquid outlet of the condensation tower through a second discharge pipe; A heat transfer component, wherein the heat transfer component is a metal wire, and the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe, and the outer wall of the liquid product receiving tank, or the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the second discharge pipe, and the outer wall of the liquid impurity receiving tank, or the metal wire is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe, the outer wall of the second discharge pipe, the outer wall of the liquid product receiving tank, and the outer wall of the liquid impurity receiving tank; A heat-insulating component, wherein the heat-insulating component is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a first discharge pipe wrapped with copper wire, and the outer wall of a liquid product receiving tank wrapped with copper wire, or the heat-insulating component is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a second discharge pipe wrapped with copper wire, and the outer wall of a liquid impurity receiving tank wrapped with copper wire, or the heat-insulating component is wrapped on the outer wall of a connecting pipe wrapped with copper wire, the outer wall of a first discharge pipe wrapped with copper wire, the outer wall of a second discharge pipe wrapped with copper wire, the outer wall of a liquid product receiving tank wrapped with copper wire, and the outer wall of a liquid impurity receiving tank wrapped with copper wire.

2. The heat preservation separation device according to claim 1, characterized in that: The metal wire is a copper wire, which is composed of a plurality of copper wires, and the diameter of each copper wire is 4.4 mm.

3. The heat preservation separation device according to claim 1, characterized in that: The liquid outlet of the condensation tower is connected to the condensation tower discharge pipe; The liquid inlet of the liquid product receiving tank is connected to the condensation tower discharge pipe through the product discharge pipe; The liquid inlet of the liquid impurity receiving tank is connected to the condensation tower discharge pipeline through an impurity discharge pipe.

4. Use of the heat preservation separation device according to any one of claims 1 to 3 in the separation of tantalum ethoxide.

5. A method for separating tantalum ethoxide, characterized in that: The thermal insulation separation device according to any one of claims 1 to 3 is used to separate tantalum ethoxide, wherein the metal wire of the thermal insulation separation device is simultaneously wound on the outer wall of the connecting pipe, the outer wall of the first discharge pipe and the outer wall of the liquid product receiving tank; the thermal insulation component is wrapped on the outer wall of the connecting pipe wound with copper wire, the outer wall of the first discharge pipe wound with copper wire and the outer wall of the liquid product receiving tank wound with copper wire; The following steps are involved: placing a synthetic liquid in a distillation kettle for a first distillation, the synthetic liquid comprising ethanol, tantalum ethoxide and an intermediate product, obtaining ethanol gas and a first impurity-removed synthetic liquid, the ethanol gas entering the condensation tower for a first condensation, obtaining ethanol liquid, and the ethanol liquid being collected in a liquid impurity receiving tank; The first impurity-removed synthetic liquid in the distillation kettle is subjected to a second distillation to obtain an intermediate product gas and a second impurity-removed synthetic liquid, the intermediate product gas enters the condensation tower for a second condensation to obtain an intermediate product liquid, and the intermediate product liquid is collected in a liquid impurity receiving tank; The second impurity-removed synthetic liquid in the distillation kettle is subjected to a third distillation to obtain tantalum ethoxide gas, and the tantalum ethoxide gas enters the condensation tower for a third condensation to obtain tantalum ethoxide liquid, which is collected in a liquid product receiving tank.

6. The method for separating tantalum ethoxide according to claim 5, characterized in that: The mass concentration of tantalum ethoxide in the synthetic solution is 250-300 g / L.

7. The method for separating tantalum ethoxide according to claim 5 or 6, characterized in that: The pressure of the first distillation is normal pressure, and the temperature is 130-170° C.; the temperature at the end of the first distillation is 60-90° C.; The temperature of the first condensation is 23-25°C.

8. The method for separating tantalum ethoxide according to claim 5 or 6, characterized in that: The pressure of the second distillation is 50-100 Pa, the temperature is 100-150° C., and the temperature at which the second distillation ends is 120-150° C.; The temperature of the second condensation is 23-25°C.

9. The method for separating tantalum ethoxide according to claim 5 or 6, characterized in that: The pressure of the third distillation is 0-20 Pa, the temperature is 150-230° C., and the temperature at which the third distillation ends is 150-200° C.; The temperature of the third condensation is 17-25°C.

10. The method for separating tantalum ethoxide according to claim 5 or 6, characterized in that: The synthetic liquid is obtained by electrolyzing an anode tantalum plate and ethanol.

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