WO2022122029A1 - 麦芽酚升华工段的冷却装置及冷却方法 - Google Patents

麦芽酚升华工段的冷却装置及冷却方法 Download PDF

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Publication number
WO2022122029A1
WO2022122029A1 PCT/CN2021/137216 CN2021137216W WO2022122029A1 WO 2022122029 A1 WO2022122029 A1 WO 2022122029A1 CN 2021137216 W CN2021137216 W CN 2021137216W WO 2022122029 A1 WO2022122029 A1 WO 2022122029A1
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Prior art keywords
sublimation
throttle plate
reaction kettle
reactor
gas phase
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PCT/CN2021/137216
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English (en)
French (fr)
Inventor
詹见
陈金林
肖建芳
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安徽金禾实业股份有限公司
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Application filed by 安徽金禾实业股份有限公司 filed Critical 安徽金禾实业股份有限公司
Priority to CN202180065863.5A priority Critical patent/CN116710184A/zh
Priority to EP21902734.9A priority patent/EP4238625A4/en
Publication of WO2022122029A1 publication Critical patent/WO2022122029A1/zh
Priority to US18/207,726 priority patent/US20230311024A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D7/00—Sublimation
    • B01D7/02—Crystallisation directly from the vapour phase
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0003—Condensation of vapours; Recovering volatile solvents by condensation by using heat-exchange surfaces for indirect contact between gases or vapours and the cooling medium
    • B01D5/0024—Rotating vessels or vessels containing movable parts

Definitions

  • the invention relates to a cooling device and a cooling method for a maltol sublimation section.
  • maltol methyl or ethyl
  • the material is sublimated in gaseous state and absorbed by cooling water to form an aqueous solution.
  • the absorbed aqueous solution is cooled again at low temperature into a solid, and dehydrated by a centrifuge to take out the material. for use in the next section.
  • Chinese patent document CN108355372A discloses a sublimation receiving method of maltol, which adopts a method of contacting and absorbing the steam material with the cooling water in the kettle after the sublimation steam enters the receiving kettle.
  • Chinese patent document CN208244148U discloses a sublimation reaction device in the production of ethyl maltol, including a sublimation kettle and a receiving tank, the sublimation kettle and the receiving tank are connected through a pipeline, and a titanium condenser tube is sleeved on the pipeline, and the titanium condensation
  • the pipe includes a condenser pipe and a jacketed pipe.
  • the condenser pipe is a straight transparent pipe body, and both ends of the condenser pipe are connected to the pipe through flanges.
  • the central axis of the straight transparent pipe body is parallel to the central axis of the pipe.
  • a number of partitions are arranged equidistantly along the axial direction, and a plurality of through holes are evenly arranged on the partitions; the jacket tube is sleeved outside the condensation tube, and a closed annular space is formed between the jacket tube and the condensation tube .
  • the first technical problem to be solved by the present invention is to provide a cooling device for the sublimation section of maltol, which has a simple structure, is convenient to use, simplifies the process and improves the production efficiency.
  • the second technical problem to be solved by the present invention is to provide a cooling method for the cooling device of the above-mentioned maltol sublimation section, which avoids water cooling in the prior art, does not generate a large amount of sewage, and saves resources.
  • the present invention provides a cooling device for the sublimation section of maltol, including a reaction kettle with an enamel inner wall, the reaction kettle is in the shape of a vertically arranged cylinder, and the side walls and bottom walls of the reaction kettle are provided with There is a jacket, the position of the jacket is provided with a condensed water inlet corresponding to the lower part of the reaction kettle, the upper part of the corresponding reaction kettle is provided with a condensed water outlet at the position of the jacket, the top wall of the reaction kettle is provided with a gas phase port that penetrates the top wall, and the bottom wall of the reaction kettle is provided with a condensed water outlet.
  • a discharge butterfly valve is arranged on the discharge port, and the surface of the discharge butterfly valve is covered with PTFE.
  • the upper part is provided with four circular throttle plates with enamel surface arranged at intervals up and down.
  • the diameter of the throttle plate matches the inner diameter of the reactor.
  • the throttle plate is a hollow plate, and the inner cavity of the throttle plate is communicated with the jacket.
  • the middle of the flow plate is provided with a first through hole vertically penetrating the throttle plate, each throttle plate is also provided with a number of second through holes arranged around the first through hole, a motor is arranged above the reactor, and the motor shaft It extends vertically downward into the reaction kettle and passes through all the first through holes in sequence.
  • the lower end of the rotating shaft is located at the lower part of the reaction kettle, and the lower end of the rotating shaft is provided with a stirring paddle.
