CN110964190B - Raw material conveying and blending device used in polycarbonate synthesis process - Google Patents
Raw material conveying and blending device used in polycarbonate synthesis process Download PDFInfo
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- CN110964190B CN110964190B CN201911165112.1A CN201911165112A CN110964190B CN 110964190 B CN110964190 B CN 110964190B CN 201911165112 A CN201911165112 A CN 201911165112A CN 110964190 B CN110964190 B CN 110964190B
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- 238000002156 mixing Methods 0.000 title claims abstract description 66
- 239000004417 polycarbonate Substances 0.000 title claims abstract description 55
- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 49
- 230000008569 process Effects 0.000 title claims abstract description 38
- 239000002994 raw material Substances 0.000 title claims abstract description 36
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 27
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 27
- 239000000203 mixture Substances 0.000 claims abstract description 106
- 238000002360 preparation method Methods 0.000 claims abstract description 79
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- 239000003054 catalyst Substances 0.000 claims abstract description 33
- 239000002002 slurry Substances 0.000 claims abstract description 32
- 238000004891 communication Methods 0.000 claims abstract description 21
- 238000007599 discharging Methods 0.000 claims abstract description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 128
- 238000005406 washing Methods 0.000 claims description 48
- 239000000463 material Substances 0.000 claims description 37
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- 239000007789 gas Substances 0.000 claims description 34
- 238000005303 weighing Methods 0.000 claims description 27
- 238000004519 manufacturing process Methods 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 16
- 230000035484 reaction time Effects 0.000 claims description 15
- 150000002148 esters Chemical class 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000002912 waste gas Substances 0.000 claims description 14
- 230000001276 controlling effect Effects 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000006068 polycondensation reaction Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 125000004185 ester group Chemical group 0.000 claims 3
- 238000010924 continuous production Methods 0.000 abstract description 5
- ROORDVPLFPIABK-UHFFFAOYSA-N diphenyl carbonate Chemical compound C=1C=CC=CC=1OC(=O)OC1=CC=CC=C1 ROORDVPLFPIABK-UHFFFAOYSA-N 0.000 description 72
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 238000006384 oligomerization reaction Methods 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000005809 transesterification reaction Methods 0.000 description 3
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 description 2
- CLBRCZAHAHECKY-UHFFFAOYSA-N [Co].[Pt] Chemical compound [Co].[Pt] CLBRCZAHAHECKY-UHFFFAOYSA-N 0.000 description 2
- 150000001339 alkali metal compounds Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 2
- 238000012696 Interfacial polycondensation Methods 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- NBPNLFQRKVSROV-UHFFFAOYSA-N [NH4+].[OH-].C=C.C=C.C=C.C=C Chemical compound [NH4+].[OH-].C=C.C=C.C=C.C=C NBPNLFQRKVSROV-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
- C08G64/20—General preparatory processes
- C08G64/205—General preparatory processes characterised by the apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
- C08G64/20—General preparatory processes
- C08G64/30—General preparatory processes using carbonates
- C08G64/307—General preparatory processes using carbonates and phenols
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention relates to a raw material conveying and blending device used in a polycarbonate synthesis process, which comprises: a DPC conveying device; a BPA transport device; a slurry blending tank in communication with the BPA transport device and the DPC transport device, respectively; the mixture preparation tank is communicated with the slurry mixing tank and is provided with a first catalyst feeding port; a mixture surge tank in communication with the mixture preparation tank; the discharging heater is communicated with the mixture buffer tank; a reaction system in communication with the discharge heater; and the tail gas treatment system is respectively communicated with the mixture preparation tank and the mixture buffer tank. The raw materials are fully mixed, the mixing temperature is lower, and the conversion rate of preparing the polycarbonate is high; the generated tail gas is less, and the environment is protected and the energy is saved; realizing continuous production of DPC and PC.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a raw material conveying and blending device used in a polycarbonate synthesis process.
