WO2020088294A1 - Device for evaporation and crystallization - Google Patents
Device for evaporation and crystallization Download PDFInfo
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- WO2020088294A1 WO2020088294A1 PCT/CN2019/112400 CN2019112400W WO2020088294A1 WO 2020088294 A1 WO2020088294 A1 WO 2020088294A1 CN 2019112400 W CN2019112400 W CN 2019112400W WO 2020088294 A1 WO2020088294 A1 WO 2020088294A1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0031—Evaporation of components of the mixture to be separated by heating
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- the invention relates to the field of chemical equipment, in particular to a device for evaporation and crystallization.
- the corresponding device In the continuous crystallization process, the method of evaporating solvent crystallization is often used.
- the corresponding device generally includes an evaporation container, a crystallization container and a circulation circuit.
- the device is difficult to effectively control the particle size of the crystal, resulting in uneven distribution of crystal size, poor crystal regularity, and low crystal purity, which affects the quality of the product .
- the crystallization efficiency of the device is relatively low.
- the present invention provides a device for evaporative crystallization with high crystallization efficiency.
- the present invention provides an apparatus for evaporative crystallization, which includes:
- An evaporation container the evaporation container is used to evaporate the solvent, a guide tube is provided at the bottom of the evaporation container, and an evaporation gas outlet is also provided at the top of the evaporation container;
- a crystallization container the crystallization container is used for crystallization, the crystallization container is located below the evaporation container, the guide tube extends into the crystallization container, and communicates with the crystallization container, the bottom of the crystallization container is provided There is a crystal slurry outlet; wherein, the side wall of the crystallization container is connected with a circulating material outlet pipe, and the circulating material outlet pipe is branched into a first branch pipe and a second branch pipe;
- the device for evaporating and crystallization further includes a first circulation unit and a second circulation unit.
- the first circulation unit includes the first branch pipe, the first circulation pump, the first circulation inlet pipe, and the first branch pipe The first circulation pump is connected;
- the first circulation inlet pipe has a first end and a second end, the first end of the first circulation inlet pipe is connected to the first circulation pump, the first circulation inlet pipe The second end of the is connected to the evaporation container;
- the second circulation unit includes the second branch pipe, a second circulation pump, a heater, and a second circulation inlet pipe.
- the second branch pipe is connected to the second circulation pump and the heater in sequence, and the second circulation inlet
- the tube has a third end and a fourth end, the third end of the second circulation inlet tube is connected to the heater, and the fourth end of the second circulation inlet tube is connected to the evaporation container;
- the device for evaporating and crystallization further includes a raw material liquid inlet pipe connected to the second branch pipe and used for pumping the raw material liquid to the heater through the second circulation.
- the crystallization vessel is also provided with a rectifier classifier.
- the rectifier classifier includes a plurality of channels, and the ratio of the size of the lower end of the channel to the size of the upper end of the channel is 1.1: 1 to 10: 1.
- the size of the upper end of the channel is 3 mm to 100 mm.
- the opening rate of the channel is 5% -50%.
- a defoamer and defoamer is provided inside the evaporation container near the evaporation gas outlet.
- the side wall of the evaporation container and the side wall of the crystallization container are also provided with a balance tube, and the balance tube communicates the evaporation container and the crystallization container.
- the invention also provides the application of the device for evaporative crystallization in the field of continuous crystallization.
- the The crystallization liquid in the crystallization vessel is in a turbulent state, which can effectively avoid the occurrence of crystal agglomeration, making the size of the precipitated crystal particles controllable; at the same time, the turbulent state further promotes the separation of large and small crystals, and plays a role in the first circulation pump and the second circulation pump
- the fine crystal particles in the crystal particles are circulated and introduced into the heater and the evaporation container. Part of the fine crystal particles that are circulated and introduced into the evaporation vessel can be used as crystal nuclei for the next cycle of crystallization, so that the subsequent crystal particles precipitate faster and form crystal particles of a more uniform size.
- a heater is provided in the second branch pipe, which can give the heat of the raw material liquid or the second mother liquid transported by the second circulation unit, and cause it to evaporate part of the solvent in the evaporation container, which is more beneficial to the raw material liquid or the second mother liquid
- the crystallization vessel performs crystallization.
- the device can realize the continuous formation of crystalline particles, the crystallization efficiency is high, and it is suitable for industrial production.
- the rectifier classifier can sort out the chaotic flow field distribution in the crystallization vessel (when there is no rectifier classifier), so that the length of the liquid flow process below the rectifier classifier tends In order to be consistent, the flow velocity of each stream tends to be consistent, so that the flow field distribution is regular and orderly, which promotes more uniform precipitation of crystalline particles.
- there is a flow rate difference between the rectifier classifier channel and the rectifier classifier because the low flow rate below the rectifier classifier is unable to continuously entrain larger crystalline particles, the larger crystalline particles are in the low-flow fluid under the rectifier classifier.
- Precipitation occurs during entrainment, and the fine-grained particles entrained by the flow below the rectifier classifier near the channel of the rectifier classifier will be entrained by the high-velocity liquid flow in the channel of the rectifier classifier and recirculated into the heater for reheating Dissolve, and circulate into the evaporation vessel as crystal nuclei.
- the role of screening and separating crystals can be achieved, so that the final product with more uniform and controllable crystal size can be obtained.
- FIG. 1 is a schematic structural diagram of an apparatus for evaporative crystallization according to Embodiment 1 of the present invention.
- FIG. 2 is a schematic structural diagram of an apparatus for evaporative crystallization according to Embodiment 2 of the present invention.
