CN101648938B - Recrystallization purifying device for lactide - Google Patents
Recrystallization purifying device for lactide Download PDFInfo
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- CN101648938B CN101648938B CN200910102212XA CN200910102212A CN101648938B CN 101648938 B CN101648938 B CN 101648938B CN 200910102212X A CN200910102212X A CN 200910102212XA CN 200910102212 A CN200910102212 A CN 200910102212A CN 101648938 B CN101648938 B CN 101648938B
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- recrystallization
- chamber
- lactide
- rac
- tank body
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- 238000001953 recrystallisation Methods 0.000 title claims abstract description 136
- JJTUDXZGHPGLLC-UHFFFAOYSA-N lactide Chemical compound CC1OC(=O)C(C)OC1=O JJTUDXZGHPGLLC-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000000746 purification Methods 0.000 claims abstract description 6
- 230000008676 import Effects 0.000 claims description 27
- 238000010992 reflux Methods 0.000 claims description 15
- 239000000284 extract Substances 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract 3
- 238000004321 preservation Methods 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 9
- 238000002425 crystallisation Methods 0.000 description 8
- 230000008025 crystallization Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 235000014655 lactic acid Nutrition 0.000 description 5
- 239000004310 lactic acid Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 229920000747 poly(lactic acid) Polymers 0.000 description 4
- 239000004626 polylactic acid Substances 0.000 description 4
- 239000003507 refrigerant Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003252 repetitive effect Effects 0.000 description 2
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
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Abstract
The invention provides a recrystallization purifying device for lactide, which has the advantages of seal operation, high recrystallization purity, economic and efficient running, and the like and mainly comprises a tank body, wherein the tank body is supported by a rotating shaft and can rotate along the rotating shaft; an inner cavity of the tank body is formed a recrystallization chamber; the inner wall of the tank body is provided with a filter plate for dividing the recrystallization chamber into an upper recrystallization chamber and a lower recrystallization chamber; the upper recrystallization chamber is provided with a recrystallization solvent inlet and a drawing outlet; the lower recrystallization chamber is provided with a lactide inlet and a lactide outlet; a heat preservation sleeve filled with cooling and heating media is fixed on the outer wall of the tank body at the outer side of the lower recrystallization chamber and provided with a cooling and heating media inlet and a cooling and heating media outlet. The whole pumping filter process is carried out in a seal or vacuum environment and has no stirring and mechanical power in running, the recrystallized liquid is uniformly mixed fully in a cavity body without residual undissolved lactide crystals, and the recrystallization purification is more complete.
Description
Technical field
The invention belongs to crystal recrystallization purifying device technical field, relate in particular to a kind of recrystallization purifying device that is used for rac-Lactide.
Background technology
Rac-Lactide is the precursor of POLYACTIC ACID.Synthesis of polylactic acid with lactide opened loop is the traditional classical method, compares with other synthesis mode, and ring-opening polymerization has the molecular weight height, the productive rate advantages of higher.High molecular weight polylactic acid is normally obtained by highly purified rac-Lactide ring-opening polymerization.Usually, rac-Lactide by aqueous lactic acid through low molecular weight as midbody, obtain through the cracked method again.But the rac-Lactide that generally obtains all contains impurity such as a small amount of lactic acid monomer, lactic acid dipolymer and water.
These impurity can have a negative impact to the polyreaction of rac-Lactide, can make the rac-Lactide hydrolysis obtain lactic acid like the existence of water, and can make polylactic acid molecule chain hydrolytic cleavage; The existence of acid such as lactic acid and dimer thereof can make the polylactic acid molecule chain degraded etc. because of acidolysis.Patent of invention: a kind of method of lactide recrystallization, the patent No.: 200510094845.2 disclose a kind of method that lactide recrystallization is obtained more highly purified rac-Lactide.
But the lactide recrystallization suitability for industrialized production is relatively more difficult at present, mainly is that the rac-Lactide generation is accompanied by a large amount of side reactions, and the impurity of removing the side reaction generation needs the certain process flow process.And in the impurity elimination process, existing flow process all is in open environment, has sneaked into other impurity again.The technical grade purifying of rac-Lactide still belongs to a difficult problem in China.
