CN205575974U - Screw extruder and have this screw extruder's cyclic annular lactide preparation facilities - Google Patents
Screw extruder and have this screw extruder's cyclic annular lactide preparation facilities Download PDFInfo
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- CN205575974U CN205575974U CN201620269851.0U CN201620269851U CN205575974U CN 205575974 U CN205575974 U CN 205575974U CN 201620269851 U CN201620269851 U CN 201620269851U CN 205575974 U CN205575974 U CN 205575974U
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Abstract
The utility model relates to a screw extruder and have this screw extruder's cyclic annular lactide preparation facilities, the draw ratio of screw extruder (1) be 25~110, from screw rod top portion place at the beginning, be 2~20 position in screw extruder (1) draw ratio and locate the interval and be equipped with at least one vacuum blow vent, cyclic annular lactide preparation facilities, including screw extruder group to reach the collecting system that connecting screw rod extruded the unit, screw extruder group form by at least one screw extruder (1) tandem compound, the collecting system including bank of condensers (2), collection tank (3), cryrogenic cold -trap (4) and vacuum decompression subassembly (5) connected, wherein, bank of condensers (2) are and connecting screw rod extrudes the vacuum blow vent in the unit. Compared with the prior art, the utility model discloses a screw extruder's shear effect is strong, does not have the coking phenomenon during reaction liquid schizolysis and takes place, and glycolide / lactide yield of formation is high, the quality is high.
Description
Technical field
This utility model relates to a kind of screw extruder and the ring-type lactide preparation facilities with this screw extruder,
Especially relate to a kind of for polyglycolic acid/polylactic acid continuous cracking prepare ring-type lactide screw extruder and with
The ring-type lactide preparation facilities of this screw extruder.
Background technology
Polyglycolic acid/polylactic acid is the high molecular polymer comprising aliphatic ester bond in strand, be known can be native
Microorganism or zymolytic biodegradable polymer present in earth or the nature such as in the sea, this kind of material by
Can be applied to that there are the packaging material such as the film of single or multiple lift structure, sheet, bottle in its excellent biodegradability energy
Purposes, in order to reduce white pollution.Simultaneously as it has good biocompatibility and decomposition in vivo
Absorbability, thus also serve as the medical bioabsorbable polymer material such as surgical suture or artificial skin.Raw in reality
In product, it will usually first prepare the cyclic ester Acetic acid, hydroxy-, bimol. cyclic ester/lactide of raw material monomer as intermediate product, then by Acetic acid, hydroxy-, bimol. cyclic ester/
The mode of lactide ring-opening polymerisation prepares the polyglycolic acid/polylactic acid of high molecular further.
General people can take the polyglycolic acid/polylactic resin of low-molecular-weight under conditions of certain catalyst exists
Pintsch process prepares Acetic acid, hydroxy-, bimol. cyclic ester/lactide.These cracking reactors can be reactor or the continuous print of interval
Circulating evaporator, falling film evaporator, membrane evaporator etc..As US2668162 discloses a kind of method, wherein
That glycolic acid oligomer is broken into powder, and under ultrahigh vacuum (12-15 holds in the palm (1.6-2.0kPa)) in 270-285 DEG C
Heating, and it is fed in reaction vessel with depolymerization in the way of a small amount of many parts (about 20g/ hour), trapping gained contains
The steam of Acetic acid, hydroxy-, bimol. cyclic ester.Although the method is suitable to small-scale production, however, it was found that it is difficult to large-scale production, the most not
Be suitable to produce in a large number.Additionally, the method causes oligomer to become weight, then with the form of abundant residues thing when heating
It is retained in reaction vessel, causes glycolide yields to decline and it needs to remove residue.CN202022870U carries
Having supplied a kind of device for preparing hydroxycarboxylic acid cyclic dipolymer, this device has horizontally disposed reactant liquor stream and anti-
Answer the thermal medium stream that liquid stream road contacts and the decompressor reduced pressure by reactant liquor stream.Can be while making reactant liquor exist
Horizontally disposed reactant liquor stream flows, under reduced pressure utilizes the heat transfer from thermal medium stream by reactant liquor
Heating.Due to while making reactant liquor flatly flow by its depolymerization, the hydroxyls such as lactide can be efficiently generated
Carboxylic acid cyclic dimer.The method and device are particularly suitable for carrying out continuously depolymerization operation, have the scale of being easier
The advantage of extension.US5326887 and WO9215572 disclose by glycolic acid oligomers anti-in fixed bed
Answer and on device, add thermal depolymerization, prepare gas shape cyclic ester, then the method being allowed to cool, solidifying collection.