- FIG. 3 is a schematic structural view of a rectifier and classifier in the device for evaporative crystallization of FIG. 2.
- Embodiment 1 of the present invention provides an apparatus for evaporative crystallization.
- the device for evaporating and crystallization includes an evaporating container 6 and a crystallization container 8.
- the crystallization container 8 is located below the evaporating container 6.
- the evaporating container 6 is used to evaporate the solvent, and the crystallization container 8 is used for crystallization.
- the top of the evaporating container 6 is provided with The evaporation gas outlet 10, the bottom of the evaporation container 6 is provided with a guide tube 7, the guide tube 7 extends into the crystallization container 8 and communicates with the crystallization container 8, and the side wall of the crystallization container 8 is connected with a circulating material outlet tube 12, circulating The material outlet pipe 12 branches into a first branch pipe 2a and a second branch pipe 2b.
- the evaporative crystallization also includes a first circulation unit and a second circulation unit, the first circulation unit includes a first branch 2a, a first circulation pump 13, a first circulation inlet pipe 14, the first branch 2a and the first circulation The pump 13 is connected, and the first circulation inlet pipe 14 has a first end and a second end. The first end of the first circulation inlet pipe 14 is connected to the first circulation pump 13, and the second end of the first circulation inlet pipe 14 is connected to the evaporation Container 6.
- the second circulation unit includes the second branch pipe 2b, the second circulation pump 3, the heater 4 and the second circulation inlet pipe 5.
- the second branch pipe 2b is connected to the second circulation pump 3 and the heater 4 in sequence, and the second circulation inlet
- the tube 5 has a third end and a fourth end.
- the third end of the second circulation inlet 5 is connected to the heater 4, and the fourth end of the second circulation inlet 5 is connected to the evaporation container 6.
- the device for evaporating and crystallization further includes a raw material liquid inlet pipe 1, which is connected to the second branch pipe 2b, and is used to send the raw material liquid to the heater 4 through the second circulation pump 3.
- the first circulation circuit (corresponding to the first circulation unit) is: crystallization vessel 8, circulation material outlet pipe 12, first branch pipe 2a, first circulation pump 13, first circulation inlet pipe 14, evaporation vessel 6; second circulation
- the circuit (corresponding to the second circulation unit) is: a crystallization vessel 8, a circulation material outlet pipe 12, a second branch pipe 2b, a second circulation pump 3, a heater 4, a second circulation inlet pipe 5, and an evaporation vessel 6.
- the second branch 2b is also responsible for connecting to the raw material liquid inlet pipe 1 and continuously introducing the raw material liquid into the second circulation circuit.
- the first circulation circuit is used to lead part of the mother liquor (defined as the first mother liquor) in the crystallization container 8 and part of the fine crystal particles (defined as the first fine crystal) obtained by the crystallization directly to the evaporation vessel 6, the part of the fine crystals
- the particles can be used as crystal nuclei in the next cycle, which will induce more uniform crystal particles. It should be noted that the first fine crystals can continue to grow to obtain larger and more uniform crystalline particles.
- the re-entry of the first fine crystals into the crystallization container 8 will also induce more crystalline particles to form orderly, that is, That is to say, the effect of the first circulation circuit is divided into two aspects: one is to make a larger number of crystalline particles formed; the other is to make fine-crystalline particles grow into uniform crystalline particles.
- the second circulation circuit is used to pass another part of the mother liquid (defined as the second mother liquid) in the crystallization container 8 and another part of the fine crystal particles (defined as the second fine crystal) obtained by crystallization into the evaporation container 6 through the action of the heater 4 After the solvent evaporates, it enters the crystallization vessel 8 to perform the next cycle of crystallization.
- the evaporation vessel 6 generally does not require additional heating.
- the temperature of the raw material liquid or the second mother liquid flowing from the second circulation inlet 5 after being heated by the heater 4 will increase. Therefore, the raw material liquid or the second The mother liquor evaporates part of the solvent in the evaporation container 6.
- a defoaming and defoaming device 9 is provided near the evaporation gas outlet 10 inside the evaporation container 6, and the defoaming and defoaming device 9 can be Screen structure or other types of defoamer and demister.
- the side wall of the evaporation container 6 and the side wall of the crystallization container 8 are also provided with a balance tube 11, which connects the evaporation container 6 and the crystallization container 8.
- the bottom of the crystallization container 8 is provided with a crystal slurry discharge port 15.
- Embodiment 2 of the present invention provides an apparatus for evaporative crystallization.
- the device for evaporative crystallization is basically the same in structure as the device for evaporative crystallization of Embodiment 1, except that a rectifier and classifier 17 is provided in the crystallization vessel 8.
- the rectifier classifier 17 includes multiple channels 18. The function of the rectifier classifier 17 is to obtain more uniform crystalline particles.
- the design purpose of the size of the lower end of the channel 18 is greater than the size of the upper end of the channel 18 has two aspects: (1) to prevent the phenomenon of "backmixing" of particles; (2) to avoid the possibility of the channel 18 being blocked.
- the axial section of the channel 18 may be, but not limited to, trapezoidal, bowl-shaped, or drop-shaped.
- the ratio of the size of the lower end of the channel 18 to the size of the upper end of the channel 18 is 1.1: 1 to 10: 1.
- the ratio of the size of the lower end of the channel 18 to the size of the upper end of the channel 18 It is 1.5: 1 ⁇ 5: 1.
- the size of the upper end of the channel 18 is 3 mm to 100 mm, preferably 5 mm to 50 mm.
