CN218962010U - Continuous refined production system of glycolide - Google Patents

Continuous refined production system of glycolide Download PDF

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CN218962010U
CN218962010U CN202222399643.0U CN202222399643U CN218962010U CN 218962010 U CN218962010 U CN 218962010U CN 202222399643 U CN202222399643 U CN 202222399643U CN 218962010 U CN218962010 U CN 218962010U
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kettle
glycolide
solvent
production system
filtering
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蒋永飞
张其荣
李奇
张晓龙
刘伟
丁兆华
薛凤山
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Inner Mongolia Jiutai New Material Technology Co ltd
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Inner Mongolia Jiutai New Material Technology Co ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract

The utility model relates to a glycolide refining instrument field, concretely relates to glycolide continuous refining's production system, this system includes the dissolution kettle, the dissolution kettle is connected with filtration system, filtration system is connected with concentrated cauldron, concentrated cauldron is connected with the condenser, the condenser is connected with the solvent and receives the jar, the solvent is received the jar and is connected with first vacuum pump, concentrated cauldron still is connected with filtration washing drying all-in-one, filtration washing drying all-in-one is connected with conveyer, conveyer is connected with the crystallization kettle, the crystallization kettle is connected with the centrifuge, the centrifuge is connected with vacuum dryer, be provided with the solvent collection jar on the centrifuge, the crystallization kettle, centrifuge and vacuum dryer are installed in the clean district. The beneficial effects of this application lie in: the production system has good continuous stability, the system is definite in labor division and not easy to damage, the cost and the energy consumption are reduced, the refining and the purification of the crude glycolide with low carbonization and continuity can be realized, and the purity can reach 99.9 percent.