Background
Polycarbonate (PC) is a linear polymer, is a thermoplastic engineering plastic with good transparency in five general engineering plastics, has visible light transmittance of 90 percent, simultaneously has excellent impact resistance, heat resistance and dimensional stability, and is widely applied in various fields. At present, most manufacturers in the world generally adopt an interfacial polycondensation method or a molten ester exchange method. However, phosgene has a destructive effect on the ozone layer, and particularly phosgene is used as a highly toxic gas, so that the preparation and the use of phosgene are very strictly limited by environment and safety. The melt transesterification polycondensation method is a method for synthesizing PC by reacting diphenyl carbonate (DPC) with bisphenol A (BPA), wherein the diphenyl carbonate is prepared by adopting environment-friendly dimethyl carbonate to replace phosgene as a raw material and carrying out transesterification with phenol, thereby eliminating pollution from the source and realizing clean production of polycarbonate, and the melt transesterification polycondensation method is the development direction of the polycarbonate production technology at present.
In the production of polycarbonate by the melt method from diphenyl carbonate and bisphenol A, a raw material mixed melt is first prepared by melting by heating, and the following two methods are generally used: (1) firstly, adding two solids of diphenyl carbonate and bisphenol A into a heating tank with stirring, and then simultaneously heating, melting and mixing to obtain a raw material mixed melt; (2) and (3) metering the bisphenol A solid, adding the metered bisphenol A solid into a heating tank with a stirrer, and simultaneously adding the metered diphenyl carbonate melt into the heating tank for mixing and dissolving to obtain the original mixed melt. The former is a method generally adopted in the current production and test, but bisphenol A is easy to decompose and color due to long heating time; the latter can be melted and mixed in a short time, a storage device for diphenyl carbonate is omitted, and the diphenyl carbonate discharged by the diphenyl carbonate device directly enters the mixing device to realize continuous production of the diphenyl carbonate and the polycarbonate. CN108789913A discloses a raw material mixing device for continuously producing polycarbonate, in particular to a raw material mixing device and a process for continuously producing polycarbonate, DPC is directly from DPC production line, the whole system saves DPC storage device, greatly shortens raw material mixing period, saves energy; realizing continuous production of DPC and PC.
In the polycarbonate synthesis early stage, raw materials need to be weighed, and the raw materials are well conveyed and prepared, so that the esterification reaction of DPC and BPA is performed as little as possible before entering a first esterification reactor, so as to avoid generating oligomers and influence on the subsequent polycarbonate molecular weight.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a raw material conveying and blending device used in a polycarbonate synthesis process and a process flow adopting the device.
A raw material conveying and blending device for a polycarbonate synthesis process comprises: a DPC conveying device; a BPA transport device; a slurry blending tank in communication with the BPA transport device and the DPC transport device, respectively; the mixture preparation tank is communicated with the slurry mixing tank and is provided with a first catalyst feeding port; a mixture surge tank in communication with the mixture preparation tank; the discharging heater is communicated with the mixture buffer tank; a reaction system in communication with the discharge heater; and the tail gas treatment system is respectively communicated with the mixture preparation tank and the mixture buffer tank.
Further, the DPC conveying device sequentially comprises a DPC heater which is communicated with the slurry mixing tank; a DPC feed filter in communication with the DPC heater; a flow control meter in communication with the DPC feed filter; and the discharge hole of the DPC production line is communicated with a flow control meter.
Further, BPA conveyor includes in proper order: a material dryer in communication with the slurry blending tank; a weighing system in communication with the material dryer; a BPA bin in communication with the weighing system.
Further, the mixture buffer tank is also provided with a second catalyst charging hole.
Further, the slurry preparation tank, the mixture preparation tank and the mixture mixing buffer tank are provided with outer jackets, the outer jackets are filled with liquid heating media, and the outer jackets are provided with temperature adjusting devices.
Further, the exhaust gas treatment system comprises: the mixing system emptying washing tower is respectively communicated with the mixture preparation tank and the mixture buffer tank; the system for preparing the emptying washing tower kettle liquid pump is communicated with the system for preparing the emptying washing tower kettle liquid pump; the mixing and emptying washing cooler is communicated with the mixing system emptying washing tower kettle liquid pump; and the burning device is communicated with the emptying washing tower of the allocation system.