- the aperture ratio of the plurality of channels 18 (that is, the sum of the area of the upper ends of the channels as a percentage of the area of the upper surface of the rectifier classifier) is 5% to 50%, preferably 10% to 30%.
- the evaporation container 6 is used to evaporate the solvent in the raw material liquid, and the crystallization container 8 is used for crystallization.
- the first branch pipe 2a is used to transform the raw material liquid
- the fine crystal particles in the crystal particles formed by the crystallization are redirected into the evaporation container 6, and the fine crystal particles can be used as crystal nuclei for the next cycle of crystallization, thereby inducing more and more uniform crystal particles to form; the second branch 2b
- the heater 4 is provided to give heat to the raw material liquid or the second mother liquid, and the partial evaporation of the solvent in the evaporation container 6 is more conducive to the crystallization of the raw material liquid or the second mother liquid in the crystallization container 8.
- the device can be used for the continuous formation of grains.
- it is suitable for vitamin B6, hexonic acid, sucralose, ethyl maltol, methionine, gulonic acid, citric acid, threonine, tryptophan, sodium gluconate, glucose, glutamic acid, Evaporative crystallization of lysine or sorbitol.
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Abstract
Provided by the present invention is a device used for evaporation and crystallization. The device comprises an evaporation container and a crystallization container. The device used for evaporation and crystallization further comprises a first circulation unit and a second circulation unit. The first circulation unit comprises a first branch pipe, a first circulation pump, and a first circulation inlet pipe that are successively connected. The second circulation unit comprises a second branch pipe, a second circulation pump, a heater, and a second circulation inlet pipe that are successively connected. The first circulation inlet pipe and the second circulation inlet pipe are connected to the evaporation container. By means of providing an additional first circulation loop, a portion of fine crystals are reintroduced into the crystallization container as a crystal nucleus, and a product that has more uniform particles and a controllable particle size is finally obtained.
Description
相关申请Related application
本申请要求2018年10月31日申请的,申请号为201811291575.8,名称为“用于蒸发结晶的装置”和2018年的10月31日申请的,申请号为201821784240.5,名称为“用于蒸发结晶的装置”的中国专利申请的优先权,在此将其全文引入作为参考。This application requires the application on October 31, 2018, the application number is 201811291575.8, the name is "device for evaporative crystallization" and the application on October 31, 2018, the application number is 201821784240.5, the name is "for evaporative crystallization The priority of the Chinese patent application of "device" is hereby incorporated by reference in its entirety.
本发明涉及化工装备领域,特别是涉及一种用于蒸发结晶的装置。The invention relates to the field of chemical equipment, in particular to a device for evaporation and crystallization.
在连续结晶过程中,经常采用蒸发溶剂结晶的方法。其对应的装置一般包括蒸发容器、结晶容器与循环回路,该装置难以对晶体的粒径进行有效调控,造成晶粒大小分布不均,晶型规整度差,结晶纯度低,从而影响产品的质量。此外,该装置的结晶效率也比较低。In the continuous crystallization process, the method of evaporating solvent crystallization is often used. The corresponding device generally includes an evaporation container, a crystallization container and a circulation circuit. The device is difficult to effectively control the particle size of the crystal, resulting in uneven distribution of crystal size, poor crystal regularity, and low crystal purity, which affects the quality of the product . In addition, the crystallization efficiency of the device is relatively low.
发明内容Summary of the invention
针对上述问题,本发明提供一种结晶效率高的用于蒸发结晶的装置。In view of the above problems, the present invention provides a device for evaporative crystallization with high crystallization efficiency.
本发明提供一种用于蒸发结晶的装置,其包括:The present invention provides an apparatus for evaporative crystallization, which includes:
蒸发容器,所述蒸发容器用于将溶剂蒸发,所述蒸发容器的底部设置导流管,所述蒸发容器的顶部还设置有蒸发气体出口;An evaporation container, the evaporation container is used to evaporate the solvent, a guide tube is provided at the bottom of the evaporation container, and an evaporation gas outlet is also provided at the top of the evaporation container;
结晶容器,所述结晶容器用于结晶,所述结晶容器位于所述蒸发容器的下方,所述导流管伸至所述结晶容器内,并与结晶容器相连通,所述结晶容器的底部设有晶浆出料口;其中,所述结晶容器的侧壁连有循环物料出管,所述循环物料出管分叉成第一分管和第二分管;A crystallization container, the crystallization container is used for crystallization, the crystallization container is located below the evaporation container, the guide tube extends into the crystallization container, and communicates with the crystallization container, the bottom of the crystallization container is provided There is a crystal slurry outlet; wherein, the side wall of the crystallization container is connected with a circulating material outlet pipe, and the circulating material outlet pipe is branched into a first branch pipe and a second branch pipe;
所述用于蒸发结晶的装置还包括第一循环单元及第二循环单元,所述第一循环单元包括所述第一分管、第一循环泵、第一循环进管,所述第一分管与该第一循环泵连接;所述第一循环进管具有第一端及第二端,所述第一循环进管的第一端与所述第一循环泵相连,所述第一循环进管的第二端连于所述蒸发容器;The device for evaporating and crystallization further includes a first circulation unit and a second circulation unit. The first circulation unit includes the first branch pipe, the first circulation pump, the first circulation inlet pipe, and the first branch pipe The first circulation pump is connected; the first circulation inlet pipe has a first end and a second end, the first end of the first circulation inlet pipe is connected to the first circulation pump, the first circulation inlet pipe The second end of the is connected to the evaporation container;
所述第二循环单元包括所述第二分管、第二循环泵、加热器及第二循环进管,所述第二分管依次与该第二循环泵、加热器连接,所述第二循环进管具有第三端及第四端,所述第二循环进管的第三端与所述加热器相连,所述第二循环进管的第四端连于所述蒸发容器;The second circulation unit includes the second branch pipe, a second circulation pump, a heater, and a second circulation inlet pipe. The second branch pipe is connected to the second circulation pump and the heater in sequence, and the second circulation inlet The tube has a third end and a fourth end, the third end of the second circulation inlet tube is connected to the heater, and the fourth end of the second circulation inlet tube is connected to the evaporation container;
所述用于蒸发结晶的装置还包括原料液进管,该原料液进管连接至该第二分管,并用于将原料液通过第二循环泵送至所述加热器。The device for evaporating and crystallization further includes a raw material liquid inlet pipe connected to the second branch pipe and used for pumping the raw material liquid to the heater through the second circulation.