  • the stirring paddle is made of stainless steel and covered with PTFE on the outside.
  • the upper side of each throttle plate is provided with a scraper matched with the throttle plate in position.
  • the cooling devices of the maltol sublimation section of the present invention are referred to as the device below.
  • the device has a simple structure, is convenient to use, simplifies the process, and improves the production efficiency.
  • the present invention provides the cooling method of the cooling device of the maltol sublimation section, comprising the following steps:
  • a cooling device for a sublimation section comprising a reactor with a smooth inner wall, a gas port on the top of the reactor, a discharge port on the bottom of the reactor, and a sublimation gas inlet in the middle of the reactor; the wall of the reactor is also provided with With jacket.
  • a throttle plate with an enamel surface is arranged in the reaction kettle, the middle of the throttle plate is provided with a first through hole vertically penetrating the throttle plate, and the throttle plate is also provided with several through holes arranged around the first through hole.
  • the throttle plate is a hollow plate, and the inner cavity of the throttle plate is communicated with the jacket.
  • the rotating shaft extending downward above the reaction kettle extends vertically downward into the reaction kettle and passes through the first through hole, and the upper side of the corresponding throttle plate at the position of the rotating shaft is provided with scrapers matching the throttle plate. plate.
  • the lower end of the rotating shaft is provided with a stirring paddle.
  • the stirring paddle is made of stainless steel and covered with polytetrafluoroethylene on the outside, and the upper side of each throttle plate is provided with a scraper matching the throttle plate at the position of the rotating shaft.
  • reaction kettle is in the shape of a vertically arranged cylinder, the throttle plate is circular, and the diameter of the throttle plate matches the inner diameter of the reactor.
  • the cooling method using the cooling device in the sublimation section includes the following steps: (1) passing cooling water of -10°C to -15°C into the inner cavity of the jacket and the throttle plate through the condensed water inlet and the condensed water outlet, And start the motor to stir, at the same time connect a vacuum pump to the gas phase port to vacuumize the reaction kettle to ensure that the vacuum degree in the kettle is -0.08MPa ⁇ -0.095MPa; (2) The sublimation kettle starts the sublimation operation, and the sublimated gas phase is directly passed through The gas phase inlet is introduced into the reactor for 4 hours; (3) the sublimated gas phase enters the reactor and condenses into solid materials, and the solid materials adhered to the upper side of the throttle plate are scraped off by the scraper and fall into the second through hole. (4) Finally, open the butterfly valve of the material opening, and release the solid material into the next step.
  • a cooling method for a sublimation section comprising the following steps: step 1: evacuate the inside of the reaction kettle to ensure that the vacuum degree in the kettle is -0.08MPa ⁇ -0.095MPa; step 2: introduce the sublimated gas phase into the reaction kettle through the gas phase inlet Step 3: The gas phase after sublimation enters the reactor and sublimates into solid material.
  • step 3 the solid material that is sublimated into a solid material and adhered to the upper side of the throttle plate of the reactor is scraped and dropped into the bottom of the reactor by a scraper.
  • step 3 the solid material adhered to the upper side of the throttle plate is scraped off by a scraper and falls into the bottom of the reaction kettle from the second through hole.
  • step 1 cooling water of -10°C to -15°C is introduced into the jacket of the reactor and the inner cavity of the throttle plate through the condensed water inlet and the condensed water outlet.
  • the cooling method of the cooling device of the maltol sublimation section of the present invention is abbreviated as the method below.
  • This method directly cools the sublimated gas phase material into a solid state, and directly sends it to the next post for use. Avoid the existing sublimation water to cool down and absorb materials, freeze and spin dry with a centrifuge, and generate a large amount of sewage, while wasting a lot of manpower and material resources. By using the method, the speed is faster, the efficiency is higher, the production yield is greatly improved, and the production cost is saved.
  • Figure 1 is a schematic diagram of the structure of the device.
  • FIG. 2 is a schematic diagram of the structure of the throttle plate of the device.
  • the cooling device of the maltol sublimation section includes a reaction kettle 1 with an enamel inner wall, and the inner wall is made of enamel material.
  • the reaction kettle needs a certain strength and can withstand a certain external force, thereby ensuring the normal progress of condensation; on the other hand , the condensed maltol (containing ethyl maltol) adheres to the inner wall, and the inner wall of the enamel material avoids the generation of peculiar smell.
  • the reaction kettle 1 is in a vertically arranged cylindrical shape.
  • the side wall and the bottom wall of the reaction kettle 1 are provided with a jacket 2.
