CN211199085U - Full-continuous PBS production equipment - Google Patents

Full-continuous PBS production equipment Download PDF

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Publication number
CN211199085U
CN211199085U CN201922261522.8U CN201922261522U CN211199085U CN 211199085 U CN211199085 U CN 211199085U CN 201922261522 U CN201922261522 U CN 201922261522U CN 211199085 U CN211199085 U CN 211199085U
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kettle
polymerization
bdo
micromolecule
prepolymerization
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卢旭坤
张宗正
季学广
张弛
季锋
王志军
高剑
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Polytex Chemical Engineering Co ltd
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Polytex Chemical Engineering Co ltd
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Abstract

The utility model relates to a production facility of full continuous PBS, including joining in marriage the thick liquid cauldron, the cauldron of esterifying, the cauldron of prepolymerization, prepolymerization vacuum system, polymeric kettle, polymeric vacuum system, cut grain system, technology tower, the little molecule desorption device of prepolymerization, the little molecule desorption device of polymerization, the BDO recycling system that the retrieval and utilization BDO jar is constituteed etc. join in marriage the thick liquid cauldron top and be provided with gas phase condenser, the bottom passes through the thick liquid pump and links to each other with the cauldron of esterifying, the cauldron top links to each other with technology tower lower part, the cauldron bottom of esterifying links to each other through esterifying thing delivery pump and prepolymerization cauldron middle part; the gas phase of the prepolymerization kettle is sequentially connected with a prepolymerization micromolecule removing device and a prepolymerization vacuum system, and the bottom of the prepolymerization kettle is connected with the bottom of the front end of the polymerization kettle through a prepolymer delivery pump and a prepolymer filter; the gas phase of the polymerization kettle is sequentially connected with a polymerization micromolecule removing device and a polymerization vacuum system, and the bottom of the polymerization kettle is connected with a grain cutting system through a melt pump and a melt filter; the pre-polymerization micromolecule removing device and the polymerization micromolecule removing device are connected with the recycling BDO tank.

Description

Full-continuous PBS production equipment
Technical Field
The utility model belongs to the biodegradable high polymer material field especially relates to a full continuous PBS's production facility.
Background
With the problem of white pollution and the increasing risk of non-renewable energy sources, the development and use of biodegradable plastics has become one of the effective ways to alleviate this problem.
The poly (butylene succinate) (PBS) is an aliphatic polyester material with excellent performance, the existence of carbonyl in the structure endows the PBS with excellent degradation performance, the PBS can be completely degraded into H2O and CO2 with good environmental compatibility under natural conditions, the PBS also has excellent mechanical property and processing performance, the application is wide, and the PBS can be used for preparing disposable shopping bags, biomedical high polymer materials, packaging bottles and the like. The PBS product waste can be quickly degraded in soil or water, the degradation product is non-toxic, the raw material succinic acid can be obtained by biological fermentation of crops, and the PBS product waste is an ecologically recyclable polymer synthetic material.
PBS can be obtained by direct esterification of succinic acid and BDO, but the PBS prepared by the production equipment has low yield, low viscosity, large raw material consumption and poor economy.
SUMMERY OF THE UTILITY MODEL
The utility model aims at solving the above difficult point, provide a reasonable in process, degree of automation is high, and production efficiency is high, product quality is stable, moves the full continuous PBS's of safety and stability production facility.