Further, a filter is arranged between the mixture buffer tank and the discharge heater, and preferably, the filter is a basket filter.
The invention also provides a process for conveying and blending raw materials in the polycarbonate synthesis process, which comprises the following steps:
s101: weighing bisphenol A in a BPA bin by using a weighing instrument, and drying by using a material dryer;
s102: DPC flowing out of a discharge port of the DPC production line enters a DPC feeding filter after being regulated and controlled by a flow control meter, and then enters a DPC heater to be heated to 130-140 ℃;
s103: adding the bisphenol A obtained in the step S101 and the DPC obtained in the step S102 into the slurry preparation tank with the temperature of 140-150 ℃, and stirring and uniformly mixing;
s104: adding the materials in the slurry preparation tank into the mixture preparation tank, controlling the temperature in the mixture preparation tank to be 140-150 ℃ under the protection of nitrogen, and introducing a catalyst through a first catalyst feed inlet, wherein the waste gas generated in the mixture preparation tank enters the tail gas treatment system;
s105: adding the materials in the mixture preparation tank into the mixture buffer tank, and controlling the temperature in the mixture buffer tank to be 150-160 ℃ under the protection of nitrogen; wherein the waste gas generated in the mixture buffer tank enters the tail gas treatment system;
s106: and heating the materials in the mixture buffer tank by a discharge heater, and then, reacting in a reaction system.
Further, the process also comprises the following steps:
s107: and (3) firstly emptying the tail gas in the step S104 and the step S105 to a washing tower through a preparation system, emptying the washing tower through the preparation system, and conveying the kettle liquid pump of the washing tower to a preparation emptying washing cooler.
Specifically, in the step S106, the material is heated to 190 to 220 ℃ by a discharge heater.
Has the advantages that:
1. by adopting the raw material conveying and blending device in the polycarbonate synthesis process, the raw materials are fully mixed, the mixing time is short, and the decomposition of bisphenol A is reduced; meanwhile, the catalyst is added after the DPC and the BPA are fully mixed, so that oligomerization is avoided, polycarbonate with ideal quality can be obtained, and the yield of the polycarbonate is improved.
2. By adopting the raw material conveying and blending device in the polycarbonate synthesis process, the raw materials are premixed before reaction in a reasonable temperature range, so that oligomerization is avoided, and polycarbonate with ideal quality can be obtained.
3. In addition, DPC melt is directly introduced into a PC production line, investment of a DPC drying and granulating device is saved, and energy consumption, time consumption and the like of DPC melting are saved.
And 4, drying the BPA and then feeding the BPA into a slurry preparation tank. The BPA subjected to drying treatment reduces the entrainment of water, so that the water in the whole PC synthesis process is reduced, and the instability of the generated polycarbonate is avoided.
Drawings
FIG. 1 is a schematic diagram of the BPA transport and blending apparatus of the present invention for use in a polycarbonate synthesis process;
1-DPC conveying apparatus; 2-a BPA transport means; 3-a tail gas treatment system; 4-slurry blending tank; 5-a mixture preparation tank; 6-mixture buffer tank; 7-a discharge heater; 8-a reaction system; a discharge port of the 11-DPC production line; 12-a flow control meter; 13-DPC feed filter; a 14-DPC heater; a 21-BPA silo; 22-BPA scale; a 23-BPA bunker emptying gas filter; 24-BPA weighing instrument vent gas filter; 25-a material dryer; 31-the preparation system empties the washing tower; 32-an incineration unit; 33-make-up system wash cooler; 51-a first catalyst addition port; 61-second catalytic addition port.
Detailed Description
The process flow of the present invention is described in detail below, and the apparatuses involved in the process flow are shown in the drawings, wherein the same or similar reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The following description, with reference to the drawings, is exemplary in nature and is intended to be illustrative of the invention and is not to be construed as limiting the invention.