But, no matter using any cracking apparatus, the coking produced during being all difficult to avoid that Pintsch process is existing
As, polyglycolic acid/polylactic acid is cracked for continuous high-efficient and prepares the response system of Acetic acid, hydroxy-, bimol. cyclic ester/lactide and still suffer from needing
Ask.
Utility model content
Defect that the purpose of this utility model is contemplated to overcome above-mentioned prior art to exist and provide a kind of screw rod to squeeze
Go out machine and the ring-type lactide preparation facilities with this screw extruder.
The purpose of this utility model can be achieved through the following technical solutions:
A kind of screw extruder, prepares ring-type lactide for continuous cracking, and the draw ratio of described screw extruder is
25～110, from the beginning of at place, screw top end, set at the interval, position that screw extruder draw ratio is 2～20
There is at least one vacuum venting mouth.
Preferably, the draw ratio of described screw extruder is 40～80.
Being additionally provided with least one set kneading block in described screw extruder, described kneading block is forward kneading block or anti-
To kneading block.
Least one set reverse-flight elements it is additionally provided with in screw extruder.
Discharge outlet at screw extruder is additionally provided with the gear pump for stable reactant liquor flow field.
Described screw extruder is double screw extruder.
A kind of ring-type lactide preparation facilities with screw extruder, including Screw Extrusion unit, and connects screw rod
Extrusion unit is also used for collecting the collection system of pyrolysis product, and described Screw Extrusion unit is squeezed by least one screw rod
Going out machine tandem compound to form, described collection system includes condenser group and the collecting tank being sequentially connected with, and described is cold
Condenser group is also sequentially connected with deep cooling cold-trap and vacuum decompression assembly, and it is true that condenser group is also connected with in Screw Extrusion unit
Empty blow vent.
The condenser that described condenser group is arranged side by side by least one forms, and the quantity of described condenser does not surpasses
Cross the quantity of vacuum venting mouth on Screw Extrusion unit.
Described vacuum decompression assembly includes at least one vacuum equipment being arranged side by side, such as sliding vane rotary vacuum pump or jet
Formula vacuum pump etc..
The top of described deep cooling cold-trap is tightly connected condenser group and vacuum decompression assembly respectively.So can be effective
Avoid the condensed fluid in condenser group is adsorbed onto in vacuum decompression assembly during evacuation simultaneously, thus
Vacuum decompression assembly is caused damage.
Ring-type lactide preparation facilities of the present utility model is prepared Acetic acid, hydroxy-, bimol. cyclic ester/the third at cracking polyglycolic acid/polylactic acid and is handed over
During ester, first raw material polyglycolic acid/polylactic acid is conveyed into screw rod uniformly by the feed system of screw extruder and squeezes
Go out machine screw rod to be carried out carry, compress, melted, melted polyglycolic acid/polylactic acid reactant liquor is at screw extruder
Middle being fed forward by level, through the intensive shear effect of high-temperature heating and screw rod, the PVOH in reactant liquor
Acid/polylactic acid is partially converted into Acetic acid, hydroxy-, bimol. cyclic ester, when this partial reaction liquid is carried the vacuum venting when screw rod leading portion is arranged
During mouth, Acetic acid, hydroxy-, bimol. cyclic ester or lactide in reactant liquor are collected through condenser condensation by abjection because reducing pressure, second in reactant liquor
Lactide or lactide reduce promotion residue polyglycolic acid/polylactic acid continuation cracking further and are converted into Acetic acid, hydroxy-, bimol. cyclic ester or the third friendship
Ester and deviate from, until remaining reactant liquor discharged by gear pump.
