CN117180849A - Separation system and separation method for glycolide solid-liquid mixture - Google Patents
Separation system and separation method for glycolide solid-liquid mixture Download PDFInfo
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- CN117180849A CN117180849A CN202311167235.5A CN202311167235A CN117180849A CN 117180849 A CN117180849 A CN 117180849A CN 202311167235 A CN202311167235 A CN 202311167235A CN 117180849 A CN117180849 A CN 117180849A
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- glycolide
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- 238000000926 separation method Methods 0.000 title claims abstract description 93
- RKDVKSZUMVYZHH-UHFFFAOYSA-N 1,4-dioxane-2,5-dione Chemical compound O=C1COC(=O)CO1 RKDVKSZUMVYZHH-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000007788 liquid Substances 0.000 title claims abstract description 69
- 239000000203 mixture Substances 0.000 title claims abstract description 45
- 239000002904 solvent Substances 0.000 claims abstract description 68
- 238000011084 recovery Methods 0.000 claims abstract description 18
- 239000000706 filtrate Substances 0.000 claims description 48
- 239000000047 product Substances 0.000 claims description 29
- 239000002002 slurry Substances 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 19
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 abstract description 16
- 239000007791 liquid phase Substances 0.000 abstract description 7
- 239000002245 particle Substances 0.000 description 21
- 238000003825 pressing Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000007790 solid phase Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Centrifugal Separators (AREA)
Abstract
The invention discloses a separation system and a separation method of glycolide solid-liquid mixture, wherein the separation system comprises the following components: horizontal decanter centrifuges, intermediate tanks, disk centrifuges, solvent recovery tanks, and glycolide product tanks. The invention utilizes the cooperation of two centrifuges to roughly separate the solid-liquid mixture of glycolide and solvent in a grading way, so as to obtain purified solid glycolide with lower moisture content and liquid phase solvent with lower solid content.
Description
Technical Field
The invention relates to the technical field of crude glycolide purification, in particular to a system and a method for separating a solid-liquid mixture of glycolide, which are used for purifying crude glycolide and interweaving, and the solid-liquid mixture of glycolide and a solvent is separated in a grading way by utilizing the cooperation of two centrifuges so as to obtain purified solid glycolide with lower moisture content and a liquid-phase solvent with lower solid content.
Background
The centrifugal machine is one of the main equipment of chemical equipment, and is also solid-liquid separation equipment commonly applied in the field of coal chemical industry. The main task of the centrifugal machine is to separate solid particles from liquid phase in the feed liquid by the action of centrifugal force.
In general, the feed liquid of the centrifugal machine is a solid-liquid mixture generated in the production process, and solid phase and liquid phase in the feed liquid produced in the production device are separated and recycled. The material liquid is directly conveyed to the centrifugal machine through a pipeline, the sedimentation speed of particles in the liquid is accelerated by utilizing the strong centrifugal force generated by the high-speed rotation of the rotor of the centrifugal machine, substances with different sedimentation coefficients and buoyancy densities in the sample are separated, and the separated substances with different phases are conveyed to a subsequent production unit through different pipelines.
In the actual production process, as different centrifuges have different separation particle size ranges, the sizes and densities of solid particles are different, the centrifugal separation effect is also different, and the load of the centrifuges is sometimes increased when the particle size is too large; when the particle size is too small, solid particles with smaller particle size cannot be separated out, and liquid phase is sent to subsequent equipment, so that the load of the subsequent equipment is increased or blocked, abnormal operation of the equipment is caused, and the service life of the equipment is even shortened.
In the existing solid-liquid separation scheme, two centrifuges of the same type are often connected in series to sequentially centrifugally separate feed liquid, and as the separation particle size ranges of the two centrifuges of the same type are the same, the secondary separation effect is poor, when the particle size range of solid particles in the feed liquid is larger, the solid particles with smaller particle size cannot be removed, the expected effect cannot be achieved, turbidity and precipitation of the feed liquid are easy to occur, and the subsequent equipment is blocked, so that the normal operation of production is influenced; and two centrifuges with large separation particle size range are connected in series, so that the load of the centrifuges is overlarge, the normal operation of equipment is influenced, and the service life of the equipment is shortened.