The diphenyl carbonate adopted in the invention is directly provided on a production line, and the purity which meets the requirement is more than or equal to 99.9 percent, and the color number of the platinum-cobalt is less than or equal to 5. The purity of the purchased bisphenol A is more than or equal to 99.8 percent, and the color number of the platinum-cobalt is less than or equal to 20. The catalyst is a compound catalyst prepared from an alkali metal compound and a quaternary ammonium base compound according to the molar ratio of 1:1, wherein the alkali metal compound can be selected from lithium hydroxide, potassium hydroxide, sodium hydroxide and the like, and preferably sodium hydroxide; the organic amine can be selected from tetrabutyl ammonium hydroxide, tetraethylene ammonium hydroxide, and tetramethylammonium hydroxide, preferably tetramethylammonium hydroxide. When the catalyst is added, the catalyst and deionized water are prepared into 0.5 percent solution, and then the solution is injected into a raw material preparation tank through a high-pressure spray pump. The catalyst is prepared into an aqueous solution and injected into a raw material tank through high-pressure spraying, so that the catalyst and the raw materials are uniformly mixed.
Example 1
As shown in fig. 1, example 1 discloses a raw material conveying and blending apparatus for polycarbonate synthesis process, comprising: a DPC conveying device 1; a BPA transport apparatus 2; the slurry mixing tank 4 is communicated with the BPA conveying device 2 and the DPC conveying device 1 respectively; a mixture preparation tank 5, wherein the mixture preparation tank 5 is communicated with the slurry preparation tank 4, and the mixture preparation tank 5 is provided with a first catalyst feeding port 51; a mixture buffer tank 6, the mixture buffer tank 6 being in communication with the mixture preparation tank 5; the discharging heater 7 is communicated with the mixture buffer tank 6; the reaction system 8 is communicated with the discharging heater 7; and the tail gas treatment system 3 is respectively communicated with the mixture preparation tank 5 and the mixture buffer tank 6.
By adopting the raw material conveying and blending device in the polycarbonate synthesis process described in embodiment 1, the raw materials are fully mixed, the mixing time is short, and the decomposition of bisphenol A is reduced; meanwhile, the catalyst is added after the DPC and the BPA are fully mixed, so that premature oligomerization is avoided, polycarbonate with ideal quality can be obtained, and the yield of the polycarbonate is improved. In addition, the additive mixture preparation tank may serve as a temporary storage.
Preferably, the DPC delivery apparatus 1 comprises, in sequence: a DPC heater 14, the DPC heater 14 being in communication with the slurry conditioning tank 4; a DPC feed filter 13, the DPC feed filter 13 being in communication with the DPC heater 14; a flow control meter 12, said flow control meter 12 being in communication with said DPC feed filter 13; DPC production line discharge gate 11, DPC production line discharge gate 11 communicates with flow control meter 12. The device of the invention is adopted to produce polycarbonate, saves DPC storage devices, greatly shortens the raw material mixing period and saves energy; realizing continuous production of DPC and PC. Meanwhile, the melt DPC prepared by the DPC production line can enter the PC production line through a flow control meter, and the added DPC amount can be accurately calculated through controlling the flow because the concentration of the DPC is certain at a specific temperature, and meanwhile, the pollution in the processes of DPC drying granulation, storage, transportation, unpacking and weighing in the prior art can also be avoided.
Preferably, the BPA conveying device 2 sequentially comprises a material dryer 25, and the material dryer 25 is communicated with the slurry mixing tank 4; the weighing system is communicated with the material drying device 25, the BPA bin 21 is communicated with the weighing system, and the BPA bin 21 is communicated with the weighing system.
The BPA bin 21 is provided with a discharge valve, and the BPA bin 21 is externally connected with a BPA bin vent gas filter 23; the weighing system comprises a BPA weighing instrument 22, the BPA weighing instrument 22 is provided with a blanking valve, and the BPA weighing instrument 22 is externally connected with a BPA weighing instrument vent gas filter 24.
Specifically, BPA enters a BPA bin 21 through a chain basket conveying system, a certain amount of BPA is weighed by a BPA weighing instrument 22, enters a material dryer 25 through a BPA bin blanking valve and a weighing instrument blanking valve, and enters a slurry mixing tank 4 after being dried. The BPA subjected to drying treatment reduces the entrainment of water, so that the water in the whole PC synthesis process is reduced, and the instability of the generated polycarbonate is avoided.
