CN208426686U - A kind of lactide purification devices and lactide purification system - Google Patents
A kind of lactide purification devices and lactide purification system Download PDFInfo
- Publication number
- CN208426686U CN208426686U CN201820512606.7U CN201820512606U CN208426686U CN 208426686 U CN208426686 U CN 208426686U CN 201820512606 U CN201820512606 U CN 201820512606U CN 208426686 U CN208426686 U CN 208426686U
- Authority
- CN
- China
- Prior art keywords
- lactide
- tube
- side fluid
- purification devices
- tank
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The utility model belongs to organic chemical industry's separation technology field more particularly to a kind of lactide purification devices and lactide purification system.Purification devices provided by the utility model include: vertical tank and the vertically disposed several heat exchanger tubes in vertical tank；Tube side fluid inlet is provided at the top of the vertical tank, bottom is provided with tube side fluid outlet；The both ends of the heat exchanger tube are respectively arranged with the upper perforated plate and lower perforated plate closed with vertical top tank structure, the lower surface of the upper perforated plate, the upper surface of lower perforated plate, the outer wall of heat exchanger tube and vertical tank inner wall be formed by enclosure space and be provided with shell side fluid inlet and shell side fluid outlet；The vertical tank is provided with vacuum orifice between tube side fluid inlet and upper perforated plate；Heating tube is provided in the inner cavity of the heat exchanger tube.Efficiently separating-purifying can be carried out to lactide crude product using device provided by the utility model, reduce the number of lactide fusion-crystallization.
Description
Technical field
The utility model belongs to organic chemical industry's separation technology field more particularly to a kind of lactide purification devices and lactide
Purification system.
Background technique
Fused junction crystallization is a kind of common isolation technics, it is led to according to the difference of freezing point between substance to be separated
It crosses and gradually reduces the temperature of molten mixture and reach constituent part and crystallize the solid phase for crystallizing precipitation come what is realized and have and raffinate
Different chemical compositions, thereby achieving the purpose of separation and purification.
Currently, it is pure to generally use the progress of fused junction crystallization in the industrial production of high-purity L- lactide and/or D- lactide
Change, this method can effectively remove the impurity in lactide, as water, the lactic acid of monomer, lactic acid linear dimerization body and polymer
Equal impurity, while can effectively remove meso- lactide component therein.But efficiency of this method in purifying lactide compared with
It is low, need to obtain the L- lactide and/or D- lactide of high-purity by multiple melting and crystallization process.
Utility model content
In view of this, the purpose of this utility model is to provide a kind of lactide purification devices and lactide purification system,
Efficiently separating-purifying can be carried out to lactide crude product using the device, reduce the number of lactide fusion-crystallization.
The utility model provides a kind of lactide purification devices, comprising: vertical tank and in vertical tank it is vertically disposed
Several heat exchanger tubes；Tube side fluid inlet is provided at the top of the vertical tank, bottom is provided with tube side fluid outlet；The heat exchange
The both ends of pipe are respectively arranged with the upper perforated plate and lower perforated plate closed with vertical top tank structure, the lower surface of the upper perforated plate, lower perforated plate
Upper surface, the outer wall of heat exchanger tube and the inner wall of vertical tank be formed by enclosure space and be provided with shell side fluid inlet and shell side
Fluid outlet；
The vertical tank is provided with vacuum orifice between tube side fluid inlet and upper perforated plate；
Heating tube is provided in the inner cavity of the heat exchanger tube.
Preferably, the heating tube is located on the axis of the heat exchanger tube.
Preferably, the distance of the heating pipe outer wall to heat transfer tube wall is 2~15cm.
Preferably, described device further includes the umbrella shape flow apron that vertical tank inner cavity is arranged in, the umbrella shape flow apron
It is concentric with the heat exchanger tube above the heat exchanger tube.
Preferably, the base angle of the umbrella shape flow apron is 5~15 °, and diameter is 1~1.2 times of heat exchange bore.
Preferably, the lower edge of the umbrella shape flow apron is 3~20cm apart from the heat exchanger tube top edge.