The purpose of the utility model is realized like this:
a full-continuous PBS production device comprises a pulping system for mixing and pulping oxalic acid melt and BDO, an esterification reaction system for carrying out esterification reaction on the mixed pulp, a polycondensation reaction system for carrying out pre-polycondensation and polymerization reaction on the esterified substance, a granulating system for granulating the melt after the pre-polycondensation and polymerization, a recycling BDO system for recycling coarse BDO such as a pre-polymerization micromolecule removing device and a polymerization micromolecule removing device, it is characterized in that the pulping system comprises a pulp preparation kettle, a BDO metering device, an oxalic acid melt metering device and a gas phase condenser, the BDO metering device, the oxalic acid melt metering device and the gas phase condenser are all arranged at the top of the slurry preparation kettle, the BDO metering device is arranged at the junction of the recycled BDO and the fresh BDO, the device comprises a slurry preparation kettle, a BDO amount used for metering the amount of the oxalic acid melt entering the slurry preparation kettle, and an oxalic acid melt metering device used for metering the amount of the oxalic acid melt entering the slurry preparation kettle;
the esterification reaction system comprises an esterification kettle, a process tower and an esterification product delivery pump, wherein the top of the esterification kettle is connected with the bottom of a slurry preparation kettle through a slurry pump, the top of the esterification kettle is connected with the middle of the process tower through a pipeline gas phase, gas generated by the esterification kettle enters the process tower through a pipeline to be separated, the gas is separated into a light component and BDO, the light component is discharged through a gas outlet at the upper part of the process tower, and the BDO is delivered back to the esterification kettle and the slurry preparation kettle again through a recycling BDO pump arranged right below the process tower;
the polycondensation reaction system comprises a prepolymerization kettle, a prepolymer delivery pump, a prepolymer filter, a polymerization kettle, a melt pump and a melt filter, wherein the middle part of the prepolymerization kettle is connected with the bottom of the esterification kettle through an esterified substance delivery pump, the esterified substance delivery pump is used for delivering esterified substances in the esterification kettle to the prepolymerization kettle for a prepolycondensation reaction, the prepolymer delivery pump and the prepolymer filter are both arranged at the lower part of the prepolymerization kettle, the bottom of the prepolymerization kettle is sequentially connected with the bottom of the front end of the polymerization kettle through the prepolymer delivery pump and the prepolymer filter, prepolymers in the prepolymerization kettle are pressurized through the prepolymer delivery pump and then filtered through the prepolymer filter and then sent into the polymerization kettle for a polymerization reaction, the melt pump and the melt filter are arranged below the polymerization kettle, the bottom of the polymerization kettle is sequentially connected with a pelletizing system through the melt pump and the melt filter, melts in the polymerization kettle are pressurized through the melt pump, Filtering the mixture by a melt filter, and then feeding the mixture into a granulating system for granulating;
the recycling BDO system comprises a recycling BDO tank, a pre-polymerization micromolecule removing device and a polymerization micromolecule removing device, the prepolymerization micromolecule removing device is connected with the top of the prepolymerization kettle, the tops of the prepolymerization micromolecule removing device and the polymerization micromolecule removing device are respectively connected with a prepolymerization vacuum system and a polymerization vacuum system, the bottoms of the prepolymerization micromolecule removing device and the polymerization micromolecule removing device are respectively connected with a recycling BDO tank, the gas generated after the reaction of the prepolymerization reactor and the polymerization reactor respectively enters a prepolymerization vacuum system and a polymerization vacuum system after BDO, water and micromolecules are removed in a prepolymerization micromolecule removing device and a polymerization micromolecule removing device, the pre-polymerization micromolecule removing device and the polymerization micromolecule removing device remove BDO, water and the like and enter a recycling BDO tank, the recycling BDO tank is connected with the middle part of the process tower through a pump pipeline, and the recycling liquid in the recycling BDO is refined by the process tower and then is conveyed back to the esterification kettle and the slurry preparation kettle again;
furthermore, the BDO and the oxalic acid melt are metered by the slurry preparation kettle through the BDO metering device and the oxalic acid melt metering device and then are added into the slurry preparation kettle simultaneously according to a certain proportion, so that full-automatic pulping is realized.
Furthermore, a pipeline for connecting the process tower and the esterification kettle is provided with a catalyst feeding port which is a main catalyst feeding point of the whole device process;
furthermore, the prepolymerization reactor adopts a chamber-divided structure, so that the combination of two reaction forms of horizontal pushing and full mixing is realized, the efficiency of the reactor is improved, and the bottom of the reactor is provided with a catalyst feeding port, so that the reaction is convenient to adjust;
furthermore, the polymerization kettle is a double-shaft disc stirring vacuum reactor, a plurality of film forming discs are arranged on two stirring shafts to form two disc stirring systems, so that the viscosity of the product can be conveniently adjusted;
further, the BDO entering the slurry preparation kettle mainly comes from recycled BDO sent out by the process tower, and the insufficient part is supplemented by fresh BDO in front of the BDO metering device.
