Continuous production device and method for rare earth chloride solid

Abstract

The invention discloses a continuous production device and method for rare earth chloride solids. The device comprises a rare earth chloride solution heater, a rare earth chloride solution separator, a jacket reaction kettle and a flaker, and no pump is arranged between the rare earth chloride solution separator and the rare earth chloride solution heater. By adopting the device and the method disclosed by the invention, continuous production of the rare earth chloride solid can be realized, the production efficiency is high, and the material leakage phenomenon is basically avoided.

Description

Technical Field

[0001] The invention relates to a continuous production device and method for rare earth chloride solids, and in particular to a continuous production device and method for flaky rare earth chloride solids. Background Art

[0002] Solid rare earth chloride is widely used as an important raw material or product in the rare earth smelting process. Among them, solid mixed rare earth chloride is easy to transport and can be used as a raw material for downstream separation, and solid single rare earth chloride can be sold as a terminal product.

[0003] At present, the production process of rare earth chloride solid generally includes evaporation concentration, water-cooling crystallization, crystal crushing and packaging, but the existing production process has problems such as low production efficiency, leakage, easy blockage during crystallization, low heat exchange efficiency, and slightly poor resistance to chlorine corrosion. Specifically:

[0004] Some use a jacketed enamel reactor + a flaker for production. The jacket of the jacketed enamel reactor uses steam or heat transfer oil as a heat source for heating, and a venturi vacuum pump is used to reduce pressure in the reactor. The concentration of the rare earth chloride solution gradually increases until it reaches the concentration requirement, and then is placed in the flaker for cooling, flake making, and crushing. However, the production equipment is not operated continuously, and a single reactor can only produce 5T (REO) products in 24 hours, with low production efficiency and high labor intensity.

[0005] Some use triple-effect evaporator + centrifuge equipment. The rare earth chloride solution is pre-concentrated through a multi-effect evaporation system. When the pre-concentration reaches a certain concentration, it is transported to a centrifuge for solid-liquid separation. The solid is used as the product, and the mother liquor continues to be concentrated. However, the operation of this equipment is discontinuous, the equipment is complicated and prone to leakage, and the material is easily blocked by the pump to circulate, affecting production. In addition, the centrifuge has a high speed and is very dangerous.

[0006] CN103172102A discloses a production process for granular rare earth chloride crystallization using a rare earth chloride solution, comprising: adding hydrochloric acid to adjust the pH value of the rare earth chloride solution and then evaporating it, condensing the water vapor and the escaped hydrogen chloride gas and then reusing it, the evaporated solution enters the cooling system by gravity and is cooled to room temperature for crystallization, and then is pumped into a centrifuge for solid-liquid separation, the mother liquor is reused, and the solid is a granular rare earth chloride crystal. The production process is an intermittent process, and the effect body is circulated by a pump, which is prone to leaking points (i.e., there is a leakage phenomenon), and the energy consumption is large and easy to damage, the heat exchange efficiency is low, and the corrosion resistance of chlorine-containing materials still needs to be further improved. In addition, it uses a centrifuge for solid-liquid separation, which is prone to blockage.

[0007] CN112499661A discloses a method for preparing flaky rare earth chloride, which is realized by a system for preparing flaky rare earth chloride, wherein the system comprises a melting unit, a continuous discharging unit, a conveying unit and a crushing unit connected in sequence, and the method comprises: in the melting unit, after the rare earth chloride solution is transferred into an evaporation concentration tank, molten rare earth chloride is formed by vacuum evaporation and concentration. The molten rare earth chloride is transferred into a storage tank, and the temperature in the storage tank is controlled to be 128°C, so that the rare earth chloride remains in a molten state; the molten rare earth chloride is transported to the conveying unit through the continuous discharging unit, and the temperature is reduced to below 40°C on the conveying unit, so that the rare earth chloride is cooled and crystallized; the cooled and crystallized rare earth chloride is transported to the crushing unit for crushing to obtain flaky rare earth chloride. The flaky rare earth chloride obtained in the patent document has a low REO content. In addition, the patent document adopts an evaporation concentration tank, which has a small processing capacity and low production efficiency.

[0008] CN217052344U discloses a rare earth liquid concentration device, including rare earth chloride pipeline, steam pipeline, vacuum concentration preheating tank, vacuum concentration tank, transfer tank and vacuum system, the vacuum concentration preheating tank is provided with a preheating jacket, the vacuum concentration tank is provided with a heating coil, the steam pipeline is connected to the preheating jacket, the preheating jacket is connected to the heating coil, the rare earth chloride pipeline is connected to the feed port of the vacuum concentration preheating tank, the discharge port of the vacuum concentration preheating tank is connected to the feed port of the vacuum concentration tank, the discharge port of the vacuum concentration tank is connected to the transfer tank, and the vacuum concentration tank is connected to the vacuum system. The device has a small processing capacity, low production efficiency, many types of intermediate equipment, and if mass production requires multiple sets of equipment, it occupies a large area. Summary of the invention

[0009] In view of this, one object of the present invention is to provide a continuous production device for rare earth chloride solids, which can realize the continuous production of rare earth chloride solids, has high production efficiency, and basically has no leakage. Furthermore, it has high heat exchange efficiency and good chlorine corrosion resistance. In addition, it is not easy to clog. Another object of the present invention is to provide a method for continuously producing rare earth chloride solids using the continuous production device as described above. The present invention adopts the following technical scheme to achieve the above purpose.

[0010] In one aspect, the present invention provides a continuous production device for rare earth chloride solids, comprising a rare earth chloride solution heater, a rare earth chloride solution separator, a jacketed reactor and a flake forming machine;

[0011] The rare earth chloride solution heater is used to receive the preheated rare earth chloride solution and further heat it to obtain a concentrated rare earth chloride solution;

[0012] The lower part of the rare earth chloride solution separator is connected to the top of the rare earth chloride solution heater through a pipeline, and the bottom of the rare earth chloride solution separator is connected to the bottom of the rare earth chloride solution heater through a pipeline, so that the concentrated rare earth chloride solution is continuously separated into gas and liquid in the rare earth chloride solution separator, and the pre-concentrated rare earth chloride solution and the primary feed liquid steam are continuously obtained; no pump is arranged between the rare earth chloride solution heater and the rare earth chloride solution separator;

[0013] The rare earth chloride solution separator is configured as a steel cylinder lined with graphite structure; the rare earth chloride solution heater is configured as a round block hole impermeable graphite structure;

[0014] The top of the jacketed reactor is connected to the bottom of the rare earth chloride solution separator through a pipeline, and is used to further concentrate the pre-concentrated rare earth chloride solution to obtain a rare earth chloride solution concentrated to a target concentration; the jacketed reactor is configured as a graphite reactor;

[0015] The flake forming machine is configured to cool, crystallize and flake the rare earth chloride solution concentrated to a target concentration to obtain a rare earth chloride solid.

