CN214693958U - Post-treatment device for production of semi-aromatic polyester-polycarbonate copolymer - Google Patents
Post-treatment device for production of semi-aromatic polyester-polycarbonate copolymer Download PDFInfo
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Abstract
The utility model discloses a post-production treatment device for semi-aromatic polyester-polycarbonate copolymer, which comprises a polymerization reaction kettle, a product outlet, a gas outlet, a glue solution storage tank, a product inlet, a gas outlet, a liquid inlet, a glue solution outlet, a washing condensation devolatilization kettle, a glue solution inlet, a gas outlet, a washing coagulant inlet, a vibrating screen, a horizontal grinding machine, a horizontal screw centrifuge, a drying machine, a cyclone separator, a storage bin, an ethanol recovery tank, an epoxy propane recovery tank, a delivery pump, a first condenser, a second condenser and the like; at least two washing, condensing and devolatilizing kettles are connected in parallel between the glue solution storage tank and the vibrating screen, and the lower parts of the kettles are provided with hot water inlets. The device has the advantages that the epoxypropane as a reactant and a solvent is efficiently recovered, the condensation devolatilization time after polymerization is greatly shortened, the production post-treatment efficiency is obviously improved, the cost of the PPC product is greatly reduced, the negative influence on the performance of the PPC product caused by micromolecule residues is obviously reduced, and the quality of the PPC product is obviously improved.
Description
Technical Field
The utility model relates to a processing apparatus after production of polycarbonate copolymer and process field thereof especially relate to a processing apparatus after production of semi-aromatic polyester-polycarbonate copolymer.
Background
Since the industrial revolution, greenhouse gases with strong heat absorptivity, such as carbon dioxide and the like discharged into the atmosphere by human beings, are increased year by year, the greenhouse effect of the atmosphere is enhanced, and a series of environmental problems are caused to attract attention of countries all over the world; carbon dioxide, which is the main gas causing the greenhouse effect, is also one of the most abundant carbon sources on the earth, how to reasonably utilize the carbon dioxide can effectively reduce the greenhouse effect and change waste into valuable, for example, the carbon dioxide can be fixed by using a chemical method, carbon dioxide is taken as a raw material and is copolymerized with alkylene oxide under the action of a catalyst to prepare polycarbonate, the inventor of Mengdong et al discloses a Chinese prior patent document CN111378101A, a commercial, simple and efficient catalytic initiation system is adopted to catalytically initiate propylene oxide, carbon dioxide and phthalic anhydride to carry out ternary copolymerization reaction, an aromatic polyester structure with the content of 10-40 percent is successfully introduced into polymethyl ethylene carbonate (PPC), the product has good biodegradability, light transmittance, barrier property and the like by synthesizing modified PPC, and is used for agricultural mulching films, food packaging bags, disposable medical materials and the like; however, because the glass transition temperature of PPC is low (30-40 ℃), it also has certain disadvantages in the links of industrial processing, transportation, etc., and related researchers have also utilized various methods to increase the glass transition temperature, such as: ternary polymerization, crosslinking, blending with other polymers, inorganic filler and organic compounding.
In the prior patent document CN111378101A, aromatic acid anhydride is introduced as a reaction monomer, and the aromatic acid anhydride, propylene oxide and carbon dioxide are synthesized under a certain reaction condition under the action of a catalyst to obtain a semi-aromatic polyester-polycarbonate copolymer polymer, so that the glass transition temperature of the material can be effectively increased, the melt index of the material can be reduced, and the subsequent processing and transportation are facilitated; and by adding the polymerization assistant, the molecular weight and the distribution of the polymer product can be effectively improved.
However, some mature post-production treatment processes in the existing market have certain limitations, such as difficult complete removal of catalyst residues, complex process, high production cost and the like, and are not suitable for all PPC products. Under the condition of bulk polymerization process, the propylene oxide is used as both monomer and solvent, and when the polymerization reaction is finished, the crude product contains 30-70% of propylene oxide, and the raw materials are required to be recovered to reduce the production cost. The residual propylene oxide also imparts a strong irritating odor to the polymer, which is a health hazard. It is to be noted that, in the course of the polymerization reaction, with the formation of cyclic carbonates as by-products, residues thereof in the product may also adversely affect the properties of the product, and thus need to be thoroughly removed.
Therefore, there is still a need for improvement and development of the prior art.
SUMMERY OF THE UTILITY MODEL
In order to solve the technical problem, the utility model provides a semi-aromatic polyester-polycarbonate copolymer's production aftertreatment device, reducible polymerization back is condensed and is devolatilized the time, obviously improves production aftertreatment efficiency, is showing the quality that improves the PPC product to be applicable to all PPC products.
And simultaneously, the utility model also provides a semi-aromatic polyester-polycarbonate copolymer's production aftertreatment method, but the cost of greatly reduced PPC product obviously reduces the micromolecule and remains the negative effects that can cause PPC product property, is showing the quality that improves PPC product to be applicable to all PPC products.