  • the position of the jacket 2 corresponds to the lower part of the reactor 1 with a condensed water inlet 21.
  • the position of the jacket 2 is provided with a condensed water inlet 21.
  • the upper part of the corresponding reaction kettle 1 is provided with a condensed water outlet 22 .
  • the top wall of the reactor 1 is provided with a gas phase port 11 penetrating the top wall.
  • a vacuum pump is connected to the gas phase port. After the vacuum pump is turned on, a negative pressure can be formed in the reactor.
  • the gaseous substances include sublimed maltol and gaseous components of the solvent. After the maltol is condensed, solid substances can be obtained, and impurities such as the gaseous components of the solvent are in the negative pressure. Under the action and extraction action, it is discharged out of the kettle through the pipeline.
  • the bottom wall of the reaction kettle 1 is provided with a discharge port 12 penetrating the bottom wall, the discharge port 12 is provided with a discharge butterfly valve 121, the surface of the discharge butterfly valve 121 is covered with polytetrafluoroethylene, and the middle of the reaction kettle 1 in the height direction is provided with a through reaction
  • the sublimation gas phase inlet is set in the middle of the reactor. After the sublimated maltol gas phase enters, part of it condenses quickly, and part of it continues upward under the action of negative pressure. As the sublimated maltol gradually cools down and contacts the inside of the reactor and the throttle plate , the maltol gradually solidified and adhered to the unfolded surface inside the reactor.
  • the upper part of the reaction kettle 1 is provided with four circular throttle plates 3 with enamel surfaces arranged at intervals up and down.
  • the diameter of the throttle plate 3 matches the inner diameter of the reactor 1.
  • the throttle plate 3 is a hollow plate, and the throttle plate 3 The cavity communicates with the jacket 2 . Through the setting of the throttle plate, the air temperature in the reactor is lower, and the maltol can be solidified.
  • the middle of each throttle plate 3 is provided with a first through hole 31 that vertically penetrates the throttle plate 3 , and each throttle plate 3 is further provided with four second through holes 32 arranged around the first through hole 31 .
  • the first through hole on the throttle plate is mainly used to form an accommodating space for the rotating shaft, and the second through hole is used to scrape off the maltol adhering to the throttle plate.
  • the first and second through holes also form channels for gas to circulate in the reactor.
  • a motor 4 is arranged above the reaction kettle 1 , and the rotating shaft 41 of the motor 4 extends vertically downward into the reaction kettle 1 and passes through all the first through holes 31 in sequence. With this setup, the shaft does not affect the throttle plate.
  • the lower end of the rotating shaft 41 is located at the lower part of the reaction kettle 1, the lower end of the rotating shaft 41 is provided with a stirring paddle 42, the stirring paddle 42 is made of stainless steel and the outer side is covered with polytetrafluoroethylene, and the upper side of each throttle plate 3 corresponding to the position of the rotating shaft 41 is provided.
  • the set scraper and stirring paddle enable the solidified maltol to be scraped off in time and gradually.
  • the second through hole enables the maltol above each condensation layer (throttle plate, the bottom of the kettle) to fall through it.
  • a multi-layered condensation space can be formed to avoid uncondensed maltol sublimation gas being sucked away by negative pressure under vacuum operation, resulting in a decrease in yield, and the maltol can be removed from the kettle in time. , instead of having to stop and reclaim the material.
  • the amount of maltol solidified on the side wall of the kettle and under the throttle plate is relatively small.
  • the treatment method may be to introduce high-temperature steam, and gradually dissolve the unscratchable maltol and flow out from the first through hole and the second through hole. After cleaning, high-temperature steam is continuously introduced, and then hot water is introduced into the jacket and the vacuum pump is turned on to dry the inner wall of the kettle to complete the cleaning.
  • Embodiment 2 is a diagrammatic representation of Embodiment 1:
  • the cooling method of the cooling device of the maltol sublimation section comprises the following steps:
  • the obtained solid material has an impurity content of 2.5%.
  • the cooling method of the cooling device of the maltol sublimation section comprises the following steps:
  • the obtained solid material has an impurity content of 1.7%.
  • Embodiment 4 is a diagrammatic representation of Embodiment 4:
  • the cooling method of the cooling device of the maltol sublimation section comprises the following steps:
  • the method of the present application does not need to introduce water, thereby reducing the steps of separating maltol from water.
  • the condensation is realized under negative pressure, the low-melting-point impurities generated during the sublimation of maltol can be directly separated, which reduces the difficulty of separating impurities.
  • the obtained solid material has an impurity content of 1.6%.