Compared with prior art, this utility model has the advantage that
(1) kneading block in screw extruder and reverse-flight elements can greatly strengthen what screw rod rotation was formed
Shear action, and then horizontal feed the polyglycolic acid/poly-breast by high-temperature heating in screw extruder can be promoted
Acid reaction liquid is cracked to form Acetic acid, hydroxy-, bimol. cyclic ester/lactide.
(2) Acetic acid, hydroxy-, bimol. cyclic ester/lactide being cracked to form can be taken off from reactant liquor by the setting of vacuum venting mouth timely
Go out, such that it is able to promote that polyglycolic acid/polylactic acid reactant liquor cracks direction to the reaction of Acetic acid, hydroxy-, bimol. cyclic ester/lactide and carries out,
And then improve the yield of Acetic acid, hydroxy-, bimol. cyclic ester/lactide.
(3) meeting between the process of screw extruder conveying material, screw rod and extruder barrel or screw rod and screw rod
There is stronger friction, it is possible to effectively reduce coking residual in reactor, further increase Acetic acid, hydroxy-, bimol. cyclic ester/
The yield of lactide and quality, be particularly suitable for carrying out continuously cracking operation.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model；
In figure, 1-screw extruder, 2-condenser group, 3-collecting tank, 4-deep cooling cold-trap, 5-vacuum decompression assembly,
6-gear pump.
Detailed description of the invention
With specific embodiment, this utility model is described in detail below in conjunction with the accompanying drawings.
Embodiment 1
A kind of ring-type lactide preparation facilities with screw extruder, its structure is as it is shown in figure 1, include Screw Extrusion
Unit, and connect Screw Extrusion unit and for collecting the collection system of pyrolysis product, Screw Extrusion unit is by list
Platform screw extruder 1 tandem compound forms, and collection system includes condenser group 2 and the collecting tank 3 being sequentially connected with,
Condenser group 2 is also sequentially connected with deep cooling cold-trap 4 and vacuum decompression assembly 5, and condenser group 2 is arranged side by side by three
Condenser group 2 become, condenser group 2 is also connected with the vacuum venting mouth in Screw Extrusion unit, deep cooling cold-trap 4
Top be tightly connected condenser group 2 and vacuum decompression assembly 5 respectively, vacuum decompression assembly 5 includes two side by side
The vacuum decompression device arranged, can be sliding vane rotary vacuum pump or jet-propelled vacuum pump.
Screw extruder 1 is double screw extruder 1, and the draw ratio of screw extruder 1 is 25, from screw top end
Start at place, be interval with three vacuum venting mouths in the position that screw extruder 1 draw ratio is 2～20,
Being additionally provided with kneading block in screw extruder 1, kneading block is forward kneading block or reverse kneading block, at screw extruder
Being additionally provided with reverse-flight elements in 1, the discharge outlet at screw extruder 1 is additionally provided with for stable reactant liquor flow field
Gear pump 6.
Ring-type lactide preparation facilities of the present utility model is prepared Acetic acid, hydroxy-, bimol. cyclic ester/the third at cracking polyglycolic acid/polylactic acid and is handed over
During ester, first raw material polyglycolic acid/polylactic acid is conveyed into screw rod uniformly by the feed system of screw extruder 1
Extruder 1 screw rod carried out carry, compress, melted, melted polyglycolic acid/polylactic acid reactant liquor squeezes at screw rod
Go out being fed forward by level in machine 1, through the intensive shear effect of high-temperature heating and screw rod, in reactant liquor
Polyglycolic acid/polylactic acid is partially converted into Acetic acid, hydroxy-, bimol. cyclic ester, when this partial reaction liquid by carry when screw rod leading portion arrange true
During empty blow vent, Acetic acid, hydroxy-, bimol. cyclic ester or lactide in reactant liquor are collected through condenser condensation by abjection because reducing pressure, reaction
In liquid, Acetic acid, hydroxy-, bimol. cyclic ester or lactide minimizing promote residue polyglycolic acid/polylactic acid to continue further cracking and are converted into Acetic acid, hydroxy-, bimol. cyclic ester
Or lactide and deviate from, until remaining reactant liquor discharged by gear pump 6.