Preferably, described device further includes the fluid distributor that vertical tank inner cavity is arranged in, the height of the fluid distributor
Degree is between tube side fluid inlet and vacuum orifice.
Preferably, drain is additionally provided at the top of the vertical tank.
Preferably, several pieces of shell-side fluid flow aprons are provided in the enclosure space.
The utility model provides a kind of lactide purification system, comprising:
Among lactide purification devices, circulating pump described in above-mentioned technical proposal, lactide mother liquor tank and lactide product
Tank；
The entrance of the lactide mother liquor tank is connected with the outlet of the tube side fluid of the lactide purification devices, and described third
The discharge port of lactide mother liquor tank is connected by circulating pump with the tube side fluid inlet of the lactide purification devices；
The feed inlet of the lactide product pans is connected with the outlet of the tube side fluid of the lactide purification devices.
Compared with prior art, the utility model provides a kind of lactide purification devices and lactide purification system.This
The purification devices that utility model provides include: vertical tank and the vertically disposed several heat exchanger tubes in vertical tank；It is described vertical
Tank top is provided with tube side fluid inlet, and bottom is provided with tube side fluid outlet；The both ends of the heat exchanger tube be respectively arranged with
Vertical top tank structure closed upper perforated plate and lower perforated plate, the lower surface of the upper perforated plate, the upper surface of lower perforated plate, heat exchanger tube outer wall
It is formed by enclosure space with the inner wall of vertical tank and is provided with shell side fluid inlet and shell side fluid outlet；The vertical tank exists
Vacuum orifice is provided between tube side fluid inlet and upper perforated plate；Heating tube is provided in the inner cavity of the heat exchanger tube.The device
The course of work include: that device is preheating to demand temperature first；Then lactide crude product is entered into dress from tube side fluid inlet
It sets, lactide crude product flows down along heat transfer tube wall, and the L- lactide and/or D- lactide in lactide crude product are in heat exchanger tube
It crystallizes and is precipitated on wall；Evacuated mouth vacuumizes device later, and steps up heating tube temperature, make crystallization lactide from
Surface starts slowly to melt, and the remaining evacuated mouth of meso- lactide in the lactide of melting enters vacuum system, remaining
Lactide flows down along heat transfer tube wall.Device provided by the utility model at runtime can purify the fusion-crystallization of lactide
It is coupled with the vacuum removal method of meso- lactide, makes L- lactide and/or D- lactide from containing meso- first
It crystallizes and is precipitated in the crude lactide melt of lactide and a small amount of other impurity, L- lactide and/or D- lactide quilt is then precipitated
Slowly melting is heated from surface, while under a high vacuum, remaining meso- lactide quilt in L- lactide and/or D- lactide
Further removing obtains the L- lactide and/or D- lactide product of high-purity of the meso- lactide content less than 0.3%.This
The number of fusion-crystallization, energy saving when the device that utility model provides can reduce fused junction crystallization purifying lactide, reduces
Cost.
Detailed description of the invention
In order to illustrate the embodiment of the utility model or the technical proposal in the existing technology more clearly, below will be to embodiment
Or attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is only
It is the embodiments of the present invention, for those of ordinary skill in the art, without creative efforts, also
Other attached drawings can be obtained according to the attached drawing of offer.
Fig. 1 is lactide purification devices structural schematic diagram provided by the embodiment of the utility model；
Fig. 2 is lactide purification system structural schematic diagram provided by the embodiment of the utility model.
Specific embodiment
The following will be combined with the drawings in the embodiments of the present invention, carries out the technical scheme in the embodiment of the utility model
Clearly and completely describe, it is clear that the described embodiments are only a part of the embodiments of the utility model, rather than whole
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are without making creative work
Every other embodiment obtained, fall within the protection scope of the utility model.