  • the impurity content of the obtained product is less than 3%, which is far lower than the material obtained by absorbing sublimation gas by water. At the same time, energy consumption, water consumption and equipment usage are reduced.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Apparatus Associated With Microorganisms And Enzymes (AREA)

Abstract

一种升华工段的冷却装置及冷却方法，冷却装置包括设有光滑内壁的反应釜（1），反应釜（1）顶部设有气相口（11），反应釜（1）底部设有放料口（12），反应釜（1）中部设有升华气相进口（13），反应釜（1）的壁还设置有夹套（2）。

Description

麦芽酚升华工段的冷却装置及冷却方法
本申请要求申请日为2020年12月11日，申请号为202011451921.1，发明名称为麦芽酚升华工段的冷却装置及冷却方法的中国专利申请的优先权。
技术领域
本发明涉及麦芽酚升华工段的冷却装置及冷却方法。
背景技术
在麦芽酚(甲基或乙基)生产过程中，在升华工段是提纯，将物料升华气态在经过降温水吸收，成水溶液，将吸收水溶液再次用低温冷却成固体，经过离心机脱水，取出物料给下一工段使用。
中国专利文献CN108355372A公开了一种麦芽酚的升华接收方法，其采用将升华蒸汽进入接收釜后使得蒸汽物料与釜内冷却水接触吸收的方式。
中国专利文献CN208244148U公开了乙基麦芽酚生产中的升华反应装置，包括升华釜和受槽，所述升华釜与受槽之间通过管道相连，所述管道上套接有钛冷凝管，所述钛冷凝管包括冷凝管和夹套管，所述冷凝管为直线透明管体，冷凝管的两端均通过法兰与管道相连，所述直线透明管体的中心轴线与管道的中心轴线平行，冷凝管内沿轴向等距地设有若干个隔板，所述隔板上均匀设有多个通孔；所述夹套管套设在冷凝管外，夹套管与冷凝管之间形成封闭环形空间。
以上专利文献是传统的麦芽酚(甲基或乙基)的升华处理方式，均将升华后的气体溶解在水中。麦芽酚为冷却水吸收后需要进一步的分离处理，可能引入杂质，且本身需要与水分离，生产效率低、分离成本高。用水进行降温吸收物料，需要大量水，再将物料用一冷冻釜进行冷却后离心脱水，形成大量污水污染，同时用离心脱水浪费大量人力物力，物料再放入离心机过程 中经常性堵管情况，需要拆管清理，不仅浪费大量人力物力，还会有物料污染和浪费，同时在离心脱水会产生大量气味，造成环境污染。
发明内容
本发明所要解决的第一个技术问题是提供麦芽酚升华工段的冷却装置，该装置结构简单，使用方便，简化工艺，提高生产效率。
本发明所要解决的第二个技术问题是提供上述麦芽酚升华工段的冷却装置的冷却方法，避免现有技术中用水冷却，不会产生大量污水，节约资源。
为解决上述第一个技术问题，本发明提供了麦芽酚升华工段的冷却装置，包括内壁搪瓷的反应釜，所述的反应釜呈竖直布置的圆筒形，反应釜侧壁和底壁设有夹套，夹套位置上对应反应釜下部设有冷凝水进口，夹套位置上对应反应釜上部设有冷凝水出口，反应釜顶壁设有贯穿顶壁的气相口，反应釜底壁设有贯穿底壁的放料口，放料口上设有放料蝶阀，放料蝶阀表面覆有聚四氟乙烯，反应釜高度方向中部设有贯穿反应釜侧壁的升华气相进口，反应釜内的上部设有四个上下间隔布置的表面搪瓷的圆形节流板，节流板直径与反应釜内径相匹配，节流板为中空板，节流板内空腔与夹套连通，每个节流板中部设有沿竖直向贯穿节流板的第一通孔，每个节流板上还设有环绕第一通孔布置的若干第二通孔，反应釜上方设有电机，电机转轴竖直向下伸入反应釜内，并依次穿过所有第一通孔，转轴下端位于反应釜的下部，转轴下端设有搅拌桨，搅拌桨为不锈钢材质外侧包覆有聚四氟乙烯，转轴位置上对应每个节流板的上侧均设有与节流板相匹配的刮板。
为简单说明问题起见，以下对本发明所述的麦芽酚升华工段的冷却装置均简称为本装置。
本装置的优点：本装置结构简单，使用方便，简化工艺，提高生产效率。
为解决上述第二个技术问题，本发明提供了麦芽酚升华工段的冷却装置的冷却方法，包括以下步骤：
(1)通过冷凝水进口、冷凝水出口向夹套和节流板内腔通入-10℃～-15℃的冷却水，并启动电机进行搅拌，同时在气相口上连接真空泵对反应釜内抽真空，保证釜内真空度为-0.08MPa～-0.095MPa；