所述结晶容器内还设有整流分级器,所述整流分级器包括多个通道,所述通道的下端的尺寸与所述通道的上端的尺寸之比值为1.1:1~10:1。The crystallization vessel is also provided with a rectifier classifier. The rectifier classifier includes a plurality of channels, and the ratio of the size of the lower end of the channel to the size of the upper end of the channel is 1.1: 1 to 10: 1.
所述通道的上端的尺寸为3毫米~100毫米。The size of the upper end of the channel is 3 mm to 100 mm.
所述通道的开孔率为5%~50%。The opening rate of the channel is 5% -50%.
所述蒸发容器的内部靠近所述蒸发气体出口处设有消泡除沫器。A defoamer and defoamer is provided inside the evaporation container near the evaporation gas outlet.
所述蒸发容器的侧壁以及所述结晶容器的侧壁还设有平衡管,所述平衡管连通所述蒸发容器与结晶容器。The side wall of the evaporation container and the side wall of the crystallization container are also provided with a balance tube, and the balance tube communicates the evaporation container and the crystallization container.
本发明还提供所述用于蒸发结晶的装置在连续结晶领域的应用。The invention also provides the application of the device for evaporative crystallization in the field of continuous crystallization.
所述用于蒸发结晶的装置具有以下优点:The device for evaporative crystallization has the following advantages:
由于多股作用力(从所述蒸发容器中而来的流体作用力,由出料带来的作用力,由第一循环泵、第二循环泵带来的作用力)作用下,使得所述结晶容器中结晶液呈湍流状态,能有效避免晶体团聚的发生,使得析出结晶颗粒大小可控;同时,湍流状态更促使了大小晶体的分离,并在第一循环泵、第二循环泵的作用下,使得结晶颗粒中的细晶颗粒循环导入到加热器和蒸发容器中。循环导入到蒸发容器的部分细晶颗粒可作为下一周期结晶的晶核,使得后续结晶颗粒更快析出,且形成大小更均匀的结晶颗粒。Due to multiple forces (fluid force from the evaporation container, force caused by discharge, force caused by the first circulation pump and the second circulation pump), the The crystallization liquid in the crystallization vessel is in a turbulent state, which can effectively avoid the occurrence of crystal agglomeration, making the size of the precipitated crystal particles controllable; at the same time, the turbulent state further promotes the separation of large and small crystals, and plays a role in the first circulation pump and the second circulation pump Next, the fine crystal particles in the crystal particles are circulated and introduced into the heater and the evaporation container. Part of the fine crystal particles that are circulated and introduced into the evaporation vessel can be used as crystal nuclei for the next cycle of crystallization, so that the subsequent crystal particles precipitate faster and form crystal particles of a more uniform size.
所述第二分管中设置加热器,可给予第二循环单元所运送的原料液或第二母液热量,而促使其在蒸发容器中蒸发部分溶剂,更有利于原料液或第二母液在所述结晶容器进行结晶。该装置可实现结晶颗粒的连续形成,结晶效率较高,可适用于工业化生产。A heater is provided in the second branch pipe, which can give the heat of the raw material liquid or the second mother liquid transported by the second circulation unit, and cause it to evaporate part of the solvent in the evaporation container, which is more beneficial to the raw material liquid or the second mother liquid The crystallization vessel performs crystallization. The device can realize the continuous formation of crystalline particles, the crystallization efficiency is high, and it is suitable for industrial production.
进一步,当所述结晶容器内还设有整流分级器时,该整流分级器可梳理结晶容器(不带整流分级器时)中混乱的流场分布,使得整流分级器下方的液流流程长度趋于一致,各股液流流速趋于一致,使流场分布规则有序,促进结晶颗粒更均匀的析出。同时,整流分级器通道内与整流分级器下方形成了流速差,由于整流分级器下方的低流速无力持续夹带较大的结晶颗粒,使得较大的结晶颗粒在被整流分级器下方的低流速流体夹带过程中发生沉淀,而被整流分级器下方液流夹带到整流分级器通道附近的细晶颗粒,则会被整流分级器通道内高流速的液流夹带,并循环导入到加热器中重新加热溶解,和循环导入到蒸发容器中作为晶核。整个过程通过调整通道的开孔率及通道上下尺寸比,就能达到筛选、分离晶体的作用,使得最终得到晶体粒径更加均匀且可控的产品。Further, when a rectifier classifier is also provided in the crystallization vessel, the rectifier classifier can sort out the chaotic flow field distribution in the crystallization vessel (when there is no rectifier classifier), so that the length of the liquid flow process below the rectifier classifier tends In order to be consistent, the flow velocity of each stream tends to be consistent, so that the flow field distribution is regular and orderly, which promotes more uniform precipitation of crystalline particles. At the same time, there is a flow rate difference between the rectifier classifier channel and the rectifier classifier. Because the low flow rate below the rectifier classifier is unable to continuously entrain larger crystalline particles, the larger crystalline particles are in the low-flow fluid under the rectifier classifier. Precipitation occurs during entrainment, and the fine-grained particles entrained by the flow below the rectifier classifier near the channel of the rectifier classifier will be entrained by the high-velocity liquid flow in the channel of the rectifier classifier and recirculated into the heater for reheating Dissolve, and circulate into the evaporation vessel as crystal nuclei. In the whole process, by adjusting the opening ratio of the channel and the ratio of the upper and lower dimensions of the channel, the role of screening and separating crystals can be achieved, so that the final product with more uniform and controllable crystal size can be obtained.