The BPA bunker emptying gas filter 23 is of a college coating pulse type and is made of 316L. The vent gas filter 24 of the BPA weighing instrument is of a college coated film pulse type and is made of 316L.
Preferably, the slurry preparation tank 4, the mixture preparation tank 5 and the mixture buffer tank 6 are provided with outer jackets, the outer jackets are filled with liquid heating media, and the outer jackets are provided with temperature adjusting devices. The slurry mixing tank 4 may be vertical, the jacket of the slurry mixing tank being Q345R. The mixture preparation tank 5 can be vertical, and the jacket material of the mixture preparation tank is Q345R. The mixture buffer tank 6 can be vertical, and the jacket material of the mixture buffer tank is Q345R.
Preferably, the exhaust gas treatment system 3 comprises: the preparation system emptying washing tower 31 is communicated with the mixture preparation tank 5 and the mixture buffer tank 6 respectively; the blending system emptying washing tower kettle liquid pump is communicated with the blending system emptying washing tower 31; a blending emptying washing cooler 33, wherein the blending emptying washing cooler 33 is communicated with the blending system emptying washing tower kettle liquid pump; an incineration device 32, the incineration device 32 is communicated with the blending system emptying washing tower 31. The main components of the tail gas in the whole production process are nitrogen, phenol and water vapor, and the tail gas enters a tail gas treatment system through a pipeline, so that the generation of pollutants is reduced, and meanwhile, available substances are recycled. Nitrogen and a small amount of phenol are discharged to the washing tower 31 through the preparation system for treatment, warm water of 45-65 ℃ is introduced into the preparation discharge washing cooler 33, pure phenol is used during washing, tail gas mainly comprises reaction byproducts and generated phenol, when pure phenol is washed, a certain cooling effect is firstly achieved, but the temperature is not reduced to be very low, part of waste gas with a boiling point which is not very low can smoothly escape in a gaseous form, the waste gas discharged to the washing tower 31 through the preparation system is introduced into the preparation discharge washing cooler 33 through a preparation discharge washing tower kettle liquid pump for cooling, most of the phenol is cooled, and the phenol can be continuously recycled after cooling. Finally, the residual nitrogen and residual waste gas enter the incineration device 32 for final incineration treatment.
Preferably, a filter is arranged between the mixture buffer tank 6 and the discharge heater 7, and the filter is preferably a basket filter.
Example 2
Example 2 differs from example 1 in that: the mixture buffer tank 6 is provided with a second catalyst charging port 61.
Example 3
An experiment conducted using the apparatus described in example 1 provided a process for raw material delivery and blending in a polycarbonate synthesis process comprising the steps of:
s101: weighing bisphenol A in a BPA bin by using a weighing instrument, and drying by using a material dryer;
s102: DPC flowing out of a discharge port of the DPC production line enters a DPC feeding filter after being regulated and controlled by a flow control meter, and then enters a DPC heater to be heated to 130-140 ℃;
s103: adding the bisphenol A obtained in the step S101 and the DPC obtained in the step S102 into a slurry mixing tank at the temperature of 140-150 ℃, and uniformly stirring;
s104: adding the materials in the slurry preparation tank into the mixture preparation tank, controlling the temperature in the mixture preparation tank to be 140-150 ℃ under the protection of nitrogen, introducing a catalyst through a first catalyst feeding port, wherein waste gas generated in the mixture preparation tank enters the tail gas treatment system, wherein the feeding molar ratio of the bisphenol A, the diphenyl carbonate and the catalyst in unit time is 1: 1.02: 5X 10 -4 ；
S105: adding the materials in the mixture preparation tank into the mixture buffer tank, and controlling the temperature in the mixture buffer tank to be 150-160 ℃ under the protection of nitrogen; wherein the waste gas generated in the mixture buffer tank enters the tail gas treatment system;
s106: and heating the materials in the mixture buffer tank to 190-220 ℃ through a discharge heater, and then entering a reaction system for reaction.