Compared with the prior art, the beneficial effects of the utility model reside in that:
the utility model discloses compact structure, reasonable in process, degree of automation is high, and production efficiency is high, product quality is stable, operation safety and stability. The full-automatic slurry preparation of BDO and oxalic acid is realized; the prepolymerization reactor adopts a chamber-divided structure, so that the combination of two reaction forms of horizontal pushing and full mixing is realized, and the efficiency of the reactor is improved; the polymerization kettle is a double-shaft disc stirring vacuum reactor, and a plurality of film forming discs are arranged on two stirring shafts to form two disc stirring systems, so that the viscosity of the product can be conveniently adjusted; good BDO recycling mechanism and reduced BDO consumption. Thereby realizing efficient and economic PBS production.
Drawings
Fig. 1 is a schematic flow chart of the present invention.
1. A slurry preparation kettle; 2. a slurry delivery pump; 3. an esterification kettle; 4. a process tower; 5 an ester delivery pump; 6. a prepolymerization kettle; 7. a prepolymer delivery pump; 8. a prepolymer filter; 9. a polymerization kettle; 10. a melt pump; 11. a melt filter; 12. a pelletizing system; 13. a BDO metering device; 14. an oxalic acid melt metering device; 15. a gas phase condenser; 16. recycling the BDO tank; 17. a pre-polymerization micromolecule removing device; 18. a prepolymerization vacuum system; 19. a polymerized micromolecule removing device; 20. polymerization vacuum system.
Detailed Description
As shown in figure 1, the pulping system of the production equipment of the fully continuous PBS comprises a pulp preparation kettle 1, a BDO metering device 13, an oxalic acid melt metering device 14 and a gas phase condenser 15, wherein the BDO metering device 13, the oxalic acid melt metering device 14 and the gas phase condenser 15 are all arranged at the top of the pulp preparation kettle 1, recycled BDO and fresh BDO are mixed, are metered by the BDO metering device 13 and then are added into the pulp preparation kettle with oxalic acid metered by the oxalic acid melt metering device 14 according to a certain proportion, and the pulped pulp is conveyed into an esterification kettle 3 through a pulp conveying pump 2.
As shown in figure 1, the esterification reaction system of the fully continuous PBS production equipment comprises an esterification kettle 3, a process tower 4 and an esterification product delivery pump 5, wherein slurry delivered by the slurry delivery pump 2 enters the esterification kettle 3 to perform esterification reaction, the reaction temperature is controlled to be 160-220 ℃, the reaction pressure is 30-90 KPa (A), a catalyst and reflux BDO are added at the bottom of the reaction kettle, and an esterified product is delivered to a pre-polycondensation reaction kettle 6 through the esterification product delivery pump 5. The water produced by the esterification, tetrahydrofuran and a large amount of BDO are separated by a gas phase pipeline to a process tower 4.
As shown in FIG. 1, a polycondensation reaction system of a full-continuous PBS production device comprises a prepolymerization reactor 6, a prepolymer delivery pump 7, a prepolymer filter 8, a polymerization reactor 9, a melt pump 10 and a melt filter 11. After the esterified substance enters a prepolymerization kettle 6, a prepolymerization reaction is carried out, the reaction temperature of the prepolymerization kettle is controlled to be 230-250 ℃, the reaction pressure is 1-10 KPa (A), and the reacted prepolymer passes through a prepolymer delivery pump 7, is filtered by a prepolymer filter 8 and enters a polymerization kettle 9. And (3) after the prepolymer enters a final polymerization kettle, carrying out polymerization reaction, wherein the reaction temperature is controlled to be 230-250 ℃, and the reaction pressure is 0.02-1 KPa (A). The melt after reaction has high viscosity, is conveyed by a melt pump 10, is filtered by a melt filter 11, and is sent to a granulating system 12 for granulation.