The technical scheme of the utility model as follows:
a post-production treatment device for a semi-aromatic polyester-polycarbonate copolymer comprises a polymerization reaction kettle, a product outlet, a gas outlet, a glue solution storage tank, a product inlet, a gas outlet, a liquid inlet, a glue solution outlet, a washing, condensing and devolatilizing kettle, a glue solution inlet, a gas outlet, a washing and condensing agent inlet, a product outlet, a vibrating screen, a horizontal grinder, a horizontal screw centrifuge, a dryer, a cyclone separator, a storage bin, an ethanol recovery tank, an epoxy propane recovery tank, a delivery pump, a first condenser, a second condenser, a hot air inlet, a product outlet and a gas outlet; a product outlet, a product first inlet and a product second inlet; the cooling temperature of the first condenser is matched with the liquefaction temperature of the gaseous propylene oxide monomer, and the propylene oxide recovery tank is communicated with the outlet end of the first condenser; the lower part of the polymerization reaction kettle is provided with a product outlet, and the upper part of the polymerization reaction kettle is provided with a gas outlet; a gas outlet of the polymerization reactor is communicated to the inlet end of the first condenser through a corresponding pipeline; the upper part of the glue solution storage tank is provided with a product inlet and a gas outlet, and the lower part is provided with a glue solution outlet; the gas outlet of the glue solution storage tank is converged into a pipeline communicated with the gas outlet of the polymerization reaction kettle through a corresponding pipeline; a product inlet of the glue solution storage tank is communicated to a product outlet of the polymerization reaction kettle through a corresponding pipeline; the lower part of the washing, condensing and devolatilizing kettle is provided with a glue solution inlet and a hot water inlet, and the upper part is provided with a gas outlet and a product outlet; the gas outlet of the washing, condensing and devolatilizing kettle is also converged into a pipeline communicated with the gas outlet of the polymerization reaction kettle through a corresponding pipeline; a glue solution inlet of the washing, condensing and devolatilizing kettle is communicated to a glue solution outlet of a glue solution storage tank through a corresponding pipeline; the delivery pump is arranged on a pipeline which is communicated between a glue solution outlet of the glue solution storage tank and a glue solution inlet of the washing, condensing and devolatilizing kettle; the product outlet of the washing, condensing and devolatilizing kettle is communicated to the inlet end of the vibrating screen through a corresponding pipeline; the outlet end of the vibrating screen is communicated with the inlet end of the horizontal grinding machine, the outlet end of the horizontal grinding machine is communicated with the inlet end of the horizontal screw centrifuge, the outlet end of the horizontal screw centrifuge is communicated with the inlet end of the dryer, the outlet end of the dryer is communicated with the inlet end of the cyclone separator, the outlet end of the cyclone separator is communicated with the inlet end of the second condenser, the outlet end of the second condenser is communicated with the ethanol recovery tank, and the outlet end of the dryer is also communicated with the inlet end of the storage bin; the outlet end of the cyclone separator is also communicated with the inlet end of the storage bin;
a liquid inlet is formed in the middle of the glue solution storage tank, and is used for adding 5-15 wt% of water into the glue solution storage tank through a corresponding pipeline, and mixing the water with the glue solution in the glue solution storage tank to terminate the polymerization reaction;
at least two washing, condensing and devolatilizing kettles are connected in parallel between a glue solution storage tank and a vibrating screen, the glue solution inlet of each washing, condensing and devolatilizing kettle is gathered to a corresponding pipeline through a parallel pipeline and then is communicated with a conveying pump, and the product outlet of each washing, condensing and devolatilizing kettle is gathered to a corresponding pipeline through a parallel pipeline and then is communicated with the inlet end of the vibrating screen;
and the lower part of each washing, condensing and devolatilizing kettle is provided with a hot water inlet for injecting hot water of 60-90 ℃ into the washing, condensing and devolatilizing kettle through a corresponding pipeline so as to remove the propylene oxide component in the glue solution.
Further, in the above condensation and devolatilization apparatus for a semi-aromatic polyester-polycarbonate copolymer: three washing, condensing and devolatilizing kettles are connected in parallel between the glue solution storage tank and the vibrating screen.
Further, the coolant of the condenser No. one in the above condensation and devolatilization apparatus for a semi-aromatic polyester-polycarbonate copolymer was brine at 7 ℃.
Further, in the above-mentioned condensation and devolatilization apparatus for a semi-aromatic polyester-polycarbonate copolymer, the capacity of the polymerization reactor was 30L, the capacity of the dope solution tank was 40L, and the capacity of each washing condensation and devolatilization reactor was 30L.
Further, in the above-mentioned condensation and devolatilization apparatus for a semi-aromatic polyester-polycarbonate copolymer, a stirring apparatus is provided in the polymerization reaction tank.
Further, in the above-mentioned condensation and devolatilization apparatus for a semi-aromatic polyester-polycarbonate copolymer, a stirring apparatus is provided in the dope solution tank.