Specifically, the reaction in the reaction system is as follows: under the protection of nitrogen, the mixture enters a first ester exchange reactor, the reaction temperature is 190-220 ℃, the reaction time is 1h, then the mixture enters a second ester exchanger, the reaction temperature is 220-240 ℃, the reaction time is 1h, and then the mixture enters a third ester exchange reactor, the reaction temperature is 240-265 ℃, and the reaction time is 1 h. After the ester exchange reaction is finished, the reaction product enters a pre-polycondensation reactor, the reaction temperature is 285-298 ℃ for 1h, and finally the reaction product enters a final polycondensation reactor, the reaction temperature is 290-298 ℃ for 0.5 h.
Example 4
An experiment conducted using the apparatus described in example 1 provided a process for raw material delivery and blending in a polycarbonate synthesis process comprising the steps of:
s101: weighing bisphenol A in a BPA bin by using a weighing instrument, and drying by using a material dryer;
s102: DPC flowing out of a discharge port of the DPC production line enters a DPC feeding filter after being regulated and controlled by a flow control meter, and then enters a DPC heater to be heated to 130-140 ℃;
s103: adding the bisphenol A obtained in the step S101 and the DPC obtained in the step S102 into the slurry preparation tank with the temperature of 140-150 ℃, and stirring and uniformly mixing;
s104: adding the materials in the slurry preparation tank into the mixture preparation tank, controlling the temperature in the mixture preparation tank to be 140-150 ℃ under the protection of nitrogen, introducing a catalyst through a first catalyst feeding port, wherein waste gas generated in the mixture preparation tank enters the tail gas treatment system, wherein the feeding molar ratio of the bisphenol A, the diphenyl carbonate and the catalyst in unit time is 1: 1.02: 5X 10 -4 ；
S105: adding the materials in the mixture preparation tank into the mixture buffer tank, and controlling the temperature in the mixture buffer tank to be 150-160 ℃ under the protection of nitrogen; wherein the waste gas generated in the mixture buffer tank enters the tail gas treatment system;
s106: and heating the materials in the mixture buffer tank to 190-220 ℃ through a discharge heater, and then entering a reaction system for reaction.
S107: and (5) firstly emptying the tail gas in the step S104 and the step S105 to a washing tower through a preparation system, emptying the washing tower through a preparation system after washing, conveying the washing tower to a preparation emptying washing cooler through a kettle liquid pump of the preparation emptying washing tower, recycling the gas cooled by the preparation emptying washing cooler, and feeding the escaped waste gas into an incineration device for final incineration treatment.
Specifically, the reaction in the reaction system is as follows: under the protection of nitrogen, the mixture enters a first ester exchange reactor, the reaction temperature is 190-220 ℃, the reaction time is 1h, then the mixture enters a second ester exchanger, the reaction temperature is 220-240 ℃, the reaction time is 1h, and then the mixture enters a third ester exchange reactor, the reaction temperature is 240-265 ℃, and the reaction time is 1 h. After the ester exchange reaction is finished, the mixture enters a pre-polycondensation reactor, the reaction temperature is 285-298 ℃ for 1h, and finally the mixture enters a final polycondensation reactor, the reaction temperature is 290-298 ℃ for 0.5 h.
Example 5
An experiment conducted using the apparatus described in example 2 provided a process for raw material delivery and blending in a polycarbonate synthesis process, comprising the steps of:
s101: weighing bisphenol A in a BPA bin by using a weighing instrument, and drying by using a material dryer;
s102: DPC flowing out of a discharge port of the DPC production line enters a DPC feeding filter after being regulated and controlled by a flow control meter, and then enters a DPC heater to be heated to 130-140 ℃;
s103: adding the bisphenol A obtained in the step S101 and the DPC obtained in the step S102 into the slurry preparation tank with the temperature of 140-150 ℃, and stirring and uniformly mixing;
s104: adding the material in the slurry blending tank to the mixtureIn a configuration tank, under the protection of nitrogen, controlling the temperature in the mixture configuration tank to be 140-150 ℃, and introducing a catalyst through a first catalyst feed inlet, wherein waste gas generated in the mixture configuration tank enters the tail gas treatment system; wherein the molar ratio of bisphenol A to diphenyl carbonate to catalyst fed per unit time is 1: 1.02: 2X 10 -4 ；
S105: adding the materials in the mixture preparation tank into the mixture buffer tank, controlling the temperature in the mixture buffer tank to be 150-160 ℃ under the protection of nitrogen, and introducing a catalyst through a second catalyst feeding port; wherein the exhaust gas generated in the mixture buffer tank enters the tail gas treatment system, wherein the molar ratio of the bisphenol A, the diphenyl carbonate and the catalyst fed per unit time is 1: 1.02: 3X 10 -4 ；
S106: and heating the materials in the mixture buffer tank to 190-220 ℃ through a discharge heater, and then entering a reaction system for reaction.
