Continuous recovery and reuse apparatus and method for organic alkalis

Abstract

To provide a device and a method for continuously recycling organic alkali.SOLUTION: According to the invention, inline mixing, rapid neutralization, inline separation and continuous dewatering and drying are adopted, and a feeding pump, a micro-mixer, a micro-channel reactor, a liquid-liquid separator and a continuous stirring kettle are connected in sequence, so that inline recycling and reuse of an organic alkali in an alkali-containing waste liquid are achieved.EFFECT: By means of this full-continuous inline alkali recovery device, an organic alkali with reliable recovery quality can be obtained at a high recovery rate and can be directly reused without batch additional treatment, and the device has a high degree of integration, occupies a small floor area and has good operation stability, and such defects are avoided that a large floor area is occupied and recovery efficiency is low because a plurality of standing tanks and storage tanks need to be used in a kettle-type process.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] The present invention belongs to the technical field of fine chemicals, and specifically relates to an apparatus and method for continuously recovering and reusing organic alkalis.

Background Art

[0002] Organic alkalis are often used as catalysts or acid binders in condensation reactions and substitution reactions, and are reagents widely used in synthetic reactions. After the reaction, complex salts with hydrochloric acid, sulfuric acid, and phosphoric acid are often formed, and they dissolve in water during post-extraction processing, generating a large amount of waste liquid containing organic alkalis. These waste liquids containing organic alkalis are not only difficult to treat but also have high treatment costs and consume a large amount of organic alkalis. Therefore, extracting, recovering, and reusing organic alkalis from waste liquids containing organic alkalis is a necessary measure to reduce the discharge of chemical waste and lower production costs.

[0003] Prior documents such as CN218951289U, CN103304423B, CN103304423A, and CN208104264U provide recovery processes and equipment for recovering triethylamine. However, due to the need for numerous storage tanks and settling tanks, the occupied floor area is large, the recovery efficiency is low, or a constant-boiling distillation column needs to be used to achieve continuous recovery of triethylamine. This results in high energy consumption and high recovery costs. Therefore, there is an urgent need to develop an innovative system specialized for efficient recovery and reuse of organic alkalis in liquid separation. Such a system can optimize the recovery rate, simplify the operation process, ensure the purity of the recovered alkali, enable direct reuse, and reduce potential safety risks, thus realizing a situation beneficial to both environmental protection and economic benefits.

Summary of the Invention

[0004] In view of the problems existing in the prior art, the object of the present invention is to provide an apparatus and method for continuously recovering and reusing organic alkalis with high recovery efficiency and low operating costs.

[0005] The continuous recovery and reuse apparatus and method for organic alkalis provided in the present invention, by sequentially connecting a matched feed pump, micromixer, microchannel reactor, liquid-liquid separator, and continuous kettle according to the characteristics of the reaction process, achieves a high alkali recovery rate (over 99%), high alkali recovery purity, direct reuse, elimination of the need for patch-type additional processing, high level of integration, small occupied floor space, and high operational stability. It avoids the shortcomings of the kettle-type process, such as the large occupied floor space and low recovery efficiency that are required when using multiple stationary tanks and storage tanks.

[0006] The present invention provides a continuous organic alkali recovery and reuse method using a fully continuous organic alkali in-line recovery and drying apparatus comprising one microchannel reactor, one continuous liquid-liquid separator, and one continuous kettle, which are sequentially connected according to the alkali recovery process. The method includes the following steps. (1) The first alkaline solution 1 (waste liquid; transported by the third pump 3) obtained by reacting the pre-prepared reaction material with alkali 1 to be recovered and reused, followed by a post-treatment operation, and the second alkaline solution 2 transported by the first pump 1 are thoroughly mixed in a micromixer, and then introduced into a microchannel reactor to carry out an alkalinization reaction, controlling the residence time to 0.1-30 minutes and controlling the temperature of the microchannel reactor to 0-90°C. (2) The alkalizing liquid discharged from the microchannel reactor enters a continuous liquid-liquid separator, where it is rapidly separated into layers by gravity. The lower layer is an aqueous solution of the second alkaline solution 2, which is reused after some water is removed by concentration. The upper layer of the continuous liquid-liquid separator is the first alkaline solution 1, which contains a small amount of water. The first alkaline solution 1 is then introduced directly into a continuous vessel equipped with a stirring device and a heat exchanger. A water removal agent is placed in the continuous vessel, and after stirring, the water contained in the first alkaline solution 1 is adsorbed. The first alkaline solution 1 is then drawn out by a second pump connected by piping from the upper outlet of the continuous vessel and enters a storage tank for the first alkaline solution 1, where it becomes recovered alkali.