CN202110960873.7 discloses a method for purifying crude glycolide, comprising a step of washing and separating crude glycolide with a solvent a and a solvent B, respectively, and optionally a step of recrystallizing and separating the washed crude glycolide with a solvent B; the solid-liquid separation operation can be performed in a nitrogen filter pressing device, a plate-frame filter pressing device, a centrifugal filter pressing device or various centrifuges, and is preferably performed in the plate-frame filter pressing device and the centrifugal filter pressing device, so that the separation effect is poor.
Disclosure of Invention
The invention aims to provide a separation system and a separation method of a glycolide solid-liquid mixture, so as to obtain purified solid glycolide with low moisture content and a liquid phase solvent with low solid content.
In order to achieve the above object, the separation system provided by the present invention adopts the following technical scheme:
a separation system for a glycolide solid-liquid mixture, the separation system comprising:
the horizontal decanter centrifuge is respectively connected with a mixture feeding pipe and a slurry outlet of the disk centrifuge at a feeding inlet, and is used for carrying out solid-liquid separation on a mixture of coarse ethyl interweaving and solvent from the mixture feeding pipe and glycolide slurry from the disk centrifuge so as to obtain a first filtrate and glycolide product;
the inlet of the intermediate tank is connected with the filtrate outlet of the horizontal decanter centrifuge and is used for receiving the first filtrate;
a bowl centrifuge configured to perform solid-liquid separation of the feed liquid from the intermediate tank to obtain a second filtrate and glycolide slurry;
a solvent recovery tank for receiving the second filtrate; and
a glycolide product tank for receiving the glycolide product.
Preferably, the separation system according to the present invention further comprises a transfer pump for feeding the feed liquid from the intermediate tank to the bowl centrifuge.
According to the separation system of the present invention, preferably, the separation system further includes a plate filter press disposed between the intermediate tank and the decanter centrifuge, and configured to perform solid-liquid separation on the first filtrate from the decanter centrifuge, and send the obtained third filtrate to the intermediate tank, and press-filtered material enters the decanter centrifuge, for example, directly enters the decanter centrifuge or enters the decanter centrifuge after being mixed with the mixture, so as to reduce the solid content entering the disk centrifuge, and finally reduce the solid content in the recovered solvent.
The separation system according to the present invention preferably further comprises a mixing tank for mixing coarse b-interweaving with solvent, connected to the decanter centrifuge by the mixture feed pipe.
According to the separation system of the invention, preferably, the intermediate tank is a settling tank for settling the received filtrate, and sending the settled lower-layer feed liquid into the disc centrifuge and the supernatant liquid into the mixing tank as part of the solvent, so that the solid-liquid separation effect of the invention is improved, on one hand, the supernatant liquid removing mixing tank is beneficial to combining the difficult-to-separate fine particles in the supernatant liquid with the rest solid particles so as to facilitate the subsequent separation, and on the other hand, the two-phase cooperation can obviously improve the separation effect due to the relatively reduced feed liquid amount going to the disc centrifuge, the reduced processing load and the reduced difficult-to-separate particle amount.
According to the separation system of the present invention, preferably, the separation system is further provided with a plurality of solvent flushing pipes for introducing a solvent to flush the equipment in the separation system and a nitrogen pipe for introducing nitrogen protection into the equipment for performing solid-liquid separation in the separation system.
In order to achieve the other aspect of the above object, the present invention also provides a separation method for performing solid-liquid separation on a mixture of coarse b-interweaving and solvent by using the above separation system.
Preferably, the glycolide content in the mixture is 5-40wt%, such as 10wt%, 20wt% or 35wt%, preferably 10-30wt%.
Preferably, the solvent is isopropanol.
In some embodiments, the glycolide product has a solvent content of no more than 15wt%, preferably no more than 10wt%; the glycolide content of the second filtrate is not more than 10wt%, such as 8wt%, preferably not more than 5wt%.
Compared with the prior art, the invention has the following advantages:
in the invention, when the crude glycolide is treated, the mixture of the crude glycolide and the solvent is treated by using a horizontal screw-disc type centrifuge, the advantages of the two centrifuges are fully utilized, and the solid particles with different particle size ranges are subjected to targeted centrifugal separation in sequence. The feed liquid is firstly sent to a horizontal screw centrifuge to separate coarse glycolide with larger particle size, the content of the coarse glycolide in the feed liquid is reduced, then clear liquid is sent to a disk centrifuge again, the coarse glycolide with smaller particle size is subjected to secondary centrifugal separation, the glycolide in the feed liquid is fully recovered, the content of solid particles in a solvent is reduced, and the influence on subsequent equipment is reduced; and meanwhile, the solid phase separated by the disc type centrifugal machine returns to the inlet of the horizontal decanter centrifugal machine for continuous concentration, only one clear liquid is discharged from the whole system, and only one solid phase discharge port is provided, so that the effective separation of solid and liquid phases is realized, and the material recovery rate and the production efficiency are improved.
