WO2020088294A1 - Dispositif d'évaporation et de cristallisation - Google Patents

Dispositif d'évaporation et de cristallisation Download PDF

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Publication number
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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WO
WIPO (PCT)
Prior art keywords
crystallization
container
circulation
evaporation
inlet pipe
Prior art date
Application number
PCT/CN2019/112400
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English (en)
Chinese (zh)
Inventor
陈志荣
刘金龙
邱贵生
王志轩
马啸
周有桂
陈卫勇
刘晓庆
Original Assignee
浙江新和成股份有限公司
浙江大学
山东新和成氨基酸有限公司
山东新和成精化科技有限公司
山东新和成药业有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from CN201821784240.5U external-priority patent/CN209286707U/zh
Priority claimed from CN201811291575.8A external-priority patent/CN109173329B/zh
Application filed by 浙江新和成股份有限公司, 浙江大学, 山东新和成氨基酸有限公司, 山东新和成精化科技有限公司, 山东新和成药业有限公司 filed Critical 浙江新和成股份有限公司
Priority to DE112019001119.7T priority Critical patent/DE112019001119T5/de
Publication of WO2020088294A1 publication Critical patent/WO2020088294A1/fr

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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
    • 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

Definitions

  • 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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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

La présente invention concerne un dispositif utilisé pour l'évaporation et la cristallisation. Le dispositif comprend un récipient d'évaporation et un récipient de cristallisation. Le dispositif utilisé pour l'évaporation et la cristallisation comprend en outre une première unité de circulation et une seconde unité de circulation. La première unité de circulation comprend un premier tuyau de dérivation, une première pompe de circulation et un premier tuyau d'entrée de circulation qui sont connectés successivement. La seconde unité de circulation comprend un second tuyau de dérivation, une seconde pompe de circulation, un dispositif de chauffage et un second tuyau d'entrée de circulation qui sont connectés successivement. Le premier tuyau d'entrée de circulation et le second tuyau d'entrée de circulation sont reliés au récipient d'évaporation. Au moyen de la fourniture d'une première boucle de circulation supplémentaire, une partie de cristaux fins est réintroduite dans le récipient de cristallisation sous la forme d'un noyau cristallin, et un produit qui a des particules plus uniformes et une taille de particule contrôlable est finalement obtenu.
PCT/CN2019/112400 2018-10-31 2019-10-22 Dispositif d'évaporation et de cristallisation WO2020088294A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE112019001119.7T DE112019001119T5 (de) 2018-10-31 2019-10-22 Vorrichtung zur Verdampfungskristallisation

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
CN201821784240.5 2018-10-31
CN201811291575.8 2018-10-31
CN201821784240.5U CN209286707U (zh) 2018-10-31 2018-10-31 用于蒸发结晶的装置
CN201811291575.8A CN109173329B (zh) 2018-10-31 2018-10-31 用于蒸发结晶的装置

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Publication Number Publication Date
WO2020088294A1 true WO2020088294A1 (fr) 2020-05-07

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DE (1) DE112019001119T5 (fr)
WO (1) WO2020088294A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116271944A (zh) * 2023-05-23 2023-06-23 山东冠森高分子材料科技股份有限公司 一种连续性对硝基苯酚钠结晶装置

Citations (7)

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Publication number Priority date Publication date Assignee Title
SU1457200A1 (ru) * 1987-04-23 1996-06-10 В.Ц. Гонионский Кристаллизатор
CN202951276U (zh) * 2012-10-31 2013-05-29 天津中科化工有限公司 一种节能蒸发结晶器
CN204447382U (zh) * 2015-02-11 2015-07-08 张诗山 新型粒度分级型结晶器
CN205796596U (zh) * 2016-05-22 2016-12-14 泉州金翊科技有限公司 一种太阳能加热蒸发结晶器
CN206793092U (zh) * 2017-06-06 2017-12-26 南昌金轩科技有限公司 一种用于回收醋酸钠的连续蒸发结晶装置
CN109173329A (zh) * 2018-10-31 2019-01-11 浙江新和成股份有限公司 用于蒸发结晶的装置
CN209286707U (zh) * 2018-10-31 2019-08-23 浙江新和成股份有限公司 用于蒸发结晶的装置

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1457200A1 (ru) * 1987-04-23 1996-06-10 В.Ц. Гонионский Кристаллизатор
CN202951276U (zh) * 2012-10-31 2013-05-29 天津中科化工有限公司 一种节能蒸发结晶器
CN204447382U (zh) * 2015-02-11 2015-07-08 张诗山 新型粒度分级型结晶器
CN205796596U (zh) * 2016-05-22 2016-12-14 泉州金翊科技有限公司 一种太阳能加热蒸发结晶器
CN206793092U (zh) * 2017-06-06 2017-12-26 南昌金轩科技有限公司 一种用于回收醋酸钠的连续蒸发结晶装置
CN109173329A (zh) * 2018-10-31 2019-01-11 浙江新和成股份有限公司 用于蒸发结晶的装置
CN209286707U (zh) * 2018-10-31 2019-08-23 浙江新和成股份有限公司 用于蒸发结晶的装置

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116271944A (zh) * 2023-05-23 2023-06-23 山东冠森高分子材料科技股份有限公司 一种连续性对硝基苯酚钠结晶装置
CN116271944B (zh) * 2023-05-23 2023-07-21 山东冠森高分子材料科技股份有限公司 一种连续性对硝基苯酚钠结晶装置

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