[0016] The continuous production device according to the present invention preferably further comprises a rare earth chloride solution preheater and a liquid steam condenser;

[0017] The rare earth chloride solution preheater is used to preheat the rare earth chloride solution, and one end of the rare earth chloride solution preheater is connected to the bottom of the rare earth chloride solution heater; the rare earth chloride solution preheater is a horizontal graphite jacket heat exchanger;

[0018] The top of the feed liquid steam condenser is connected to the top of the rare earth chloride solution separator through a pipeline, and is used to receive the primary feed liquid steam and cool it; the feed liquid steam condenser is configured as a round block hole impermeable graphite structure;

[0019] The rare earth chloride solution heater is also configured to generate steam condensed water by heat exchange, and transport the steam condensed water to the rare earth chloride solution preheater, thereby preheating the rare earth chloride solution.

[0020] The continuous production device according to the present invention preferably further comprises a steam supply unit and a cooling water supply unit;

[0021] The steam supply unit is connected to the top of the rare earth chloride solution heater and the top of the jacketed reactor through pipelines, respectively, for supplying hot steam to them;

[0022] The cooling water supply unit is connected to the bottom of the feed liquid steam condenser through a pipeline, and is used to supply cooling water to the feed liquid steam condenser, thereby cooling the primary feed liquid steam.

[0023] The continuous production device according to the present invention preferably further comprises a liquid condensate storage tank and a horizontal closed-circuit vacuum device;

[0024] The top of the feed liquid condensate storage tank is respectively connected to the bottom of the feed liquid steam condenser and the top of the jacketed reactor through pipelines;

[0025] The feed liquid condensate storage tank is connected to the horizontal closed-circuit vacuum equipment through a pipeline, so that vacuum is formed in both the rare earth chloride solution separator and the jacketed reactor.

[0026] According to the continuous production device of the present invention, preferably, it also includes a steam condensate storage tank, which is connected to one end of the rare earth chloride solution preheater and the bottom of the jacketed reactor through pipelines respectively.

[0027] According to the continuous production device of the present invention, preferably, it also includes a rare earth chloride solution storage tank, which is connected to the rare earth chloride solution preheater through a pipeline and is used to provide rare earth chloride solution to the rare earth chloride solution preheater.

[0028] According to the continuous production device of the present invention, preferably, an insertion type differential pressure level gauge, an insertion type specific gravity meter and a pressure transmitter are arranged in the rare earth chloride solution separator; and a pressure transmitter is arranged in the jacketed reactor.

[0029] On the other hand, the present invention also provides a method for continuously producing rare earth chloride solids using the continuous production device as described above, comprising the following steps:

[0030] 1) supplying a rare earth chloride solution to the rare earth chloride solution preheater, wherein the rare earth chloride solution preheater preheats the rare earth chloride solution to a temperature greater than or equal to 75° C. to obtain a preheated rare earth chloride solution; wherein the rare earth chloride solution has a REO content greater than or equal to 30 wt % and a pH value of 1.5 to 2;

[0031] 2) conveying the preheated rare earth chloride solution to the rare earth chloride solution heater for further heating to obtain a concentrated rare earth chloride solution; wherein the temperature of the concentrated rare earth chloride solution is 130-140° C.;

[0032] 3) introducing the concentrated rare earth chloride solution into the rare earth chloride solution separator to perform gas-liquid separation, thereby obtaining a pre-concentrated rare earth chloride solution; wherein the REO content of the pre-concentrated rare earth chloride solution is greater than 50 wt %;

[0033] 4) discharging the pre-concentrated rare earth chloride solution into the jacketed reactor for further concentration to obtain a rare earth chloride solution concentrated to a target concentration; wherein the rare earth chloride solution concentrated to the target concentration has a REO content of more than 65 wt %;

[0034] 5) introducing the rare earth chloride solution concentrated to the target concentration into the flake machine for cooling, crystallization and flake making to obtain rare earth chloride solid.

[0035] According to the method of the present invention, preferably, the pressure in the rare earth chloride solution separator is set to -60 to -90 kPa.

[0036] According to the method of the present invention, preferably, the REO content in the concentrated rare earth chloride solution is 50-55wt%; the REO content in the rare earth chloride solution concentrated to the target concentration is 65-70wt%.

[0037] The continuous production device of rare earth chloride solid of the present invention can realize the continuous production of solid rare earth chloride with high production efficiency. The REO content of the obtained rare earth chloride solid is relatively high. Furthermore, it has high heat exchange efficiency and good chlorine corrosion resistance. Furthermore, no pump is required to provide circulation power between the rare earth chloride solution heater and the rare earth chloride solution separator of the present invention, which can reduce leakage points, that is, reduce leakage. The device of the present invention is not easy to be blocked during concentration and discharge. In addition, the device of the present invention does not use multi-effect evaporation equipment and does not use multiple evaporation concentration tanks, which can reduce the floor space and reduce investment costs. The device and method of the present invention are conducive to popularization and application. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] Figure 1 It is a schematic structural diagram of the continuous production device of rare earth chloride solid of the present invention.

[0039] The following are the descriptions of the reference numerals:

[0040] 1-rare earth chloride solution storage tank, 2-rare earth chloride solution preheater, 3-rare earth chloride solution heater, 4-rare earth chloride solution separator, 5-jacketed reactor, 6-flaking machine, 7-liquid steam condenser, 8-liquid condensate storage tank, 9-steam condensate storage tank, CW-cooling water supply unit, VW-steam supply unit, HW-cooling water recovery unit, Va-horizontal closed-circuit vacuum equipment. DETAILED DESCRIPTION

[0041] The present invention is further described below in conjunction with specific embodiments, but the protection scope of the present invention is not limited thereto.

[0042] <Continuous production device for rare earth chloride solid>

[0043] The present invention provides a continuous production device for rare earth chloride solids, comprising a rare earth chloride solution preheater, a rare earth chloride solution heater, a rare earth chloride solution separator, a jacketed reactor, a flake machine, a liquid steam condenser, a steam supply unit, a cooling water supply unit, a liquid condensate storage tank, a steam condensate storage tank, and a cooling water recovery unit. Preferably, it also includes a rare earth chloride solution storage tank and a horizontal closed-circuit vacuum device. The following is a detailed description.

[0044] Rare earth chloride solution storage tank

[0045] The rare earth chloride solution storage tank is used to store the rare earth chloride solution and supply the rare earth chloride solution to the rare earth chloride solution preheater. In certain specific embodiments, the rare earth chloride solution storage tank can supply the rare earth chloride solution to the rare earth chloride solution preheater via an output pump.

[0046] Rare earth chloride solution preheater

[0047] The rare earth chloride solution preheater is used to preheat the rare earth chloride solution to obtain the preheated rare earth chloride solution, which is beneficial to improve the pre-concentration efficiency and recycle the heat energy of the steam condensed water generated by the rare earth chloride solution heater, thereby improving the steam utilization rate and reducing energy consumption.