The utility model provides a kind of lactide purification devices, comprising: vertical tank and in vertical tank it is vertically disposed
Several heat exchanger tubes；Tube side fluid inlet is provided at the top of the vertical tank, bottom is provided with tube side fluid outlet；The heat exchange
The both ends of pipe are respectively arranged with the upper perforated plate and lower perforated plate closed with vertical top tank structure, the lower surface of the upper perforated plate, lower perforated plate
Upper surface, the outer wall of heat exchanger tube and the inner wall of vertical tank be formed by enclosure space and be provided with shell side fluid inlet and shell side
Fluid outlet；
The vertical tank is provided with vacuum orifice between tube side fluid inlet and upper perforated plate；
Heating tube is provided in the inner cavity of the heat exchanger tube.
It is lactide purification devices structural schematic diagram provided by the embodiment of the utility model referring to Fig. 1, Fig. 1.In Fig. 1, a is
Vertical tank, b are heat exchanger tube, and c is upper perforated plate, and d is lower perforated plate, and e is tube side fluid inlet, and f is vacuum orifice, and g is tube side fluid
Outlet, h are heating tube, and i is heating tube fluid inlet, and j is heating tube fluid outlet, and k is fluid distributor, and m is umbrella shape water conservancy diversion
Baffle, n are shell side fluid inlet, and p is shell side fluid outlet, and q is shell-side fluid flow apron, and r is drain.
Lactide purification devices provided by the utility model include vertical tank a and several heat exchanger tube b, and heat exchanger tube b is vertical
It is arranged in vertical tank a, the both ends of heat exchanger tube b are respectively arranged with the upper perforated plate c and lower perforated plate d closed with vertical top tank structure, on
The upper surface of tube sheet c, the lower surface of lower perforated plate d, the inner wall of heat exchanger tube b and vertical tank a inner wall be formed by enclosure space and be
Tube side region, the lower surface of upper perforated plate c, the upper surface of lower perforated plate d, heat exchanger tube b the inner wall of outer wall and vertical tank a be formed by
Enclosure space is shell side region.
In the tube side region, tube side fluid inlet e, vacuum orifice f and tube side fluid outlet g are provided on vertical tank a.
Wherein, tube side fluid inlet e be arranged at the top of vertical tank a, vacuum orifice f setting tube side fluid inlet e and upper perforated plate c it
Between, tube side fluid exports g and is arranged in the bottom vertical tank a.In one embodiment provided by the utility model, the vertical tank a
On be additionally provided with drain r, drain r is arranged at the top of vertical tank a.
In the tube side region, the inner cavity of heat exchanger tube b is provided with heating tube h.Implement at one provided by the utility model
In example, heating tube h is located on the axis of heat exchanger tube b, and the distance of the inner wall of the outer wall of heating tube h to heat exchanger tube b is preferably 2~
15cm.In one embodiment provided by the utility model, heating tube h obtains heat by flowing through the fluid of heat, on heating tube h
The connection type being provided between heating tube fluid inlet i and heating tube fluid outlet j, heating tube h includes series, parallel, portion
Divide series connection or part in parallel.
In one embodiment provided by the utility model, in the tube side region, it is additionally provided with fluid distributor k, is flowed
The height of body distributor k is located at below tube side fluid inlet e, above vacuum orifice f.In the present invention, liquid distribution trough k
On be distributed uniform circular hole, guarantee that tube side fluid flows uniformly in each heat exchanger tube.
In one embodiment provided by the utility model, in the tube side region, it is additionally provided with umbrella shape flow apron m,
Umbrella shape flow apron m is located above heat exchanger tube b, concentric with heat exchanger tube b.In one embodiment provided by the utility model, umbrella
Shape flow apron m is located at below vacuum orifice f.In one embodiment provided by the utility model, the bottom of umbrella shape flow apron m
Angle is 5~15 °, and diameter is 1~1.2 times of heat exchange bore.In one embodiment provided by the utility model, umbrella shape water conservancy diversion
The lower edge of baffle m is 3~20cm apart from the heat exchanger tube top edge.In the present invention, umbrella shape flow apron m can guarantee pipe
Cheng Liuti uniformly flows down along heat transfer tube wall.