(2)升华釜开始升华作业，并将升华后的气相直接通过气相进口导入反应釜内持续4h；
(3)升华后的气相进入反应釜内凝华成固态物料，粘接在节流板上侧的固态物料经刮板刮落并从第二通孔落入反应釜底部；
(4)最后打开放料口的蝶阀，将固态物料放出进入下一步工序。
一种升华工段的冷却装置，包括设有光滑内壁的反应釜，反应釜顶部设有气口，反应釜底部设有放料口，反应釜中部设有升华气相进口；所述反应釜的壁还设置有夹套。
进一步的，反应釜内设有表面搪瓷的节流板，节流板中部设有沿竖直向贯穿节流板的第一通孔，节流板上还设有环绕第一通孔布置的若干第二通孔
进一步的，节流板为中空板，节流板内空腔与夹套连通。
进一步的，反应釜上方延伸向下的转轴竖直向下伸入反应釜内，并穿过第一通孔，转轴位置上对应节流板的上侧均设有与节流板相匹配的刮板。
进一步的，转轴下端设有搅拌桨。
进一步的，搅拌桨为不锈钢材质外侧包覆有聚四氟乙烯，转轴位置上对应每个节流板的上侧均设有与节流板相匹配的刮板。
进一步的，反应釜呈竖直布置的圆筒形，节流板为圆形，节流板直径与反应釜内径相匹配。
使用所述的升华工段的冷却装置的冷却方法，包括以下步骤：(1)通过冷凝水进口、冷凝水出口向夹套和节流板内腔通入-10℃～-15℃的冷却水，并启动电机进行搅拌，同时在气相口上连接真空泵对反应釜内抽真空，保证釜内真空度为-0.08MPa～-0.095MPa；(2)升华釜开始升华作业，并将升华后的气相直接通过气相进口导入反应釜内持续4h；(3)升华后的气相进入反应釜内凝华成固态物料，粘接在节流板上侧的固态物料经刮板刮落并从第二通孔落入反应釜底部；(4)最后打开放料口的蝶阀，将固态物料放出进入下一步工序。
一种升华工段的冷却方法，包括以下步骤：步骤1：对反应釜内抽真空，保证釜内真空度为-0.08MPa～-0.095MPa；步骤2：将升华后的气相通过气相进口导入反应釜内；步骤3：升华后的气相进入反应釜内凝华成固态物料。
进一步的，步骤3中，凝华成固态物料并粘接在反应釜的节流板上侧的固态物料经刮板刮落入反应釜底部。
进一步的，步骤3中，粘接在节流板上侧的固态物料经刮板刮落从第二通孔落入反应釜底部。
进一步的，步骤1中，通过冷凝水进口、冷凝水出口向反应釜的夹套和节流板内腔通入-10℃～-15℃的冷却水。
为简单说明问题起见，以下对本发明所述的麦芽酚升华工段的冷却装置的冷却方法均简称为本方法。
本方法的优点：本方法直接将升华气相物料冷却成固态，直接送下一岗位使用。避免现有升华用水进行降温并吸收物料，在进行冷冻并用离心机甩干，并产生大量污水，同时浪费大量人力物力。利用本方法，速度更快、效率更高，生产得率大大提高，并节约生产成本。
附图说明
图1是本装置的结构示意图。
图2是本装置节流板的结构示意图。
具体实施方式
实施例一：
参见图1，麦芽酚升华工段的冷却装置，包括内壁搪瓷的反应釜1，内壁使用搪瓷材质，一方面反应釜需要一定的强度，能够承受一定的外力，从而确保冷凝的正常进行；另一方面，冷凝的麦芽酚(含乙基麦芽酚)粘附在内壁，搪瓷材质的内壁避免异味的产生。
所述的反应釜1呈竖直布置的圆筒形，反应釜1侧壁和底壁设有夹套2，夹套2位置上对应反应釜1下部设有冷凝水进口21，夹套2位置上对应反应釜1上部设有冷凝水出口22。这样的结构使得反应釜内能够形成较低温度，升华的麦芽酚可以在壁部能够冷凝获得固态物质。
反应釜1顶壁设有贯穿顶壁的气相口11。气相口接有真空泵，开启真空泵后，可以在反应釜内形成负压。在真空度为-0.08MPa～-0.095MPa的负压情况下，气体物质中包括了升华的麦芽酚、溶剂的气态成分，麦芽酚冷凝后可以获得固态物质，溶剂的气态成分等杂质在负压作用下及抽取作用下，经由管道排出釜外。在真空负压情况下，麦芽酚的升华时减压的升华过程，因此在较低温度下即可实现升华，从而降低了高温加热升华导致的产品分解，产量下降，杂质增多的问题。
反应釜1底壁设有贯穿底壁的放料口12，放料口12上设有放料蝶阀121，放料蝶阀121表面覆有聚四氟乙烯，反应釜1高度方向中部设有贯穿反应釜1侧壁的升华气相进口13。升华气相进口设置在反应釜中部，升华的麦芽酚气相进入后，部分很快冷凝，一部分在负压作用下持续向上，随着升华的麦芽酚逐渐的冷却以及接触到反应釜内部和节流板，麦芽酚逐渐的凝固，粘附在反应釜内部展开的表面上。
