CN113577814B - Diphenyl carbonate recovery device and method for industrial production of polycarbonate - Google Patents
Diphenyl carbonate recovery device and method for industrial production of polycarbonate Download PDFInfo
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- CN113577814B CN113577814B CN202110934686.1A CN202110934686A CN113577814B CN 113577814 B CN113577814 B CN 113577814B CN 202110934686 A CN202110934686 A CN 202110934686A CN 113577814 B CN113577814 B CN 113577814B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/145—One step being separation by permeation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
Abstract
The invention provides a diphenyl carbonate recovery device and method for polycarbonate industrial production, which comprises a DPC rectifying tower, wherein the middle feed end at one side of the DPC rectifying tower is connected with a DPC recovery material pipe through a connecting pipeline, the DPC recovery material pipe is communicated with the liquid outlet end of a phenol recovery system, a feed valve is further installed at the connecting part of a connecting pipe and the DPC rectifying tower, the top discharge end of the DPC rectifying tower is connected with a phenol recovery pipe, and the discharge end of the DPC rectifying tower is also communicated with a DPC recovery pipe for recovering DPC.
Description
Technical Field
The invention belongs to the technical field of polycarbonate production, and particularly relates to a diphenyl carbonate recovery device and method for industrial production of polycarbonate.
Background
Polycarbonates (abbreviated as PC in english) are high molecular polymers containing carbonate groups in their molecular chains, and are classified into various types such as aliphatic, aromatic, aliphatic-aromatic, and the like, depending on the structure of the ester group. Among them, aliphatic and aliphatic-aromatic polycarbonates have limited their use as engineering plastics due to their low mechanical properties.
At present, two main methods for the industrial production of polycarbonate are available, one is a phosgene method, and the other is non-phosgene. The non-phosgene method adopts bisphenol A and diphenyl carbonate (DPC) as raw materials to prepare Polycarbonate (PC) through ester exchange and polycondensation, in the production process, phenol generated in the reaction process needs to be continuously extracted, in the process, a small part of raw material bisphenol A, raw material DPC and generated oligomers are extracted together with the phenol and enter a phenol recovery system, the phenol is separated and recovered in the phenol recovery system and then enter the DPC recovery system to recover the DPC, in the existing DPC recovery technology, the recovery rate of the DPC is lower than 80 percent, a large amount of DPC is discharged into a waste liquid treatment system together with waste liquid to be treated, the consumption of the DPC is increased, meanwhile, certain pollution is caused to the environment, and the production cost of enterprises is increased invisibly.
Disclosure of Invention
The invention aims to provide a diphenyl carbonate recovery device and a diphenyl carbonate recovery method for industrial production of polycarbonate, and aims to solve the problems that in the DPC recovery technology in the prior art, the recovery rate of DPC is lower than 80%, a large amount of DPC is discharged into a waste liquid treatment system along with waste liquid for treatment, the consumption of DPC is increased, meanwhile, certain pollution is caused to the environment, and the production cost of enterprises is increased invisibly.
In order to achieve the purpose, the invention provides the following technical scheme: a diphenyl carbonate recovery device for industrial production of polycarbonate comprises a DPC rectifying tower, wherein a DPC recovery material pipe is connected to a feed end in the middle of one side of the DPC rectifying tower through a connecting pipeline, the DPC recovery material pipe is communicated with a liquid outlet end of a phenol recovery system, a feed valve is further installed at the joint of the connecting pipeline and the DPC rectifying tower, a phenol recovery pipe is connected to a discharge end at the top of the DPC rectifying tower, a DPC recovery pipe for recovering DPC is further communicated with a discharge end of the DPC rectifying tower, a kettle pump is connected to a liquid outlet end of the DPC rectifying tower through a pipeline, the kettle pump is communicated with a liquid inlet end of a flash tank through a pipeline, a liquid outlet end of the flash tank is communicated with a liquid inlet end of a membrane vaporizer through a pipeline, a liquid outlet end of the membrane vaporizer is communicated with a DPC recovery tank through a pipeline, a waste liquid outlet end of the membrane vaporizer is communicated with a waste liquid waste collection tank through a pipeline, the waste liquid outlet recovery tank is connected to a DPC recovery pump through a waste liquid outlet end of the membrane vaporizer through a waste liquid pump, and a waste liquid discharge pipe are communicated with a waste liquid waste collection tank, and a waste discharge pipe, and a waste liquid discharge pipe is communicated with a waste liquid discharge pipe
In order to communicate the recovery device with the phenol recovery system, it is preferable that the phenol recovery pipe is communicated with a liquid inlet end of the phenol recovery system.