Drawings
FIG. 1 shows a schematic view of one embodiment of a separation system of the present invention;
FIG. 2 shows a schematic view of another embodiment of the separation system of the present invention;
FIG. 3 shows a schematic view of yet another embodiment of the separation system of the present invention;
reference numerals illustrate:
1-an intermediate tank; 2-a delivery pump; 3-horizontal decanter centrifuge; a 4-glycolide product tank; 5-disc centrifuge; 6-a solvent recovery tank; 7-a plate and frame filter press; 8-a mixing tank;
(1) -a mixture of crude glycolide and isopropanol solvent; (2) -isopropanol solvent; (3) -depressurising nitrogen.
Detailed Description
In order that those skilled in the art will better understand the present invention, a technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and the claims of the present invention and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate in order to describe the embodiments of the invention herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
FIG. 1 shows a schematic diagram of one embodiment of a separation system provided by the present invention, including decanter centrifuges, intermediate tanks, disk centrifuges, solvent recovery tanks, glycolide product tanks, feed pumps, and mixing tanks; the feeding port of the horizontal decanter centrifuge is respectively connected with the mixture feeding pipe and the slurry outlet of the disk centrifuge and is used for carrying out solid-liquid separation on the mixture of coarse ethyl interweaving and solvent from the mixture feeding pipe and glycolide slurry from the disk centrifuge so as to obtain first filtrate and glycolide products. The glycolide product tank is for receiving the glycolide product.
The mixing tank is used for mixing coarse b interweaving and solvent, and is connected to the decanter centrifuge through the mixture feeding pipe. And an inlet of the intermediate tank is connected with a filtrate outlet of the horizontal decanter centrifuge and is used for receiving the first filtrate. The delivery pump is used for delivering the feed liquid from the intermediate tank into the disc centrifuge.
The disk centrifuge is configured to perform solid-liquid separation of the feed liquid from the intermediate tank to obtain a second filtrate and glycolide slurry. The solvent recovery tank is used for receiving the second filtrate for subsequent solvent recovery and utilization.
In addition, the separation system is also provided with a plurality of solvent flushing pipes and a nitrogen pipe, wherein the solvent flushing pipes are used for introducing solvents to flush equipment in the separation system, and the nitrogen pipe is used for introducing nitrogen protection into the equipment for solid-liquid separation in the separation system.
In operation, the mixture of crude glycolide and solvent is sent to a decanter centrifuge 3 for centrifugal separation, the separated slurry is sent to a glycolide dissolution tank 4 as a glycolide product, and the separated first filtrate is sent to an intermediate tank 1. The feed liquid in the intermediate tank 1 is sent to a disk centrifuge 5 for centrifugal separation by a delivery pump 2, the separated second filtrate is sent to a solvent recovery tank 6, and the separated glycolide slurry is returned to a horizontal decanter centrifuge 3 for centrifugal separation. In addition, the horizontal decanter centrifuge 3, the disk centrifuge 5 and the conveying pump 2 are also washed intermittently or with isopropanol solvent during shutdown, so that the deposition of solid-phase materials in equipment and pipelines is reduced, and the normal operation of the equipment is ensured; in addition, during operation, the operation of decanter centrifuge 3 and disk centrifuge 5 is protected with reduced pressure nitrogen to avoid air leaking into the system to form an explosive mixture with the vapor phase solvent, and nitrogen is also used for centrifuge mechanical seal protection.
FIG. 2 shows a schematic diagram of another embodiment of the separation system provided by the present invention, including decanter centrifuges, intermediate tanks, disk centrifuges, solvent recovery tanks, glycolide product tanks, feed pumps, mixing tanks, and plate and frame filter presses; the feeding port of the horizontal decanter centrifuge is respectively connected with the mixture feeding pipe and the slurry outlet of the disk centrifuge and is used for carrying out solid-liquid separation on the mixture of coarse ethyl interweaving and solvent from the mixture feeding pipe and glycolide slurry from the disk centrifuge so as to obtain first filtrate and glycolide products. The glycolide product tank is for receiving the glycolide product.