反应釜1内的上部设有四个上下间隔布置的表面搪瓷的圆形节流板3，节流板3直径与反应釜1内径相匹配，节流板3为中空板，节流板3内空腔与夹套2连通。通过节流板的设置，使反应釜内空气温度较低，能够凝固麦芽酚。每个节流板3中部设有沿竖直向贯穿节流板3的第一通孔31，每个节流板3上还设有环绕第一通孔31布置的四个第二通孔32。节流板上的第一通孔主要用于形成转轴的容纳空间，第二通孔用于将节流板上粘附的麦芽酚刮下。第一和第二通孔还形成了供气体在反应釜内流通的通道。反应釜1上方设有电机4，电机4转轴41竖直向下伸入反应釜1内，并依次穿过所有第一通孔31。这种设置方式，转轴不会影响节流板。转轴41下端位于反应釜1的下部，转轴41下端设有搅拌桨42，搅拌桨42为不锈钢材质外侧包覆有聚四氟乙烯，转轴41位置上对应每个节流板3的上侧均设有与节流板4相匹配的刮板43。本申请通过设置的刮板、搅拌桨，使得凝固的麦芽酚能够及时的、逐步的被刮下。在反应釜 内部具有多层的冷凝收集层的情况下，第二通孔使每层冷凝层(节流板、釜底)上方的麦芽酚能够通过其落下。通过这样的设置，既能够形成多层次化的冷凝空间，避免在真空操作情况下有未冷凝的麦芽酚升华气体被负压抽吸走造成产量降低，也能够及时的将麦芽酚从釜内排除，而不必采用停机取料的方式。麦芽酚凝固在釜的侧壁以及节流板下方的料，相对较少，随着堆积的量增加，发现影响传热时，可停机进行处理。处理方式可以是采用通入高温水蒸汽，逐渐的无法刮擦的麦芽酚溶解并从第一通孔和第二通孔流出。清洁完毕后持续通入高温水蒸气，随后向夹套内通入热水并开启真空泵，将釜内壁烘干，完成清洁。
实施例二：
麦芽酚升华工段的冷却装置的冷却方法，包括以下步骤：
(1)通过冷凝水进口、冷凝水出口向夹套和节流板内腔通入-10℃的冷却水，并启动电机进行搅拌，同时在气相口上连接真空泵对反应釜内抽真空，保证釜内真空度为-0.08MPa；
(2)升华釜开始升华作业，并将升华后的气相直接通过气相进口导入反应釜内持续4h；
(3)升华后的气相进入反应釜内凝华成固态物料，粘接在节流板上侧的固态物料经刮板刮落并从第二通孔落入反应釜底部；
(4)最后打开放料口的蝶阀，将固态物料放出进入下一步工序。
经过检测，获得固态物料中，杂质含量为2.5％。
实施例三：
麦芽酚升华工段的冷却装置的冷却方法，包括以下步骤：
(1)通过冷凝水进口、冷凝水出口向夹套和节流板内腔通入-12.5℃的冷却水，并启动电机进行搅拌，同时在气相口上连接真空泵对反应釜内抽真空，保证釜内真空度为-0.09MPa；
(2)升华釜开始升华作业，并将升华后的气相直接通过气相进口导入反应釜内持续4h；
(3)升华后的气相进入反应釜内凝华成固态物料，粘接在节流板上侧的固态物料经刮板刮落并从第二通孔落入反应釜底部；
(4)最后打开放料口的蝶阀，将固态物料放出进入下一步工序。
经过检测，获得固态物料中，杂质含量为1.7％。
实施例四：
麦芽酚升华工段的冷却装置的冷却方法，包括以下步骤：
(1)通过冷凝水进口、冷凝水出口向夹套和节流板内腔通入-15℃的冷却水，并启动电机进行搅拌，同时在气相口上连接真空泵对反应釜内抽真空，保证釜内真空度为-0.095MPa；
(2)升华釜开始升华作业，并将升华后的气相直接通过气相进口导入反应釜内持续4h；
(3)升华后的气相进入反应釜内凝华成固态物料，粘接在节流板上侧的固态物料经刮板刮落并从第二通孔落入反应釜底部；
(4)最后打开放料口的蝶阀，将固态物料放出进入下一步工序。
相较于将麦芽酚蒸汽通入水中从而使其结晶，本申请方式不需要引入水，从而减少了将麦芽酚从水中分离的步骤。此外，由于是在负压状态下实现冷凝，因此麦芽酚升华过程中产生的低熔点杂质均可直接分离，降低了分离杂质的难度。
经过检测，获得固态物料中，杂质含量为1.6％。
在实施例二、三、四中，获得产品的杂质含量低于3％，这一杂质含量远低于采用水吸收升华气体方式方式获得的物料。同时，降低了能耗、水耗以及设备使用。
以上所述，仅为本申请的具体实施方式，在本申请的上述教导下，本领域技术人员可以在上述实施例的基础上进行其他的改进或变形。本领域技术人员应该明白，上述的具体描述只是更好的解释本申请的目的，本申请的保护范围应以权利要求的保护范围为准。
此外，本领域的技术人员能够理解，尽管在此所述的一些实施例包括其它实施例中所包括的某些特征而不是其它特征，但是不同实施例的特征的组合意味着处于本申请的范围之内并且形成不同的实施例。例如，在下面的权利要求书中，所要求保护的实施例的任意之一都可以以任意的组合方式来使用。

Claims (12)

  1. 一种升华工段的冷却装置，其特征在于：包括设有光滑内壁的反应釜，反应釜顶部设有气口，反应釜底部设有放料口，反应釜中部设有升华气相进口；所述反应釜的壁还设置有夹套。