In the shell side region, shell side fluid inlet n and shell side fluid outlet p are provided on vertical tank a.It is practical new at this
In one embodiment that type provides, so shell side region is provided with several pieces of shell-side fluid flow apron q, for changing in shell side
The flow path of fluid makes heat exchanger tube thermally equivalent.
The course of work of lactide purification devices provided by the utility model includes: that device is preheating to demand temperature first
Degree；Then lactide crude product is entered into device from tube side fluid inlet, lactide crude product flows down along heat transfer tube wall, lactide
L- lactide and/or D- lactide in crude product crystallize precipitation in heat transfer tube wall；Evacuated mouth is taken out device true later
Sky, and heating tube temperature is stepped up, melt the lactide of crystallization slowly since surface, the remnants in the lactide of melting
The evacuated mouth of meso- lactide enters vacuum system, and remaining lactide flows down along heat transfer tube wall.
Device provided by the utility model at runtime can purify the fusion-crystallization of lactide true with meso- lactide
Empty removal methods are coupled, and make L- lactide and/or D- lactide from containing meso- lactide and a small amount of other miscellaneous first
It crystallizes and is precipitated in the crude lactide melt of matter, L- lactide and/or D- lactide is then precipitated and is heated slowly melting from surface,
Simultaneously under a high vacuum, remaining meso- lactide is further removed in L- lactide and/or D- lactide, obtains meso-
The L- lactide and/or D- lactide product of high-purity of the lactide content less than 0.3%.Device provided by the utility model can
The number of fusion-crystallization, energy saving when reducing fused junction crystallization purifying lactide, reduces cost.
The utility model provides a kind of lactide purification system, comprising:
Among lactide purification devices, circulating pump described in above-mentioned technical proposal, lactide mother liquor tank and lactide product
Tank；
The entrance of the lactide mother liquor tank is connected with the outlet of the tube side fluid of the lactide purification devices, and described third
The discharge port of lactide mother liquor tank is connected by circulating pump with the tube side fluid inlet of the lactide purification devices；
The feed inlet of the lactide product pans is connected with the outlet of the tube side fluid of the lactide purification devices.
Referring to fig. 2, Fig. 2 is lactide purification system structural schematic diagram provided by the embodiment of the utility model.In Fig. 2,1 is
Tube side fluid inlet valve, 2 be lactide product pans inlet valve, and 3 be lactide mother liquor tank to lactide disposing mother liquor
Tank valve, 4 be lactide product pans, and 5 be lactide product pans outlet valve, and 6 be circulating pump, and 7 pump out for circulation
Mouth valve, 8 be lactide mother liquor tank to pump entry valve, and 9 export total valve for lactide mother liquor tank, and 10 be lactide mother
Flow container, 11 be lactide raw materials mouth valve, and 12 export to lactide mother liquor tank inlet valve for tube side fluid, and 13 be vacuum
Valve, 14 be emptying valve, and 15 be lactide purification devices.
Lactide purification system provided by the utility model includes lactide mother liquor tank 10, circulating pump 6, in lactide product
Between tank 4 and lactide purification devices 15.Wherein, the tube side fluid of the entrance of lactide mother liquor tank 10 and lactide purification devices 15
It exports g to be connected, tube side fluid is provided on connecting line and exports to lactide mother liquor tank inlet valve 12；Lactide mother liquor tank
10 discharge port is connected by circulating pump 6 with the tube side fluid inlet e of lactide purification devices 15, along fluid on connecting line
The direction of motion is disposed with lactide mother liquor tank outlet total valve 9, lactide mother liquor tank to pump entry valve 8, circulation
Pump 6, circulating-pump outlet valve 7 and tube side fluid inlet valve 1.In one embodiment provided by the utility model, lactide
The discharge port of mother liquor tank 10 connects lactide disposing mother liquor tank, is disposed with the third friendship along fluid direction of motion on connecting line
Ester mother liquor tank exports total valve 9 and lactide mother liquor tank to lactide disposing mother liquor tank valve 3.Provided by the utility model one
In a embodiment, lactide raw materials mouth is additionally provided on lactide mother liquor tank 10, with lactide raw materials pipeline phase
Even, lactide raw materials mouth valve 11 is provided on the pipeline.