Description

Continuous refined production system of glycolide
Technical Field
The application belongs to the field of glycolide refining apparatuses, and particularly relates to a continuous glycolide refining production system.
Background
Polyglycolic acid (PGA) is a common biodegradable polyester and is often used in high value-added fields such as surgical sutures, bone materials, and controlled drug release carriers.
The synthetic method commonly employed in the industry for the preparation of higher relative molecular mass polyglycolic acid (PGA) is the "two-step process": firstly, glycolic acid is polycondensed to obtain glycolic acid oligomer, then the glycolic acid oligomer is depolymerized to obtain cyclic glycolide, and the glycolide is used for ring-opening polymerization to obtain the product with relative molecular weight of 10 5 ~10 6 Glycolide is an important monomer for preparing polyglycolic acid as a degradable surgical suture material in a two-step process, and thus, the purification of glycolide is a key in preparing polyglycolic acid of high relative molecular mass and polyglycolic lactide.
Glycolide is usually produced by depolymerization of glycolic acid oligomers at high temperature and under vacuum, which gives the crude product called crude glycolide (purity. Gtoreq.85%). Crude glycolide contains impurities such as free water, glycolic acid and linear oligomers of glycolic acid, which can cause polymerization inhibition on ring opening polymerization, so that the relative molecular quality of the polymer obtained by ring opening polymerization of glycolide is reduced, and the mechanical properties of the polymer are reduced. To obtain at least a relative molecular mass greater than 10 5 Polyglycolic acid (PGA) for surgical suture of (2) and glycolide for ring-opening polymerization are required to have a purity of 99.9%As above, however, there is no corresponding production system for producing glycolide having such a high purity in the prior art.
In view of the above, there is a need for a large-scale continuous glycolide purification production system.
Disclosure of Invention
In order to solve the problem, the application provides a continuous refined production system of glycolide, this system is including dissolving the cauldron, it is connected with filtration system to dissolve the cauldron, filtration system is connected with concentrated cauldron, concentrated cauldron is connected with the condenser, the condenser is connected with the solvent and receives the jar, the solvent is received the jar and is connected with first vacuum pump, concentrated cauldron still is connected with filtration washing drying all-in-one, filtration washing drying all-in-one is connected with conveyer, conveyer is connected with crystallization cauldron, crystallization cauldron is connected with centrifuge, centrifuge is connected with vacuum dryer, be provided with the solvent collection jar on the centrifuge, crystallization cauldron, centrifuge and vacuum dryer are installed in the clean area.
The dissolution tank, the concentration tank, the condenser, the filtration system, the filtration, washing and drying integrated machine, the crystallization tank, the centrifuge, the vacuum dryer and other devices are all in the prior art, and the necessary structure not mentioned in the application in the above system is still provided in the system of the application.
The dissolving kettle is provided with an inert gas inlet, and inert gas is introduced into the dissolving kettle to protect substances in the dissolving kettle from reacting with the outside.
The filtration system is a metal or ceramic membrane filtration system, two ends of the filtration system are connected with the dissolution kettle and the concentration kettle through pipelines, the pipelines are soft stainless steel pipelines, the filtration system and the pipelines are connected in a clamping mode, the clamping connection is detachable, the filtration system can be detached, and replacement and cleaning are facilitated.
The concentration kettle comprises a solvent outlet and a material outlet, wherein a solvent outlet pipeline is connected with a condenser, a material outlet pipeline is connected with a filtering, washing and drying integrated machine, and the concentration kettle is a jacketed concentration kettle.
The filtering, washing and drying integrated machine is divided into a washing filtering part and a drying part, the filtering part is provided with a filtrate outlet, a filtrate storage tank is connected at the filtrate outlet, and the filtrate storage tank is connected with a second vacuum pump.
The conveying device is a conveying belt or a push conveyor.
A buffer tank is arranged between the solvent receiving tank and the first vacuum pump, and can protect the first vacuum pump and prevent the first vacuum pump from being damaged.
The crystallization kettle, the centrifugal machine and the vacuum dryer are arranged in a clean area of a clean environment and used for guaranteeing the obtained product to be clean and sanitary and reducing the influence of moisture on the product.
The denuded zone is an area that meets at least the D-class denuded zone criteria.
The solvent receiving tank is a stainless steel tank or a transparent glass tank with a window, and the solvent receiving tank is provided with accurate scales.
The inlet and the outlet of each device are controlled by valves, each device operates as an independent unit, and enters the next unit to operate after corresponding operation is completed in one unit until a qualified product is obtained.
The beneficial effects of this application lie in:
(1) The production system has good continuous stability, the system is definite in labor division and not easy to damage, the cost and the energy consumption are reduced, the refining and the purification of the crude glycolide with low carbonization and continuity can be realized, and the purity can reach 99.9 percent.
(2) The application is provided with the solvent receiving tank and realizes the recycle of solvent to be provided with filtrate holding vessel, centrifuge department when filtering and be provided with solvent collecting tank, make the material further retrieve, reduction in production cost, further improve the productivity ratio when little to environmental impact.
(3) The equipment adopted by the method is equipment with mature technology and low cost requirement, is simple and safe to operate, has low equipment investment, and can realize continuous and large-scale production of glycolide refining.
Drawings
FIG. 1 is a system equipment connection diagram of example 1;
in the figure: 100-dissolution kettle, 102-inert gas inlet, 200-filtration system, 300-concentration kettle, 302-material outlet, 303-solvent outlet, 400-condenser, 401-solvent receiving tank, 402-buffer tank, 403-first vacuum pump, 500-filtration washing and drying integrated machine, 502-filtrate outlet, 503-filtrate storage tank, 504-second vacuum pump, 600-conveying device, 700-crystallization kettle, 800-centrifuge, 801-solvent collection tank, 900-vacuum dryer, 1000-clean zone.
Detailed Description
The present application will now be further described in connection with particular embodiments in order to enable those skilled in the art to better understand the present application.
Example 1
The continuous glycolide refining production system comprises a dissolution kettle 100, wherein the dissolution kettle 100 is connected with a filtering system 200, the filtering system 200 is connected with a concentration kettle 300, the concentration kettle 300 is connected with a condenser 400, the condenser 400 is connected with a solvent receiving tank 401, the solvent receiving tank 401 is connected with a first vacuum pump 403, the concentration kettle 300 is also connected with a filtering, washing and drying integrated machine 500, the filtering, washing and drying integrated machine 500 is connected with a conveying device 600, the conveying device 600 is connected with a crystallization kettle 700, the crystallization kettle 700 is connected with a centrifugal machine 800, the centrifugal machine 800 is connected with a vacuum dryer 900, the centrifugal machine 800 is provided with a solvent collecting tank 801, and the crystallization kettle 700, the centrifugal machine 800 and the vacuum dryer 900 are arranged in a clean zone 1000.
The dissolution vessel 100 is provided with an inert gas inlet 102.
The filtering system 200 is a metal or ceramic membrane filtering system, two ends of the filtering system 200 are connected with the dissolution kettle 100 and the concentration kettle 300 through pipelines, the pipelines are soft stainless steel pipelines, and the filtering system 200 is connected with the pipelines in a clamping mode.
The concentration kettle 300 comprises a solvent outlet 303 and a material outlet 302, wherein a solvent outlet pipeline is connected with a condenser 400, the material outlet pipeline is connected with a filtering, washing and drying integrated machine 500, and the concentration kettle 300 is a jacketed concentration kettle.
The integrated filtering, washing and drying machine 500 is divided into a washing filtering part and a drying part, the filtering part is provided with a filtrate outlet, a filtrate storage tank 503 is connected at the filtrate outlet, and a second vacuum pump 504 is connected to the filtrate storage tank 503.
The conveyor 600 is a conveyor belt or pusher conveyor.
Denuded zone 1000 is an area that meets at least the class D denuded zone criteria.
A buffer tank 402 is provided between the solvent receiving tank 401 and the first vacuum pump 403.
The solvent receiving tank 401 is a stainless steel tank or a transparent glass tank with a window, and the solvent receiving tank 401 has accurate graduations.
Adding crude glycolide as a solid material into a dissolution kettle 100, adding a polar solvent, starting stirring, dissolving a solid product, introducing inert gas after the solid product is dissolved completely, introducing the dissolved material solution into a filtering system 200, and introducing the solution into a concentration kettle 300 after the filtering is completed; all the solution enters the concentration kettle 300, stirring is started, heating and concentration are carried out, a first vacuum pump 403 is started, the evaporated light component solvent is concentrated in vacuum, and the light component solvent is cooled by a condenser 400 and then is recycled into a solvent receiving tank 401; stopping concentrating when the volume of the light component solvent received in the solvent receiving tank 401 reaches 85-90% of the volume of the added polar solvent; turning off the first vacuum pump 403, placing the concentrated residual material into the filtering, washing and drying integrated machine 500, and performing filtering, washing and drying operations in the filtering, washing and drying integrated machine 500, wherein the filtering and drying operations need to be performed in a vacuum state, namely turning on the vacuum pump; in addition, the filtered and washed filtrate is collected and stored by a filtrate storage tank 503 to be treated and recovered; the solid remained after filtration is dried, the dried solid material is sent into a crystallization kettle 700 through a conveying device 600, a recrystallization solvent is added, then the temperature is raised, the solution is heated and dissolved, after the solution is dissolved, the temperature is reduced, crystallization is completed, the solution enters a centrifuge 800, centrifugal filtration operation is completed, and the centrifuged liquid is placed in a solvent collection tank 801 for treatment and recovery; and then transferring the solid material into a vacuum dryer 900 for vacuum drying, and packaging the product after the drying is finished to obtain the final refined glycolide product.
Wherein, the crystallization kettle 700, the centrifugal machine 800, the vacuum dryer 900 and other devices are arranged in the clean area 1000, so that the operations of recrystallization, centrifugal throwing filtration, vacuum drying and packaging are all carried out in the clean area 1000.