  2. 如权利要求1所述的升华工段的冷却装置，其特征在于：反应釜内设有表面搪瓷的节流板，节流板中部设有沿竖直向贯穿节流板的第一通孔，节流板上还设有环绕第一通孔布置的若干第二通孔
  3. 如权利要求2所述的升华工段的冷却装置，其特征在于：节流板为中空板，节流板内空腔与夹套连通。
  4. 如权利要求2所述的升华工段的冷却装置，其特征在于：反应釜上方延伸向下的转轴竖直向下伸入反应釜内，并穿过第一通孔，转轴位置上对应节流板的上侧均设有与节流板相匹配的刮板。
  5. 如权利要求4所述的升华工段的冷却装置，其特征在于：转轴下端设有搅拌桨。
  6. 如权利要求5所述的升华工段的冷却装置，其特征在于：搅拌桨为不锈钢材质外侧包覆有聚四氟乙烯，转轴位置上对应每个节流板的上侧均设有与节流板相匹配的刮板。
  7. 如权利要求1所述的升华工段的冷却装置，其特征在于：反应釜呈竖直布置的圆筒形，节流板为圆形，节流板直径与反应釜内径相匹配。
  8. 使用如权利要求1-7中所述的升华工段的冷却装置的冷却方法，其特征在于，包括以下步骤：
    (1)通过冷凝水进口、冷凝水出口向夹套和节流板内腔通入-10℃～-15℃的冷却水，并启动电机进行搅拌，同时在气相口上连接真空泵对反应釜内抽真空，保证釜内真空度为-0.08MPa～-0.095MPa；
    (2)升华釜开始升华作业，并将升华后的气相直接通过气相进口导入反应釜内持续4h；
    (3)升华后的气相进入反应釜内凝华成固态物料，粘接在节流板上侧的固态物料经刮板刮落并从第二通孔落入反应釜底部；
    (4)最后打开放料口的蝶阀，将固态物料放出进入下一步工序。
  9. 一种升华工段的冷却方法，包括以下步骤：
    步骤1：对反应釜内抽真空，保证釜内真空度为-0.08MPa～-0.095MPa；
    步骤2：将升华后的气相通过气相进口导入反应釜内；
    步骤3：升华后的气相进入反应釜内凝华成固态物料。
  10. 如权利要求9所述的升华工段的冷却方法，其特征在于：步骤3中，凝华成固态物料并粘接在反应釜的节流板上侧的固态物料经刮板刮落入反应釜底部。
  11. 如权利要求10所述的升华工段的冷却方法，其特征在于：步骤3中，粘接在节流板上侧的固态物料经刮板刮落从第二通孔落入反应釜底部。
  12. 如权利要求9所述的升华工段的冷却方法，其特征在于：步骤1中，通过冷凝水进口、冷凝水出口向反应釜的夹套和节流板内腔通入-10℃～-15℃的冷却水。
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Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112742061A (zh) * 2020-12-11 2021-05-04 安徽金禾实业股份有限公司 麦芽酚升华工段的冷却装置及冷却方法

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2993764A (en) * 1956-12-07 1961-07-25 Cfmc Apparatus for purification by sublimation
GB1275232A (en) * 1969-04-16 1972-05-24 Diamond Shamrock Corp Improvements in or relating to sublimation processes
CN102671412A (zh) * 2012-05-16 2012-09-19 六盘水神驰生物科技有限公司 升华法焦性没食子酸冷阱回收装置
CN102671415A (zh) * 2012-05-16 2012-09-19 六盘水神驰生物科技有限公司 升华法焦性没食子酸一步作业法升华装置
CN202709776U (zh) * 2012-08-09 2013-01-30 山东盛华电子新材料有限公司 一种高真空蒸馏系统中的冷却装置
CN108355372A (zh) 2018-01-13 2018-08-03 安徽金禾实业股份有限公司 一种麦芽酚的升华接收方法及装置
CN208244148U (zh) 2018-04-18 2018-12-18 陕西天汉生物科技有限公司 乙基麦芽酚生产中的升华反应装置
CN210030506U (zh) * 2019-05-24 2020-02-07 湖北开元化工科技股份有限公司 一种对苯醌连续高效升华结晶系统