Further, in the above-mentioned condensation and devolatilization apparatus for a semi-aromatic polyester-polycarbonate copolymer, a stirring apparatus is provided in the washing condensation and devolatilization vessel.
Further, in the above-mentioned condensation and devolatilization apparatus for a semi-aromatic polyester-polycarbonate copolymer, the grinding medium used in the horizontal grinder is ethanol having a temperature of 30 ± 10 ℃.
Furthermore, the diameters of pipelines communicated with the glue solution inlets of all washing and condensing devolatilization kettles in the semi-aromatic polyester-polycarbonate copolymer condensing devolatilization device are all between 50 and 100 mm.
Further, in the condensation and devolatilization apparatus for a semi-aromatic polyester-polycarbonate copolymer, 2 to 5 wt% of a dispersant is contained in the hot water of 60 to 90 ℃.
A production post-treatment method of a semi-aromatic polyester-polycarbonate copolymer, which adopts the production post-treatment device of the semi-aromatic polyester-polycarbonate copolymer, comprises the following steps:
A. adding 5-15 wt% of water into the glue solution storage tank, and stirring and mixing the water and the crude product in the glue solution storage tank to terminate the polymerization reaction;
B. injecting hot water at 60-90 ℃ containing 2-5 wt% of a dispersing agent into the washing, condensing and devolatilizing kettle to remove the epoxypropane component in the glue solution; the flow rate of hot water injected into the washing, condensing and devolatilizing kettle is regulated to be matched with the flow rate of glue solution pumped into the washing, condensing and devolatilizing kettle, so that the mass ratio of water to the glue solution is controlled to be 95: 5-80: 20, and the residence time of the glue solution in the washing, condensing and devolatilizing kettle is more than 30 minutes;
C. the grinding balls added into the horizontal grinding machine are ceramic balls, the diameter of each grinding ball is 1-5 cm, the adding amount of the grinding balls accounts for 30-60% of the volume of the horizontal grinding machine, and the particle size of the ground material is smaller than 5 mm;
D. centrifuging the polymer and ethanol by using a horizontal spiral separator to obtain a polymer containing 10-15 wt% of ethanol, drying the separated ethanol by using a dryer, and returning the dried ethanol to an ethanol storage tank for reuse;
E. and drying the polymer separated by the horizontal spiral separator by a dryer to obtain powdery solid, and feeding the powdery solid into a storage bin to finally obtain the powdery semi-aromatic polyester-polycarbonate copolymer after washing, condensation and devolatilization.
The utility model provides a semi-aromatic polyester-polycarbonate copolymer's production aftertreatment device and production aftertreatment method, owing to adopt 5 ~ 15 wt% water termination polymerization earlier, adopt 60 ~ 90 ℃ of hot water as the washing coagulant again, the epoxypropane as reactant and solvent has been retrieved to the high efficiency, the back condensation devolatilization time of polymerization has greatly been shortened, production aftertreatment efficiency has obviously been improved, greatly reduced the cost of PPC product, the micromolecule has obviously been reduced and has remained the negative effects that can cause PPC product property, the quality that PPC product has been showing and is improved, and be applicable to all PPC products.
Drawings
The drawings described herein are for illustration purposes only and are not intended to limit the scope of the present disclosure in any way; the shapes, the proportional sizes and the like of the various components in the drawings are only schematic and are used for helping the understanding of the invention, and the shapes, the proportional sizes and the like of the various components of the invention are not particularly limited; the skilled person in the art can, under the teaching of the present invention, choose various possible shapes and proportional dimensions to implement the invention according to the specific situation.
FIG. 1 is a schematic structural view of an example of a post-production treatment apparatus for a semi-aromatic polyester-polycarbonate copolymer according to the present invention.
The various reference numbers in the figures are summarized:
a polymerization reaction kettle 1, a polymerization reaction kettle product outlet 1-1, a polymerization reaction kettle gas outlet 1-2, a glue solution storage tank product inlet 2-1, a glue solution storage tank gas outlet 2-2, a glue solution storage tank liquid inlet 2-3, a glue solution storage tank glue solution outlet 2-4, a washing coagulation devolatilization kettle 3, a washing coagulation devolatilization kettle glue solution inlet 3-1, a washing coagulation devolatilization kettle gas outlet 3-2, a washing coagulation devolatilization kettle hot water (washing coagulant) inlet 3-3, a washing coagulation devolatilization kettle product outlet 3-4, a vibrating screen 4, a horizontal grinder 5, a horizontal screw centrifuge 6, a dryer 7, a dryer hot air inlet 7-3, a dryer product outlet 7-4, a cyclone separator 8 and a cyclone separator gas outlet 8-2; cyclone product outlet 8-3, silo 9, silo product first inlet 9-1, silo product second inlet 9-2, ethanol recovery tank 10, propylene oxide recovery tank 11, transfer pump 12, condenser No. one 13, condenser No. two 14, pipes (15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33).
Detailed Description
The following detailed description and examples of the present invention are provided in connection with the accompanying drawings, which are set forth for the purpose of illustration only and are not intended to limit the invention.