图1为本发明实施例1的用于蒸发结晶的装置的结构示意图。FIG. 1 is a schematic structural diagram of an apparatus for evaporative crystallization according to Embodiment 1 of the present invention.
图2为本发明实施例2的用于蒸发结晶的装置的结构示意图。FIG. 2 is a schematic structural diagram of an apparatus for evaporative crystallization according to Embodiment 2 of the present invention.
图3为图2用于蒸发结晶的装置中的整流分级器的结构示意图。3 is a schematic structural view of a rectifier and classifier in the device for evaporative crystallization of FIG. 2.
其中,1、原料液进管;2a、第一分管;2b、第二分管;3、第二循环泵;4、加热器;5、第二循环进管;6、蒸发容器;7、导流管;8、结晶容器;9、消泡除沫器;10、蒸发气体出口;11、平衡管;12、循环物料出管;13、第一循环泵;14、第一循环进管;15、晶浆出料口;16、离心机;17、整流分级器;18、通道。Among them, 1. raw material liquid inlet pipe; 2a, first branch pipe; 2b, second branch pipe; 3. second circulation pump; 4. heater; 5. second circulation inlet pipe; 6. evaporation vessel; 7. diversion Pipe; 8. Crystallization vessel; 9. Defoaming and demister; 10. Evaporation gas outlet; 11. Balance pipe; 12. Circulation material outlet pipe; 13. First circulation pump; 14. First circulation inlet pipe; 15. Crystal slurry discharge port; 16, centrifuge; 17, rectifier classifier; 18, channel.
下面将对本发明实施方式中的技术方案进行清楚、完整地描述,显然,所描述的实施方式仅仅是本发明一部分实施方式,而不是全部的实施方式。基于本发明中的实施方式,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施方式,都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are only a part of the embodiments of the present invention, but not all the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person of ordinary skill in the art without making creative efforts fall within the protection scope of the present invention.
请参阅图1,本发明实施例1提供一种用于蒸发结晶的装置。所述用于蒸发结晶的装置包括蒸发容器6、结晶容器8,结晶容器8位于蒸发容器6的下方,蒸发容器6用于将溶剂蒸发,结晶容器8用于结晶,蒸发容器6的顶部设置有蒸发气体出口10,蒸发容器6的底部设置导流管7,导流管7伸至结晶容器8内,并与结晶容器8相连通,结晶容器8的侧壁连有循环物料出管12,循环物料出管12分叉成第一分管2a和第二分管2b。Please refer to FIG. 1, Embodiment 1 of the present invention provides an apparatus for evaporative crystallization. The device for evaporating and crystallization includes an evaporating container 6 and a crystallization container 8. The crystallization container 8 is located below the evaporating container 6. The evaporating container 6 is used to evaporate the solvent, and the crystallization container 8 is used for crystallization. The top of the evaporating container 6 is provided with The evaporation gas outlet 10, the bottom of the evaporation container 6 is provided with a guide tube 7, the guide tube 7 extends into the crystallization container 8 and communicates with the crystallization container 8, and the side wall of the crystallization container 8 is connected with a circulating material outlet tube 12, circulating The material outlet pipe 12 branches into a first branch pipe 2a and a second branch pipe 2b.
所述用于蒸发结晶的还包括第一循环单元及第二循环单元,第一循环单元包括第一分管2a、第一循环泵13、第一循环进管14,第一分管2a与第一循环泵13连接,第一循环进管14具有第一端及第二端,第一循环进管14的第一端与第一循环泵13相连,第一循环进管14的第二端连于蒸发容器6。The evaporative crystallization also includes a first circulation unit and a second circulation unit, the first circulation unit includes a first branch 2a, a first circulation pump 13, a first circulation inlet pipe 14, the first branch 2a and the first circulation The pump 13 is connected, and the first circulation inlet pipe 14 has a first end and a second end. The first end of the first circulation inlet pipe 14 is connected to the first circulation pump 13, and the second end of the first circulation inlet pipe 14 is connected to the evaporation Container 6.
第二循环单元包括所述第二分管2b、第二循环泵3、加热器4及第二循环进管5,第二分管2b依次与第二循环泵3、加热器4连接,第二循环进管5具有第三端及第四端,第二循环进管5的第三端与所述加热器4相连,第二循环进管5的第四端连于蒸发容器6。The second circulation unit includes the second branch pipe 2b, the second circulation pump 3, the heater 4 and the second circulation inlet pipe 5. The second branch pipe 2b is connected to the second circulation pump 3 and the heater 4 in sequence, and the second circulation inlet The tube 5 has a third end and a fourth end. The third end of the second circulation inlet 5 is connected to the heater 4, and the fourth end of the second circulation inlet 5 is connected to the evaporation container 6.