Summary of the invention
Technical problem to be solved by this invention is to above-mentioned prior art present situation, provides a kind of sealing operation, recrystallization purifying degree height, economical operation to be used for the recrystallization purifying device of rac-Lactide efficiently.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: the recrystallization purifying device that is used for rac-Lactide; Comprise a tank body that rotates by the rotation axis supporting and the moving axis that can rotate; Tank inner chamber constitutes the recrystallization chamber, is provided with a screen plate that the recrystallization chamber is divided into recrystallization chamber and following recrystallization chamber in inner tank wall; Be provided with a recrystallization solvent import and an extraction mouth in last recrystallization chamber; Be provided with a rac-Lactide inlet and a rac-Lactide outlet in following recrystallization chamber; Be fixed with a muff that feeds cold and hot matchmaker on the tank wall of following recrystallization outside, muff is provided with cold and hot matchmaker's import and cold and hot matchmaker's outlet; Tank body rotates and extracts liquid out from extracting mouth out after moving axis rotates 180 degree.
In order to improve from extracting mouthful utilising efficiency of the solvent of discharging out; Quicken the mixing of the indoor solution of recrystallization down simultaneously; The present invention has done further improvement on the technique scheme basis, is provided with a refluxing opening in last recrystallization chamber, extracts mouthful outer end connects refluxing opening through a purification devices outer end out; With extracting mouthful solvent of extracting out that can utilize again out, when a next recrystallization, inject the recrystallization chamber through refluxing opening through behind the purification devices purifying.
For optimizing technique scheme, the measure of taking also comprises:
At the following indoor interceptor that is fixed with of recrystallization, when tank body rotates moving axis when waving, but the indoor mixed solution accelerate dissolution of following recrystallization.
Tank body is designed oval tank body, can make the operational efficiency of tank body reach the highest.
Above-mentioned extraction mouth is arranged on the top of recrystallization chamber, and refluxing opening and recrystallization solvent import are arranged on the sidewall of recrystallization chamber.
Above-mentioned rac-Lactide outlet is arranged on down the bottom of recrystallization chamber, and the rac-Lactide inlet is arranged on down the sidewall of recrystallization chamber.
Above-mentioned screen plate is arranged on the middle part of recrystallization chamber, and rotation axis is fixed on the middle part of tank body.
Cold and hot matchmaker's import on the above-mentioned muff exports into the diagonal angle setting with cold and hot matchmaker.
Above-mentioned screen plate order number is 200 order to 400 orders.
Compared with prior art, the above-mentioned designing institute of the present invention have advantage:
1, whole suction filtration process was carried out under airtight or vacuum environment in the dissolving suction filtration stage, made whole flow process not receive outside contamination, can improve crystallization purity;
2, do not have to stir, do not have mechanical power, the stirring action with interceptor of rocking of rotation axis makes recrystallization liquid abundant mixing in cavity, does not have remaining undissolved rac-Lactide crystal to exist, and makes recrystallization complete;
3, when rac-Lactide need dissolve, feed heating agent, feed refrigerant, make it accelerate crystallisation, and go out more polycrystal than crystallization under the normal temperature in the recrystallization stage.
Description of drawings
Fig. 1 is the structural representation of the embodiment of the invention 1;
Fig. 2 be Fig. 1 partly cut open structural representation;
Fig. 3 is the structural representation of the embodiment of the invention 2;
Fig. 4 be Fig. 3 partly cut open structural representation.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are described in further detail.
Fig. 1 is extremely shown in Figure 4 to be structural representation of the present invention.
Reference numeral wherein is: rotation axis 1, tank body 2, recrystallization chamber 3, go up recrystallization chamber 3a, recrystallization chamber 3b, screen plate 4, recrystallization solvent import 5 down, extract mouthfuls 6 out, refluxing opening 7, rac-Lactide inlet 8, rac-Lactide outlet 9, muff 10, cold and hot matchmaker's import 11, cold and hot matchmaker export 12, interceptor 13.