As shown in figure 1, figure 1 is the structure schematic diagram of the embodiment of the post-treatment device for semi-aromatic polyester-polycarbonate copolymer production of the present invention, the post-treatment device for semi-aromatic polyester-polycarbonate copolymer production of the present invention comprises a polymerization reaction kettle 1, a polymerization reaction kettle product outlet 1-1, a polymerization reaction kettle gas outlet 1-2, a glue solution storage tank product inlet 2-1, a glue solution storage tank gas outlet 2-2, a glue solution storage tank liquid inlet 2-3, a glue solution storage tank glue solution outlet 2-4, a washing coagulation devolatilization kettle 3, a washing coagulation devolatilization kettle glue solution inlet 3-1, a washing coagulation devolatilization kettle gas outlet 3-2, a washing coagulation devolatilization kettle washing coagulant inlet 3-3, a washing coagulation devolatilization kettle product outlet 3-4, The device comprises a vibrating screen 4, a horizontal grinder 5, a horizontal screw centrifuge 6, a dryer 7, a cyclone separator 8, a storage bin 9, an ethanol recovery tank 10, a propylene oxide recovery tank 11, a delivery pump 12, a first condenser 13, a second condenser 14, a hot air inlet 7-3 of the dryer, a product outlet 7-4 of the dryer and a gas outlet 8-2 of the cyclone separator; a cyclone product outlet 8-3, a first bin product inlet 9-1 and a second bin product inlet 9-2; the cooling temperature of the first condenser 13 is matched with the liquefaction temperature of the gaseous propylene oxide monomer, and the propylene oxide recovery tank 11 is communicated with the outlet end of the first condenser 13; the lower part of the polymerization reaction kettle 1 is provided with a polymerization reaction kettle product outlet 1-1, and the upper part is provided with a polymerization reaction kettle gas outlet 1-2; a gas outlet of the polymerization reactor 1 is communicated to an inlet end of a first condenser 13 through a corresponding pipeline; the upper part of the glue solution storage tank 2 is provided with a product inlet 2-1 of the glue solution storage tank and a gas outlet 2-2 of the glue solution storage tank, and the lower part is provided with a glue solution outlet 2-4 of the glue solution storage tank; a gas outlet of the glue solution storage tank 2 is converged into a pipeline communicated with a gas outlet 1-2 of the polymerization reaction kettle through a corresponding pipeline; a product inlet 2-1 of the glue solution storage tank is communicated to a product outlet 1-1 of the polymerization reaction kettle through a corresponding pipeline; the lower part of the washing, condensing and devolatilizing kettle 3 is provided with a washing, condensing and devolatilizing kettle glue solution inlet 3-1, and the upper part is provided with a gas outlet 3-2 of the washing, condensing and devolatilizing kettle and a product outlet 3-4 of the washing, condensing and devolatilizing kettle; the gas outlet of the washing, condensing and devolatilizing kettle 3 is also converged into a pipeline communicated with the gas outlet 1-2 of the polymerization reaction kettle through a corresponding pipeline; a glue solution inlet 3-1 of the washing, condensing and devolatilizing kettle is communicated to a glue solution outlet 2-4 of the glue solution storage tank through a corresponding pipeline; the delivery pump 12 is arranged on a pipeline between a glue solution outlet 2-4 communicated with the glue solution storage tank and a glue solution inlet 3-1 of the washing, condensing and devolatilizing kettle; a product outlet 3-4 of the washing, condensing and devolatilizing kettle is communicated to the inlet end of the vibrating screen 4 through a corresponding pipeline; the outlet end of the vibrating screen 4 is communicated with the inlet end of a horizontal grinding machine 5, the outlet end of the horizontal grinding machine 5 is communicated with the inlet end of a horizontal screw centrifuge 6, the outlet end of the horizontal screw centrifuge 6 is communicated with the inlet end of a dryer 7, the outlet end of the dryer 7 is communicated with the inlet end of a cyclone separator 8, the outlet end of the cyclone separator 8 is communicated with the inlet end of a second condenser 14, the outlet end of the second condenser 14 is communicated with an ethanol recovery tank 10, and the outlet end of the dryer 7 is also communicated with the inlet end of a storage bin 9; the outlet end of the cyclone separator 8 is also communicated with the inlet end of a storage bin 9;
a liquid inlet 2-3 is formed in the middle of the glue solution storage tank 2 and is used for adding 5-15 wt% of water into the glue solution storage tank through a corresponding pipeline, and the water is mixed with the glue solution in the glue solution storage tank to terminate the polymerization reaction;
at least two washing coagulation devolatilization kettles are connected in parallel between a glue solution storage tank 2 and a vibrating screen 4, a glue solution inlet 3-1 of each washing coagulation devolatilization kettle 3 is gathered to a corresponding pipeline through a parallel pipeline and then communicated with a delivery pump 12, and a product outlet 3-4 of each washing coagulation devolatilization kettle is gathered to a corresponding pipeline through a parallel pipeline and then communicated with an inlet end of the vibrating screen 4;
and the lower part of each washing, condensing and devolatilizing kettle is provided with a hot water inlet 3-3 which is used for injecting 60-90 ℃ hot water containing 2-5 wt% of dispersing agent into the washing, condensing and devolatilizing kettle through a corresponding pipeline so as to remove the propylene oxide component in the glue solution.