所述用于蒸发结晶的装置还包括原料液进管1,原料液进管1连接至该第二分管2b,并用于将原料液通过第二循环泵3送至加热器4。The device for evaporating and crystallization further includes a raw material liquid inlet pipe 1, which is connected to the second branch pipe 2b, and is used to send the raw material liquid to the heater 4 through the second circulation pump 3.
所述结晶容器8与蒸发容器6之外有两个循环回路。第一个循环回路(对应第一循环单元)为:结晶容器8、循环物料出管12、第一分管2a、第一循环泵13、第一循环进管14、蒸发容器6;第二个循环回路(对应第二循环单元)为:结晶容器8、循环物料出管12、第二分管2b、第二循环泵3、加热器4、第二循环进管5、蒸发容器6。其中,第二分管2b也 承担着与原料液进管1连接,而将原料液持续引入第二循环回路的作用。There are two circulation circuits outside the crystallization vessel 8 and the evaporation vessel 6. The first circulation circuit (corresponding to the first circulation unit) is: crystallization vessel 8, circulation material outlet pipe 12, first branch pipe 2a, first circulation pump 13, first circulation inlet pipe 14, evaporation vessel 6; second circulation The circuit (corresponding to the second circulation unit) is: a crystallization vessel 8, a circulation material outlet pipe 12, a second branch pipe 2b, a second circulation pump 3, a heater 4, a second circulation inlet pipe 5, and an evaporation vessel 6. Among them, the second branch 2b is also responsible for connecting to the raw material liquid inlet pipe 1 and continuously introducing the raw material liquid into the second circulation circuit.
该第一循环回路用于将结晶容器8内的部分母液(定义为第一母液)以及结晶得到的部分细晶颗粒(定义为第一细晶)直接引至蒸发容器6,该部分的细晶颗粒可作为下一周期的结晶晶核,从而会诱导得到更均匀的结晶颗粒。需要说明的是,该第一细晶可继续长大得到更大及更均匀的结晶颗粒,同时,第一细晶重新进入结晶容器8也会诱导更多的结晶颗粒有序地形成,也就是说,该第一循环回路的效果分为两个方面:一是使得数量更多的结晶颗粒形成;二是使得细晶颗粒生长为均匀的结晶颗粒。The first circulation circuit is used to lead part of the mother liquor (defined as the first mother liquor) in the crystallization container 8 and part of the fine crystal particles (defined as the first fine crystal) obtained by the crystallization directly to the evaporation vessel 6, the part of the fine crystals The particles can be used as crystal nuclei in the next cycle, which will induce more uniform crystal particles. It should be noted that the first fine crystals can continue to grow to obtain larger and more uniform crystalline particles. At the same time, the re-entry of the first fine crystals into the crystallization container 8 will also induce more crystalline particles to form orderly, that is, That is to say, the effect of the first circulation circuit is divided into two aspects: one is to make a larger number of crystalline particles formed; the other is to make fine-crystalline particles grow into uniform crystalline particles.
该第二循环回路用于将结晶容器8内的另一部分母液(定义为第二母液)及结晶得到的另一部分细晶颗粒(定义为第二细晶)经过加热器4的作用进入蒸发容器6,溶剂蒸发后,进入结晶容器8而进行下一周期的结晶。The second circulation circuit is used to pass another part of the mother liquid (defined as the second mother liquid) in the crystallization container 8 and another part of the fine crystal particles (defined as the second fine crystal) obtained by crystallization into the evaporation container 6 through the action of the heater 4 After the solvent evaporates, it enters the crystallization vessel 8 to perform the next cycle of crystallization.
所述蒸发容器6通常无需额外的加热,由所述第二循环进管5流入的原料液或者第二母液在经过加热器4的加热之后,其温度均会上升,因此,原料液或者第二母液会在所述蒸发容器6内蒸发掉部分的溶剂。为了避免溶剂蒸发过程中产生的泡沫夹带走部分的产品,造成收率损失,在蒸发容器6的内部靠近蒸发气体出口10处设有消泡除沫器9,消泡除沫器9可为筛网结构或者其它类型的消泡除沫器。The evaporation vessel 6 generally does not require additional heating. The temperature of the raw material liquid or the second mother liquid flowing from the second circulation inlet 5 after being heated by the heater 4 will increase. Therefore, the raw material liquid or the second The mother liquor evaporates part of the solvent in the evaporation container 6. In order to avoid that the foam generated during the evaporation of the solvent entrains part of the product and causes loss of yield, a defoaming and defoaming device 9 is provided near the evaporation gas outlet 10 inside the evaporation container 6, and the defoaming and defoaming device 9 can be Screen structure or other types of defoamer and demister.
所述蒸发容器6的侧壁以及结晶容器8的侧壁还设有平衡管11,平衡管11连通蒸发容器6与结晶容器8。The side wall of the evaporation container 6 and the side wall of the crystallization container 8 are also provided with a balance tube 11, which connects the evaporation container 6 and the crystallization container 8.
所述结晶容器8的底部设有晶浆出料口15。The bottom of the crystallization container 8 is provided with a crystal slurry discharge port 15.
请参阅图2,本发明实施例2提供一种用于蒸发结晶的装置。该用于蒸发结晶的装置与实施例1的用于蒸发结晶的装置的结构基本相同,其区别在于:在结晶容器8内设整流分级器17。请参阅图3,所述整流分级器17包括多个通道18。所述整流分级器17的作用为得到更均匀的结晶颗粒。Please refer to FIG. 2, Embodiment 2 of the present invention provides an apparatus for evaporative crystallization. The device for evaporative crystallization is basically the same in structure as the device for evaporative crystallization of Embodiment 1, except that a rectifier and classifier 17 is provided in the crystallization vessel 8. Referring to FIG. 3, the rectifier classifier 17 includes multiple channels 18. The function of the rectifier classifier 17 is to obtain more uniform crystalline particles.