[0048] In certain specific embodiments, the rare earth chloride solution storage tank, the rare earth chloride solution preheater and the rare earth chloride solution heater are connected in sequence by pipelines. An output pump is arranged between the rare earth chloride solution storage tank and the rare earth chloride solution preheater. No pump is arranged between the rare earth chloride solution preheater and the rare earth chloride solution heater. The rare earth chloride solution storage tank supplies the rare earth chloride solution to the rare earth chloride solution heater via the output pump, and during the transportation process, the rare earth chloride solution flows through the rare earth chloride solution preheater, thereby being preheated. This is conducive to reducing leak points, recycling steam condensate and improving heating efficiency.

[0049] In the present invention, the rare earth chloride solution preheater has a rare earth chloride solution feed port, a rare earth chloride solution discharge port, a heat source condensed water inlet and a heat source condensed water outlet.

[0050] The rare earth chloride solution feed port is located at one end of the rare earth chloride solution preheater, and is used to pass the rare earth chloride solution, and the rare earth chloride solution enters the intermediate cavity. The rare earth chloride solution discharge port is located at the other end of the rare earth chloride solution preheater, and is used to discharge the preheated rare earth chloride solution and discharge it to the rare earth chloride solution heater. The heat source condensate water inlet is located at one end of the rare earth chloride solution preheater, and is used to pass steam condensate water, and the steam condensate water enters the jacket cavity. The heat source condensate water outlet is located at the other end of the rare earth chloride solution preheater. The steam condensate water can be steam condensate water from the rare earth chloride solution heater. This is conducive to realizing countercurrent heat exchange of the rare earth chloride solution, and recycling steam condensate water to reduce costs.

[0051] The rare earth chloride solution and steam condensate are countercurrently exchanged in the rare earth chloride solution preheater, thereby preheating the rare earth chloride solution to obtain a preheated rare earth chloride solution. The steam condensate is cooled after heat exchange and discharged from the heat source condensate outlet to the steam condensate storage tank.

[0052] In the present invention, the rare earth chloride solution preheater is a horizontal graphite jacket heat exchanger, which is beneficial to improving the heat exchange efficiency and the chlorine corrosion resistance.

[0053] Rare earth chloride solution heater, rare earth chloride solution separator and steam supply unit

[0054] In the present invention, the rare earth chloride solution heater is used to receive the preheated rare earth chloride solution and further heat it to obtain a concentrated rare earth chloride solution.

[0055] Specifically, the bottom of the rare earth chloride solution heater is connected to the rare earth chloride solution preheater through a pipeline, and is used to receive the preheated rare earth chloride solution and further heat it to obtain a concentrated rare earth chloride solution.

[0056] In the present invention, the lower part of the rare earth chloride solution separator is connected to the top of the rare earth chloride solution heater through a pipeline, and the bottom of the rare earth chloride solution separator is connected to the bottom of the rare earth chloride solution heater through a pipeline, so that the concentrated rare earth chloride solution is continuously separated from the gas and liquid in the rare earth chloride solution separator, and the pre-concentrated rare earth chloride solution and the primary feed liquid steam are continuously obtained; no pump is provided between the rare earth chloride solution heater and the rare earth chloride solution separator. This is conducive to gas-liquid separation and reduces leakage points.

[0057] In the present invention, a circulation route is formed between the rare earth chloride solution separator and the rare earth chloride solution heater, which is used to realize continuous gas-liquid separation of the concentrated rare earth chloride solution in the rare earth chloride solution separator, and at the same time, the rare earth chloride solution that does not meet the pre-concentration requirements is re-transported to the rare earth chloride solution heater to realize continuous concentration. The temperature of the rare earth chloride solution in the rare earth chloride solution heater is high, and the temperature of the rare earth chloride solution in the rare earth chloride solution separator is low. The hot liquid goes up and the cold liquid goes down to form a circulation power, and there is no need to rely on a pump to provide power. Single-effect self-circulation concentration is realized.

[0058] In the present invention, the rare earth chloride solution heater has a feed port for the preheated rare earth chloride solution, a feed port for the circulating concentrated rare earth chloride solution heater, a discharge port for the concentrated rare earth chloride solution heater, a heater steam inlet, and a heater steam condensate outlet. The feed port for the preheated rare earth chloride solution and the feed port for the circulating concentrated rare earth chloride solution heater are both located at the bottom of the rare earth chloride solution heater, and the discharge port for the concentrated rare earth chloride solution heater is located at the top of the rare earth chloride solution heater. The heater steam inlet is located at the top of the rare earth chloride solution heater, and the heater steam condensate outlet is located at the bottom of the rare earth chloride solution heater.

[0059] According to one embodiment of the present invention, the feed port of the rare earth chloride solution heater after preheating is connected to the rare earth chloride solution discharge port of the rare earth chloride solution preheater through a heater feed pipeline, and is used to receive the preheated rare earth chloride solution. A flow meter and a pneumatic regulating valve are provided on the heater feed pipeline to adjust the feed amount so that the feed amount of the rare earth chloride solution heater is balanced with the discharge amount of the rare earth chloride solution separator to the jacketed reactor, that is, to maintain the inlet and outlet balance.

[0060] In the present invention, the rare earth chloride solution heater is connected to the steam supply unit. Specifically, the steam supply unit supplies hot steam to the rare earth chloride solution heater through the steam inlet of the heater. The hot steam and the preheated rare earth chloride solution are countercurrently exchanged to further heat the preheated rare earth chloride solution, thereby obtaining a concentrated rare earth chloride solution. At the same time, the hot steam is cooled to form steam condensate.

[0061] In the present invention, the steam condensate can be transported to the rare earth chloride solution preheater through the steam condensate outlet of the heater and the condensate inlet of the heat source in sequence, so as to preheat the rare earth chloride solution. This can save energy consumption and reduce costs.

[0062] According to one embodiment of the present invention, the steam inlet of the heater is connected to the steam supply unit through a heater steam inlet pipeline. A pneumatic regulating valve is arranged on the heater steam inlet pipeline to adjust the size of the steam inlet and control the heat exchange amount.

[0063] According to one embodiment of the present invention, the concentrated rare earth chloride solution heater outlet is connected to the rare earth chloride solution separator through a heater outlet pipeline. A thermal resistor can be set on the heater outlet pipeline to measure the feed temperature of the rare earth chloride solution heater.

[0064] In the present invention, the rare earth chloride solution heater is a round block hole impermeable graphite structure, which can improve the heat exchange efficiency and enhance the chlorine corrosion resistance.

[0065] In the present invention, the discharge port of the circulating concentrated rare earth chloride solution separator is connected to the feed port of the circulating concentrated rare earth chloride solution heater through a machine-made glass fiber reinforced plastic pipe. The machine-made glass fiber reinforced plastic pipe can withstand high temperatures above 150°C and negative pressure. In this way, the rare earth chloride solution that does not meet the pre-concentration requirements can be re-transported to the rare earth chloride solution heater for further pre-concentration until the concentration requirements are met.

[0066] In the present invention, the rare earth chloride solution separator has a feed inlet of the rare earth chloride solution separator for cyclic concentration, a discharge port of the rare earth chloride solution separator for cyclic concentration, a discharge port of the rare earth chloride solution separator after final concentration, and a primary liquid steam outlet. The feed inlet of the rare earth chloride solution separator for cyclic concentration is located at the lower part of the rare earth chloride solution separator, the discharge port of the rare earth chloride solution separator for cyclic concentration is located at the bottom of the rare earth chloride solution separator, the discharge port of the rare earth chloride solution separator after final concentration is located at the bottom of the rare earth chloride solution separator, and the primary liquid steam outlet is located at the top of the rare earth chloride solution separator.