Preferably, the polymerization reaction kettle 1, the glue solution storage tank 2 and the washing, condensing and devolatilizing kettle 3 are respectively provided with respective stirring devices, so as to be more beneficial to realizing the better volatilization functions of the polymerization reaction kettle 1, the glue solution storage tank 2 and the washing, condensing and devolatilizing kettle 3.
Different from the post-production treatment device in the prior art, the post-production treatment device of the semi-aromatic polyester-polycarbonate copolymer of the present invention has the improvement point that: on one hand, the middle part of the glue solution storage tank 2 is provided with a liquid inlet 2-3, which is used for adding water which is 5-15 wt% of the total amount of the glue solution into the glue solution storage tank 2 through a corresponding pipeline 17, stirring and mixing the water with a crude product in the glue solution storage tank 2 to terminate the polymerization reaction, volatilizing part of monomer solvent such as a propylene oxide monomer into gas, entering a corresponding pipeline 16 from a gas outlet 2-2 of the glue solution storage tank, converging the gas into a pipeline communicated with a gas outlet 1-2 of the polymerization reaction kettle 1, cooling the gas by a first condenser 13, and then entering a propylene oxide recovery tank 11; the glue solution obtained by the method is sprayed into a washing, condensing and devolatilizing kettle 3 from a glue solution inlet 3-1 of the washing, condensing and devolatilizing kettle from a glue solution outlet 2-4 of a glue solution storage tank through a corresponding pipeline 18 under the action of a delivery pump 12; on the other hand, at least two washing coagulation devolatilization kettles 3 (for example, three washing coagulation devolatilization kettles 3 shown in the embodiment of fig. 1) are connected in parallel between the glue solution storage tank 2 and the vibrating screen 4, the glue solution inlet 3-1 of each washing coagulation devolatilization kettle 3 is gathered to the corresponding pipeline 18 through the parallel pipeline and then communicated with the delivery pump 12, and the product outlet 3-4 of each washing coagulation devolatilization kettle 3 is gathered to the corresponding pipeline 21 through the parallel pipeline and then communicated with the vibrating screen 4; the lower part of each washing, condensing and devolatilizing kettle 3 is provided with a hot water (washing coagulant) inlet 3-3 which is used for injecting hot water with the temperature of 60-90 ℃ into the washing, condensing and devolatilizing kettle 3 through a corresponding pipeline, so that residual propylene oxide in the glue solution is volatilized into gas to the maximum extent, and the gas enters the corresponding pipeline from a gas outlet 3-2, is converged into a pipeline 20 communicated with a gas outlet 1-2 of the polymerization reaction kettle 1, is cooled by a first condenser 13, and then enters a propylene oxide recovery tank 11; and the components such as the catalyst, the cyclic carbonate and the like are washed out, the obtained semi-aromatic polyester-polycarbonate copolymer blocky solid suspended substance is gathered to a corresponding pipeline 21 from a product outlet 3-4 of the washing condensation devolatilization kettle 3 through parallel pipelines, enters a vibrating screen 4, enters a horizontal grinder 5 for grinding to obtain semi-aromatic polyester-polycarbonate copolymer powdery solid, the ground powdery solid enters a horizontal spiral separator 6, the horizontal spiral separator 6 separates ethanol from the polymer, the ethanol and the polymer are dried through a dryer 7, the powder enters a bin 9, and part of fine particle powder also enters the bin 9 after being settled through a cyclone separator 8. Finally, the powdery semi-aromatic polyester-polycarbonate copolymer after washing, condensation and devolatilization is obtained, so as to facilitate the subsequent processing and transportation. The ethanol removed in the drying process is recovered to the ethanol recovery tank 10 through the second condenser 14 together with the hot air. The dryer 7 may be a drying device such as tubular air flow drying, fluidized bed drying, spouted drying, tank/tub/drum paddle/non-paddle drying, expansion drying, centrifugal liquefaction drying, or a combination thereof, preferably a combination of drum paddle drying and tray drying. The device for post-production treatment of the semi-aromatic polyester-polycarbonate copolymer of the utility model also comprises an ethanol recovery tank 10 and a second condenser 14, the cooling temperature of the second condenser 14 is matched with the liquefaction temperature of the gaseous ethanol, and the ethanol recovery tank 10 is communicated with the outlet end of the second condenser 14;
the outlet end of the vibrating screen 4 is communicated with the inlet end of a horizontal grinding machine 5, the outlet end of the horizontal grinding machine 5 is communicated with the inlet end of a horizontal screw centrifuge 6, the outlet end of the horizontal screw centrifuge 6 is communicated with the inlet end of a dryer 7, the outlet end of the dryer 7 is communicated with the inlet end of a cyclone separator 8, the outlet end of the cyclone separator 8 is communicated with the inlet end of a second condenser 14, the outlet end of the second condenser 14 is communicated with an ethanol recovery tank 10, and the outlet end of the dryer 7 is also communicated with the inlet end of a storage bin 9; the outlet end of the cyclone separator 8 is also communicated with the inlet end of a storage bin 9; after the separation of the cyclone separator 8, the ethanol is cooled by a second condenser 14 and then enters an ethanol recovery tank 10.