The mixing tank is used for mixing coarse b interweaving and solvent, and is connected to the decanter centrifuge through the mixture feeding pipe.
The plate filter press is arranged between the intermediate tank and the decanter centrifuge and is used for carrying out solid-liquid separation on the first filtrate from the decanter centrifuge, and sending the obtained third filtrate into the intermediate tank and the filter pressing material to enter the decanter centrifuge.
And an inlet of the intermediate tank is connected with a filtrate outlet of the plate-and-frame filter press and is used for receiving the third filtrate. The delivery pump is used for delivering the feed liquid from the intermediate tank into the disc centrifuge.
The disk centrifuge is configured to perform solid-liquid separation of the feed liquid from the intermediate tank to obtain a second filtrate and glycolide slurry. The solvent recovery tank is used for receiving the second filtrate for subsequent solvent recovery and utilization.
FIG. 3 shows a schematic diagram of one embodiment of a separation system provided by the present invention, including decanter centrifuges, intermediate tanks, disk centrifuges, solvent recovery tanks, glycolide product tanks, feed pumps, and mixing tanks; the feeding port of the horizontal decanter centrifuge is respectively connected with the mixture feeding pipe and the slurry outlet of the disk centrifuge and is used for carrying out solid-liquid separation on the mixture of coarse ethyl interweaving and solvent from the mixture feeding pipe and glycolide slurry from the disk centrifuge so as to obtain first filtrate and glycolide products. The glycolide product tank is for receiving the glycolide product.
The mixing tank is used for mixing coarse b interweaving and solvent, and is connected to the decanter centrifuge through the mixture feeding pipe.
The middle tank is a settling tank, an inlet of the middle tank is connected with a filtrate outlet of the decanter centrifuge and is used for settling the received filtrate, and the settled lower-layer feed liquid is pumped into the dish-type centrifuge and the supernatant liquid is used as a part of solvent (namely, replaces a part of original solvent) to be sent into the mixing tank by a conveying pump.
The disk centrifuge is configured to perform solid-liquid separation of the feed liquid from the intermediate tank to obtain a second filtrate and glycolide slurry. The solvent recovery tank is used for receiving the second filtrate for subsequent solvent recovery and utilization.
The invention is further illustrated by the following examples:
example 1
The mixture of crude glycolide and isopropanol solvent (glycolide content 25 wt%) was subjected to separation treatment at room temperature using the separation system described in fig. 1.
The mixture is first sent to a decanter centrifuge 3 for centrifugation, the separated slurry is sent as glycolide product to a glycolide dissolution tank 4, and the separated first filtrate is sent to an intermediate tank 1. The feed liquid in the intermediate tank 1 is sent to a disk centrifuge 5 for centrifugal separation by a delivery pump 2, the separated second filtrate is sent to a solvent recovery tank 6, and the separated glycolide slurry is returned to a horizontal decanter centrifuge 3 for centrifugal separation.
The glycolide product was tested for a solvent content of about 12wt%; the glycolide content of the second filtrate is 9wt%
Example 2
The mixture of crude glycolide and isopropanol solvent (glycolide content 25 wt%) was subjected to separation treatment at room temperature using the separation system described in fig. 2.
The mixture is firstly sent to a horizontal decanter centrifuge 3 for centrifugal separation, the separated slurry is sent to a glycolide dissolving tank 4 as glycolide product, the separated first filtrate is sent to a plate filter press for solid-liquid separation, and the separated third filtrate is sent to a middle tank 1 and the filter pressing material is sent to the horizontal decanter centrifuge. The feed liquid in the intermediate tank 1 is sent to a disk centrifuge 5 for centrifugal separation by a delivery pump 2, the separated second filtrate is sent to a solvent recovery tank 6, and the separated glycolide slurry is returned to a horizontal decanter centrifuge 3 for centrifugal separation.
The glycolide product was tested for a solvent content of about 12wt%; the glycolide content of the second filtrate was about 8wt%.
Example 3
The mixture of crude glycolide and isopropanol solvent (glycolide content 25 wt%) was subjected to separation treatment at room temperature using the separation system described in fig. 3.