In the present invention, the tube side fluid of the feed inlet of lactide product pans 4 and lactide purification devices 15
It exports g to be connected, lactide product pans inlet valve 2 is provided on connecting line.At one provided by the utility model
In embodiment, the discharge port of lactide product pans 4 connects lactide product storage tank, is provided with lactide on connecting line
Product pans outlet valve 5.
In one embodiment provided by the utility model, the vacuum orifice f of lactide purification devices 15 is connected by cold-trap
Vacuum system is connect, vacuum valve 13 is provided on connecting line.
In one embodiment provided by the utility model, the drain r connection blowdown piping of lactide purification devices 15,
Emptying valve 14 is provided on pipeline.
The course of work of lactide purification system provided by the utility model includes (1) fusion-crystallization process and (2) vacuum
Remove meso- lactide process:
(1) fusion-crystallization process: first by system warm-up to demand temperature；Then the crude lactide in lactide mother liquor tank
Melt enters purification devices from the tube side fluid inlet of lactide purification devices by circulating pump, flows down simultaneously along heat transfer tube wall
It crystallizes and is precipitated in heat transfer tube wall, uncrystallized mother liquor is flowed into lactide mother liquor tank, the liquid level in lactide mother liquor tank
When being reduced to the 1/5~1/2 of inventory, fusion-crystallization process terminates.
(2) vacuum removal meso- lactide process: after fusion-crystallization, evacuated mouth is to lactide purification devices
It vacuumizes, and steps up lactide purification devices heating tube temperature, melt the lactide of crystallization slowly since surface, melt
The evacuated mouth of meso- lactide in the lactide melted enters vacuum system, remaining lactide (L- lactide and/or D-
Lactide) along being flowed under heat transfer tube wall in lactide product pans.
System provided by the utility model at runtime can purify the fusion-crystallization of lactide true with meso- lactide
Empty removal methods are coupled, it is possible to reduce the number of fusion-crystallization when fused junction crystallization purifying lactide, energy saving, drop
Low cost realizes the efficient purification of lactide.
For the sake of becoming apparent from, it is described in detail below by following embodiment.
Embodiment 1
Lactide purification system
A kind of lactide purification system as shown in Figure 2 is present embodiments provided, including, tube side fluid inlet valve 1, third
Lactide product pans inlet valve 2, lactide mother liquor tank to lactide disposing mother liquor tank valve 3, lactide product pans
4, lactide product pans outlet valve 5, circulating pump 6, circulating-pump outlet valve 7, lactide mother liquor tank to pump entry
Valve 8, lactide mother liquor tank export total valve 9, lactide mother liquor tank 10, lactide raw materials mouth valve 11, tube side fluid
Lactide mother liquor tank inlet valve 12, vacuum valve 13 are exported to, valve 14 and lactide purification devices 15 are vented, wherein each portion
Point position and connection relationship hereinbefore by the agency of, details are not described herein.
In the present embodiment, the structure of lactide purification devices 15 is as shown in Figure 1, include vertical tank a, heat exchanger tube b, upper tube
Plate c, lower perforated plate d, tube side fluid inlet e, vacuum orifice f, tube side fluid outlet g, heating tube h, heating tube fluid inlet i, add
Heat-pipe-fluid exports j, fluid distributor k, umbrella shape flow apron m, shell side fluid inlet n, shell side fluid outlet p, shell-side fluid
Flow apron q and drain r, the wherein position of each section and connection relationship hereinbefore by the agency of, details are not described herein.
In the present embodiment, the temperature of heat exchanger tube b is controlled that (shell side conduction oil flows through shell by the thermally conductive oil temperature of shell side
Journey fluid inlet n and shell side fluid outlet p)；The temperature of heating tube h is controlled (heating tube by the thermally conductive oil temperature of heating tube
Conduction oil flows through heating tube fluid inlet i and heating tube fluid outlet j)；Lactide mother liquor tank 10 and lactide product pans 4
It is equipped with heating and temperature controlling device；Each connecting line is equipped with thermal jacket.