[0067] Specifically, the feed port of the circulating concentrated rare earth chloride solution separator is connected to the discharge port of the concentrated rare earth chloride solution heater through a pipeline, and is used to receive the concentrated rare earth chloride solution from the rare earth chloride solution heater. The discharge port of the circulating concentrated rare earth chloride solution separator is connected to the feed port of the circulating concentrated rare earth chloride solution heater through a pipeline. This is conducive to achieving continuous pre-concentration.

[0068] The pre-concentrated rare earth chloride solution is discharged to the jacketed reactor through the discharge port of the rare earth chloride solution separator after final concentration. Specifically, the discharge port of the rare earth chloride solution after final concentration is connected to the jacketed reactor through the separator discharge pipeline. A thermal resistor is arranged on the separator discharge pipeline to measure the temperature of the feed liquid discharged from the rare earth chloride solution separator.

[0069] A thermal resistor, an insertion differential pressure level gauge, an insertion specific gravity meter, and a pressure transmitter can be installed in the rare earth chloride solution separator. The thermal resistor is used to measure the liquid temperature. The insertion differential pressure level gauge is used to measure the liquid level inside it. The insertion specific gravity meter is used to measure the ratio of the feed liquid to the standard water density. The pressure transmitter is used to control the pressure inside it. This is conducive to achieving interlocking control and better controlling the balance of feed liquid concentration.

[0070] In the present invention, the rare earth chloride solution separator is a steel cylinder lined with graphite structure, which is beneficial to improve the impact resistance and chlorine corrosion resistance.

[0071] The outlet of the steam supply unit is provided with a temperature gauge and a pressure transmitter. The temperature gauge is used to control the temperature. The pressure transmitter is used to control the pressure.

[0072] Liquid steam condenser, cooling water supply unit, cooling water recovery unit and horizontal closed-circuit vacuum equipment

[0073] The top of the feed liquid steam condenser is connected to the top of the rare earth chloride solution separator through a pipeline, and is used to receive the primary feed liquid steam and cool it to form acidic condensed water, which is recorded as the primary feed liquid condensed water. The feed liquid steam condenser is set as a round block hole impermeable graphite structure.

[0074] The cooling water supply unit is connected to the bottom of the feed liquid steam condenser through a pipeline, and is used to supply cooling water to the feed liquid steam condenser, thereby cooling the primary feed liquid steam. In this way, the primary feed liquid steam generated by the rare earth chloride solution separator can be cooled.

[0075] In the present invention, the feed liquid steam condenser has a feed liquid steam inlet, a feed liquid condensed water and non-condensable gas outlet, a cooling water inlet, and a cooling water outlet. The feed liquid steam inlet is located at the top of the feed liquid steam condenser, the feed liquid condensed water and non-condensable gas outlet are located at the bottom of the feed liquid steam condenser, the cooling water inlet is located at the bottom of the feed liquid steam condenser, and the cooling water outlet is located at the top of the feed liquid steam condenser.

[0076] According to one embodiment of the present invention, the feed liquid steam inlet of the feed liquid steam condenser is connected to the primary feed liquid steam outlet of the rare earth chloride solution separator through a pipeline. The cooling water inlet of the feed liquid steam condenser is connected to the cooling water supply unit through a pipeline. The cooling water outlet is connected to the cooling water recovery unit through a pipeline. The feed liquid condensed water and non-condensable gas outlet are connected to the feed liquid condensed water storage tank through a pipeline.

[0077] In the liquid steam condenser, the cooling water is converted into hot water after heat exchange. The hot water can be transported to the cooling water recovery unit through the cooling water outlet, and then used as cooling water after centralized cooling in the cooling tower. The inlet of the cooling water recovery unit is provided with a thermometer for controlling the temperature; a pressure transmitter is provided for controlling the pressure. The outlet of the cooling water supply unit is provided with a thermometer for controlling the temperature; a pressure transmitter is provided for controlling the pressure.

[0078] The primary liquid condensate and non-condensable gas produced in the liquid steam condenser and the secondary liquid steam produced in the jacketed reactor first enter the liquid condensate storage tank. The gas phase outlet at the top of the liquid condensate storage tank is connected to the horizontal closed-circuit vacuum equipment through a pipeline. The non-condensable gas and the secondary liquid steam are condensed in the horizontal closed-circuit vacuum equipment to form acidic wastewater. Only a small amount of non-condensable gas is discharged into the atmosphere.

[0079] The liquid steam condenser is a round hole impermeable graphite structure, which can improve the heat exchange efficiency and has good chlorine corrosion resistance.

[0080] As the horizontal closed-circuit vacuum equipment, known ones can be used.

[0081] Jacketed Reactor

[0082] The top of the jacketed reactor is connected to the bottom of the rare earth chloride solution separator through a pipeline, which is used to further concentrate the pre-concentrated rare earth chloride solution to obtain a rare earth chloride solution concentrated to a target concentration. The jacketed reactor is a graphite reactor. The jacketed reactor is formed of graphite as a whole. This is conducive to improving heat exchange efficiency, is not easy to be blocked during discharge, and improves chlorine corrosion resistance.

[0083] In the present invention, the jacketed reactor has a reactor feed port, a reactor discharge port, a reactor heat source inlet, a secondary feed liquid steam outlet, and a reactor heat source condensed water outlet. The reactor feed port is located at the top of the jacketed reactor, the reactor discharge port is located at the bottom of the jacketed reactor, the reactor heat source inlet is located at the top of the jacketed reactor, the secondary feed liquid steam outlet is located at the top of the jacketed reactor, and the reactor heat source condensed water outlet is located at the bottom of the jacketed reactor.

[0084] In the present invention, there may be more than one jacketed reactor, for example, more than two, so as to improve production efficiency.

[0085] According to one embodiment of the present invention, the feed port of the reactor is connected to the discharge port of the rare earth chloride solution after the final concentration of the rare earth chloride solution separator through a pipeline, which is used to receive the pre-concentrated rare earth chloride solution and further concentrate it to obtain the rare earth chloride solution concentrated to the target concentration and the secondary feed liquid steam. The concentration in the jacketed reactor is vacuum concentration.

[0086] The discharge port of the reactor is used to discharge the rare earth chloride solution concentrated to the target concentration and supply it to the flake machine. The secondary feed liquid steam outlet is connected to the feed liquid condensate water storage tank through a pipeline. The secondary feed liquid steam is discharged to the feed liquid condensate water storage tank through the secondary feed liquid steam outlet.

[0087] The jacketed reactor is also connected to the steam supply unit through a pipeline. Specifically, the steam supply unit supplies hot steam (i.e., heat source) to the jacketed reactor through the reactor heat source inlet, and the hot steam forms condensed water after heat exchange with the pre-concentrated rare earth chloride solution. The condensed water is discharged to the steam condensed water storage tank through the reactor heat source condensed water outlet.