Above-mentioned preparation facilities in running, condenser circulatory mediator temperature at 60～150 DEG C, preferably 80～98 DEG C
Between；Vacuum in collection system need to reach between 10Pa～5KPa, preferably 10Pa～2KPa；Collecting tank needs
Insulation is at 60～150 DEG C, and between preferably 80～98 DEG C, collecting tank is equipped with liquidometer；The transfer rate of gear pump 6
For extruder feed rate 5%～50%.
Embodiment 2
A kind of ring-type lactide preparation facilities with screw extruder, including Screw Extrusion unit, and connects screw rod
Extrusion unit is also used for collecting the collection system of pyrolysis product, and Screw Extrusion unit is connected by separate unit screw extruder 1
Combining, collection system includes condenser group 2 and the collecting tank 3 being sequentially connected with, and condenser group 2 connects the most successively
Connecing deep cooling cold-trap 4 and vacuum decompression assembly 5, condenser group 2 is become by three condenser groups 2 being arranged side by side, cold
Condenser group 2 is also connected with the vacuum venting mouth in Screw Extrusion unit, and the top of deep cooling cold-trap 4 is tightly connected cold respectively
Condenser group 2 and vacuum decompression assembly 5, vacuum decompression assembly 5 includes two vacuum decompression devices being arranged side by side,
Can be sliding vane rotary vacuum pump or jet-propelled vacuum pump.
Screw extruder 1 is double screw extruder 1, and the draw ratio of screw extruder 1 is 110, from screw tip
Portion starts at place, is interval with three vacuum venting mouths in the position that screw extruder 1 draw ratio is 2～20,
Being additionally provided with kneading block in screw extruder 1, kneading block is forward kneading block or reverse kneading block, at screw extruder
Being additionally provided with reverse-flight elements in 1, the discharge outlet at screw extruder 1 is additionally provided with for stable reactant liquor flow field
Gear pump 6.
Embodiment 3
A kind of ring-type lactide preparation facilities with screw extruder, including Screw Extrusion unit, and connects screw rod
Extrusion unit is also used for collecting the collection system of pyrolysis product, and Screw Extrusion unit is connected by separate unit screw extruder 1
Combining, collection system includes condenser group 2 and the collecting tank 3 being sequentially connected with, and condenser group 2 connects the most successively
Connecing deep cooling cold-trap 4 and vacuum decompression assembly 5, condenser group 2 is become by three condenser groups 2 being arranged side by side, cold
Condenser group 2 is also connected with the vacuum venting mouth in Screw Extrusion unit, and the top of deep cooling cold-trap 4 is tightly connected cold respectively
Condenser group 2 and vacuum decompression assembly 5, vacuum decompression assembly 5 includes two vacuum decompression devices being arranged side by side,
Can be sliding vane rotary vacuum pump or jet-propelled vacuum pump.
Screw extruder 1 is double screw extruder 1, and the draw ratio of screw extruder 1 is 40, from screw top end
Start at place, be interval with three vacuum venting mouths in the position that screw extruder 1 draw ratio is 2～20,
Being additionally provided with kneading block in screw extruder 1, kneading block is forward kneading block or reverse kneading block, at screw extruder
Being additionally provided with reverse-flight elements in 1, the discharge outlet at screw extruder 1 is additionally provided with for stable reactant liquor flow field
Gear pump 6.
Embodiment 4
A kind of ring-type lactide preparation facilities with screw extruder, including Screw Extrusion unit, and connects screw rod
Extrusion unit is also used for collecting the collection system of pyrolysis product, and Screw Extrusion unit is connected by separate unit screw extruder 1
Combining, collection system includes condenser group 2 and the collecting tank 3 being sequentially connected with, and condenser group 2 connects the most successively
Connecing deep cooling cold-trap 4 and vacuum decompression assembly 5, condenser group 2 is become by three condenser groups 2 being arranged side by side, cold
Condenser group 2 is also connected with the vacuum venting mouth in Screw Extrusion unit, and the top of deep cooling cold-trap 4 is tightly connected cold respectively
Condenser group 2 and vacuum decompression assembly 5, vacuum decompression assembly 5 includes two vacuum decompression devices being arranged side by side,
Can be sliding vane rotary vacuum pump or jet-propelled vacuum pump.
