CN205323272U - Multistage crystallization system - Google Patents

Multistage crystallization system Download PDF

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Publication number
CN205323272U
CN205323272U CN201521126270.3U CN201521126270U CN205323272U CN 205323272 U CN205323272 U CN 205323272U CN 201521126270 U CN201521126270 U CN 201521126270U CN 205323272 U CN205323272 U CN 205323272U
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CN
China
Prior art keywords
crystallization
conveyance conduit
crystallized product
multistage
crystallization kettle
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Legal status (The legal status 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 status listed.)
Expired - Fee Related
Application number
CN201521126270.3U
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Chinese (zh)
Inventor
赖安平
郭静威
吴朝刚
蒋小军
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Apeloa Home Pharmaceutical Co.,Ltd.
Original Assignee
PULUO MEDICINES TECH Co Ltd ZHEJIANG
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Application filed by PULUO MEDICINES TECH Co Ltd ZHEJIANG filed Critical PULUO MEDICINES TECH Co Ltd ZHEJIANG
Priority to CN201521126270.3U priority Critical patent/CN205323272U/en
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Publication of CN205323272U publication Critical patent/CN205323272U/en
Expired - Fee Related legal-status Critical Current
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  • Heterocyclic Carbon Compounds Containing A Hetero Ring Having Nitrogen And Oxygen As The Only Ring Hetero Atoms (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The utility model discloses a multistage crystallization system, including the crystallization kettle that a plurality of is established ties in proper order, the intercommunication has mother liquor pipeline and crystallized product pipeline between two adjacent crystallization kettles, wherein, the material flow direction among the mother liquor pipeline is unanimous, and the material flow direction among mother liquor pipeline and the crystallized product pipeline is opposite. Adopt the utility model discloses a multistage crystallization system can realize crystallization many times in succession, can improve crystallized product 's purity more effectively to improve crystallized product 's yield.