[0007] In the present invention, the first pump, the second pump, and the third pump are plunger pumps for transporting a solution.

[0008] In the present invention, the micromixer is specially designed and specifically a composite plate type micromixer in which 15-18 diamond-shaped conduit mixing members are connected in series. As shown in Figure 2, the diamond-shaped conduit is a fluid passage, its cross-section is circular or square, the size of the cross-section (diameter or side length) is 100 μm-20 mm, the length of the fluid passage is 1-100 cm, the applicable flow velocity is 1-3000 mL / min, preferably the size of the cross-section (diameter or side length) is 1-20 mm, the length of the fluid passage is 10-100 cm, the applicable flow velocity is 1000-3000 mL / min, and the material is one or more selected from glass, polytetrafluoroethylene, stainless steel, Hastelloy, tantalum, and zirconium.

[0009] In the present invention, the microchannel reactor is a specially designed tubular microreactor equipped with a static mixing member. Specifically, its body is a tubular cavity that serves as a fluid passage, with a reaction material inlet and a reaction material outlet at both ends of the cavity, and a series of cross-shaped members arranged axially within the tubular cavity. The outside of the cavity is a heat exchange fluid intervening layer through which the heat exchange fluid passes, with a heat exchange fluid outlet and a heat exchange fluid inlet at both ends of the heat exchange fluid intervening layer (Figure 3). The diameter of the fluid passage is 100 μm-20 mm, and the length is 1 m-5000 m, preferably the diameter of the fluid passage is 5 mm-20 mm, and the length is 1 m-5000 m, and the material is one or more selected from glass, polytetrafluoroethylene, stainless steel, Hastelloy, tantalum, and zirconium.

[0010] In the present invention, the liquid-liquid separator is a liquid-liquid separator designed according to the principle of gravity sedimentation, and its body is a vertically arranged cylindrical cavity, with an inlet for the material to be separated provided at the lower end of the cavity, a lower heavy phase outlet further provided at the lower end of the cavity, and an upper light phase outlet provided at the upper end of the cavity, and the outside of the cylindrical cavity is a heat exchange fluid intervening layer through which the heat exchange fluid passes, with a heat exchange fluid inlet provided at the bottom of the heat exchange fluid intervening layer and a heat exchange fluid outlet provided at the top (Figure 4). The inner diameter of the liquid-liquid separator is 1-20 cm, the height is 1-200 cm, and the material is one or more combinations selected from glass, polytetrafluoroethylene, stainless steel, Hastelloy, tantalum, and zirconium.

[0011] In the present invention, the continuous vessel is a vertically oriented cylindrical body with stirring blades inside and a heat exchange jacket on the outside. A material inlet is provided at the bottom of the continuous vessel and a material outlet at the top. A heat exchange fluid inlet is provided at the bottom of the heat exchange jacket and a heat exchange fluid outlet at the top. A moisture removal agent is filled inside the continuous vessel. The material inlet is connected to a continuous liquid-liquid separator via piping, and the material outlet is connected to a pump via piping (Figure 5). The inner diameter of the vessel is 5-1000 cm and its height is 5-1000 cm. The material is one or a combination of several materials selected from glass, polytetrafluoroethylene, stainless steel, Hastelloy, tantalum, and zirconium.

[0012] In the present invention, the first alkaline solution 1 is one of liquid ammonia, triethylamine, trimethylamine, tributylamine, diethylamine, and N,N-diisopropylethylamine; alkali 2 is one of potassium carbonate, sodium carbonate, sodium bicarbonate, sodium hydroxide, potassium hydroxide, and lithium hydroxide; and the water removal agent filled into the continuous vessel is one or more selected from potassium carbonate, sodium carbonate, sodium bicarbonate, sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium sulfate, magnesium sulfate, and molecular sieves.

[0013] In the present invention, the temperature of the microchannel reactor is 0-90°C, and the material residence time is 0.1-30 min. Preferably, the temperature is 20-60°C, and the material residence time is 5-20 min.