Claims (9)

1. The continuous refined production system of glycolide is characterized in that the system comprises a dissolution kettle, the dissolution kettle is connected with a filtering system, the filtering system is connected with a concentration kettle, the concentration kettle is connected with a condenser, the condenser is connected with a solvent receiving tank, the solvent receiving tank is connected with a first vacuum pump, the concentration kettle is also connected with a filtering, washing and drying integrated machine, the filtering, washing and drying integrated machine is connected with a conveying device, the conveying device is connected with a crystallization kettle, the crystallization kettle is connected with a centrifugal machine, the centrifugal machine is connected with a vacuum dryer, a solvent collecting tank is arranged on the centrifugal machine, and the crystallization kettle, the centrifugal machine and the vacuum dryer are arranged in a clean area.
2. The continuous refining production system for glycolide according to claim 1, wherein an inert gas inlet is provided on the dissolution vessel.
3. The continuous refining production system of glycolide according to claim 1, wherein the filtration system is a metal or ceramic membrane filtration system, two ends of the filtration system are connected with the dissolution kettle and the concentration kettle through pipelines, the pipelines are soft stainless steel pipelines, and the filtration system is connected with the pipelines through hoops.
4. The continuous refining production system of glycolide according to claim 1, wherein the concentration kettle comprises a solvent outlet and a material outlet, the solvent outlet is connected with a condenser through a pipeline, the material outlet is connected with a filtering, washing and drying integrated machine, and the concentration kettle is a jacketed concentration kettle.
5. The continuous refining production system of glycolide according to claim 1, wherein the filtering, washing and drying integrated machine is divided into a washing filtering part and a drying part, the filtering part is provided with a filtrate outlet, a filtrate storage tank is connected at the filtrate outlet, and the filtrate storage tank is connected with a second vacuum pump.
6. The continuous refining production system of glycolide according to claim 1, wherein the conveyor is a conveyor belt or a pusher conveyor.
7. A continuous refining production system for glycolide according to claim 1, wherein the denuded zone is a zone that meets at least the D-class denuded zone criteria.
8. The continuous refining production system for glycolide according to claim 1, wherein a buffer tank is provided between the solvent receiving tank and the first vacuum pump.
9. The continuous refining production system of glycolide according to claim 1, wherein the solvent receiving tank is a stainless steel tank or a transparent glass tank with a window, and the solvent receiving tank has a precise scale.
CN202222399643.0U 2022-09-09 2022-09-09 Continuous refined production system of glycolide Active CN218962010U (en)

Priority Applications (1)

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CN202222399643.0U CN218962010U (en) 2022-09-09 2022-09-09 Continuous refined production system of glycolide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202222399643.0U CN218962010U (en) 2022-09-09 2022-09-09 Continuous refined production system of glycolide

Publications (1)

Publication Number Publication Date
CN218962010U true CN218962010U (en) 2023-05-05

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