The mixture is first sent to a decanter centrifuge 3 for centrifugation, the separated slurry is sent as glycolide product to a glycolide dissolution tank 4, and the separated first filtrate is sent to a settling tank as intermediate tank 1. And delivering the lower-layer feed liquid settled in the settling tank into the disc-type centrifugal machine and delivering the supernatant into the mixing tank by using a delivery pump. The second filtrate of the lower layer feed liquid separated by the disk centrifuge 5 is sent to the solvent recovery tank 6, and the separated glycolide slurry is returned to the horizontal decanter centrifuge 3 for centrifugal separation.
The glycolide product was tested for a solvent content of about 11wt%; the glycolide content of the second filtrate was about 5wt%.
Comparative example 1
The difference from example 1 is that the decanter centrifuge is replaced with a plate and frame filter press, and the rest is the same.
The solvent content of the glycolide product is detected to be more than 20wt%; the glycolide content of the second filtrate exceeds 10wt%.
As is evident from the comparison of examples 1-3 and comparative example 1 above, an effective separation of glycolide from solvent can be achieved by employing the separation system of the present invention by the combination of a decanter centrifuge with a disk centrifuge. In addition, the separation effect is further improved obviously after the sedimentation tank is adopted in the example 3, and the glycolide yield is also improved obviously compared with the examples 1 and 2.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. Not all embodiments are exhaustive. All obvious variations or modifications which come within the spirit of the invention are desired to be protected.
Claims (10)
1. A system for separating a glycolide solid-liquid mixture, the system comprising:
the horizontal decanter centrifuge is respectively connected with a mixture feeding pipe and a slurry outlet of the disk centrifuge at a feeding inlet, and is used for carrying out solid-liquid separation on a mixture of coarse ethyl interweaving and solvent from the mixture feeding pipe and glycolide slurry from the disk centrifuge so as to obtain a first filtrate and glycolide product;
the inlet of the intermediate tank is connected with the filtrate outlet of the horizontal decanter centrifuge and is used for receiving the first filtrate;
a bowl centrifuge configured to perform solid-liquid separation of the feed liquid from the intermediate tank to obtain a second filtrate and glycolide slurry;
a solvent recovery tank for receiving the second filtrate; and
a glycolide product tank for receiving the glycolide product.
2. The separation system of claim 1, further comprising a transfer pump for transferring feed liquid from the intermediate tank to the bowl centrifuge.
3. The separation system according to claim 1 or 2, further comprising a plate filter press arranged between the intermediate tank and the decanter centrifuge for performing solid-liquid separation of the first filtrate from the decanter centrifuge and feeding the obtained third filtrate into the intermediate tank and press filter into the decanter centrifuge.
4. A separation system according to any one of claims 1-3, further comprising a mixing tank for mixing coarse b-interweaving with solvent, connected to the decanter centrifuge by the mixture feed pipe.
5. The separation system of claim 4 wherein the intermediate tank is a settling tank for settling the received filtrate and feeding the settled lower feed liquid to the bowl centrifuge and the supernatant liquid as part of the solvent to the mixing tank.
6. The separation system of any one of claims 1-5, further comprising a plurality of solvent flushing pipes for introducing solvent to flush equipment in the separation system and nitrogen pipes for introducing nitrogen protection into the equipment for solid-liquid separation in the separation system.
7. A separation method for solid-liquid separation of a mixture of crude ethyl interweaving and a solvent using the separation system according to any one of claims 1 to 6.
8. The method according to claim 7, characterized in that the glycolide content in the mixture is 5-40wt%, preferably 10-30wt%.
9. The method according to claim 7 or 8, wherein the solvent is isopropanol.
10. The method according to any one of claims 7 to 9, wherein the glycolide product has a solvent content of no more than 15wt%, preferably no more than 10wt%; the glycolide content in the second filtrate is not more than 10wt%, preferably not more than 5wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311167235.5A CN117180849A (en) | 2023-09-11 | 2023-09-11 | Separation system and separation method for glycolide solid-liquid mixture |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311167235.5A CN117180849A (en) | 2023-09-11 | 2023-09-11 | Separation system and separation method for glycolide solid-liquid mixture |
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| CN117180849A true CN117180849A (en) | 2023-12-08 |
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| CN202311167235.5A Pending CN117180849A (en) | 2023-09-11 | 2023-09-11 | Separation system and separation method for glycolide solid-liquid mixture |
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| Country | Link |
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| CN (1) | CN117180849A (en) |
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- 2023-09-11 CN CN202311167235.5A patent/CN117180849A/en active Pending
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