Screw extruder 1 is double screw extruder 1, and the draw ratio of screw extruder 1 is 80, from screw top end
Start at place, be interval with three vacuum venting mouths in the position that screw extruder 1 draw ratio is 2～20,
Being additionally provided with kneading block in screw extruder 1, kneading block is forward kneading block or reverse kneading block, at screw extruder
Being additionally provided with reverse-flight elements in 1, the discharge outlet at screw extruder 1 is additionally provided with for stable reactant liquor flow field
Gear pump 6.
Embodiment 5
A kind of ring-type lactide preparation facilities with screw extruder, including Screw Extrusion unit, and connects screw rod
Extrusion unit is also used for collecting the collection system of pyrolysis product, and Screw Extrusion unit is connected by two screw extruders 1
Combining, collection system includes condenser group 2 and the collecting tank 3 being sequentially connected with, and condenser group 2 connects the most successively
Connecing deep cooling cold-trap 4 and vacuum decompression assembly 5, condenser group 2 is become by six condenser groups 2 being arranged side by side, cold
Condenser group 2 is also connected with the vacuum venting mouth in Screw Extrusion unit, and the top of deep cooling cold-trap 4 is tightly connected cold respectively
Condenser group 2 and vacuum decompression assembly 5, vacuum decompression assembly 5 includes two vacuum decompression devices being arranged side by side,
Can be sliding vane rotary vacuum pump or jet-propelled vacuum pump.
Screw extruder 1 is double screw extruder 1, and the draw ratio of screw extruder 1 is 60, from screw top end
Start at place, be interval with three vacuum venting mouths in the position that screw extruder 1 draw ratio is 2～20,
Two groups of kneading blocks it are additionally provided with in screw extruder 1, respectively one group forward kneading block and one group of reverse kneading block,
Being additionally provided with reverse-flight elements in screw extruder 1, the discharge outlet at screw extruder 1 is additionally provided with for stable
The gear pump 6 in reactant liquor flow field.
Embodiment 6
The situation using the cracking polyglycolic acid of the device in embodiment 1 to prepare Acetic acid, hydroxy-, bimol. cyclic ester illustrates, but this device
It is not limited to crack polyglycolic acid and prepares Acetic acid, hydroxy-, bimol. cyclic ester, it is also possible to be corresponding for cracking other polyhydroxycarboxyliacid acid preparation
Cyclic ester:
Raw material polyglycolic acid needs fully dried, drying condition: vacuum drying；Absolute pressure 1KPa, is dried by 90 DEG C
3h；Weight average molecular weight Mw of raw material polyglycolic acid is 100～20000, and preferable weight-average molecular weight Mw is
400～15000.Raw material polyglycolic acid is sufficiently mixed with catalyst for cracking uniformly before feeding intake, and the catalyst of use does not has
It is particularly limited to, it is possible to use by the organic carboxyl acid stannum (such as tin octoate, stannous octoate, tin octoate) of wide coverage
Deng titanium sub-group compound, the acetylacetone,2,4-pentanedione zirconiums such as aluminum based compound, alkoxy titanates such as stannum based compound, aluminum alkoxides
Deng the antimony based compound such as zirconium compound, antimony halides, also or the oxide such as zinc oxide, stibium oxide etc., catalyst
Addition can add by optimum addition as seen by each report.
Screw extruder as cracker selects double screw extruder, twin screw main-machine screw diameter: Ф
35.6mm；Main frame draw ratio: L/D=40；Main-machine screw rotating speed: 50r/min；Outer screw diameter/internal diameter ratio:
DO/Di=1.55；Main frame cylinder uses building block principle design, ten cylinders of postulating, and Fen Shiqu heats, if
Surely conveying compression section heating-up temperature 190～225 DEG C, melt zone heating-up temperature 230～250 DEG C；At Section 8 cylinder
Arranging a vacuum venting mouth, controlling absolute pressure herein is 700Pa；Arranging a condenser, cooling medium is 90 DEG C
Soft water；The transfer rate controlling gear pump 6 is about 2kg/h；Collecting tank is incubated 85 DEG C.By weight average molecular weight Mw
It is with feed rate after the catalyst for cracking tin octoate mix homogeneously of 3400 raw material polyglycolic acids and 1% mass fraction
It is conveyed into double screw extruder for 10kg/h, Acetic acid, hydroxy-, bimol. cyclic ester product from collecting tank that can be stable, detects its gas phase
Chromatographic purity up to more than 85%, capillary melting point apparatus test fusing point 60～83 DEG C.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and use reality
With novel.These embodiments obviously easily can be made various amendment, and handle by person skilled in the art
General Principle described herein is applied in other embodiments without through performing creative labour.Therefore, this practicality
The novel above-described embodiment that is not limited to, those skilled in the art are according to announcement of the present utility model, new without departing from this practicality
Improvement and amendment that type category is made all should be within protection domains of the present utility model.