In order to make the recovery device integrated and modularized, as a preferable aspect of the present invention, the membrane vaporizer is mounted on the top of a mounting frame, a transverse mounting plate is mounted in the middle of the mounting frame, and the top of the transverse mounting plate is fixedly connected to the DPC recovery tank and the waste liquid collection tank.
In order to rapidly support and adjust the flash tank, as a preferred mode of the invention, the bottom of the flash tank is provided with a plurality of supports for supporting the flash tank, and the bottom ends of the supports are provided with adjusting feet.
In order to enable personnel to conveniently debug the recovery device, as a preferable mode of the invention, control valves are arranged in the middle of a connecting pipeline between the tower kettle pump and the flash tank, in the middle of a connecting pipeline between the DPC recovery pump and the feed valve and in the middle of the waste liquid discharge pipe.
In order to connect the phenol recovery system to the recovery device and recover the materials, as a preferred aspect of the present invention, the weight percentages (wt%) of the materials of the phenol recovery system are: 3% of phenol, 87% of DPC and 10% of high-boiling components, wherein the flow rates of the materials are as follows: 1600kg/h.
In order to make the DPC rectifying tower used for rectifying the material, as a preferred mode of the invention, the weight percentages (wt%) of the recovered DPC in the DPC rectifying tower are respectively: phenol 0.05%, DPC99.95% and high boiling substance 0, wherein the flow of the materials is: 1220kg/h.
In order to verify the DPC loss rate at the top of the DPC rectifying tower, as a preferable mode of the invention, the weight percentages (wt%) of phenol extracted components in a phenol recovery pipe at the top of the DPC rectifying tower are respectively as follows: 40% of phenol, 60% of DPC and 0% of high-boiling substances, wherein the flow rate of the materials is as follows: 30kg/h.
In order to verify the recovery rate of the phenol in the DPC rectifying tower, as a preferred mode of the invention, the weight percentages (wt%) of the materials in the rectifying liquid end at the tower bottom of the DPC rectifying tower are respectively as follows: phenol 0, DPC55% and high boiling point substance 45%, wherein the flow of the materials is: 350kg/h.
A diphenyl carbonate recovery method for industrial production of polycarbonate comprises any one of the diphenyl carbonate recovery devices for industrial production of polycarbonate, and the specific steps are as follows:
s1, debugging and installing a recovery device, and communicating a phenol recovery pipe with a liquid inlet end of a phenol recovery system;
s2, recovering the diphenyl carbonate by using a rectification process of a DPC rectification tower and a vaporization technology of a membrane vaporizer;
s3, counting the recovery rate of the DPC in the recovery process, and carrying out secondary debugging on a recovery device;
and S4, treating the waste liquid in the waste liquid removing discharge pipe, and saving energy and reducing emission.
Compared with the prior art, the invention has the beneficial effects that:
1) The raw material injected by the phenol recovery system can be rectified by the arranged DPC rectifying tower, and the material after flash evaporation is subjected to vaporization separation by using the membrane vaporizer, so that the DPC can be recovered to a greater extent in the production process of the polycarbonate, and the recovery rate of the DPC can be up to more than 98% by the arranged recovery device, thereby effectively reducing the loss of the DPC, reducing the DPC consumption of the whole polycarbonate device, reducing the production input cost of an enterprise, simultaneously providing technical support for industrial energy-saving and environment-friendly production of the polycarbonate, and having important creative significance in the polycarbonate production industry;
2) Through retrieving jar DPC, waste liquid collection tank and membrane vaporizer all install on the mounting bracket for possible integration and modularization of recovery unit, reduce recovery unit's space and occupy, make polycarbonate manufacturing enterprise can be more convenient assemble the use, and can carry out temporary storage to the waste liquid that produces among the recovery process through the waste liquid collection tank that sets up, make waste water carry out unified processing after going waste liquid discharge pipe discharge, reach energy saving and emission reduction's effect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a partial schematic structural view of the present invention;
FIG. 3 is a side view of FIG. 2 of the present invention;
FIG. 4 is a schematic diagram of the DPC rectifying tower structure of the present invention.