The utility model discloses semi-aromatic polyester-polycarbonate copolymer's production aftertreatment device, physical characteristic to semi-aromatic polyester-polycarbonate copolymer, 5 ~ 15 wt% water and the glue solution stirring in glue solution storage tank 2 have been adopted earlier creatively, mix with termination polymerization, 60 ~ 90 ℃ hot water that will contain 2 ~ 5 wt% dispersant again is as the washing coagulant, it volatilizes cauldron 3 interior surplus low boiling point monomer epoxypropane (34 ℃) to deviate from the glue solution as far as possible to wash the coagulation, components such as catalyst and cyclic annular carbonate, combine two at least washing coagulation to volatilize the parallel structure of cauldron 3 constitution simultaneously, can greatly shorten the coagulation time of volatilizing, obviously improve production aftertreatment efficiency, show the quality that improves the PPC product, and be applicable to all PPC products.
Preferably, hot water with the temperature of 60-90 ℃ which is equivalent to 5-15 wt% of the total amount of the glue solution is added into the glue solution storage tank 2 from a liquid inlet 2-3 of the glue solution storage tank 2 through a corresponding pipeline 17, more epoxy propane monomers are volatilized into gas by utilizing the pressure of the glue solution storage tank 2, and the gas enters a corresponding pipeline 16 from a gas outlet 2-2, so that the glue solution can be obtained more quickly.
The glue solution in the glue solution storage tank 2 comprises semi-aromatic polyester-polycarbonate copolymer, propylene oxide, cyclic carbonate, catalyst, cocatalyst and branching agent, wherein the catalyst, cocatalyst and branching agent are well known in the art and are not described in detail herein.
Preferably, the grinding medium of the horizontal grinder 5 is ethanol having a temperature of 30 ± 10 ℃, and when the semi-aromatic polyester-polycarbonate copolymer enters the horizontal grinder 5, the block polymer is hardened by cooling, thereby facilitating grinding of the semi-aromatic polyester-polycarbonate copolymer into a powdery solid.
Preferably, the diameter of the pipeline communicated with the glue solution inlet 3-1 of each washing, condensing and devolatilizing kettle 3 is 50-100 mm, and the flow rate of hot water of 60-90 ℃ injected into the washing, condensing and devolatilizing kettle 3 from the washing and coagulating agent inlet 3-3 is regulated to be matched with the flow rate of glue solution pumped into the washing, condensing and devolatilizing kettle 3 through the delivery pump 12, so that the obtained semi-aromatic polyester-polycarbonate copolymer blocky suspended solid has better fluidity and larger apparent density, is more beneficial to solid-liquid separation of the vibrating screen 4, and is more beneficial to grinding by the horizontal grinder 5.
Based on the production aftertreatment device of above-mentioned semi-aromatic polyester-polycarbonate copolymer, the utility model also provides a production aftertreatment method of semi-aromatic polyester-polycarbonate copolymer, mainly includes following step:
A. adding 5-15 wt% of water into the glue solution storage tank, and stirring and mixing the water and the crude product in the glue solution storage tank to terminate the polymerization reaction;
B. injecting hot water at 60-90 ℃ containing 2-5 wt% of a dispersing agent into the washing, condensing and devolatilizing kettle to remove the epoxypropane component in the glue solution; the flow rate of hot water injected into the washing, condensing and devolatilizing kettle is regulated to be matched with the flow rate of glue solution pumped into the washing, condensing and devolatilizing kettle, so that the mass ratio of water to the glue solution is controlled to be 95: 5-80: 20, and the residence time of the glue solution in the washing, condensing and devolatilizing kettle is more than 30 minutes;
C. the grinding balls added into the horizontal grinding machine are ceramic balls, the diameter of each grinding ball is 1-5 cm, the adding amount of the grinding balls accounts for 30-60% of the volume of the horizontal grinding machine, and the particle size of the ground material is smaller than 5 mm;
D. centrifuging the polymer and ethanol by using a horizontal spiral separator to obtain a polymer containing 10-15 wt% of ethanol, drying the separated ethanol by using a dryer, and returning the dried ethanol to an ethanol storage tank for reuse;
E. and (3) feeding the powder dried by the dryer into a storage bin to finally obtain the powdery semi-aromatic polyester-polycarbonate copolymer after washing, coagulation and devolatilization.