[0088] Flow meters and pneumatic control valves can be installed on the discharge pipes of the separators near the jacketed reactor to adjust the feed amount and control the liquid level of the jacketed reactor. Thermal resistors and pressure transmitters can be installed in the jacketed reactor. Thermal resistors are used to measure the gas-liquid phase temperature. Pressure transmitters are used to control the pressure in the jacketed reactor.

[0089] Liquid condensate storage tank and steam condensate storage tank

[0090] The feed liquid condensate storage tank is connected to the bottom of the feed liquid steam condenser through a pipeline, and is used to receive the primary feed liquid condensate and non-condensable gas generated in the feed liquid steam condenser. Specifically, the feed liquid condensate storage tank is connected to the feed liquid condensate and non-condensable gas outlet of the feed liquid steam condenser through a pipeline. The secondary feed liquid condensate generated by the jacketed reactor is also discharged to the feed liquid condensate storage tank.

[0091] The steam condensate storage tank is connected to the bottom of the rare earth chloride solution preheater and the bottom of the jacketed reactor through pipelines. Specifically, the steam condensate storage tank is connected to the heat source condensate outlet of the rare earth chloride solution preheater and the reactor heat source condensate outlet of the jacketed reactor through pipelines to receive condensate. The condensate can be recycled.

[0092] Flaking Machine

[0093] The flake forming machine is configured to cool, crystallize and flake the rare earth chloride solution concentrated to the target concentration to obtain a flake rare earth chloride solid. In the present invention, the rare earth chloride solution concentrated to the target concentration is introduced into the flake forming machine from the jacketed reactor through a guide pipe. One end of the guide pipe is connected to the reactor discharge port of the jacketed reactor, and the other end is a free end.

[0094] In the present invention, the flaker includes a distributor. The flaker may be any known one in the art.

[0095] <Method for continuous production of rare earth chloride solid>

[0096] The present invention also provides a method for continuously producing rare earth chloride solids using the continuous production device as described above, comprising the following steps:

[0097] 1) supplying a rare earth chloride solution to the rare earth chloride solution preheater, wherein the rare earth chloride solution preheater preheats the rare earth chloride solution to a temperature greater than or equal to 75° C. to obtain a preheated rare earth chloride solution; wherein the rare earth chloride solution has a REO content greater than or equal to 30 wt % and a pH value of 1.5 to 2;

[0098] 2) conveying the preheated rare earth chloride solution to the rare earth chloride solution heater for further heating to obtain a concentrated rare earth chloride solution; wherein the temperature of the concentrated rare earth chloride solution is 130-140° C.;

[0099] 3) introducing the concentrated rare earth chloride solution into the rare earth chloride solution separator to perform gas-liquid separation, thereby obtaining a pre-concentrated rare earth chloride solution; wherein the REO content of the pre-concentrated rare earth chloride solution is greater than 50 wt %;

[0100] 4) discharging the pre-concentrated rare earth chloride solution into the jacketed reactor for further concentration to obtain a rare earth chloride solution concentrated to a target concentration; wherein the rare earth chloride solution concentrated to the target concentration has a REO content of more than 65 wt %;

[0101] 5) The rare earth chloride solution concentrated to the target concentration is introduced into the flake machine for cooling, crystallization and flake making to obtain rare earth chloride solid.

[0102] In step 1) of the present invention, the rare earth chloride solution in the rare earth chloride solution storage tank is supplied to the rare earth chloride solution preheater through an output pump. The heat source of the rare earth chloride solution preheater can be steam condensed water generated by the rare earth chloride solution heater, and the rare earth chloride solution is preheated by the steam condensed water. For example, the rare earth chloride solution can be preheated to about 80°C. The REO content of the rare earth chloride solution is preferably greater than or equal to 30wt%, more preferably 32-35wt%.

[0103] In step 2) of the present invention, the heat source of the rare earth chloride solution heater can come from a steam supply unit. While obtaining the concentrated rare earth chloride solution, the hot steam (heat source) is cooled to steam condensate. The steam condensate can be used for heat exchange in the rare earth chloride solution preheater.

[0104] In step 3) of the present invention, the rare earth chloride solution separator performs gas-liquid separation to obtain a pre-concentrated rare earth chloride solution and primary liquid vapor. The pre-concentrated rare earth chloride solution is discharged to a jacketed reactor for further concentration.

[0105] The primary liquid steam is discharged to the liquid steam condenser and cooled into primary liquid condensate and non-condensable gas. The pressure in the separation chamber of the rare earth chloride solution separator is set to -60 to -90 kPa.

[0106] The REO content of the pre-concentrated rare earth chloride solution is preferably 50 to 55 wt%.

[0107] In step 4) of the present invention, the heat source of the jacketed reactor comes from the steam supply unit. While obtaining the rare earth chloride solution concentrated to the target concentration, secondary feed liquid steam is obtained. The secondary feed liquid steam is discharged to the feed liquid condensate storage tank.

[0108] The REO content of the rare earth chloride solution concentrated to the target concentration is preferably 65 to 70 wt %, more preferably 65 to 68 wt %.

[0109] In step 5), a flake machine (i.e., crystallization and flake-making equipment) is used to cool the rare earth chloride solution concentrated to the target concentration, crystallize it, and flake it to obtain flaky rare earth chloride solids.

[0110] The flaky rare earth chloride solid may be in an irregular flake shape with a thickness of 3 to 5 mm, a length of 10 to 20 mm, and a width of 10 to 20 mm.

[0111] In the present invention, the concentration of the feed solution refers to the REO content.

[0112] The present invention can realize the continuous production of rare earth chloride solid with high production efficiency. The tonnage of flaky rare earth chloride solid produced in 24 hours is more than 10t (calculated based on REO content).

[0113] Here is the test method:

[0114] REO content: determined by atomic absorption spectrometry.

[0115] Example 1

[0116] Figure 1 It is a schematic structural diagram of the continuous production device of rare earth chloride solid of the present invention.

[0117] like Figure 1 As shown, the continuous production device of rare earth chloride solid of the present invention includes a rare earth chloride solution storage tank 1, a rare earth chloride solution preheater 2, a rare earth chloride solution heater 3, a rare earth chloride solution separator 4, a jacketed reactor 5, a flake machine 6, a feed liquid steam condenser 7, a feed liquid condensate water storage tank 8, a steam condensate water storage tank 9, a cooling water supply unit CW, a steam supply unit VW, a cooling water recovery unit HW, and a horizontal closed-circuit vacuum equipment Va.

[0118] The rare earth chloride solution storage tank 1 is used to store the rare earth chloride solution and stably supply the rare earth chloride solution to the rare earth chloride solution preheater 2. Specifically, the rare earth chloride solution storage tank 1 can supply the rare earth chloride solution to the rare earth chloride solution preheater 2 through an output pump.