In the figure: 1. a DPC rectifying tower; 11. a feed valve; 12. a phenol recovery pipe; 13. a phenol recovery material pipe; 14. a DPC recovery pipe; 15. the liquid end is extracted by rectification; 16. a reboiler; 17. a condenser; 18. a condensate tank; 2. a tower kettle pump; 3. a flash tank; 31. a support; 4. a mounting frame; 41. a transverse mounting plate; 5. a DPC recovery pump; 6. a DPC recovery tank; 7. a waste liquid collection tank; 8. a membrane vaporizer; 9. a waste liquid pump; 10. to a waste liquid discharge pipe.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1-4, the present invention provides the following technical solutions: the diphenyl carbonate recovery device for the industrial production of polycarbonate comprises a DPC rectifying tower 1, wherein a DPC recovery material pipe 13 is connected to the feed end of the middle of one side of the DPC rectifying tower 1 through a connecting pipeline, the DPC recovery material pipe 13 is communicated with the liquid outlet end of a phenol recovery system, a feed valve 11 is further installed at the connecting part of the connecting pipe and the DPC rectifying tower 1, a phenol recovery pipe 12 is connected to the discharge end of the top of the DPC rectifying tower 1, the phenol recovery pipe 12 is connected with a condenser 17 through a pipeline, condensate condensed by the condenser 17 enters a condensate tank 18, meanwhile, a part of condensate inside the condensate tank 18 is pumped into the phenol recovery system through a pump to recover phenol, a part of the condensate enters the top of the DPC rectifying tower 1 to flow back, and the ratio of the backflow amount to the extracted amount (the amount entering the phenol recovery system) is 2-10. Besides, a reboiler 16 communicated with the interior of the DPC rectifying tower 1 is arranged on one side of the DPC rectifying tower 1, and the reboiler 16 is indirectly heated by adding a heating medium to provide heat required by the whole rectifying system. The discharge end of the DPC rectifying tower 1 is further communicated with a DPC recovery pipe 14 for recovering DPC, the liquid outlet end of the DPC rectifying tower 1 is connected with a tower kettle pump 2 through a pipeline, the tower kettle pump 2 is communicated with the liquid inlet end of the flash tank 3 through a pipeline, the liquid outlet end of the flash tank 3 is communicated with the liquid inlet end of the membrane vaporizer 8 through a pipeline, the liquid outlet end of the membrane vaporizer 8 is communicated with a DPC recovery tank 6 through a pipeline, the waste liquid outlet end of the membrane vaporizer 8 is communicated with a waste liquid collecting tank 7 through a pipeline, the DPC recovery tank 6 is connected with a DPC recovery pump 5 through a pipeline, the liquid outlet end of the DPC recovery pump 5 is communicated with a feed valve 11 through a pipeline, the liquid outlet end of the waste liquid collecting tank 7 is communicated with a waste liquid pump 9 through a pipeline, and the liquid outlet end of the waste liquid pump 9 is communicated with a waste liquid discharge pipe 10.
In this embodiment: the phenol recovery pipe 12 is communicated with the liquid inlet end of the phenol recovery system.
Specifically, make phenol recovery pipe 12 and phenol recovery system's feed liquor end communicate through flange joint spare for recovery unit and phenol recovery system realize being connected, and personnel can control the flow that phenol recovery system pours into through feed valve 11 simultaneously, can be better control the recovery.
In this embodiment: the membrane vaporizer 8 is arranged on the top of the mounting frame 4, the middle part of the mounting frame 4 is provided with a transverse mounting plate 41, and the top of the transverse mounting plate 41 is fixedly connected with the DPC recovery tank 6 and the waste liquid collecting tank 7.
Specifically, utilize the screw rod can retrieve DPC recovery tank 6 and waste liquid collection tank 7 horizontal installation on the horizontal mounting panel 41 at mounting bracket 4 middle part, can install diaphragm type vaporizer 8 in the top of mounting bracket 4 fast for recovery unit can accomplish miniaturization and modularization, does benefit to the polycarbonate enterprise and installs, reduces the production input of enterprise.
In this embodiment: the bottom of flash tank 3 is installed a plurality of supports 31 that are used for supporting it, the bottom of support 31 is installed and is adjusted the stabilizer blade.