Description

A kind of multistage crystallization system
Technical field
This utility model belongs to field of chemical equipment, is specifically related to a kind of reactor for heterogeneous reaction。
Background technology
The process that crystal is formed in the solution is called crystallization。The method of crystallization generally has 2 kinds: one is evaporation solvent method, and it is applicable to the material that temperature is little on dissolubility impact。Coastal area " evaporate brine " be exactly utilize this method。Another kind is to cool down hot saturated solution method。This method is applicable to temperature and raises, the material that dissolubility also increases。Such as the salt lake of northern area, summer temperature is high, and lake surface occurs without crystal;In every winter, temperature reduces, alkalium (Na2CO3·10H2O), Natrii Sulfas (Na2SO4·10H2Etc. O) material just separates out from salt lake。Under lab for obtaining bigger perfect crystal, normal use slowly reduces temperature, the method for the crystalline rate that slows down。
Crystallization operation to use special crystallization apparatus, the Chinese patent application that publication number is CN203561889U discloses a kind of crystallization apparatus with fluid level control device, including crystallization kettle and U-tube, it is provided with tapping valve bottom described crystallization kettle, described tapping valve lower end connects the conveying pipe of a transverse direction, and described conveying pipe one end is provided with urgent tapping valve, and the described conveying pipe other end connects U-tube, described U-tube is connected with discharging tube, and described U-tube top is provided with idle discharge pipe。This crystallization apparatus utilizes U-tube to realize crystallization kettle high liquid level automatic liquid-drainage function, eliminates manual operation, saves human resources, and improves the stability of liquid in crystallization kettle。
In pharmaceutical synthesis, the crude product obtained often contains a certain amount of impurity, it is necessary to just can obtain purer active substance through a series of purification。Crystallization operation is high owing to being easy to batch operation and the product purity that obtains, is one of modal operation in purifying after medicine, and substantially the medicine of more than 90% finally will experience crystallization operation and just can obtain purer product。
Complexity due to organic synthesis, the medicine obtained often contains more impurity, simultaneously, medicine to directly apply to human body, and impurity content has stricter requirement, is difficult to obtain gratifying product by single crystallization, generally require and just can obtain qualified product through repeatedly recrystallization, but directly adopting existing crystallizer that crystallization operation is repeated, process is comparatively laborious, and resource utilization is relatively low。
Utility model content
This utility model provides a kind of multistage crystallization system, and this multistage crystallization system can realize continuous crystallisation operation, it is possible to obtains high purity product easily。
A kind of multistage crystallization system, including several crystallization kettles being sequentially connected in series, is communicated with mother solution conveyance conduit and crystallized product conveyance conduit between adjacent two crystallization kettles;
Wherein, the flow direction of material in mother solution conveyance conduit is consistent, and mother solution conveyance conduit and the flow direction of material in crystallized product conveyance conduit are contrary。
In this multistage crystallization system, being joined by solution to be crystallized in certain one-level crystallization kettle middle and carry out crystallization, the crystalline mother solution obtained is input in next stage crystallization kettle through mother solution conveyance conduit and concentrates, it is possible to make target product farthest precipitate out;The crystallized product simultaneously obtained is input in upper level crystallization kettle and carries out secondary crystallization, it is possible to increase the purity of crystallized product, adopts this kind of mode can be effectively realized multistage crystallization process。
In order to prevent crystallized product from entering mother solution conveyance conduit, as preferably, the input port of mother solution conveyance conduit is provided with screen plate。
As preferably, the sidewall of described crystallization kettle is provided with Heat exchange jacekt, and the top of described crystallization kettle is provided with steam output pipe;
Steam output pipe is sequentially communicated condenser and collects the recycling can of solvent。In time needing the solution in crystallization kettle is concentrated, it is possible to input adds thermal medium in this Heat exchange jacekt, and meanwhile, the solvent of evaporation enters condenser through steam conveying pipe, after condensation, enter recycling can within the condenser;Carry out in process in crystallization, it is possible in this Heat exchange jacekt, pass into cooling medium, accelerate the precipitation process of product。
In order to improve evaporation efficiency, as further preferably, steam output pipe is with open entrance, and its diameter is gradually increased from top to bottom。
As preferably, the top of described crystallization kettle is cylindrical shape, and bottom is hollow rounding mesa-shaped, offering mother liquor outlet on the sidewall of bottom, be provided with crystallized product outlet in bottom, crystallization kettle adopts this kind of shape, crystallized product can be made to be enriched in bottom better, it is simple to collect and transfer。
As preferably, the sidewall of described crystallization kettle is provided with feed pipe, and the lower end of described feed pipe passes into the latter half of crystallization kettle, at this point it is possible to make reinforced process more successfully carry out, and can avoid in evaporation process, and solvent enters feeding tube。
Compared with the existing technology, the beneficial effects of the utility model are embodied in: adopt multistage crystallization system of the present utility model, repeatedly crystallization can be realized continuously, can more effectively improve the purity of crystallized product, and improve the yield of crystallized product, meanwhile, by the recycling to solvent, improve the utilization ratio of solvent。
Accompanying drawing explanation
Fig. 1 is the structural representation of multistage crystallization system of the present utility model;
Fig. 2 is the structural representation of the crystallization kettle adopted in the multistage crystallization system shown in Fig. 1;In figure, 1: mother solution conveyance conduit;2: crystallized product conveyance conduit;3: screen plate;4: Heat exchange jacekt;5: steam output pipe;6: recycling can;7: crystallized product exports;8: feed pipe;Arrow represents the flow direction of material。
Detailed description of the invention
Below in conjunction with accompanying drawing, multistage crystallization system of the present utility model is further described。
The schematic diagram of multistage crystallization system as shown in Figure 1, it can be seen that this multistage crystallization system includes three crystallization kettles being sequentially connected in series, is communicated with two material conveying pipes between adjacent two crystallization kettles, respectively mother solution conveyance conduit 1 and crystallized product conveyance conduit 2。
Wherein, mother solution conveyance conduit 1 is used for the mother solution after carrying crystallization, and its material transferring direction is crystallization kettle A-crystallization kettle B-crystallization kettle C, and crystallized product conveyance conduit 2 is used for the product after carrying crystallization, and its material transferring direction is crystallization kettle C-crystallization kettle B-crystallization kettle A。
In order to prevent crystallized product from entering mother solution conveyance conduit 1, it is provided with screen plate 3 in the input port of mother solution conveyance conduit 1。
The structural representation of crystallization kettle as shown in Figure 2 is known, the sidewall of this crystallization kettle is provided with the Heat exchange jacekt 4 for evaporating solvent, this Heat exchange jacekt 4 can pass into as required and add thermal medium or cooling medium, before carrying out crystallization, first pass into and add thermal medium evaporation section solvent and make solution concentrate, improve saturation;Then passing into cooling medium when crystallization is that solid is easier to crystallize out。
It is provided with steam output pipe 5 at the top of crystallization kettle, steam output pipe 5 is sequentially communicated condenser and collects the recycling can 6 of solvent, the solvent being evaporated is collected in recycling can 6, then inputs adjacent crystallization kettle with crystallized product together, carries out secondary crystallization process。
Steam output pipe 5 is with open entrance, and its diameter is gradually increased from top to bottom, so can be effectively improved evaporation efficiency。
The top of crystallization kettle is cylindrical shape, bottom is hollow rounding mesa-shaped, rounding mesa-shaped can make crystallized product be enriched in bottom effectively, the sidewall of bottom offers mother liquor outlet, crystallized product outlet 7 it is provided with in bottom, crystallized product outlet 7 is arranged on bottom can make crystal be easier to transfer, and the crystallized product of residual can use the solvent in recycling can 6 to carry out solution transfer。
Sidewall at crystallization kettle is provided with feed pipe 8, the lower end of described feed pipe 8 passes into the latter half of crystallization kettle, can be effectively prevented in evaporation process solvent and enter feed pipe 8, the entrance of feed pipe 8 is connected with recycling can 6, crystallized product transfer passage and mother solution conveyance conduit 1 independently, adds corresponding material as required。
For the multistage crystallization system shown in Fig. 1, work process is as follows: first from the feed pipe 8 of crystallization kettle B, solution to be crystallized is joined crystallization kettle B, then pass in the heat exchange jacket of crystallization kettle B and add thermal medium, treat crystallization solution and be evaporated concentration, the solvent evaporated enters the recycling can 6 of crystallization kettle B, when crystallization solution is concentrated into a certain degree, then passes into cooling medium in the heat exchange jacket of crystallization kettle B, make solid crystal out, complete first time crystallization process;Then crystalline mother solution is squeezed into crystallization kettle C from mother solution conveyance conduit 1, crystallized product is exported 7 from the crystallized product of bottom and is transferred to crystallization kettle A, the solvent collected in recycling can 6 is joined in crystallization kettle A simultaneously and crystallized product is dissolved, then in the heat exchange jacket of crystallization kettle A, cooling medium is passed into, product is carried out secondary crystallization, and the crystallized product obtained is derived from the product exit of crystallization kettle A;Meanwhile, passing into and add thermal medium, crystalline mother solution therein is concentrated in the heat exchange jacket of crystallization kettle C, solvent enters the recycling can 6 of crystallization kettle C, then passes into cooling medium again and carries out crystallization, and crystallized product returns crystallization kettle B, and crystalline mother solution is as waste collection。
In this utility model, the material mode of movement in conveyance conduit is state of the art, for instance, it is possible to adopt common feeding engine;Can arranging valve on each pipeline as required, those skilled in the art can select according to general knowledge。
The technical solution of the utility model and beneficial effect have been described in detail by above-described detailed description of the invention; it it should be understood that and the foregoing is only most preferred embodiment of the present utility model; it is not limited to this utility model; all make in spirit of the present utility model any amendment, supplement and equivalent replacement etc., should be included within protection domain of the present utility model。