Embodiment 2
Lactide crude product is purified using lactide purification system described in embodiment 1, detailed process includes:
1) preheat to system: the temperature of control heating tube conduction oil is 110~120 DEG C, and the thermally conductive oil temperature of shell side is
80~90 DEG C, connecting pipeline oil heating jacket temperature be 110~120 DEG C, lactide product pans temperature be 105~110 DEG C,
Lactide mother liquor tank temperature is 110~120 DEG C.
2) fusion-crystallization process: inspection must ensure lactide product pans inlet valve, lactide product pans
Outlet valve, vacuum valve and emptying valve are in close state.By lactide raw materials mouth valve, crude lactide is put into
(L- lactide content is 94wt%, and meso- lactide content is 5wt%), inventory is the 3/4 of lactide mother liquor tank, and is controlled
The temperature of lactide processed is 110~120 DEG C, closes lactide raw materials mouth valve.Open tube side fluid inlet valve, tube side
Fluid outlet is pumped into lactide mother liquor tank inlet valve, lactide mother liquor tank outlet total valve, lactide mother liquor tank to circulation
Mouth valve, circulating-pump outlet valve, open circulating pump；The flow of control loop pump, so that lactide is along heat transfer tube wall stream
Under, lactide is crystallized in heat transfer tube wall and is precipitated；The temperature of heat exchanger tube is slowly reduced to 40~60 DEG C, makes lactide crystal and liquid
The phase interface temperature of body is 70~90 DEG C.When lactide remaining in lactide mother liquor tank is inventory 1/4~1/3, melting
Crystallization terminates.It closes circulating pump, close tube side fluid inlet valve；To there is no material to flow into lactide in lactide purification devices
When mother liquor tank, closes tube side fluid and export to lactide mother liquor tank inlet valve, open lactide mother liquor tank to lactide mother liquor
Tank valve is recycled, the lactide mother liquor participated in is made to be all introduced into lactide disposing mother liquor tank.
3) meso- lactide vacuum removal process: after fusion-crystallization, vacuum system is opened, opens vacuum valve, is opened
The temperature control of lactide product pans inlet valve, heat exchanger tube is 85~95 DEG C, steps up the thermally conductive oil temperature of heating tube
To 160~180 DEG C, melt the L- lactide of crystallization slowly since surface, the meso- third hereafter melted in L- lactide is handed over
Ester is sublimated in cold-trap by vacuum system, realizes further separation, the L- lactide finally purified is along heat transfer tube wall stream
Under enter in lactide product pans.In meso- lactide vacuum removal process finally, heat exchanger tube temperature is controlled from 95
105 DEG C DEG C are to slowly warm up to, guarantees that lactide finally all melts, enters lactide product pans, third is finally opened and hands over
Ester product pans outlet valve exports lactide product, can be obtained the L- lactide product of high-purity.
L- lactide content is greater than 99.5wt%, meso- lactide content in the L- lactide product of the high-purity of acquisition
Less than 0.3wt%.
Embodiment 3
Lactide crude product is purified using lactide purification system described in embodiment 1, detailed process includes:
1) preheat to system: the temperature of control heating tube conduction oil is 126~135 DEG C, and the thermally conductive oil temperature of shell side is
90~110 DEG C, connecting pipeline oil heating jacket temperature is 125~135 DEG C, and lactide product pans temperature is 130~135
DEG C, lactide mother liquor tank temperature be 130~135 DEG C.