The utility model discloses a production post-treatment method of semi-aromatic polyester-polycarbonate copolymer, greatly reduced the cost of PPC product, obviously reduced the negative effects that little molecule remained and caused PPC product property, obviously improved the quality of PPC product to be applicable to all PPC products; the production process is simpler, is more suitable for automatic control, can continuously carry out post-production treatment operation, and can fully utilize material energy; the adopted post-production treatment device is basically a closed container and a pipeline with pressure, the air is not contacted with the ambient air at all, no gas phase is exhausted basically in the operation process (namely, the gas phase is collected by a condensing system), the cleaning is not needed, the product is completely deashed and devolatilized, the generated solid-liquid waste is very little, and the use requirements of raw materials in related fields are met; meanwhile, the industrial production cost is lower, and the industrial process basically meets the requirement of green chemistry.
Example 1, taking 30L polymerization reaction vessel 1, 40L glue solution storage tank 2 and three 30L washing coagulation devolatilization vessels 3 connected in parallel as an example, the diameter of the pipe connected to the glue solution inlet 3-1 of each washing coagulation devolatilization vessel 3 was 50mm, the content of propylene oxide was 40 wt% and the content of cyclic carbonate was 10 wt% in the reaction solution after the polymerization reaction of the polymerization reaction vessel 1 was completed, the reaction solution was injected into the glue solution storage tank 2, and at the same time, 85 ℃ hot water equivalent to 10 wt% of the reaction solution was added to terminate the reaction to obtain a glue solution, and then the glue solution was injected into the washing coagulation devolatilization vessel 3 through transfer pump 12, and at the same time, 85 ℃ hot water was injected, and the coolant in condenser No. 22 was 7 ℃ brine; after the semi-aromatic polyester-polycarbonate copolymer production post-treatment device is adopted for production post-treatment, the content of the propylene oxide is reduced to 0.2 wt% and the content of the cyclic carbonate is reduced to 1.2 wt% in the obtained semi-aromatic polyester-polycarbonate copolymer powdery solid; the dried powdery solid was dissolved in methylene chloride and washed by ethanol extraction without turbidity, i.e., no significant (oligomers and catalyst) residue was observed.
Meanwhile, the utility model discloses still adopt the Nuclear Magnetic Resonance Spectroscopy (Nuclear Magnetic Resonance Spectroscopy, NMR for short) of research atomic nucleus to Radio frequency Radiation (Radio-frequency Radiation) absorption to carry out analysis and verification to the composition and the structure of the semi-aromatic polyester-polycarbonate copolymer powder that example 1 obtained, can see from the verification result and adopt the utility model discloses after semi-aromatic polyester-polycarbonate copolymer's production aftertreatment device carries out the production posttreatment, the content of epoxypropane component and cyclic carbonate component all obviously reduces, and especially the epoxypropane component as monomer and solvent has basically got rid of totally from the polycarbonate product.
Example 2 is different from example 1 in that the reaction liquid after completion of the polymerization reaction in the polymerization reactor 1 contains propylene oxide in an amount of 45 wt% and cyclic carbonate in an amount of 9 wt%; after the semi-aromatic polyester-polycarbonate copolymer production post-treatment device is adopted for production post-treatment, the content of the propylene oxide is reduced to 0.3 wt% and the content of the cyclic carbonate is reduced to 1.0 wt% in the obtained semi-aromatic polyester-polycarbonate copolymer powdery solid; the dried powdery solid was dissolved in methylene chloride and washed with ethanol without turbidity, i.e., no significant (oligomers and catalyst) residue was observed.
Example 3, different from example 1, in the reaction solution after completion of the polymerization reaction in the polymerization reactor 1, the content of propylene oxide was 50 wt%, and the content of cyclic carbonate was 11 wt%; after the semi-aromatic polyester-polycarbonate copolymer production post-treatment device is adopted for production post-treatment, the content of the propylene oxide is reduced to 0.4 wt% and the content of the cyclic carbonate is reduced to 1.3 wt% in the obtained semi-aromatic polyester-polycarbonate copolymer powdery solid; the dried powdery solid was dissolved in methylene chloride and washed with ethanol without turbidity, i.e., no significant precipitation of (oligomers and catalyst) residue was observed.
From the data results of the above three examples, it can be seen that, with the gradual increase of the propylene oxide content and the cyclic carbonate content in the reaction liquid added into the polymerization reactor 1, after the post-production treatment device for semi-aromatic polyester-polycarbonate copolymer of the present invention is used for post-production treatment, the propylene oxide content and the cyclic carbonate content in the obtained powdery solid of semi-aromatic polyester-polycarbonate copolymer are not significantly increased, which shows that the post-production treatment device and method for semi-aromatic polyester-polycarbonate copolymer of the present invention have an efficient removal effect on both the propylene oxide component and the cyclic carbonate component in the semi-aromatic polyester-polycarbonate copolymer.
It should be understood that the above-mentioned embodiments are only preferred embodiments of the present invention, and are not intended to limit the technical solutions of the present invention, and those skilled in the art can add, subtract, replace, change or modify the above-mentioned embodiments within the spirit and principle of the present invention, and all such additions, substitutions, changes or modifications should fall within the scope of the appended claims.