As shown in Figure 1, present embodiment is used for the recrystallization purifying device of rac-Lactide, comprises a tank body 2 that is rotated by rotation axis 1 supporting and the moving axis 1 that can rotate.Tank body 2 inner chambers constitute recrystallization chamber 3, are provided with a screen plate 4 that recrystallization chamber 3 is divided into recrystallization chamber 3a and following recrystallization chamber 3b at tank body 2 inwalls.The order number of screen plate 4 between 200 order to 400 orders, with not through the rac-Lactide crystal, and solvent can be rapidly through for best.Tank body 2 connects to form replaceable screen plate 4 when two portions are taken apart up and down by two portions removable seal up and down.
Be provided with a recrystallization solvent import 5 and an extraction mouth 6 at last recrystallization chamber 3a.Extraction mouth 6 is arranged on the top of recrystallization chamber 3a, extracts mouth 6 out and can connect vacuum pump, and recrystallization chamber 3 is vacuumized, and after the crystallization completion, also can extract liquid out simultaneously.Recrystallization solvent import 5 operated by rotary motion are at the sidewall of last recrystallization chamber 3a.
Be provided with 8 and rac-Lactides outlets 9 of a rac-Lactide inlet at following recrystallization chamber 3b.Be fixed with a muff 10 that feeds cold and hot matchmaker on tank body 2 outer walls in the following recrystallization chamber 3b outside, muff 10 is provided with cold and hot matchmaker's import 11 and a cold and hot matchmaker exports 12.
Rac-Lactide is joined in the recrystallization chamber 3 by rac-Lactide inlet 8, and recrystallization solvent is injected in the recrystallization chamber 3 by recrystallization solvent import 5.The amount of liquid that adds in the recrystallization chamber 3 is no more than the height of rac-Lactide inlet 8.Feed heating agents from cold and hot matchmaker's import 11, heating is recrystallization chamber 3b down, and whole tank body 2 moving axis 1 that rotates is done oscillating motion simultaneously, quickens mixed solution and is dissolving in the 3b of recrystallization chamber down.After treating all dissolvings, the tank body 2 moving axis 1 whole upset that rotates, following recrystallization chamber 3b is positioned at the top of recrystallization chamber 3a.Solution in the following recrystallization chamber 3b filters the back through screen plate 4 and flows into the last recrystallization chamber 3a that is positioned at the below, changes screen plate 4, will go up recrystallization chamber 3a again and be turned to the top.Heating agent in the emptying muff 10 then, treat that solution naturally cools to normal temperature after, feed refrigerants through cold and hot matchmaker's import 11 to muff 10 again, make the further recrystallization of solution.To recrystallization fully after upset once more, solid was filtered plate 4 and held back this moment.Liquid separates rapidly with crystalline solid through extracting mouthful 6 extractions out.After solid drained, the moving axis 1 upset tank body 2 that rotates again fed heating agents fusing rac-Lactides to muff 10, and liquid rac-Lactide is extracted out from rac-Lactide outlet 9.
Above-mentioned heating agent can adopt hot water, thermal oil, warm air, steam etc., is incorporated in the muff 10 by cold and hot matchmaker's import 11, is full of muff 10, and heating agent exports 12 through cold and hot matchmaker at last and draws.Cold and hot matchmaker's import 11 exports 12 one-tenth diagonal angle settings with cold and hot matchmaker, forms circulation with external circulating system, and in muff 10, forms convection current, keeps down the temperature of recrystallization chamber 3b.Refrigerant can adopt water coolant, freezing air, cold oil etc., also is to be introduced by cold and hot matchmaker's import 11, and cold and hot matchmaker exports 12 and draws.
Be provided with a recrystallization solvent import 5, one at last recrystallization chamber 3a and extract mouthful 6 and refluxing openings 7 out.Extraction mouth 6 is arranged on the top of recrystallization chamber 3a, extracts mouth 6 during use out and can connect vacuum pump, and recrystallization chamber 3 is vacuumized, and after the crystallization completion, also can extract liquid out simultaneously.Recrystallization solvent import 5 and refluxing opening 7 are arranged on the sidewall of recrystallization chamber 3a.Extracting mouthful 6 outer ends out also can be through the outer end of a solvent purification device connection refluxing opening 7.