[0119] In this embodiment, the rare earth chloride solution storage tank 1 supplies the rare earth chloride solution to the rare earth chloride solution heater 3 through an output pump. During the supply process, the rare earth chloride solution flows through the rare earth chloride solution preheater 2 and exchanges heat with steam condensate to achieve preheating of the rare earth chloride solution. The rare earth chloride solution preheater 2 is a graphite jacketed heat exchanger with a large diameter and negligible pressure loss.

[0120] The rare earth chloride solution preheater 2 has a rare earth chloride solution feed port, a rare earth chloride solution discharge port, a heat source condensed water inlet and a heat source condensed water outlet. The rare earth chloride solution feed port is located at one end of the rare earth chloride solution preheater 2, and is used to receive the rare earth chloride solution from the rare earth chloride solution storage tank 1. The rare earth chloride solution discharge port is located at the other end of the rare earth chloride solution preheater 2, and is used to discharge the preheated rare earth chloride solution to the rare earth chloride solution heater 3. The heat source condensed water inlet is located at one end of the rare earth chloride solution preheater 2, and is used to provide a preheating heat source to the rare earth chloride solution preheater 2. The heat source condensed water outlet is located at the other end of the rare earth chloride solution preheater 2, and is used to discharge the heat source after cooling.

[0121] The rare earth chloride solution preheater 2 preheats the rare earth chloride solution through countercurrent heat exchange to obtain a preheated rare earth chloride solution. The steam condensate is discharged from the heat source condensate outlet after heat exchange and is discharged to the steam condensate storage tank 9 through a pipeline. The preheated rare earth chloride solution flows from the rare earth chloride solution outlet to the rare earth chloride solution heater 3.

[0122] The rare earth chloride solution heater 3 has a feed port for the preheated rare earth chloride solution, a feed port for the circulating concentrated rare earth chloride solution heater, a discharge port for the concentrated rare earth chloride solution heater, a heater steam inlet, and a heater steam condensate outlet. The feed port for the preheated rare earth chloride solution is located at the bottom of the rare earth chloride solution heater 3, and is used to receive the preheated rare earth chloride solution from the rare earth chloride solution preheater 2. The feed port for the circulating concentrated rare earth chloride solution is located at the bottom of the rare earth chloride solution heater 3, and is used to receive the rare earth chloride solution that does not meet the concentration requirements from the rare earth chloride solution separator 4. The concentrated rare earth chloride solution discharge port is located at the top of the rare earth chloride solution heater 3, and is used to discharge the concentrated rare earth chloride solution to the rare earth chloride solution separator 4. The heater steam inlet is located at the top of the rare earth chloride solution heater 3, and is used to pass heating steam. The heater steam condensate outlet is located at the bottom of the rare earth chloride solution heater 3, and is used to discharge the steam condensate obtained after heat exchange. In this embodiment, the steam condensed water of the rare earth chloride solution heater 3 can be transported to the rare earth chloride solution preheater 2, so as to preheat the rare earth chloride solution. Continuous production can save energy consumption and reduce costs.

[0123] Specifically, the feed port of the preheated rare earth chloride solution of the rare earth chloride solution heater 3 is connected to the rare earth chloride solution discharge port of the rare earth chloride solution preheater 2 through the heater feed pipeline. The concentrated rare earth chloride solution discharge port of the rare earth chloride solution heater 3 is connected to the lower part of the rare earth chloride solution separator 4 through the heater discharge pipeline. The steam inlet of the rare earth chloride solution heater 3 is connected to the steam supply unit VW through the heater steam inlet pipeline.

[0124] A flow meter and a pneumatic regulating valve are provided on the heater feed pipeline to adjust the feed amount so that the feed amount of the rare earth chloride solution heater 3 is balanced with the discharge amount of the rare earth chloride solution separator 4 to the jacketed reactor 5, that is, the inlet and outlet balance is maintained. A pneumatic regulating valve is provided on the heater steam inlet pipeline to adjust the size of the steam inlet and control the heat exchange amount.

[0125] In this embodiment, the rare earth chloride solution heater 3 is a round hole-type impermeable graphite structure, and the rare earth chloride solution preheater 2 is a horizontal graphite jacket structure.

[0126] The rare earth chloride solution separator 4 has a feed inlet for a cyclically concentrated rare earth chloride solution separator, a discharge port for a cyclically concentrated rare earth chloride solution separator, a discharge port for a finally concentrated rare earth chloride solution separator and a primary feed liquid steam outlet.

[0127] The feed port of the circulating concentrated rare earth chloride solution separator is located at the lower part of the rare earth chloride solution separator 4, and is used to receive the circulating concentrated rare earth chloride solution discharged from the rare earth chloride solution heater 3. The discharge port of the circulating concentrated rare earth chloride solution separator is located at the bottom of the rare earth chloride solution separator 4, and is used to transfer the rare earth chloride solution that does not meet the concentration requirement to the rare earth chloride solution heater 3. The discharge port of the final concentrated rare earth chloride solution separator is located at the bottom of the rare earth chloride solution separator 4, and is used to discharge the final concentrated rare earth chloride solution that meets the concentration requirement to the jacketed reactor 5. The primary feed liquid steam outlet is located at the top of the rare earth chloride solution separator 4, and is used to discharge the generated feed liquid steam to the feed liquid steam condenser 7.

[0128] Specifically, the circulating concentrated rare earth chloride solution feed port of the rare earth chloride solution separator 4 is connected to the circulating concentrated rare earth chloride solution heater discharge port of the rare earth chloride solution heater 3 through a pipeline. The rare earth chloride solution separator 4 receives the rare earth chloride solution after heating and circulation, and performs gas-liquid separation to obtain a pre-concentrated rare earth chloride solution (i.e., the rare earth chloride solution after final concentration) and primary liquid steam. The rare earth chloride solution separator 4 is a steel cylinder lined with graphite structure. The device of this embodiment can realize self-circulation, and a pump can be omitted between the rare earth chloride solution separator 4 and the rare earth chloride solution heater 3 to reduce leakage points.

[0129] The pre-concentrated rare earth chloride solution is discharged to the jacketed reactor 5 through the discharge port of the finally concentrated rare earth chloride solution. Specifically, the discharge port of the finally concentrated rare earth chloride solution is connected to the jacketed reactor 5 through the separator discharge pipeline.

[0130] In this embodiment, the bottom of the rare earth chloride solution separator 4 is also connected to the bottom of the rare earth chloride solution heater 3 through a pipeline. Specifically, the circulating concentrated rare earth chloride solution outlet of the rare earth chloride solution separator 4 is connected to the circulating concentrated rare earth chloride solution feed port of the rare earth chloride solution heater 3 through a pipeline, so that the rare earth chloride solution that does not meet the pre-concentration requirement is re-transported to the rare earth chloride solution heater 3, and circulated and heated to concentrate until the concentration requirement is reached.

[0131] The rare earth chloride solution separator 4 is provided with two temperature measuring ports for measuring the temperature of the liquid phase and the gas phase. The rare earth chloride solution separator 4 is provided with two liquid level gauge ports for measuring the liquid level of the liquid phase, and the constant feeding and discharging are ensured by controlling the liquid level height. The rare earth chloride solution separator 4 is provided with a pressure measuring port for measuring the pressure inside the rare earth chloride solution separator 4. The rare earth chloride solution separator 4 is provided with two specific gravity gauge ports for measuring the ratio of the feed liquid to the standard water density.