所述通道18的下端的尺寸大于所述通道18的上端的尺寸的设计目的有两个方面:(1)防止颗粒“返混”现象的发生;(2)避免了通道18堵塞的可能。所述通道18的轴截面可以为但不限于梯形、碗形、水滴形。The design purpose of the size of the lower end of the channel 18 is greater than the size of the upper end of the channel 18 has two aspects: (1) to prevent the phenomenon of "backmixing" of particles; (2) to avoid the possibility of the channel 18 being blocked. The axial section of the channel 18 may be, but not limited to, trapezoidal, bowl-shaped, or drop-shaped.
所述通道18的下端的尺寸与所述通道18的上端的尺寸之比值为1.1:1~10:1,优选的,所述通道18的下端的尺寸与所述通道18的上端的尺寸之比值为1.5:1~5:1。The ratio of the size of the lower end of the channel 18 to the size of the upper end of the channel 18 is 1.1: 1 to 10: 1. Preferably, the ratio of the size of the lower end of the channel 18 to the size of the upper end of the channel 18 It is 1.5: 1 ~ 5: 1.
所述通道18的上端的尺寸为3毫米~100毫米,优选为5毫米~50毫米。The size of the upper end of the channel 18 is 3 mm to 100 mm, preferably 5 mm to 50 mm.
多个所述通道18的开孔率(即,通道的上端的面积之和占所述整流分级器的上表面的面积的百分数)为5%~50%,优选为10%~30%。The aperture ratio of the plurality of channels 18 (that is, the sum of the area of the upper ends of the channels as a percentage of the area of the upper surface of the rectifier classifier) is 5% to 50%, preferably 10% to 30%.
所述用于蒸发结晶的装置具有以下优点:The device for evaporative crystallization has the following advantages:
所述蒸发容器6用于蒸发原料液中的溶剂,结晶容器8用于结晶,通过将循环物料出管12分叉成第一分管2a和第二分管2b,第一分管2a用于将原料液结晶形成的结晶颗粒中的细晶颗粒重新导至蒸发容器6内,该细晶颗粒可作为下一周期结晶的晶核,从而诱导更多以及更均匀的结晶颗粒形成;所述第二分管2b中设置加热器4,可给予原料液或第二母液热量,而在蒸发容器6中溶剂部分蒸发,更有利于原料液或第二母液在所述结晶容器8进行结晶。The evaporation container 6 is used to evaporate the solvent in the raw material liquid, and the crystallization container 8 is used for crystallization. By forking the circulating material outlet pipe 12 into a first branch pipe 2a and a second branch pipe 2b, the first branch pipe 2a is used to transform the raw material liquid The fine crystal particles in the crystal particles formed by the crystallization are redirected into the evaporation container 6, and the fine crystal particles can be used as crystal nuclei for the next cycle of crystallization, thereby inducing more and more uniform crystal particles to form; the second branch 2b The heater 4 is provided to give heat to the raw material liquid or the second mother liquid, and the partial evaporation of the solvent in the evaporation container 6 is more conducive to the crystallization of the raw material liquid or the second mother liquid in the crystallization container 8.
该装置可用于晶粒的连续形成。特别地,适用于维生素B6、己糖酸、三氯蔗糖、乙基麦芽酚、甲硫氨酸、古龙酸、柠檬酸、苏氨酸、色氨酸、葡萄糖酸钠、葡萄糖、谷氨酸、赖氨酸或山梨醇的蒸发结晶过程。The device can be used for the continuous formation of grains. In particular, it is suitable for vitamin B6, hexonic acid, sucralose, ethyl maltol, methionine, gulonic acid, citric acid, threonine, tryptophan, sodium gluconate, glucose, glutamic acid, Evaporative crystallization of lysine or sorbitol.
以上所述实施例的各技术特征可以进行任意的组合,为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。The technical features of the above-mentioned embodiments can be combined arbitrarily. To simplify the description, all possible combinations of the technical features in the above-mentioned embodiments are not described. However, as long as there is no contradiction in the combination of these technical features, All should be considered within the scope of this description.
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。The above-mentioned embodiments only express several embodiments of the present invention, and their descriptions are more specific and detailed, but they should not be construed as limiting the scope of the invention patent. It should be noted that, for a person of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can also be made, which all fall within the protection scope of the present invention. Therefore, the protection scope of the invention patent shall be subject to the appended claims.