Be provided with 8 and rac-Lactides outlets 9 of a rac-Lactide inlet at following recrystallization chamber 3b.Rac-Lactide outlet 9 is arranged on down the bottom of recrystallization chamber 3b, and rac-Lactide inlet 8 is arranged on down the sidewall of recrystallization chamber 3b.
Be fixed with a muff 10 that feeds cold and hot matchmaker on tank body 2 outer walls in the following recrystallization chamber 3b outside, muff 10 is provided with cold and hot matchmaker's import 11 and a cold and hot matchmaker exports 12.Cold and hot matchmaker's import 11 exports 12 one-tenth diagonal angle settings with cold and hot matchmaker.
Following recrystallization chamber 3b internal fixing has interceptor 13.Be used to stir the quantity of interceptor 11 do not have concrete restriction, shape is unrestricted, can design voluntarily according to actual mix.
Rac-Lactide is joined in the recrystallization chamber 3 by rac-Lactide inlet 8, and recrystallization solvent is injected in the recrystallization chamber 3 by recrystallization solvent import 5.The amount of liquid that adds in the recrystallization chamber 3 is no more than the height of rac-Lactide inlet 8.Feed heating agents from cold and hot matchmaker's import 11, heating is recrystallization chamber 3b down, and whole tank body 2 moving axis 1 that rotates is done oscillating motion simultaneously, and mixed solution is accelerate dissolution under interceptor 13 effects.After treating all dissolvings, the tank body 2 moving axis 1 whole upset that rotates, following recrystallization chamber 3b is positioned at the top of recrystallization chamber 3a.Solution in the following recrystallization chamber 3b filters the back through screen plate 4 and flows into the last recrystallization chamber 3a that is positioned at the below, changes screen plate 4, will go up recrystallization chamber 3a again and be turned to the top.Heating agent in the emptying muff 10 then, treat that solution naturally cools to normal temperature after, feed refrigerants through cold and hot matchmaker's import 11 to muff 10 again, further recrystallizations.To recrystallization fully after upset once more, solid was filtered plate 4 and held back this moment.Liquid behind the entering solvent purification device purifying, treats that next recrystallization injects recrystallization chamber 3 from refluxing opening 7 through extracting mouthful 6 extractions out.
Repeat aforesaid operations again four times, when behind the 4th recrystallization solid being drained, the moving axis 1 upset tank body 2 that rotates again feeds heating agents fusing rac-Lactides to muff 10, and liquid rac-Lactide is extracted out from rac-Lactide outlet 9.The reflux solvent that injects from refluxing opening 7 is used in wherein preceding twice repetitive operation, and the fresh solvent that injects from recrystallization solvent import 5 is used in twice repetitive operation in back.With respect to embodiment 1, use reflux solvent can effectively improve the utilization ratio of recrystallization solvent, reduce production costs.
The recrystallization purifying device that is used for rac-Lactide provided by the invention has solved following technical barrier: 1, owing to there is not whisking appliance, so the sealing problem of whisking appliance, failure problems, energy consumption issues have all been avoided; 2, dissolving, heat filtering, crystallization and the cold filtration with recrystallization is combined in the device equipment of saving and place; 3, in crystallisation process, be isolated from the outside, improved crystallization purity effectively.
Most preferred embodiment of the present invention is illustrated, and various variations or the remodeling made by those of ordinary skills can not depart from the scope of the present invention.
Claims (7)
1. the recrystallization purifying device that is used for rac-Lactide; Comprise a tank body (2) that rotates by rotation axis (1) supporting and the moving axis (1) that can rotate; It is characterized in that: described tank body (2) inner chamber constitutes recrystallization chamber (3), is provided with a screen plate (4) that recrystallization chamber (3) is divided into recrystallization chamber (3a) and following recrystallization chamber (3b) at tank body (2) inwall; Be provided with a recrystallization solvent import (5) and an extraction mouthful (6) in last recrystallization chamber (3a); Be provided with a rac-Lactide inlet (8) and a rac-Lactide outlet (9) in following recrystallization chamber (3b); Be fixed with a muff (10) that feeds cold and hot matchmaker on tank body (2) outer wall in the outside, following recrystallization chamber (3b), muff (10) is provided with cold and hot matchmaker's import (11) and cold and hot matchmaker's outlet (12); Described tank body (2) rotates and extracts liquid out from described extraction mouthful (6) after moving axis (1) rotates 180 degree; The described recrystallization chamber (3a) of going up is provided with a refluxing opening (7), extracts mouthful (6) outer end connects refluxing opening (7) through a purification devices outer end out; Described recrystallization chamber (3b) internal fixing down has interceptor (13).