2) fusion-crystallization process: inspection must ensure lactide product pans inlet valve, lactide product pans
Outlet valve, vacuum valve and emptying valve are in close state.By lactide raw materials mouth valve, crude lactide is put into
(L- lactide content is 60wt%, and D- lactide content is 30wt%, and meso- lactide content is 9wt%), inventory third
The 3/4 of lactide mother liquor tank, and the temperature for controlling lactide is 125~135 DEG C, closes lactide raw materials mouth valve.It opens
Tube side fluid inlet valve, tube side fluid export to lactide mother liquor tank inlet valve, the outlet of lactide mother liquor tank total valve, third
Lactide mother liquor tank opens circulating pump to pump entry valve, circulating-pump outlet valve；The flow of control loop pump, so that third
Lactide is flowed down along heat transfer tube wall, and lactide is crystallized in heat transfer tube wall and is precipitated；Slowly reduce the temperature of heat exchanger tube to 40~
60 DEG C, makes 90~110 DEG C of phase interface temperature of lactide crystal and liquid, be then down to 70~90 DEG C.When lactide mother liquor
When remaining lactide is inventory 1/4~1/3 in tank, fusion-crystallization terminates.It closes circulating pump, close tube side fluid inlet valve
Door；When there is no material to flow into lactide mother liquor tank in lactide purification devices, closes tube side fluid and export to lactide mother liquor
Tank inlet valve opens lactide mother liquor tank to lactide disposing mother liquor tank valve, fully enters the lactide mother liquor participated in
To lactide disposing mother liquor tank.
3) meso- lactide vacuum removal process: after fusion-crystallization, vacuum system is opened, opens vacuum valve, is opened
The temperature control of lactide product pans inlet valve, heat exchanger tube is 85~95 DEG C, steps up the thermally conductive oil temperature of heating tube
To 160~180 DEG C, melt the lactide of crystallization slowly since surface, hereafter the meso- lactide in molten lactide is logical
It crosses vacuum system to sublimate in cold-trap, realizes that further separation, the lactide finally purified flow down entrance along heat transfer tube wall
Into lactide product pans.In meso- lactide vacuum removal process finally, the control of heat exchanger tube temperature is slow from 95 DEG C
130 DEG C are warming up to, guarantees that lactide all melts, enters lactide product pans, finally open among lactide product
Tank outlet valve exports lactide product, can be obtained the mixing of the L- lactide and D- lactide enantiomer of high chemical purity
Produce product.
L- lactide and D- lactide is total in the mix product of L- lactide and D- lactide enantiomer after purification
Content is greater than 99.5wt%, meso- lactide content and is less than 0.3wt%.
The above is only the preferred embodiment of the utility model, it is noted that for the common skill of the art
For art personnel, without departing from the principle of this utility model, several improvements and modifications can also be made, these improve and
Retouching also should be regarded as the protection scope of the utility model.
Claims (10)
1. a kind of lactide purification devices characterized by comprising vertical tank and in vertical tank vertically disposed several change
Heat pipe；Tube side fluid inlet is provided at the top of the vertical tank, bottom is provided with tube side fluid outlet；The both ends of the heat exchanger tube
Be respectively arranged with the upper perforated plate and lower perforated plate closed with vertical top tank structure, the lower surface of the upper perforated plate, lower perforated plate upper surface,
The outer wall of heat exchanger tube and the inner wall of vertical tank are formed by enclosure space and are provided with shell side fluid inlet and shell side fluid outlet；
The vertical tank is provided with vacuum orifice between tube side fluid inlet and upper perforated plate；
Heating tube is provided in the inner cavity of the heat exchanger tube.
2. purification devices according to claim 1, which is characterized in that the heating tube is located at the axis of the heat exchanger tube
On.
3. purification devices according to claim 2, which is characterized in that the distance of the heating pipe outer wall to heat transfer tube wall
For 2~15cm.
4. purification devices according to claim 1, which is characterized in that further include the umbrella shape water conservancy diversion that vertical tank inner cavity is arranged in
Baffle, the umbrella shape flow apron is located above the heat exchanger tube, concentric with the heat exchanger tube.
5. purification devices according to claim 4, which is characterized in that the base angle of the umbrella shape flow apron is 5~15 °,
Diameter is 1~1.2 times of heat exchange bore.
6. purification devices according to claim 5, which is characterized in that changed described in the lower edge distance of the umbrella shape flow apron
Heat pipe top edge is 3~20cm.