Claims (10)
1. a screw extruder, prepares ring-type lactide for continuous cracking, it is characterised in that described screw rod
The draw ratio of extruder (1) is 25～110, from the beginning of at place, screw top end, in screw extruder (1)
Draw ratio be 2～20 position be interval with at least one vacuum venting mouth.
A kind of screw extruder the most according to claim 1, it is characterised in that described screw extruder
(1) draw ratio is 40～80.
A kind of screw extruder the most according to claim 1, it is characterised in that described screw extruder
(1) being additionally provided with least one set kneading block in, described kneading block is forward kneading block or reverse kneading block.
A kind of screw extruder the most according to claim 1, it is characterised in that in screw extruder (1)
Inside it is additionally provided with least one set reverse-flight elements.
A kind of screw extruder the most according to claim 1, it is characterised in that in screw extruder (1)
Discharge outlet be additionally provided with the gear pump (6) for stable reactant liquor flow field.
A kind of screw extruder the most according to claim 1, it is characterised in that described screw extruder
(1) it is double screw extruder (1).
7. a ring-type lactide preparation facilities for band described screw extruder arbitrary just like claim 1～6, bag
Include Screw Extrusion unit, and connect Screw Extrusion unit and for collecting the collection system of pyrolysis product, described
Screw Extrusion unit is formed by least one screw extruder (1) tandem compound, it is characterised in that described receipts
Collecting system includes condenser group (2) and the collecting tank (3) being sequentially connected with, and described condenser group (2) is the most successively
Connecting deep cooling cold-trap (4) and vacuum decompression assembly (5), condenser group (2) is also connected with in Screw Extrusion unit
Vacuum venting mouth.
One the most according to claim 7 ring-type lactide preparation facilities, it is characterised in that described condensation
The condenser that device group (2) is arranged side by side by least one forms, and the quantity of described condenser is squeezed less than screw rod
Go out the quantity of vacuum venting mouth on unit.
One the most according to claim 7 ring-type lactide preparation facilities, it is characterised in that described vacuum
Pressure relief assembly (5) includes at least one vacuum equipment being arranged side by side.
One the most according to claim 7 ring-type lactide preparation facilities, it is characterised in that described deep cooling
The top of cold-trap (4) is tightly connected condenser group (2) and vacuum decompression assembly (5) respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620269851.0U CN205575974U (en) | 2016-04-01 | 2016-04-01 | Screw extruder and have this screw extruder's cyclic annular lactide preparation facilities |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620269851.0U CN205575974U (en) | 2016-04-01 | 2016-04-01 | Screw extruder and have this screw extruder's cyclic annular lactide preparation facilities |
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| CN205575974U true CN205575974U (en) | 2016-09-14 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438411A (en) * | 2018-10-24 | 2019-03-08 | 深圳光华伟业股份有限公司 | Glycolide process units and production method |
| CN116283889A (en) * | 2023-03-29 | 2023-06-23 | 中国科学院长春应用化学研究所 | Preparation method and preparation device of glycolide |
-
2016
- 2016-04-01 CN CN201620269851.0U patent/CN205575974U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438411A (en) * | 2018-10-24 | 2019-03-08 | 深圳光华伟业股份有限公司 | Glycolide process units and production method |
| CN116283889A (en) * | 2023-03-29 | 2023-06-23 | 中国科学院长春应用化学研究所 | Preparation method and preparation device of glycolide |
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