Specifically, support 31 through the installation can support the installation fast to flash tank 3 fixed to the regulation stabilizer blade that can set up can adjust the level of flash tank 3, ensures that flash tank 3 can carry out the flash distillation to the material and handle.
In this embodiment: control valves are arranged in the middle of connecting pipelines of the tower kettle pump 2 and the flash tank 3, in the middle of connecting pipelines of the DPC recovery pump 5 and the feed valve 11 and in the middle of the waste liquid discharge pipe 10.
The utility model discloses a phenol recovery process, including phenol recovery process, control valve, material flow in the pipeline, the control valve that sets up, can adjust the material flow in the pipeline, ensure to carry out the at utmost recovery to phenol, save the manufacturing cost to polycarbonate of enterprise, realize finely tuning to phenol's recovery process simultaneously.
In this embodiment: the weight percentages (wt%) of the materials of the phenol recovery system are respectively as follows: 3% of phenol, 87% of DPC and 10% of high-boiling-point substances (containing BPA), wherein the flow rates of materials are as follows: 1600kg/h.
Specifically, the material composition in the phenol recovery system is detected in advance, and the weight percentage of each component is calculated to verify the phenol recovery rate and the DPC loss rate.
In this embodiment, the recovered DPC in DPC rectifying tower 1 has the following weight percentage (wt%) respectively: phenol 0.05%, DPC99.95% and high boiler (BPA-containing) 0, wherein the flow rates of the materials are: 1220kg/h.
Specifically, the DPC rectifying tower 1 is arranged to rectify the materials, the materials are detected again after rectification, the recovery of phenol is obviously improved, and the consumption of DPC is reduced, and it should be noted that the flow rate of the materials is controlled to be 1150-1220kg/h.
In this embodiment: the weight percentages (wt%) of phenol extraction components in the DPC rectifying tower 1 overhead phenol recovery pipe 12 are respectively as follows: phenol 40%, DPC60% and high boiling point substance (containing BPA) 0, wherein the flow rate of the materials is as follows: 30kg/h.
Specifically, after the DPC rectifying tower 1 recovers and processes the materials, the phenol recovery pipe 12 can inject phenol into the phenol recovery system again, and then secondary rectification recovery can be performed, so that the purity and recovery amount of phenol recovery are improved, and DPC generated after rectification can be recovered through the arranged DPC recovery pipe 14.
In this embodiment: the weight percentages (wt%) of the materials in the bottom rectification liquid outlet end 15 of the DPC rectification tower 1 are as follows: phenol 0, DPC55% and high boiling point substances (containing BPA) 45%, wherein the flow rates of the materials are as follows: 350kg/h.
Specifically, can pump into flash tank 3 once more with the material after DPC rectifying column 1 rectification through the tower cauldron pump 2 that sets up, through boiling vaporization rapidly to inject into membrane vaporizer 8 after the double-phase separation, carry out vaporization separation to it, rethread DPC recovery tank 6 is retrieved PDC, increases the rate of recovery of PDC, utilizes waste liquid collection tank 7 to store the collection to the waste liquid simultaneously.
A diphenyl carbonate recovery method for industrial production of polycarbonate comprises the steps of utilizing any one of the diphenyl carbonate recovery devices for industrial production of polycarbonate, and the specific steps are as follows:
s1, debugging and installing a recovery device, and communicating a phenol recovery pipe 12 with a liquid inlet end of a phenol recovery system;
s2, recovering the diphenyl carbonate by using the rectification process of the DPC rectification tower 1 and the vaporization technology of the membrane vaporizer 8;
s3, counting the recovery rate of the DPC in the recovery process, and carrying out secondary debugging on a recovery device;
and S4, treating the waste liquid in the waste liquid discharge pipe 10, and saving energy and reducing emission.