As shown in fig. 1, a recycling BDO system of a fully continuous PBS production facility includes a recycling BDO tank 16, a pre-polymerization small molecule removal device 17, a polymerization small molecule removal device 19, and the like. The process gas reacted by the prepolymerization kettle 6 and the polymerization kettle 9 respectively enters a prepolymerization vacuum system 18 and a polymerization vacuum system 20 after BDO, water and micromolecules are removed by a prepolymerization micromolecule removing device 17 and a polymerization micromolecule removing device 19, the removed BDO, water and the like enter a recycling BDO tank 16, the recycling liquid in the recycling BDO tank 16 is refined by a process tower 4 and then is conveyed back to the esterification kettle 3 for backflow and the slurry preparation kettle 1 for slurry preparation, and the part of the slurry preparation kettle 1, which needs insufficient BDO, is supplemented by fresh BDO.
The utility model discloses compact structure, reasonable in process, degree of automation is high, and production efficiency is high, product quality is stable, operation safety and stability. The full-automatic slurry preparation of BDO and oxalic acid is realized; the prepolymerization reactor adopts a chamber-divided structure, so that the combination of two reaction forms of horizontal pushing and full mixing is realized, and the efficiency of the reactor is improved; the polymerization kettle is a double-shaft disc stirring vacuum reactor, and a plurality of film forming discs are arranged on two stirring shafts to form two disc stirring systems, so that the viscosity of the product can be conveniently adjusted; good BDO recycling mechanism, reduced BDO consumption, and further realizes efficient and economic PBS production.
The present invention is not limited to the above embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some replacements and transformations for some technical features without creative labor according to the disclosed technical contents, and these replacements and transformations are all within the protection scope of the present invention.

Claims (6)

1. The full-continuous PBS production equipment comprises a pulping system for mixing and pulping oxalic acid melt and BDO, an esterification reaction system for carrying out esterification reaction on the mixed pulp, a polycondensation reaction system for carrying out pre-polycondensation and polymerization reaction on the esterified substance, a granulating system for granulating the melt after the pre-polycondensation and polymerization, and a recycling BDO system for recycling coarse BDO such as a pre-polymerization small molecule removing device and a polymerization small molecule removing device, and is characterized in that the pulping system comprises a pulp preparation kettle (1), a BDO metering device (13), an oxalic acid melt metering device (14) and a gas phase condenser (15), wherein the BDO metering device (13), the oxalic acid melt metering device (14) and the gas phase condenser (15) are all arranged at the top of the pulp preparation kettle (1), and the BDO metering device (13) is arranged at the junction of the recycling BDO and the fresh BDO, the device is used for metering the BDO amount entering the slurry preparation kettle (1), and the oxalic acid melt metering device (14) is used for metering the oxalic acid melt amount entering the slurry preparation kettle (1);
the esterification reaction system comprises an esterification kettle (3), a process tower (4) and an esterification product delivery pump (5), wherein the top of the esterification kettle (3) is connected with the bottom of a slurry preparation kettle (1) through a slurry pump (2), the top of the esterification kettle (3) is connected with the middle of the process tower (4) through a pipeline gas phase, gas generated by the esterification kettle (3) enters the process tower (4) through a pipeline for separation, the gas is separated to obtain a light component and BDO, the light component is discharged through a gas outlet at the upper part of the process tower (4), and the BDO is re-delivered back to the esterification kettle (3) and the slurry preparation kettle (1) through a BDO pump arranged right below the process tower (4);