7. purification devices according to claim 1, which is characterized in that further include the fluid distrbution that vertical tank inner cavity is arranged in
Device, the height of the fluid distributor is between tube side fluid inlet and vacuum orifice.
8. purification devices according to claim 1, which is characterized in that be additionally provided with drain at the top of the vertical tank.
9. purification devices according to claim 1, which is characterized in that be provided with several blocks of shell side streams in the enclosure space
Body flow apron.
10. a kind of lactide purification system characterized by comprising
In lactide purification devices according to any one of claims 1 to 9, circulating pump, lactide mother liquor tank and lactide product
Between tank；
The entrance of the lactide mother liquor tank is connected with the outlet of the tube side fluid of the lactide purification devices, the lactide
The discharge port of mother liquor tank is connected by circulating pump with the tube side fluid inlet of the lactide purification devices；
The feed inlet of the lactide product pans is connected with the outlet of the tube side fluid of the lactide purification devices.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820512606.7U CN208426686U (en) | 2018-04-11 | 2018-04-11 | A kind of lactide purification devices and lactide purification system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820512606.7U CN208426686U (en) | 2018-04-11 | 2018-04-11 | A kind of lactide purification devices and lactide purification system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN208426686U true CN208426686U (en) | 2019-01-25 |
Family
ID=65106252
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201820512606.7U Active CN208426686U (en) | 2018-04-11 | 2018-04-11 | A kind of lactide purification devices and lactide purification system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN208426686U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113856235A (en) * | 2021-09-29 | 2021-12-31 | 浙江大华技术股份有限公司 | Cooling crystallization control method, device, electronic equipment and system |
-
2018
- 2018-04-11 CN CN201820512606.7U patent/CN208426686U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113856235A (en) * | 2021-09-29 | 2021-12-31 | 浙江大华技术股份有限公司 | Cooling crystallization control method, device, electronic equipment and system |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104192927B (en) | Phenol-acetone waste water evaporative desalination pretreating process | |
| CN1792406A (en) | Equipment for preparing high pure organic matter by fusion-crystallization method | |
| CN208426686U (en) | A kind of lactide purification devices and lactide purification system | |
| CN108031141A (en) | The process equipment and method of refined lactide | |
| CN202155070U (en) | External-circulation evaporation crystallizer | |
| CN1027963C (en) | Parametric pump fractional crystallization method and PFC crystallizer | |
| CN109621478A (en) | One kind being used for material purification & isolation static state melting crystallizer | |
| WO2011140855A1 (en) | Process for directly obtaining anhydrous sodium sulfate by flash evaporating and crystallizing and apparatus thereof | |
| CN106048262A (en) | Purifying method and purifying apparatus for gallium | |
| CN103832986A (en) | Preparation method for polyphosphoric acid | |
| CN108905265A (en) | Sodium vanadate Continuous Cooling Crystallization equipment and its production method | |
| CN101786951B (en) | Method for purifying crude acrylic acid and device thereof | |
| CN201930572U (en) | Continuous vacuum cooling crystallizing device | |
| CN2834659Y (en) | Apparatus for preparing high-purity organism by fusion crystallization method | |
| CN1171890C (en) | Prepn process and plant of high-purity eudesmin | |
| CN115364569A (en) | Mother liquor desalting and concentrating device for preparing taurine | |
| CN105418535B (en) | Fusion-crystallization refines the method and its fusion-crystallization device of the 5-chloromethyl thiazole of 2 chlorine 5 | |
| CN208617728U (en) | A kind of crystallization apparatus for ethylene carbonate purification purification | |
| CN203763893U (en) | Continuous crystallizing device for resorcinol | |
| CN209836041U (en) | Benzoic acid refining device | |
| CN208182887U (en) | A kind of Ergol low-boiling-point substance continuous production benzoic acid system | |
| CN209405724U (en) | Continuous crystallisation device | |
| CN106866367A (en) | A kind of continuous oscillation drift tube type crystallisation by cooling method of antierythrite | |
| CN208843971U (en) | A kind of system for continuous production prometryn | |
| CN102895796A (en) | Low-temperature concentration device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |