CN201482237U - Recrystallization purification device for lactide - Google Patents
Recrystallization purification device for lactide Download PDFInfo
- Publication number
- CN201482237U CN201482237U CN2009201924995U CN200920192499U CN201482237U CN 201482237 U CN201482237 U CN 201482237U CN 2009201924995 U CN2009201924995 U CN 2009201924995U CN 200920192499 U CN200920192499 U CN 200920192499U CN 201482237 U CN201482237 U CN 201482237U
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- recrystallization
- chamber
- lactide
- tank body
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Abstract
The utility model provides a recrystallization purification device for lactide, which has the advantages of operating under sealing, high degree of recrystallization purification, economical and efficiency running, and the like, and mainly comprises a tank body supported by a rotating shaft and capable of rotating around the rotating shaft, inner cavities of the tank body form a recrystallization chamber, the inner wall of the tank body is provided with a filter plate which divides 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 an extraction port; the lower recrystallization chamber is provided with a lactide inlet and a lactide outlet; the outer wall of the tank body at the outer side of the lower recrystallization chamber is fixed with a heat preservation sleeve in which cooling/heating media are fed, and the heat preservation sleeve is provided with a cooling/heating media inlet and a cooling/heating media outlet. The entire extraction/filtration process is conducted in closed or vacuum environments without stirring and mechanical power in the operation, recrystallization liquid is sufficiently and uniformly mixed in the cavities, and no undissolved lactide crystal is remained, thus achieving more complete recrystallization purification.
Description
Technical field
The utility model belongs to crystal recrystallization purifying device technical field, relates in particular to a kind of recrystallization purifying device that is used for lactide.
Background technology
Lactide is the precursor of PLA.Synthesis of polylactic acid with lactide opened loop is the traditional classical method, compares with other synthesis mode, and ring-opening polymerisation has the molecular weight height, the productive rate advantages of higher.High molecular weight polylactic acid is normally obtained by highly purified lactide ring-opening polymerisation.Usually, lactide by moisture lactic acid through low molecular weight as intermediate, the method by cracking obtains again.But the lactide that generally obtains all contains impurity such as a small amount of lactic acid monomer, lactic acid dimer and water.
These impurity can have a negative impact to the polymerisation of lactide, can make the lactide hydrolysis obtain lactic acid as 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 be 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 lactide.
But the lactide recrystallization suitability for industrialized production is relatively more difficult at present, mainly is that the lactide generation is accompanied by a large amount of side reactions, and the impurity of removing the side reaction generation needs certain technological 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 lactide still belongs to a difficult problem in China.
Summary of the invention
Technical problem to be solved in the utility model is at 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 lactide efficiently.
The utility model solves the problems of the technologies described above the technical scheme that is adopted: the recrystallization purifying device that is used for lactide, comprise a tank body that rotates by the turning cylinder supporting and the moving axis that can rotate, tank inner chamber formation recrystallization chamber is provided with a filter that the chamber of recrystallization is divided into recrystallization chamber and the following chamber that is recrystallized in inner tank wall; Be provided with a recrystallization solvent import and an extraction mouth in last recrystallization chamber; Under the chamber of recrystallization be provided with lactide inlet and a lactide exports; Being recrystallized down is fixed with a muff that feeds cold and hot matchmaker on the tank wall of outside, and 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 utilization ratio of the solvent of discharging out, quicken the mixing of the indoor solution of recrystallization down simultaneously, the utility model has been done further improvement on the technique scheme basis, be provided with a refluxing opening in last recrystallization chamber, extract the outer end of mouthful outer end out by a purification devices connection refluxing opening, to extract mouthful recycling solvent of extracting out out by behind the purification devices purifying, when a next recrystallization, inject the recrystallization chamber by refluxing opening.
For optimizing technique scheme, the measure of taking also comprises:
Under the indoor spoiler that is fixed with that is recrystallized, when tank body rotates moving axis when waving, but the indoor mixed liquor 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 lactide outlet is arranged on down the bottom of recrystallization chamber, and the lactide inlet is arranged on down the sidewall of recrystallization chamber.
Above-mentioned filter is arranged on the middle part of recrystallization chamber, and turning cylinder 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 filter order number is 200 order to 400 orders.
Compared with prior art, the above-mentioned designing institute of the utility model 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 be subjected to outside contamination, can improve crystallization purity;
2, do not have to stir, do not have mechanical power, the stirring action with spoiler of rocking of turning cylinder makes recrystallization liquid abundant mixing in cavity, do not have remaining undissolved in the lactide crystal exist, make recrystallization fully;
3, when lactide need dissolve, feed heating agent, feed refrigerant, make it to quicken crystallization, 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 utility model embodiment 1;
Fig. 2 be Fig. 1 partly cut open structural representation;
Fig. 3 is the structural representation of the utility model embodiment 2;
Fig. 4 be Fig. 3 partly cut open structural representation.
The specific embodiment
Below in conjunction with accompanying drawing embodiment of the present utility model is described in further detail.
Fig. 1 is to Figure 4 shows that structural representation of the present utility model.
Reference numeral wherein is: turning cylinder 1, tank body 2, recrystallization chamber 3, on be recrystallized chamber 3a, down be recrystallized chamber 3b, filter 4, recrystallization solvent import 5, extract mouthfuls 6 out, refluxing opening 7, lactide inlet 8, lactide outlet 9, muff 10, cold and hot matchmaker's import 11, cold and hot matchmaker export 12, spoiler 13.
Embodiment 1
As shown in Figure 1, present embodiment is used for the recrystallization purifying device of lactide, comprises a tank body 2 that is rotated by turning cylinder 1 supporting and the moving axis 1 that can rotate.Tank body 2 inner chambers constitute recrystallization chamber 3, are provided with the filter 4 that the chamber 3 that will be recrystallized is divided into recrystallization chamber 3a and following recrystallization chamber 3b at tank body 2 inwalls.The order number of filter 4 between 200 order to 400 orders, with not by the lactide crystal, and solvent can be rapidly by for best.Tank body 2 connects to form replaceable filter 4 when two parts are taken apart up and down by two parts 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 vavuum pump, and the chamber 3 that will be recrystallized vacuumizes, and the while also can be extracted liquid out after crystallization is finished.Recrystallization solvent import 5 operated by rotary motion are at the sidewall of last recrystallization chamber 3a.
Under the chamber 3b that is recrystallized be provided with 8 and lactides outlets 9 of lactide inlet.Being recrystallized down is fixed with a muff 10 that feeds cold and hot matchmaker on tank body 2 outer walls in the chamber 3b outside, and muff 10 is provided with cold and hot matchmaker's import 11 and a cold and hot matchmaker exports 12.
Lactide is joined in the recrystallization chamber 3 by 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 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, quicken mixed liquor under be recrystallized and dissolve in the 3b of chamber.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 the chamber 3a that is recrystallized.Be recrystallized down in the 3b of chamber solution through filter 4 filter the back flow into be positioned at the below go up recrystallization chamber 3a, change filter 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, solution further is recrystallized.To recrystallization fully after upset once more, solid was filtered plate 4 and held back this moment.Liquid separates rapidly with crystalline solid by extracting mouthful 6 extractions out.After solid drained, the moving axis 1 upset tank body 2 that rotates again fed heating agents fusing lactides to muff 10, and liquid lactide is extracted out from lactide outlet 9.
Above-mentioned heating agent can adopt hot water, conduction oil, hot-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 by 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 form convection current in muff 10, keeps down the temperature of recrystallization chamber 3b.Refrigerant can adopt cooling water, cold 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 vavuum pump, and the chamber 3 that will be recrystallized vacuumizes, and the while also can be extracted liquid out after crystallization is finished.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 by the outer end of a solvent purification device connection refluxing opening 7.
Under the chamber 3b that is recrystallized be provided with 8 and lactides outlets 9 of lactide inlet.Lactide outlet 9 is arranged on down the bottom of recrystallization chamber 3b, and lactide inlet 8 is arranged on down the sidewall of recrystallization chamber 3b.
Being recrystallized down is fixed with a muff 10 that feeds cold and hot matchmaker on tank body 2 outer walls in the chamber 3b outside, and 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.
Under be recrystallized and be fixed with spoiler 13 in the 3b of chamber.Be used to stir the quantity of spoiler 11 do not have concrete restriction, shape is unrestricted, can design voluntarily according to the reality situation of mixing.
Lactide is joined in the recrystallization chamber 3 by 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 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 liquor is accelerate dissolution under spoiler 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 the chamber 3a that is recrystallized.Be recrystallized down in the 3b of chamber solution through filter 4 filter the back flow into be positioned at the below go up recrystallization chamber 3a, change filter 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 recrystallization.To recrystallization fully after upset once more, solid was filtered plate 4 and held back this moment.Liquid is extracted out by extracting mouthfuls 6 out, enter solvent purification device purifying after, treat that next time, recrystallization injected recrystallization chambers 3 from refluxing opening 7.
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 lactides to muff 10, and liquid lactide is extracted out from 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 rate of recrystallization solvent, reduce production costs.