Claims (6)

1. a multistage crystallization system, it is characterised in that include several crystallization kettles being sequentially connected in series, be communicated with mother solution conveyance conduit (1) and crystallized product conveyance conduit (2) between adjacent two crystallization kettles;
Wherein, the flow direction of material in mother solution conveyance conduit (1) is consistent, and mother solution conveyance conduit (1) and the flow direction of material in crystallized product conveyance conduit (2) are contrary。
2. multistage crystallization system according to claim 1, it is characterised in that the input port of mother solution conveyance conduit (1) is provided with screen plate (3)。
3. multistage crystallization system according to claim 1, it is characterised in that the sidewall of described crystallization kettle is provided with Heat exchange jacekt (4), the top of described crystallization kettle is provided with steam output pipe (5);
Steam output pipe (5) is sequentially communicated condenser and collects the recycling can (6) of solvent。
4. multistage crystallization system according to claim 3, it is characterised in that steam output pipe (5) is with open entrance, and its diameter is gradually increased from top to bottom。
5. multistage crystallization system according to claim 1, it is characterised in that the top of described crystallization kettle is cylindrical shape, bottom is hollow rounding mesa-shaped, offers mother liquor outlet on the sidewall of bottom, is provided with crystallized product outlet (7) in bottom。
6. multistage crystallization system according to claim 1, it is characterised in that the sidewall of described crystallization kettle is provided with feed pipe (8), the lower end of described feed pipe (8) passes into the latter half of crystallization kettle。
CN201521126270.3U 2015-12-29 2015-12-29 Multistage crystallization system Expired - Fee Related CN205323272U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201521126270.3U CN205323272U (en) 2015-12-29 2015-12-29 Multistage crystallization system

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201521126270.3U CN205323272U (en) 2015-12-29 2015-12-29 Multistage crystallization system

Publications (1)

Publication Number Publication Date
CN205323272U true CN205323272U (en) 2016-06-22

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112691402A (en) * 2020-12-23 2021-04-23 安徽英特力工业工程技术有限公司 Vertical melt crystallizer

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112691402A (en) * 2020-12-23 2021-04-23 安徽英特力工业工程技术有限公司 Vertical melt crystallizer

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Date Code Title Description
C14 Grant of patent or utility model
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20170503

Address after: 322118 No. two, 323 Jiangnan Road, Hengdian Town, Zhejiang, Dongyang

Patentee after: Zhejiang Apeloa Home Pharmaceutical Co.,Ltd.

Address before: 322118 Hengdian Industrial Zone, Jinhua, Zhejiang, China, Dongyang

Patentee before: Puluo Medicines Tech Co., Ltd., Zhejiang

CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20160622

Termination date: 20181229