the polycondensation reaction system comprises a prepolymerization kettle (6), a prepolymer delivery pump (7), a prepolymer filter (8), a polymerization kettle (9), a melt pump (10) and a melt filter (11), wherein the middle part of the prepolymerization kettle (6) is connected with the bottom of the esterification kettle (3) through an esterification delivery pump (5), the esterification delivery pump (5) is used for delivering an esterification product in the esterification kettle (3) to the prepolymerization kettle (6) for carrying out a prepolycondensation reaction, the prepolymer delivery pump (7) and the prepolymer filter (8) are both arranged at the lower part of the prepolymerization kettle (6), the bottom of the prepolymerization kettle (6) is connected with the bottom of the front end of the polymerization kettle (9) through the prepolymer delivery pump (7) and the prepolymer filter (8) in sequence, a prepolymer in the prepolymerization kettle (6) is pressurized through the prepolymer delivery pump (7), then is filtered through the prepolymer filter (8) and then is delivered to the polymerization kettle (9) for carrying out a polymerization reaction, a melt pump (10) and a melt filter (11) are arranged below the polymerization kettle (9), the bottom of the polymerization kettle (9) is connected with a granulating system (12) through the melt pump (10) and the melt filter (11) in sequence, and melt in the polymerization kettle (9) is pressurized through the melt pump (10), filtered through the melt filter (11) and then sent into the granulating system (12) for granulating;
the recycling BDO system comprises a recycling BDO tank (16), a pre-polymerization micromolecule removing device (17) and a polymerization micromolecule removing device (19), wherein the pre-polymerization micromolecule removing device (17) is connected with the top of the pre-polymerization kettle (6), the tops of the pre-polymerization micromolecule removing device (17) and the polymerization micromolecule removing device (19) are respectively connected with a pre-polymerization vacuum system (18) and a polymerization vacuum system (20), the bottoms of the pre-polymerization micromolecule removing device (17) and the polymerization micromolecule removing device (19) are respectively connected with the recycling BDO tank (16), gas generated after the reaction of the pre-polymerization kettle (6) and the polymerization kettle (9) respectively enters the pre-polymerization vacuum system (18) and the polymerization vacuum system (20) after BDO, water and micromolecule are removed in the pre-polymerization micromolecule removing device (17) and the polymerization micromolecule removing device (19), and the pre-polymerization micromolecule removing device (17) and the polymerization micromolecule removing device (19) respectively, The polymer micromolecule removing device (19) removes BDO, water and the like and enters a recycling BDO tank (16), the recycling BDO tank (16) is connected with the middle part of the process tower (4) through a pump pipeline, and recycling liquid in the recycling BDO tank (16) is refined through the process tower (4) and then is conveyed back to the esterification kettle (3) and the slurry mixing kettle (1).
2. The apparatus of claim 1, wherein: the slurry preparation kettle (1) is used for metering BDO and oxalic acid melt by using a BDO metering device (13) and an oxalic acid melt metering device (14) and then simultaneously adding the BDO and the oxalic acid melt into the slurry preparation kettle (1) according to a certain proportion, so that full-automatic pulping is realized.
3. The apparatus of claim 1, wherein: and a catalyst adding port is arranged on a pipeline connecting the process tower (4) and the esterification kettle (3), and the catalyst adding port is a main catalyst adding point of the whole device flow.
4. The apparatus of claim 1, wherein: the prepolymerization cauldron (6) adopt the locellus structure, have realized the combination of flat push with two kinds of reaction forms of mixing entirely, have improved the efficiency of reactor, and the bottom is provided with the catalyst and adds the mouth, is convenient for adjust the reaction.
5. The apparatus of claim 1, wherein: the polymerization kettle (9) is a double-shaft disc stirring vacuum reactor, and a plurality of film forming discs are arranged on two stirring shafts to form two disc stirring systems, so that the viscosity of the product can be conveniently adjusted.
6. The apparatus of claim 1, wherein: BDO entering the slurry preparation kettle (1) mainly comes from recycled BDO sent out by the process tower (4), and the insufficient part is supplemented by fresh BDO in front of the BDO metering device (13).
CN201922261522.8U 2019-12-17 2019-12-17 Full-continuous PBS production equipment Active CN211199085U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110818888A (en) * 2019-12-17 2020-02-21 扬州普立特科技发展有限公司 Production equipment and process flow of fully-continuous PBS (Poly Butylene succinate)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110818888A (en) * 2019-12-17 2020-02-21 扬州普立特科技发展有限公司 Production equipment and process flow of fully-continuous PBS (Poly Butylene succinate)

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