[0014] The present invention further provides a continuous recovery and reuse apparatus for organic alkalis, comprising three transport pumps, one micromixer, one microchannel reactor, one continuous liquid-liquid separator, and one continuous kettle, which are connected in sequence according to the recovery process. The micromixer, microchannel reactor, liquid-liquid separator, and continuous kettle are connected in sequence by piping, the first pump 1 is used to introduce the second alkaline liquid into the micromixer, the second pump 2 is used to discharge the first alkaline liquid 1 from the continuous kettle into a storage tank via a pipeline, the third pump 3 is used to introduce the first alkaline liquid 1 (waste liquid) from the storage tank into the micromixer, and in the micromixer, the second alkaline liquid introduced by the first pump 1 and the first alkaline liquid 1 (waste liquid) introduced by the third pump are mixed. Afterward, the first alkaline solution enters a microchannel reactor for alkalization. The effluent from the microchannel reactor enters a liquid-liquid separator for liquid-liquid separation. Here, the second alkaline solution refluxes from the lower outlet of the liquid-liquid separator, is concentrated, and then introduced into a second alkaline solution storage pool for continued use. The first alkaline solution enters a continuous vessel via a pipeline from the upper outlet of the liquid-liquid separator, where it is processed. Water contained in the first alkaline solution is adsorbed and removed. The first alkaline solution is then discharged by a second pump, undergoes a series of processes, and enters a storage tank. This process is repeated. [Brief explanation of the drawing]

[0015] [Figure 1] This is a flowchart of a continuous recovery and reuse apparatus and method for organic alkalis. [Figure 2] This is a schematic diagram of the structure of plate-type micromixers connected in series in a circular shape. [Figure 3] This is a schematic diagram of the structure of a tubular microreactor containing a square-shaped mixing element. [Figure 4] This is a schematic diagram of the structure of a continuous liquid-liquid separator. [Figure 5] This is a schematic diagram of the structure of a continuous boiler used to remove water from recovered alkali.

[0016] Explanation of the symbols In Figures 3-5, 1- is the reaction material inlet of the tubular microreactor, 2- is the reaction material outlet of the tubular microreactor, 3- is the heat exchange fluid outlet of the tubular microreactor, 4- is the heat exchange fluid inlet of the tubular microreactor, 5- is the cross-shaped member of the tubular microreactor, 6- is the material to be separated inlet of the liquid-liquid separator, 7- is the lower heavy phase outlet of the liquid-liquid separator, 8- is the upper light phase outlet of the liquid-liquid separator, 9- is the heat exchange fluid inlet of the liquid-liquid separator, 10- is the heat exchange fluid outlet of the liquid-liquid separator, 11- is the material inlet of the continuous vessel, 12- is the material outlet of the continuous vessel, 13- is the heat exchange fluid inlet of the continuous vessel, 14- is the heat exchange fluid outlet of the continuous vessel, and 15- is the water removal agent. [Modes for carrying out the invention]

[0017] The present invention will be further described below with reference to examples.

[0018] Example 1 The trimethylamine salt waste liquid, obtained by reacting pre-prepared reaction materials with trimethylamine (alkali 1 to be recovered and reused) followed by a post-treatment operation, was thoroughly mixed in a micromixer with a 20% sodium hydroxide solution transported by pump 1, and then introduced into a microchannel reactor for alkalization. The residence time was 5 minutes, and the reactor temperature was controlled to 40°C. The alkalized liquid was then directly entered into a continuous liquid-liquid separator, where it was rapidly separated by gravity sedimentation. The lower layer was an aqueous sodium hydroxide solution, which was concentrated to 20% by distillation to remove water and then reused. The upper layer of the continuous liquid-liquid separator was trimethylamine containing a small amount of water, and was directly introduced into a continuous vessel with stirring and heat exchange functions. Anhydrous sodium sulfate, a water removal agent, was added to the vessel. After stirring, the water contained in the trimethylamine was adsorbed. The trimethylamine was extracted from the upper outlet of the vessel by pump 2, which was connected to a piping system, and entered into a trimethylamine storage tank for reuse. The recovery rate of trimethylamine was 95.1%, the purity was higher than 99%, and the water content was less than 0.1%.