Claims (7)
1. A post-treatment device for production of semi-aromatic polyester-polycarbonate copolymer is characterized by comprising a polymerization reaction kettle, a polymerization reaction kettle product outlet, a polymerization reaction kettle gas outlet, a glue solution storage tank product inlet, a glue solution storage tank gas outlet, a glue solution storage tank liquid inlet, a glue solution storage tank glue solution outlet, a washing condensation devolatilization kettle glue solution inlet, a washing condensation devolatilization kettle gas outlet, a washing condensation devolatilization kettle washing coagulant inlet, a washing condensation devolatilization kettle product outlet, a vibrating screen, a horizontal grinder, a horizontal screw centrifuge, a dryer, a cyclone separator, a storage bin, an ethanol recovery tank, a propylene oxide recovery tank, a delivery pump, a first condenser, a second condenser, a dryer hot air inlet, a dryer product outlet and a cyclone separator gas outlet; a cyclone product outlet, a first bin product inlet and a second bin product inlet; the cooling temperature of the first condenser is matched with the liquefaction temperature of the gaseous propylene oxide monomer, and the propylene oxide recovery tank is communicated with the outlet end of the first condenser; the lower part of the polymerization reaction kettle is provided with a product outlet, and the upper part of the polymerization reaction kettle is provided with a gas outlet; a gas outlet of the polymerization reactor is communicated to the inlet end of the first condenser through a corresponding pipeline; the upper part of the glue solution storage tank is provided with a product inlet and a gas outlet, and the lower part is provided with a glue solution outlet; the gas outlet of the glue solution storage tank is converged into a pipeline communicated with the gas outlet of the polymerization reaction kettle through a corresponding pipeline; a product inlet of the glue solution storage tank is communicated to a product outlet of the polymerization reaction kettle through a corresponding pipeline; the lower part of the washing, condensing and devolatilizing kettle is provided with a glue solution inlet and a hot water inlet, and the upper part is provided with a gas outlet and a product outlet; the gas outlet of the washing, condensing and devolatilizing kettle is also converged into a pipeline communicated with the gas outlet of the polymerization reaction kettle through a corresponding pipeline; a glue solution inlet of the washing, condensing and devolatilizing kettle is communicated to a glue solution outlet of a glue solution storage tank through a corresponding pipeline; the delivery pump is arranged on a pipeline which is communicated between a glue solution outlet of the glue solution storage tank and a glue solution inlet of the washing, condensing and devolatilizing kettle; the product outlet of the washing, condensing and devolatilizing kettle is communicated to the inlet end of the vibrating screen through a corresponding pipeline; the outlet end of the vibrating screen is communicated with the inlet end of the horizontal grinding machine, the outlet end of the horizontal grinding machine is communicated with the inlet end of the horizontal screw centrifuge, the outlet end of the horizontal screw centrifuge is communicated with the inlet end of the dryer, the outlet end of the dryer is communicated with the inlet end of the cyclone separator, the outlet end of the cyclone separator is communicated with the inlet end of the second condenser, the outlet end of the second condenser is communicated with the ethanol recovery tank, and the outlet end of the dryer is also communicated with the inlet end of the storage bin; the outlet end of the cyclone separator is also communicated with the inlet end of the storage bin;
a liquid inlet is arranged in the middle of the glue solution storage tank;
at least two washing, condensing and devolatilizing kettles are connected in parallel between a glue solution storage tank and a vibrating screen, the glue solution inlet of each washing, condensing and devolatilizing kettle is gathered to a corresponding pipeline through a parallel pipeline and then is communicated with a conveying pump, and the product outlet of each washing, condensing and devolatilizing kettle is gathered to a corresponding pipeline through a parallel pipeline and then is communicated with the inlet end of the vibrating screen;
and the lower part of each washing, condensing and devolatilizing kettle is provided with a hot water inlet for injecting hot water of 60-90 ℃ into the washing, condensing and devolatilizing kettle through a corresponding pipeline so as to remove the propylene oxide component in the glue solution.
2. The post-production treatment apparatus of a semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: three washing, condensing and devolatilizing kettles are connected in parallel between the glue solution storage tank and the vibrating screen.
3. The post-production treatment apparatus of a semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: the capacity of the polymerization reaction kettle is 30L, the capacity of the glue solution storage tank is 40L, and the capacity of each washing, condensing and devolatilizing kettle is 30L.
4. The post-production treatment apparatus of a semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: a stirring device is arranged in the polymerization reaction kettle; and a stirring device is arranged in the glue solution storage tank.
5. The post-production treatment apparatus of a semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: and a stirring device is arranged in the washing, condensing and devolatilizing kettle.
6. The post-production treatment apparatus of a semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: the grinding medium adopted by the horizontal grinding machine is ethanol with the temperature of 30 +/-10 ℃.
7. The post-production treatment apparatus of a semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: the diameter of the pipeline communicated with the glue solution inlet of each washing, condensing and devolatilizing kettle is 50-100 mm.
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