[0132] The jacketed reactor 5 has a reactor feed port, a reactor discharge port, a reactor heat source inlet, a secondary feed liquid steam outlet, and a reactor heat source condensed water outlet. The reactor feed port is located at the top of the jacketed reactor 5, and is used to receive the rare earth chloride solution that meets the pre-concentration requirements from the rare earth chloride solution separator 4. The reactor discharge port is located at the bottom of the jacketed reactor 5, and is used to discharge the rare earth chloride solution concentrated to the target concentration to the flaker 6. The reactor heat source inlet is located at the top of the jacketed reactor 5, and is used to pass heating steam. The secondary feed liquid steam outlet is located at the top of the jacketed reactor 5, and is used to discharge the generated secondary feed liquid steam to the feed liquid condensed water storage tank 8. The reactor heat source condensed water outlet is located at the bottom of the jacketed reactor 5, and is used to discharge the heat source condensed water after heat exchange to the steam condensed water storage tank 9.

[0133] Specifically, the reactor feed port of the jacketed reactor 5 is connected to the discharge port of the rare earth chloride solution after the rare earth chloride solution separator 4 is finally concentrated through a pipeline, and is used to receive the pre-concentrated rare earth chloride solution, and further concentrate to obtain the rare earth chloride solution concentrated to the target concentration and the secondary feed liquid steam. The jacketed reactor 5 is a graphite jacketed reactor. In this embodiment, there can be two jacketed reactors 5, which are arranged in parallel. The steam supply unit VW supplies hot steam (i.e., heat source) to the jacketed reactor 5 through the reactor heat source inlet, and the hot steam forms condensed water after heat exchange with the pre-concentrated rare earth chloride solution. The condensed water is discharged to the steam condensed water storage tank 9 through the reactor condensed water outlet.

[0134] The rare earth chloride solution finally concentrated in the rare earth chloride solution separator 4 flows into the jacketed reactor 5 due to the different height differences of the equipment. A thermal resistor is arranged in the jacketed reactor 5 to measure the temperature of the gas and liquid phases. A pressure transmitter is arranged in the jacketed reactor 5 to control the pressure in the jacketed reactor 5.

[0135] The liquid steam condenser 7 has a liquid steam inlet, a liquid condensate and non-condensable gas outlet, a cooling water inlet, and a cooling water outlet. The liquid steam inlet is located at the top of the liquid steam condenser 7, and is used to receive the primary liquid steam from the rare earth chloride solution separator 4. The liquid condensate and non-condensable gas outlets are located at the bottom of the liquid steam condenser 7, and are used to discharge the primary liquid condensate and non-condensable gas to the liquid condensate water storage tank 8. The cooling water inlet is located at the bottom of the liquid steam condenser 7, and is used to pass cooling water. The cooling water outlet is located at the top of the liquid steam condenser 7, and is used to discharge the cooling water after heat exchange to the cooling water recovery unit HW. The liquid steam condenser 7 is a round block hole impermeable graphite structure.

[0136] The feed liquid steam condenser 7 is connected to the rare earth chloride solution separator 4, the feed liquid condensed water storage tank 8 and the cooling water supply unit CW respectively. Specifically, the feed liquid steam inlet of the feed liquid steam condenser 7 is connected to the primary feed liquid steam outlet of the rare earth chloride solution separator 4 through a pipeline to receive the primary feed liquid steam. The cooling water inlet of the feed liquid steam condenser 7 is connected to the cooling water supply unit CW. The cooling water outlet is connected to the cooling water recovery unit HW.

[0137] The feed liquid steam condenser 7 can cool the primary feed liquid steam by the cooling water supplied by the cooling water supply unit CW to form primary feed liquid condensed water and non-condensable gas.

[0138] In the liquid vapor condenser 7, the cooling water is converted into 90°C hot water after heat exchange. The hot water can be transported to the cooling water recovery unit HW through the cooling water outlet, and then recycled as cooling water after centralized cooling in the cooling tower.

[0139] The primary liquid condensate and non-condensable gas generated in the liquid steam condenser 7 and the secondary liquid steam generated in the jacketed reactor 5 enter the liquid condensate storage tank 8. The gas phase outlet at the top of the liquid condensate storage tank 8 is connected to the horizontal closed-circuit vacuum equipment Va through a pipeline. The non-condensable gas and the secondary liquid steam are condensed in the horizontal closed-circuit vacuum equipment Va to form acidic wastewater. Only a small amount of non-condensable gas is discharged into the atmosphere.

[0140] The steam condensate storage tank 9 is respectively connected to the heat source condensate outlet of the rare earth chloride solution preheater 2 and the reactor heat source condensate outlet of the jacketed reactor 5 through pipelines for receiving condensate.

[0141] The flake forming machine 6 cools and crystallizes the rare earth chloride solution concentrated to the target concentration to obtain rare earth chloride solid.

[0142] The outlet of the steam supply unit VW is provided with a temperature gauge for controlling the temperature; a pressure transmitter is provided for controlling the pressure. The outlet of the cooling water supply unit CW is provided with a temperature gauge for controlling the temperature; a pressure transmitter is provided for controlling the pressure. The inlet of the cooling water recovery unit HW is provided with a temperature gauge for controlling the temperature; a pressure transmitter is provided for controlling the pressure.

[0143] The interlocking control between the instruments in this embodiment realizes the automatic continuous feeding and discharging production of the device. Each instrument can be those known in the art.

[0144] Example 2

[0145] This embodiment provides a method for continuously producing rare earth chloride solids using the continuous production device described in Embodiment 1, comprising the following steps:

[0146] The cerium chloride solution in the rare earth chloride solution storage tank 1 is supplied to the rare earth chloride solution preheater 2 (flowing in from the rare earth chloride solution feed port) through an output pump, and the cerium chloride solution is preheated to about 80° C. by heat exchange with steam condensate to obtain a preheated cerium chloride solution; wherein the REO content in the cerium chloride solution is 32wt%, and the pH value of the cerium chloride solution is 1.5-2.

[0147] The preheated cerium chloride solution is transported to the rare earth chloride solution heater 3 (through the preheated rare earth chloride solution feed port), and countercurrent heat exchange is performed with the hot steam supplied by the steam supply unit VW to obtain a concentrated cerium chloride solution. At the same time, the hot steam is cooled to form steam condensate. The temperature of the concentrated cerium chloride solution is 130-140°C; the temperature of the steam condensate is about 90°C. The steam condensate is supplied to the rare earth chloride solution preheater 2.