The recrystallization purifying device that is used for lactide that the utility model provides has solved following technical barrier: 1, owing to there is not agitator, so the sealing problem of agitator, failure problems, energy consumption issues have all been avoided; 2, the dissolving that will be recrystallized, heat filtering, crystallization and cold filtration are combined in the device, the equipment of saving and place; 3, in crystallization process, be isolated from the outside, improved crystallization purity effectively.
Most preferred embodiment of the present utility model is illustrated, and various variations or the remodeling made by those of ordinary skills can not break away from scope of the present utility model.
Claims (9)
1. the recrystallization purifying device that is used for lactide, comprise a tank body (2) that rotates by turning cylinder (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 the filter (4) that the chamber (3) that will be recrystallized 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); Under be recrystallized that chamber (3b) is provided with lactide inlet (8) and a lactide exports (9); Being recrystallized down is fixed with a muff (10) that feeds cold and hot matchmaker on tank body (2) outer wall in chamber (3b) outside, and muff (10) is provided with cold and hot matchmaker's import (11) and a cold and hot matchmaker exports (12); Described tank body (2) rotates and extracts liquid out from described extraction mouthful (6) after moving axis (1) rotates 180 degree.
2. the recrystallization purifying device that is used for lactide according to claim 1 is characterized in that: the described recrystallization chamber (3a) of going up is provided with a refluxing opening (7), extracts mouthful (6) outer end connects refluxing opening (7) by a purification devices outer end out.
3. the recrystallization purifying device that is used for lactide according to claim 2 is characterized in that: be fixed with spoiler (13) in the described chamber (3b) that is recrystallized down.
4. according to claim 1 or the 2 or 3 described recrystallization purifying devices that are used for lactide, it is characterized in that: described tank body (2) is oval tank body.
5. the recrystallization purifying device that is used for lactide according to claim 4, it 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).
6. the recrystallization purifying device that is used for lactide according to claim 4 is characterized in that: described lactide outlet (9) is arranged on down the bottom of recrystallization chamber (3b), and lactide inlet (8) is arranged on down the sidewall of recrystallization chamber (3b).
7. according to claim 1 or the 2 or 3 described recrystallization purifying devices that are used for lactide, it is characterized in that: described filter (4) is arranged on the middle part of recrystallization chamber (3), and described turning cylinder (1) is fixed on the middle part of tank body (2).
8. according to claim 1 or the 2 or 3 described recrystallization purifying devices that are used for lactide, it 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.
9. according to claim 1 or the 2 or 3 described recrystallization purifying devices that are used for lactide, it is characterized in that: described filter (4) order number is 200 order to 400 orders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009201924995U CN201482237U (en) | 2009-09-03 | 2009-09-03 | Recrystallization purification device for lactide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009201924995U CN201482237U (en) | 2009-09-03 | 2009-09-03 | Recrystallization purification device for lactide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201482237U true CN201482237U (en) | 2010-05-26 |
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ID=42421131
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009201924995U Expired - Lifetime CN201482237U (en) | 2009-09-03 | 2009-09-03 | Recrystallization purification device for lactide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN201482237U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104043264A (en) * | 2014-06-18 | 2014-09-17 | 阚梦诗 | Crystallization kettle for preventing crystals from flowing out from overflowing hole |
| CN112090108A (en) * | 2020-09-22 | 2020-12-18 | 安徽英特力工业工程技术有限公司 | Lactide circulating crystallization drying equipment in polylactic acid synthesis process |
| 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 |
-
2009
- 2009-09-03 CN CN2009201924995U patent/CN201482237U/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104043264A (en) * | 2014-06-18 | 2014-09-17 | 阚梦诗 | Crystallization kettle for preventing crystals from flowing out from overflowing hole |
| CN112090108A (en) * | 2020-09-22 | 2020-12-18 | 安徽英特力工业工程技术有限公司 | Lactide circulating crystallization drying equipment in polylactic acid synthesis process |
| 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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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee | ||
| CP02 | Change in the address of a patent holder |
Address after: 315104 Zhejiang city of Ningbo province Yinzhou District Qiming road 677 Lane 166 Ningbo Boshuo times medical instrument limited company Patentee after: Ningbo BSB Medical Devices Co., Ltd. Address before: 315192 Zhejiang city of Ningbo province Yinzhou District Zhonggongmiao street lamp Hui Temple Village Ningbo Boshuo times medical instrument limited company Patentee before: Ningbo BSB Medical Devices Co., Ltd. |
|
| AV01 | Patent right actively abandoned |
Granted publication date: 20100526 Effective date of abandoning: 20090903 |