[0019] Example 2 The triethylamine salt waste liquid, obtained by reacting pre-prepared reaction materials with triethylamine (alkali 1 to be recovered and reused) followed by a post-treatment operation, was thoroughly mixed in a micromixer with a 20% potassium hydroxide solution transported by pump 1, and then introduced into a microchannel reactor for alkalization. The residence time was 3 minutes, and the reactor temperature was controlled to 40°C. The alkalized liquid was then directly entered into a continuous liquid-liquid separator, where it was rapidly separated by gravity sedimentation. The lower layer was an aqueous solution of potassium hydroxide, which was concentrated to 20% by distillation to remove water and then reused. The upper layer of the continuous liquid-liquid separator was triethylamine containing a small amount of water, and was directly introduced into a continuous vessel with stirring and heat exchange functions. Anhydrous sodium sulfate, a water removal agent, was added to the vessel. After stirring, the water contained in the triethylamine was adsorbed. The triethylamine was extracted from the upper outlet of the vessel by pump 2, which was connected to a piping system, and entered into a triethylamine storage tank for reuse. The recovery rate of triethylamine was 96.3%, the purity was higher than 99%, and the water content was less than 0.1%.

[0020] Example 3 The triethylamine salt waste liquid, obtained by reacting pre-prepared reaction materials with triethylamine (alkali 1 to be recovered and reused) followed by a post-treatment operation, was thoroughly mixed in a micromixer with a 20% potassium hydroxide solution transported by pump 1, and then introduced into a microchannel reactor for alkalization. The residence time was 3 minutes, and the reactor temperature was controlled to 40°C. The alkalized liquid was then directly entered into a continuous liquid-liquid separator, where it was rapidly separated by gravity sedimentation. The lower layer was an aqueous solution of potassium hydroxide, which was concentrated to 20% by distillation to remove water and then reused. The upper layer of the continuous liquid-liquid separator was triethylamine containing a small amount of water, and was directly introduced into a continuous vessel with stirring and heat exchange functions. Anhydrous potassium hydroxide, a water removal agent, was added to the vessel. After stirring, the water contained in the triethylamine was adsorbed. The triethylamine was extracted from the upper outlet of the vessel by pump 2, which was connected to a piping system, and entered into a triethylamine storage tank for reuse. The recovery rate of triethylamine was 99.1%, the purity was higher than 99%, and the water content was less than 0.1%.

[0021] Example 4 The pre-prepared reaction material was reacted with triethylamine, which is the alkali 1 to be recovered and reused, and then post-treated. The waste liquid of triethylamine salt obtained in this way was thoroughly mixed with a 25% sodium hydroxide solution transported by pump 1 in a micro mixer, and then introduced into a microchannel reactor for alkalization. The residence time was 4 min, and the temperature of the reactor was controlled at 35°C. The alkalized liquid directly entered a continuous liquid-liquid separator and was quickly separated into layers by gravity sedimentation. The lower layer was an aqueous solution of sodium hydroxide, which was concentrated to 25% by distilling off the water and then reused. The upper layer of the continuous liquid-liquid separator was triethylamine containing a small amount of water, which was directly introduced into a continuous kettle having stirring and heat exchange functions. Anhydrous sodium hydroxide, which is a water remover, was placed in the kettle. After stirring, the water contained in the triethylamine was adsorbed. Triethylamine was withdrawn by pump 2 connected by piping from the upper outlet of the kettle and entered a storage tank for triethylamine, thereby realizing reuse. The recovery rate of triethylamine was 99.6%, the purity was higher than 99%, and the water content was less than 0.1%.

[0022] Example 5 The tributylamine salt waste liquid, obtained by reacting pre-prepared reaction materials with tributylamine (alkali 1 to be recovered and reused) followed by a post-treatment operation, was thoroughly mixed in a micromixer with a 25% sodium hydroxide solution transported by pump 1, and then introduced into a microchannel reactor for alkalization. The residence time was 4 minutes, and the reactor temperature was controlled to 35°C. The alkalized liquid was then directly entered into a continuous liquid-liquid separator, where it was rapidly separated by gravity sedimentation. The lower layer was an aqueous sodium hydroxide solution, which was concentrated to 25% by distillation to remove water and then reused. The upper layer of the continuous liquid-liquid separator was tributylamine containing a small amount of water, and was directly introduced into a continuous vessel with stirring and heat exchange functions. Anhydrous sodium hydroxide, a water removal agent, was added to the vessel. After stirring, the water contained in the tributylamine was adsorbed. The tributylamine was extracted from the upper outlet of the vessel by pump 2, which was connected to a piping system, and entered into a tributylamine storage tank for reuse. The recovery rate of tributylamine was 99.8%, the purity was higher than 99%, and the water content was less than 0.1%.