Claims (7)
- 一种用于蒸发结晶的装置,其包括:A device for evaporative crystallization, including:蒸发容器(6),所述蒸发容器(6)用于将溶剂蒸发,所述蒸发容器(6)的底部设置导流管(7),所述蒸发容器(6)的顶部还设置有蒸发气体出口(10);An evaporation container (6) is used to evaporate the solvent, a guide tube (7) is provided at the bottom of the evaporation container (6), and an evaporation gas is also provided at the top of the evaporation container (6) Export (10);结晶容器(8),所述结晶容器(8)用于结晶,所述结晶容器(8)位于所述蒸发容器(6)的下方,所述导流管(7)伸至所述结晶容器(8)内,并与结晶容器(8)相连通,所述结晶容器(8)的底部设有晶浆出料口(15);其特征在于,A crystallization container (8), the crystallization container (8) is used for crystallization, the crystallization container (8) is located below the evaporation container (6), and the guide tube (7) extends to the crystallization container (8) 8) inside and communicate with the crystallization container (8), the bottom of the crystallization container (8) is provided with a crystal slurry discharge port (15);所述结晶容器(8)的侧壁连有循环物料出管(12),所述循环物料出管(12)分叉成第一分管(2a)和第二分管(2b);A circulating material outlet pipe (12) is connected to the side wall of the crystallization container (8), and the circulating material outlet pipe (12) branches into a first branch pipe (2a) and a second branch pipe (2b);所述用于蒸发结晶的装置还包括第一循环单元及第二循环单元,所述第一循环单元包括所述第一分管(2a)、第一循环泵(13)、第一循环进管(14),所述第一分管(2a)与该第一循环泵(13)连接;所述第一循环进管(14)具有第一端及第二端,所述第一循环进管(14)的第一端与所述第一循环泵(13)相连,所述第一循环进管(14)的第二端连于所述蒸发容器(6);The device for evaporative crystallization also includes a first circulation unit and a second circulation unit, the first circulation unit includes the first branch (2a), a first circulation pump (13), and a first circulation inlet ( 14), the first branch pipe (2a) is connected to the first circulation pump (13); the first circulation inlet pipe (14) has a first end and a second end, and the first circulation inlet pipe (14) ) Has a first end connected to the first circulation pump (13), and a second end of the first circulation inlet pipe (14) is connected to the evaporation vessel (6);所述第二循环单元包括所述第二分管(2b)、第二循环泵(3)、加热器(4)及第二循环进管(5),所述第二分管(2b)依次与该第二循环泵(3)、加热器(4)连接,所述第二循环进管(5)具有第三端及第四端,所述第二循环进管(5)的第三端与所述加热器(4)相连,所述第二循环进管(5)的第四端连于所述蒸发容器(6);The second circulation unit includes the second branch pipe (2b), a second circulation pump (3), a heater (4) and a second circulation inlet pipe (5). The second branch pipe (2b) is A second circulation pump (3) and a heater (4) are connected, the second circulation inlet pipe (5) has a third end and a fourth end, and the third end of the second circulation inlet pipe (5) is connected to all The heater (4) is connected, and the fourth end of the second circulation inlet tube (5) is connected to the evaporation container (6);所述用于蒸发结晶的装置还包括原料液进管(1),该原料液进管(1)连接至该第二分管(2b),并用于将原料液通过第二循环泵(3)送至所述加热器(4)。The device for evaporating and crystallization further includes a raw material liquid inlet pipe (1), the raw material liquid inlet pipe (1) is connected to the second branch pipe (2b), and is used to send the raw material liquid through the second circulation pump (3) To the heater (4).
- 如权利要求1所述的用于蒸发结晶的装置,其特征在于,所述结晶容器(8)内还设有整流分级器(17),所述整流分级器(17)包括多个通道(18),所述通道(18)的下端的尺寸与所述通道(18)的上端的尺寸之比值为1.1:1~10:1。The device for evaporative crystallization according to claim 1, characterized in that a rectifying classifier (17) is further provided in the crystallization vessel (8), and the rectifying classifier (17) includes a plurality of channels (18) ), The ratio of the size of the lower end of the channel (18) to the size of the upper end of the channel (18) is 1.1: 1 to 10: 1.
- 如权利要求2所述的用于蒸发结晶的装置,其特征在于,所述通道(18)的上端的尺寸为3毫米~100毫米。The device for evaporative crystallization according to claim 2, characterized in that the size of the upper end of the channel (18) is 3 mm to 100 mm.
- 如权利要求2所述的用于蒸发结晶的装置,其特征在于,所述通道(18)的开孔率为5%~50%。The device for evaporative crystallization according to claim 2, characterized in that the opening rate of the channel (18) is 5% to 50%.
- 如权利要求1所述的用于蒸发结晶的装置,其特征在于,所述蒸发容器(6)的内部靠近所述蒸发气体出口(10)处设有消泡除沫器(9)。The device for evaporative crystallization according to claim 1, characterized in that a defoamer and defoamer (9) is provided inside the evaporation container (6) near the evaporation gas outlet (10).
- 如权利要求1所述的用于蒸发结晶的装置,其特征在于,所述蒸发容器(6)的侧壁以及所述结晶容器(8)的侧壁还设有平衡管(11),所述平衡管(11)连通所述蒸发容器(6)与结晶容器(8)。The device for evaporative crystallization according to claim 1, characterized in that a side wall of the evaporation container (6) and the side wall of the crystallization container (8) are further provided with a balance tube (11), The balance tube (11) communicates the evaporation container (6) and the crystallization container (8).
- 如权利要求1-6中任一项所述的用于蒸发结晶的装置在连续结晶领域的应用。The application of the evaporative crystallization device according to any one of claims 1 to 6 in the field of continuous crystallization.
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CN109173329A (en) * | 2018-10-31 | 2019-01-11 | 浙江新和成股份有限公司 | Device for evaporative crystallization |
CN209286707U (en) * | 2018-10-31 | 2019-08-23 | 浙江新和成股份有限公司 | Device for evaporative crystallization |
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2019
- 2019-10-22 DE DE112019001119.7T patent/DE112019001119T5/en active Granted
- 2019-10-22 WO PCT/CN2019/112400 patent/WO2020088294A1/en active Application Filing
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CN116271944A (en) * | 2023-05-23 | 2023-06-23 | 山东冠森高分子材料科技股份有限公司 | Continuity paranitrophenol sodium crystallization device |
CN116271944B (en) * | 2023-05-23 | 2023-07-21 | 山东冠森高分子材料科技股份有限公司 | Continuity paranitrophenol sodium crystallization device |
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