Specifically, after being detected by testers, the weight percentages (wt%) of the materials in the DPC recovery tank 6 are respectively as follows: phenol 0, DPC85% and high boiling point substances (containing BPA) 15%, wherein the flow rates of the materials are as follows: 200kg/h;
the weight percentages (wt%) of the materials in the waste liquid collecting tank 7 are as follows: phenol 0, DPC15% and high boiling point substance (containing BPA) 85%, wherein the flow rate of the materials is as follows: 150kg/h.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A diphenyl carbonate recovery unit for polycarbonate industrial production, includes DPC rectifying column (1), characterized by that, one side middle feed end of DPC rectifying column (1) is connected with DPC recovery material pipe (13) through the connecting tube, DPC recovery material pipe (13) and phenol recovery system's play liquid end intercommunication, and the junction of the said connecting tube and DPC rectifying column (1) still installs feed valve (11), the top discharge end of DPC rectifying column (1) is connected with phenol recovery tube (12), the discharge end of DPC rectifying column (1) still communicates DPC recovery pipe (14) that are used for retrieving DPC, the play liquid end of DPC rectifying column (1) is connected with column cauldron pump (2) through the pipeline, the said DPC cauldron pump (2) communicates with the feed liquor end of flash drum (3) through the pipeline, the play liquid end of flash drum (3) communicates with the feed liquor end of membrane vaporizer (8) through the pipeline, the vaporizer (8) communicates with the waste liquid inlet end of DPC vaporizer (6), the waste liquid recovery pot (7) communicates with waste liquid collection tank (7) through the waste liquid collection tank (7), the waste liquid recovery tank (7) communicates with waste liquid recovery tank (7) through the waste liquid pump (7), and the liquid outlet end of the waste liquid pump (9) is communicated with a waste liquid discharge pipe (10).
2. The diphenyl carbonate recycling device for industrial production of polycarbonate according to claim 1, wherein: and the phenol recovery pipe (12) is communicated with the liquid inlet end of the phenol recovery system.
3. The diphenyl carbonate recycling device for industrial production of polycarbonate according to claim 1, wherein: the membrane vaporizer (8) is installed at the top of a mounting rack (4), a transverse mounting plate (41) is installed in the middle of the mounting rack (4), and the top of the transverse mounting plate (41) is fixedly connected with a DPC recovery tank (6) and a waste liquid collection tank (7).
4. The diphenyl carbonate recycling device for industrial production of polycarbonate according to claim 1, wherein: a plurality of supports (31) that are used for supporting it are installed to the bottom of flash tank (3), the regulation stabilizer blade is installed to the bottom of support (31).
5. The diphenyl carbonate recycling apparatus according to claim 1, wherein the diphenyl carbonate recycling apparatus comprises: and control valves are arranged in the middle of a connecting pipeline between the tower kettle pump (2) and the flash tank (3), in the middle of a connecting pipeline between the DPC recovery pump (5) and the feed valve (11) and in the middle of the waste liquid removal discharge pipe (10).
6. The diphenyl carbonate recycling device for industrial production of polycarbonate according to claim 1, wherein: the weight percentages (wt%) of the recovered DPC in the DPC rectifying tower (1) are respectively as follows: 0.05% of phenol, 99.95% of DPC and 0% of high-boiling substances, wherein the flow rates of materials are as follows: 1220kg/h.
7. The diphenyl carbonate recycling device for industrial production of polycarbonate according to claim 1, wherein: the weight percentages (wt%) of phenol extraction components in the DPC rectifying tower (1) overhead phenol recovery pipe (12) are respectively as follows: 40% of phenol, 60% of DPC and 0% of high-boiling substances, wherein the flow rate of the materials is as follows: 30kg/h.
8. The diphenyl carbonate recycling device according to claim 1, wherein the diphenyl carbonate recycling device comprises: the weight percentages (wt%) of materials in the bottom distillation liquid outlet end (15) of the DPC rectifying tower (1) are respectively as follows: phenol 0, DPC55% and high boiling substance 45%, wherein the flow rate of the materials is: 350kg/h.
9. A diphenyl carbonate recycling method for industrial production of polycarbonate, comprising the diphenyl carbonate recycling apparatus for industrial production of polycarbonate according to any one of claims 2 to 8, characterized by comprising the following steps:
s1, debugging and installing a recovery device, and communicating a phenol recovery pipe (12) with a liquid inlet end of a phenol recovery system;
s2, recovering the diphenyl carbonate by using a rectification process of the DPC rectification tower (1) and a vaporization technology of the membrane vaporizer (8);
s3, counting the recovery rate of the DPC in the recovery process, and carrying out secondary debugging on a recovery device; and S4, treating the waste liquid in the waste liquid discharge pipe (10), and saving energy and reducing emission.
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