[0148] The concentrated cerium chloride solution enters the rare earth chloride solution separator 4 (through the feed port of the circulating concentrated rare earth chloride solution separator), and is separated into gas and liquid, thereby obtaining a pre-concentrated cerium chloride solution and a primary liquid steam. Among them, the REO content in the pre-concentrated cerium chloride solution is 50-55wt%. The pressure in the separation chamber of the rare earth chloride solution separator 4 is -60--90kPa. The primary liquid steam is discharged from the primary liquid steam outlet to the liquid steam condenser 7, and is cooled into primary liquid condensate and non-condensable gas in the liquid steam condenser 7. The primary liquid condensate and non-condensable gas are discharged to the liquid condensate storage tank 8 through the liquid condensate and non-condensable gas outlets.

[0149] The pre-concentrated cerium chloride solution flows into the jacketed reactor 5 for further concentration to obtain a cerium chloride solution concentrated to the target concentration and secondary feed liquid steam. Among them, the jacketed reactor 5 is negatively pressurized by the horizontal closed-circuit vacuum equipment Va. The REO content in the cerium chloride solution concentrated to the target concentration is 67-68wt%. The secondary feed liquid steam is discharged to the feed liquid condensate storage tank 8, and then passes through the horizontal closed-circuit vacuum equipment Va to form acidic wastewater.

[0150] The cerium chloride solution concentrated to the target concentration is introduced into the flake machine 6 for cooling, crystallization, and flake formation to obtain flake cerium chloride solid. The process parameters and product performance data are shown in Table 1 and Table 2, respectively.

[0151] Table 1

[0152]

[0153] Table 2

[0154]

[0155] It can be seen from this that the present invention can continuously produce flaky rare earth chloride solids with high production efficiency, and the REO content in the obtained product is relatively high.

[0156] The present invention is not limited to the above-mentioned embodiments. Without departing from the essential content of the present invention, any deformation, improvement and substitution that can be conceived by those skilled in the art shall fall within the scope of the present invention.

Claims

1. A continuous production device for rare earth chloride solids, characterized in that: It includes a rare earth chloride solution heater, a rare earth chloride solution separator, a jacketed reactor and a flake machine; The rare earth chloride solution heater is used to receive the preheated rare earth chloride solution and further heat it to obtain a concentrated rare earth chloride solution; The lower part of the rare earth chloride solution separator is connected to the top of the rare earth chloride solution heater through a pipeline, and the bottom of the rare earth chloride solution separator is connected to the bottom of the rare earth chloride solution heater through a pipeline, so that the concentrated rare earth chloride solution is continuously separated into gas and liquid in the rare earth chloride solution separator, and the pre-concentrated rare earth chloride solution and the primary feed liquid steam are continuously obtained; no pump is arranged between the rare earth chloride solution heater and the rare earth chloride solution separator; The rare earth chloride solution separator is configured as a steel cylinder lined with graphite structure; the rare earth chloride solution heater is configured as a round block hole impermeable graphite structure; The top of the jacketed reactor is connected to the bottom of the rare earth chloride solution separator through a pipeline, and is used to further concentrate the pre-concentrated rare earth chloride solution to obtain a rare earth chloride solution concentrated to a target concentration; the jacketed reactor is configured as a graphite reactor; The flake forming machine is configured to cool, crystallize and flake the rare earth chloride solution concentrated to a target concentration to obtain a rare earth chloride solid.

2. The continuous production device according to claim 1, characterized in that: It also includes a rare earth chloride solution preheater and a liquid steam condenser; The rare earth chloride solution preheater is used to preheat the rare earth chloride solution, and one end of the rare earth chloride solution preheater is connected to the bottom of the rare earth chloride solution heater; the rare earth chloride solution preheater is a horizontal graphite jacket heat exchanger; The top of the feed liquid steam condenser is connected to the top of the rare earth chloride solution separator through a pipeline, and is used to receive the primary feed liquid steam and cool it; the feed liquid steam condenser is configured as a round block hole impermeable graphite structure; The rare earth chloride solution heater is also configured to generate steam condensed water by heat exchange, and transport the steam condensed water to the rare earth chloride solution preheater, thereby preheating the rare earth chloride solution.

3. The continuous production device according to claim 2, characterized in that: Also includes a steam supply unit and a cooling water supply unit; The steam supply unit is connected to the top of the rare earth chloride solution heater and the top of the jacketed reactor through pipelines, respectively, for supplying hot steam to them; The cooling water supply unit is connected to the bottom of the feed liquid steam condenser through a pipeline, and is used to supply cooling water to the feed liquid steam condenser, thereby cooling the primary feed liquid steam.

4. The continuous production device according to claim 2, characterized in that: It also includes liquid condensate storage tanks and horizontal closed-circuit vacuum equipment; The top of the feed liquid condensate storage tank is respectively connected to the bottom of the feed liquid steam condenser and the top of the jacketed reactor through pipelines; The feed liquid condensate storage tank is connected to the horizontal closed-circuit vacuum equipment through a pipeline, so that vacuum is formed in both the rare earth chloride solution separator and the jacketed reactor.

5. The continuous production device according to claim 2, characterized in that: It also includes a steam condensate storage tank, which is connected to one end of the rare earth chloride solution preheater and the bottom of the jacketed reactor through pipelines.

6. The continuous production device according to claim 2, characterized in that: It also includes a rare earth chloride solution storage tank, which is connected to the rare earth chloride solution preheater through a pipeline and is used to provide rare earth chloride solution to the rare earth chloride solution preheater.

7. The continuous production device according to claim 2, characterized in that: The rare earth chloride solution separator is provided with an insertion type differential pressure level gauge, an insertion type specific gravity meter and a pressure transmitter; the jacketed reactor is provided with a pressure transmitter.

8. A method for continuously producing rare earth chloride solids using the continuous production device according to any one of claims 2 to 7, characterized in that: The steps include: 1) supplying a rare earth chloride solution to the rare earth chloride solution preheater, wherein the rare earth chloride solution preheater preheats the rare earth chloride solution to a temperature greater than or equal to 75° C. to obtain a preheated rare earth chloride solution; wherein the rare earth chloride solution has a REO content greater than or equal to 30 wt % and a pH value of 1.5 to 2; 2) conveying the preheated rare earth chloride solution to the rare earth chloride solution heater for further heating to obtain a concentrated rare earth chloride solution; wherein the temperature of the concentrated rare earth chloride solution is 130-140° C.; 3) introducing the concentrated rare earth chloride solution into the rare earth chloride solution separator to perform gas-liquid separation, thereby obtaining a pre-concentrated rare earth chloride solution; wherein the REO content of the pre-concentrated rare earth chloride solution is greater than 50 wt %; 4) discharging the pre-concentrated rare earth chloride solution into the jacketed reactor for further concentration to obtain a rare earth chloride solution concentrated to a target concentration; wherein the rare earth chloride solution concentrated to the target concentration has a REO content of more than 65 wt %; 5) introducing the rare earth chloride solution concentrated to the target concentration into the flake machine for cooling, crystallization and flake making to obtain rare earth chloride solid.

9. The method according to claim 8, characterized in that The pressure in the rare earth chloride solution separator is set to -60 to -90 kPa.

10. The method according to claim 8, characterized in that The REO content in the concentrated rare earth chloride solution is 50-55wt%; the REO content in the rare earth chloride solution concentrated to the target concentration is 65-70wt%.

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