S107: and (5) firstly emptying the tail gas in the step S104 and the step S105 to a washing tower through a preparation system, emptying the washing tower through a preparation system after washing, conveying the washing tower to a preparation emptying washing cooler through a kettle liquid pump of the preparation emptying washing tower, recycling the gas cooled by the preparation emptying washing cooler, and feeding the escaped waste gas into an incineration device for final incineration treatment.
Specifically, the reaction in the reaction system is as follows: under the protection of nitrogen, the mixture enters a first ester exchange reactor, the reaction temperature is 190-220 ℃, the reaction time is 1h, then the mixture enters a second ester exchanger, the reaction temperature is 220-240 ℃, the reaction time is 1h, and then the mixture enters a third ester exchange reactor, the reaction temperature is 240-265 ℃, and the reaction time is 1 h. After the ester exchange reaction is finished, the reaction product enters a pre-polycondensation reactor, the reaction temperature is 285-298 ℃ for 1h, and finally the reaction product enters a final polycondensation reactor, the reaction temperature is 290-298 ℃ for 0.5 h.
Comparative example 1
Comparative example 1 differs from example 4 in that the BPA transport equipment did not include a material dryer.
Comparative example 2
Experiments were carried out using the preparation method of example 2 in CN108789913A and the apparatus described in example 1.
Experimental example 1
In order to better highlight the advantages of the present invention, the properties of the polycarbonate prepared in each example, such as intrinsic viscosity and number average molecular weight, were determined, and are shown in Table 1.
1. Intrinsic viscosity measurement method: 0.125g of the objective product polycarbonate was dissolved in 25mL of a 1:1 by weight mixed solution of 1,1,2, 2-tetrachloroethane and phenol, and measured at 20 ℃ by an Ubbelohde viscometer.
2. Method for measuring viscosity average molecular weight: and (3) calculating the viscosity average molecular weight by referring to the intrinsic viscosity measuring method through a Mark-Houwink equation: [ eta ]]＝KM α Wherein, K is 1.11 x 10 -2 ，α＝0.82；
TABLE 1 polycarbonate Performance test results
| Viscosity average molecular weight | Intrinsic viscosity (mL/g) | |
| Example 3 | 38945 | 53.57 |
| Example 4 | 39102 | 53.24 |
| Example 5 | 39949 | 55.45 |
| Comparative example 1 | 35547 | 47.78 |
| Comparative example 2 | 37858 | 49.25 |
By adopting the raw material conveying and blending device in the polycarbonate synthesis process, the raw materials are fully mixed, the mixing time is short, and the decomposition of bisphenol A is reduced; meanwhile, the DPC and the BPA are fully mixed and then added with the catalyst, so that oligomerization is avoided, and the polycarbonate prepared by the method has higher molecular weight and excellent comprehensive performance. In addition, the running process flow of the raw material conveying and blending device in the polycarbonate synthesis process can realize continuous production of PC, simultaneously ensure the purity of the raw materials, reduce unnecessary steps of purification and the like.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that changes, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (7)
1. A polycarbonate synthesis process is characterized in that a raw material conveying and blending device comprises:
a DPC conveying device;
a BPA transport unit;
a slurry blending tank in communication with the BPA transport device and the DPC transport device, respectively;
the mixture preparation tank is communicated with the slurry mixing tank and is provided with a first catalyst feeding port;
the mixture buffer tank is communicated with the mixture preparation tank and is provided with a second catalyst feeding port;
the discharging heater is communicated with the mixture buffer tank;
a reaction system in communication with the discharge heater;
the tail gas treatment system is respectively communicated with the mixture preparation tank and the mixture buffer tank; the process of the raw material conveying and blending device comprises the following steps:
s101: weighing bisphenol A in a BPA bin by using a weighing instrument, and drying by using a material dryer;
s102: DPC flowing out of a discharge port of the DPC production line enters a DPC feeding filter after being regulated and controlled by a flow control meter, and then enters a DPC heater to be heated to 130-140 ℃;
s103: adding the bisphenol A obtained in the step S101 and the DPC obtained in the step S102 into the slurry mixing tank with the temperature of 140-150 ℃, and stirring and uniformly mixing;
s104: adding the materials in the slurry preparation tank into the mixture preparation tank, controlling the temperature in the mixture preparation tank to be 140-150 ℃ under the protection of nitrogen, and introducing a catalyst through a first catalyst feed inlet, wherein the waste gas generated in the mixture preparation tank enters the tail gas treatment system;
s105: adding the materials in the mixture preparation tank into the mixture buffer tank, and controlling the temperature in the mixture buffer tank to be 150-160 ℃ under the protection of nitrogen; wherein the waste gas generated in the mixture buffer tank enters the tail gas treatment system;
s106: heating the materials in the mixture buffer tank to 190-220 ℃ after the materials are heated by a discharge heater, and then entering a reaction system for reaction;
under the protection of nitrogen, the mixture enters a first ester exchange reactor, the reaction temperature is 190-plus-220 ℃, the reaction time is 1h, then the mixture enters a second ester exchanger, the reaction temperature is 220-plus-240 ℃, the reaction time is 1h, then the mixture enters a third ester exchange reactor, the reaction time is 1h, the temperature is 240-plus-265 ℃, the reaction time is 1h, the mixture enters a pre-polycondensation reactor after the ester exchange reaction is finished, the reaction temperature is 285-plus-290 ℃, the reaction time is 1h, and finally the mixture enters a final polycondensation reactor, the reaction temperature is 290-plus-298 ℃, and the reaction time is 0.5 h.
2. The polycarbonate synthesis process of claim 1, wherein: the DPC conveying device sequentially comprises a DPC heater, a DPC conveying device and a DPC conveying device, wherein the DPC heater is communicated with the slurry mixing tank;
a DPC feed filter in communication with the DPC heater;
a flow control meter in communication with the DPC feed filter;
DPC production line discharge gate, DPC production line discharge gate and the flow control meter intercommunication.
3. The polycarbonate synthesis process of claim 1, wherein: the BPA conveying device sequentially comprises a material dryer, and the material dryer is communicated with the slurry mixing tank;
a weighing system in communication with the material dryer;
a BPA bin in communication with the weighing system.
4. The polycarbonate synthesis process of claim 1, wherein: the slurry preparation tank, the mixture preparation tank and the mixture buffer tank are provided with outer jackets, the outer jackets are communicated with liquid heating media, and the outer jackets are provided with temperature adjusting devices.
5. The polycarbonate synthesis process of claim 1, wherein: the tail gas treatment system includes: the mixing system emptying washing tower is respectively communicated with the mixture preparation tank and the mixture buffer tank;
the system for preparing the emptying washing tower kettle liquid pump is communicated with the system for preparing the emptying washing tower kettle liquid pump; the mixing and emptying washing cooler is communicated with the mixing system emptying washing tower kettle liquid pump;
and the burning device is communicated with the emptying washing tower of the allocation system.
6. The polycarbonate synthesis process of claim 1, wherein: a filter is arranged between the mixture buffer tank and the discharging heater, and the filter is a basket filter.
7. The polycarbonate synthesis process of claim 1, wherein: further comprising the steps of: s107: and (5) firstly emptying the tail gas in the step S104 and the step S105 to the washing tower through the preparation system, emptying the washing tower through the preparation system, and conveying the kettle liquid pump of the washing tower to the preparation emptying washing cooler.
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