CN112742061A (zh) * 2020-12-11 2021-05-04 安徽金禾实业股份有限公司 麦芽酚升华工段的冷却装置及冷却方法

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2538540A (en) * 1944-06-22 1951-01-16 Kraft Foods Co Distillation apparatus
GB949161A (en) * 1959-04-30 1964-02-12 Maruzen Sekiyu Kabushiki Kaish A process and apparatus for manufacturing high purity p-xylene
BE880930A (nl) * 1979-12-28 1980-06-30 Vandekerckhove Constr Inwendig verwarmd roerwerk
NO307957B1 (no) * 1998-05-29 2000-06-26 Norsk Hydro As Fremgangsmate for desorpsjon av ±n eller flere komponenter fra en absorbentlosning og anvendelse derav
CN101972556B (zh) * 2010-11-18 2012-07-04 唐山中材重型机械有限公司 立式蒸馏塔
CN203899596U (zh) * 2014-05-30 2014-10-29 建水德福再生资源利用有限公司 化工反应结晶装置
WO2017056472A1 (ja) * 2015-09-30 2017-04-06 Ｊｆｅスチール株式会社 晶析槽のスクレーパー装置
CN207877830U (zh) * 2018-01-30 2018-09-18 赣州齐畅新材料有限公司 一种稀土用循环冷却装置
WO2020106397A1 (en) * 2018-11-20 2020-05-28 Exxonmobil Upstream Research Company Methods and apparatus for improving multi-plate scraped heat exchangers
CN111330300A (zh) * 2020-03-04 2020-06-26 上海缘昌医药化工装备有限公司 一种刮壁式连续蒸发、结晶、干燥和反应多用途机

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2993764A (en) * 1956-12-07 1961-07-25 Cfmc Apparatus for purification by sublimation
GB1275232A (en) * 1969-04-16 1972-05-24 Diamond Shamrock Corp Improvements in or relating to sublimation processes
CN102671412A (zh) * 2012-05-16 2012-09-19 六盘水神驰生物科技有限公司 升华法焦性没食子酸冷阱回收装置
CN102671415A (zh) * 2012-05-16 2012-09-19 六盘水神驰生物科技有限公司 升华法焦性没食子酸一步作业法升华装置
CN202709776U (zh) * 2012-08-09 2013-01-30 山东盛华电子新材料有限公司 一种高真空蒸馏系统中的冷却装置
CN108355372A (zh) 2018-01-13 2018-08-03 安徽金禾实业股份有限公司 一种麦芽酚的升华接收方法及装置
CN208244148U (zh) 2018-04-18 2018-12-18 陕西天汉生物科技有限公司 乙基麦芽酚生产中的升华反应装置
CN210030506U (zh) * 2019-05-24 2020-02-07 湖北开元化工科技股份有限公司 一种对苯醌连续高效升华结晶系统
CN112742061A (zh) * 2020-12-11 2021-05-04 安徽金禾实业股份有限公司 麦芽酚升华工段的冷却装置及冷却方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP4238625A4

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