[0023] Furthermore, any modification or alteration of the embodiments described herein based on the concept of the present invention, or equivalent structural or process transformations made in accordance with the contents of this specification and drawings, or direct or indirect application of the above technical means to other related technologies, are all within the scope of protection of the present invention.

Claims

1. A continuous recovery and reuse method for organic alkali, using a continuous recovery and reuse apparatus for organic alkali, comprising: a first pump, a second pump and a third pump; one micromixer; one microchannel reactor; one liquid-liquid separator; and one kettle having an agitator and a heat exchange jacket and filled with a moisture removal agent, wherein the micromixer, the microchannel reactor, the liquid-liquid separator and the kettle are sequentially connected by piping, the first pump is used to introduce a second alkaline liquid into the micromixer, the second pump is used to discharge the first alkaline liquid from the kettle and introduce it into a storage tank via a pipeline, and the third pump is used to introduce the first alkaline liquid from the storage tank into the micromixer. This includes steps (1) and (2) below, (1) The first alkali solution, which is a waste alkali liquid obtained by reacting the pre-prepared reaction material with the first alkali to be recovered and reused, and the second alkali solution transported by the first pump are mixed in a micromixer, and then introduced into a microchannel reactor to carry out an alkalinization reaction, controlling the residence time to 0.1-30 minutes and controlling the temperature of the microchannel reactor to 0-90°C. (2) A method characterized in that the alkalizing liquid discharged from the microchannel reactor enters a liquid-liquid separator, separates into layers by gravity, the lower layer is an aqueous solution of the second alkali, which is reused as the second alkali after some water is removed by concentration, the upper layer of the liquid-liquid separator is the first alkali solution containing water, the first alkali solution is introduced directly into the kettle and stirred, the water contained in the first alkali is adsorbed, the first alkali solution is drawn out by a second pump connected by piping from the upper outlet of the kettle and enters a storage tank for the first alkali solution to recover the alkali, thereby enabling reuse.

2. The method according to claim 1, characterized in that the first pump, second pump, and third pump are plunger pumps for transporting a solution.

3. The method according to claim 1, wherein the micromixer is a composite plate type micromixer comprising 15 to 18 diamond-shaped conduits connected in series, the diamond-shaped conduits having a circular or square cross-section as fluid passages, a cross-sectional size of 100 μm to 20 mm, a fluid passage length of 1 to 100 cm, and an applicable flow velocity of 1 to 3000 mL / min.

4. The method according to claim 1, wherein the microchannel reactor is a tubular microreactor provided with a static mixing member, and specifically its body is a tubular cavity that serves as a fluid passage, with a reaction material inlet and a reaction material outlet provided at both ends of the cavity, and a series of cross-shaped members arranged axially within the tubular cavity, and the outside of the cavity is a heat exchange fluid intervening layer through which a heat exchange fluid passes, with a heat exchange fluid outlet and a heat exchange fluid inlet provided at both ends of the heat exchange fluid intervening layer, and the diameter of the fluid passage is 100 μm to 20 mm and the length is 1 m to 5000 m.

5. The liquid-liquid separator is a liquid-liquid separator designed according to the principle of gravity sedimentation, the body of which is a vertically arranged cylindrical cavity, an inlet for the material to be separated is provided at the lower end of the cavity, a lower heavy phase outlet is further provided at the lower end of the cavity, and an upper light phase outlet is provided at the upper end of the cavity, the outside of the cylindrical cavity is a heat exchange fluid intervening layer through which the heat exchange fluid passes, a heat exchange fluid inlet is provided at the lower part of the heat exchange fluid intervening layer, and a heat exchange fluid outlet is provided at the upper part, the inner diameter of the liquid-liquid separator is 1 to 20 cm and the height is 1 to 200 cm, the method according to claim 1.

6. The method according to claim 1, characterized in that the kettle is a cylindrical body arranged vertically, has stirring blades inside, has a heat exchange jacket on the outside, has a material inlet at the bottom of the kettle and a material outlet at the top, has a heat exchange fluid inlet at the bottom of the heat exchange jacket and a heat exchange fluid outlet at the top, has a moisture removal agent filled inside the kettle, has a material inlet connected to a liquid-liquid separator via piping, has a material outlet connected to a pump via piping, has an inner diameter of 5-1000 cm and a height of 5-1000 cm.