2. the recrystallization purifying device that is used for rac-Lactide according to claim 1 is characterized in that: described tank body (2) is oval tank body.
3. the recrystallization purifying device that is used for rac-Lactide according to claim 2 is characterized in that: described extraction mouthful (6) is arranged on the top of recrystallization chamber (3a), and refluxing opening (7) and recrystallization solvent import (5) are arranged on the sidewall of recrystallization chamber (3a).
4. the recrystallization purifying device that is used for rac-Lactide according to claim 3 is characterized in that: described rac-Lactide outlet (9) is arranged on down the bottom of recrystallization chamber (3b), and rac-Lactide inlet (8) is arranged on down the sidewall of recrystallization chamber (3b).
5. the recrystallization purifying device that is used for rac-Lactide according to claim 1 is characterized in that: described screen plate (4) is arranged on the middle part of recrystallization chamber (3), and described rotation axis (1) is fixed on the middle part of tank body (2).
6. the recrystallization purifying device that is used for rac-Lactide according to claim 1 is characterized in that: the cold and hot matchmaker's import (11) on the described muff (10) exports (12) with cold and hot matchmaker and becomes the diagonal angle setting.
7. the recrystallization purifying device that is used for rac-Lactide according to claim 1 is characterized in that: described screen plate (4) order number is 200 order to 400 orders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910102212XA CN101648938B (en) | 2009-09-03 | 2009-09-03 | Recrystallization purifying device for lactide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910102212XA CN101648938B (en) | 2009-09-03 | 2009-09-03 | Recrystallization purifying device for lactide |
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| Publication Number | Publication Date |
|---|---|
| CN101648938A CN101648938A (en) | 2010-02-17 |
| CN101648938B true CN101648938B (en) | 2012-07-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200910102212XA Expired - Fee Related CN101648938B (en) | 2009-09-03 | 2009-09-03 | Recrystallization purifying device for lactide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105396349B (en) * | 2015-11-24 | 2024-05-14 | 重庆欣欣向荣精细化工有限公司 | Filter device for ethyl vanillin |
| CN106397388B (en) * | 2016-09-07 | 2019-02-01 | 南京大学科技园发展有限公司 | A kind of technique of crude product cyclic ester purifying preparation high-purity cyclic ester |
| CN106621443B (en) * | 2016-11-14 | 2019-02-22 | 森田新能源材料（张家港）有限公司 | The Crystallization Separation device of lithium hexafluoro phosphate |
| CN113289371A (en) * | 2021-06-17 | 2021-08-24 | 马鞍山同杰良生物材料有限公司 | Suspension crystallization continuous purification L-lactide system in polylactic acid synthesis process |
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Address after: Yinzhou District Zhonggongmiao Street copper basin Zha Cun 315192 Zhejiang province Ningbo city Zhejiang Boshuo times Biotechnology Co. Ltd. Patentee after: Zhejiang Boshuobei Biological Technology Co.,Ltd. Address before: 315104 Zhejiang city of Ningbo province Yinzhou District Qiming road 677 Lane 166 Ningbo Boshuo times medical instrument limited company Patentee before: NINGBO BSB MEDICAL DEVICES Co.,Ltd. |
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Effective date of registration: 20160427 Address after: 300401 Tianjin city Wuqing District Chen Zui town Mei Shi Road No. 486 Patentee after: Tianjin Boshuobei Biological Technology Co.,Ltd. Address before: Yinzhou District Zhonggongmiao Street copper basin Zha Cun 315192 Zhejiang province Ningbo city Zhejiang Boshuo times Biotechnology Co. Ltd. Patentee before: Zhejiang Boshuobei Biological Technology Co.,Ltd. |
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