7. The method according to claim 1, characterized in that the first alkali is one of liquid ammonia, triethylamine, trimethylamine, tributylamine, diethylamine, and N,N-diisopropylethylamine, the second alkali is one of potassium carbonate, sodium carbonate, sodium bicarbonate, sodium hydroxide, potassium hydroxide, and lithium hydroxide, and the water removal agent filled in the kettle is one or more selected from potassium carbonate, sodium carbonate, sodium bicarbonate, sodium hydroxide, potassium hydroxide, lithium hydroxide, sodium sulfate, magnesium sulfate, and molecular sieves.

8. A continuous recovery and reuse apparatus for organic alkalis comprising a first pump, a second pump and a third pump, one micromixer, one microchannel reactor, one liquid-liquid separator, and one kettle having an agitator and a heat exchange jacket and filled with a moisture removal agent, wherein the micromixer, the microchannel reactor, the liquid-liquid separator and the kettle are sequentially connected by piping, The apparatus is characterized in that a first pump is used to introduce a second alkaline solution into a micromixer, a second pump is used to discharge the first alkaline solution from the kettle into a storage tank via a pipeline, a third pump is used to introduce the first alkaline solution from the storage tank into the micromixer, in the micromixer the second alkaline solution introduced by the first pump and the first alkaline solution introduced by the third pump are mixed and then enter a microchannel reactor for alkalization, the effluent from the microchannel reactor enters a liquid-liquid separator for liquid-liquid separation, the second alkaline solution is refluxed from the lower outlet of the liquid-liquid separator, concentrated and then introduced into a second alkaline solution storage pool for continued use, the first alkaline solution enters the kettle via a pipeline from the upper outlet of the liquid-liquid separator, is processed in the kettle, and water contained in the first alkaline solution is adsorbed and removed, the first alkaline solution is discharged by the second pump, undergoes a series of processes and then enters a storage tank, and thus circulates.

9. The aforementioned first pump, second pump, and third pump are plunger pumps for transporting the solution. The aforementioned micromixer is a composite plate type micromixer in which the rhomboid conduit mixing members 15-18 are connected in series, and the rhomboid conduit has a circular or square cross-section as a fluid passage, a cross-sectional size of 100 μm-20 mm, a fluid passage length of 1-100 cm, and an applicable flow velocity of 1-3000 mL / min. The aforementioned microchannel reactor is a tubular microreactor equipped with a static mixing member. Specifically, its body is a tubular cavity that serves as a fluid passage, with a reaction material inlet and a reaction material outlet at both ends of the cavity, and a series of cross-shaped members arranged axially within the tubular cavity. The outside of the cavity is a heat exchange fluid intervening layer through which the heat exchange fluid passes, with a heat exchange fluid outlet and a heat exchange fluid inlet at both ends of the heat exchange fluid intervening layer, and the fluid passage has a diameter of 100 μm to 20 mm and a length of 1 m to 5000 m. The aforementioned liquid-liquid separator is a liquid-liquid separator designed according to the principle of gravity sedimentation, and its body is a cylindrical cavity arranged vertically, with an inlet for the material to be separated provided at the lower end of the cavity, a lower heavy phase outlet further provided at the lower end of the cavity, and an upper light phase outlet provided at the upper end of the cavity, the outside of the cylindrical cavity being a heat exchange fluid intervening layer through which the heat exchange fluid passes, with a heat exchange fluid inlet provided at the bottom of the heat exchange fluid intervening layer and a heat exchange fluid outlet provided at the top, the inner diameter of the liquid-liquid separator being 1-20 cm and the height being 1-200 cm. The apparatus according to claim 8, characterized in that the aforementioned vessel is a cylindrical body arranged vertically, with stirring blades provided inside, the outside being a heat exchange jacket, a material inlet provided at the bottom of the vessel, a material outlet provided at the top, a heat exchange fluid inlet provided at the bottom of the heat exchange jacket, a heat exchange fluid outlet provided at the top, a moisture removal agent filled inside the vessel, the material inlet connected to a liquid-liquid separator by piping, the material outlet connected to a pump by piping, and the inner diameter of the vessel being 5-1000 cm and the height being 5-1000 cm.

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