CN112898552B - Condensation devolatilization device and method for semi-aromatic polyester-polycarbonate copolymer - Google Patents

Abstract

The invention discloses a device and method for condensation and devolatilization of semi-aromatic polyester-polycarbonate copolymer. The method includes adding 5 to 15 wt% water into a glue storage tank, and mixing it with the glue in the glue storage tank. Mixing terminates the polymerization reaction; injects hot water of 60 to 90°C into the washing coagulation and devolatilization kettle to remove the propylene oxide component in the glue; and regulates the flow rate of hot water injected into the washing coagulation and devolatilization kettle and the flow rate of the hot water into the washing coagulation and devolatilization kettle. The flow rate of the glue liquid pumped into the devolatilization kettle matches; because 5 to 15 wt% water is first used to terminate the polymerization reaction, and then hot water of 60 to 90°C is used as the washing coagulant, the epoxy as the reactant and solvent is efficiently recovered Propane. It can reduce the coagulation and devolatilization time after polymerization, significantly improve the coagulation and devolatilization efficiency, significantly improve the quality of PPC products, and is applicable to all PPC products.

Description

Condensation devolatilization device and method for semi-aromatic polyester-polycarbonate copolymer

Technical field

The present invention relates to a condensation devolatilization device for polycarbonate copolymers and the technical field thereof, and in particular to a condensation devolatilization device and a condensation devolatilization method for semi-aromatic polyester-polycarbonate copolymers.

Background technique

Since the Industrial Revolution, the amount of heat-trapping greenhouse gases such as carbon dioxide emitted by humans into the atmosphere has increased year by year, and the greenhouse effect of the atmosphere has also increased, which has triggered a series of environmental problems and attracted the attention of countries around the world; as Carbon dioxide, the main gas causing the greenhouse effect, is also one of the most abundant carbon sources on the earth. How to rationally utilize carbon dioxide can effectively reduce the greenhouse effect and turn waste into treasure. For example, it can be fixed by chemical methods and use carbon dioxide as raw material. Polycarbonate is prepared by copolymerizing alkylene oxide with alkylene oxide under the action of a catalyst. The existing Chinese patent document CN111378101A disclosed by the inventor Meng Yuezhong uses a commercial, simple and efficient catalytic initiation system to catalytically initiate propylene oxide, carbon dioxide and ophthalmic acid. Phthalic anhydride performs ternary copolymerization and successfully introduces an aromatic polyester structure with a content of 10-40% into polymethylethylene carbonate (PPC). This product is synthetically modified PPC and has good biological properties. Degradability, light transmittance and barrier properties, etc., are used in agricultural mulch films, food packaging bags, and disposable medical materials; however, due to the low glass transition temperature of PPC (30~40°C), it also makes it difficult to process in industrial processes. There are certain shortcomings in transportation, transportation and other links. Relevant researchers have also used various methods to increase their glass transition temperature, such as: ternary copolymerization, cross-linking, blending with other polymers, inorganic fillers and organic composites.

The existing patent document CN111378101A synthesizes a semi-aromatic polyester-polycarbonate copolymer polymer under certain reaction conditions by introducing aromatic anhydride as a reaction monomer, propylene oxide and carbon dioxide through the action of a catalyst, which can effectively improve the material's properties. The glass transition temperature and the reduction of its melt index are very beneficial to subsequent processing and transportation; and by adding polymerization aids, the molecular weight and distribution of polymer products can also be effectively increased.

However, there are some relatively mature condensation devolatilization processes on the existing market, which all have certain limitations, such as difficulty in completely removing catalyst residues, complex processes, and high production costs. They are not suitable for all PPC products. Under bulk polymerization process conditions, propylene oxide is used as both a monomer and a solvent. At the end of the polymerization reaction, the crude product contains 30% to 70% propylene oxide, and this part of the raw material needs to be recycled to reduce production costs. Residual propylene oxide will also cause the polymer to have a strong pungent odor, which is harmful to human health. It is worth noting that during the polymerization reaction, the by-product cyclic carbonate is produced, and its residue in the product will also have a negative impact on the performance of the product, so it needs to be completely removed.

Therefore, the existing technology still needs to be improved and developed.

Contents of the invention

In order to solve the above technical problems, the present invention provides a condensation and devolatilization device for semi-aromatic polyester-polycarbonate copolymer, which can reduce the condensation and devolatilization time after polymerization, significantly improve the condensation and devolatilization efficiency, and significantly improve the quality of PPC products. , and applies to all PPC products.

At the same time, the present invention also provides a condensation and devolatilization method of semi-aromatic polyester-polycarbonate copolymer, which can greatly reduce the cost of PPC products, significantly reduce the negative impact of small molecule residues on the performance of PPC products, and significantly improve the performance of PPC products. product quality and applies to all PPC products.

The technical solution of the present invention is as follows:

A coagulation and devolatilization device for semi-aromatic polyester-polycarbonate copolymer, including a polymerization reaction kettle, a glue storage tank, a washing coagulation and devolatilization kettle, a transfer pump, a vibrating screen, a horizontal grinder and a decanter separator ; The lower part of the polymerization reactor is provided with a product outlet, and the upper part is provided with a gas outlet; the upper part of the glue storage tank is provided with a product inlet and a gas outlet, and the lower part is provided with a glue outlet; the product inlet of the glue storage tank is connected through a corresponding pipeline to the product outlet of the polymerization reactor; the lower part of the washing, condensation and devolatilization kettle is provided with a glue inlet, and the upper part is provided with a product outlet and a gas outlet; the glue inlet of the washing, condensation and devolatilization kettle is connected to the glue storage tank through corresponding pipelines Glue outlet; the transfer pump is installed on the pipeline between the glue outlet of the glue storage tank and the glue inlet of the washing, condensation and devolatilization kettle; the product outlet of the washing, condensation and devolatilization kettle is connected to the vibrating screen through the corresponding pipe, and the vibration The screen is connected to the horizontal grinder through corresponding pipes, and the horizontal grinder is connected to the inlet end of the decanter separator through corresponding pipes;

There is a liquid inlet in the middle of the glue storage tank, which is used to add 5~15wt% water into the glue storage tank through the corresponding pipeline, and mix it with the glue in the glue storage tank to terminate the polymerization reaction;

At least two washing, condensation and devolatilization kettles are connected in parallel between the glue storage tank and the vibrating screen. The glue inlet of each washing, condensation and devolatilization kettle is collected through parallel pipelines to the corresponding pipeline and then connected to the transfer pump. The product outlet of each washing, condensation and devolatilization kettle is collected through parallel pipelines to the corresponding pipeline and then connected to the inlet end of the vibrating screen;

And the lower part of each washing, condensation and devolatilization kettle is provided with a hot water inlet, which is used to inject 60-90°C hot water into the washing, condensation and devolatilization kettle through corresponding pipelines to remove the propylene oxide component in the glue solution. .

Further, in the above-mentioned coagulation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer: three washing coagulation and devolatilization kettles are connected in parallel between the glue storage tank and the vibrating screen.

Further, in the above-mentioned condensation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer, the capacity of the polymerization reactor is 30L, the capacity of the glue storage tank is 40L, and each washing condensation and devolatilization kettle The capacity is 30L.

Further, in the above-mentioned coagulation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer, a stirring device is provided in the polymerization reaction kettle.

Further, in the above-mentioned coagulation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer, a stirring device is provided in the glue storage tank.

Further, in the above-mentioned coagulation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer, a stirring device is provided in the washing coagulation and devolatilization tank.

Further, in the above-mentioned condensation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer, the grinding medium used in the horizontal grinder is ethanol with a temperature of 30±10°C.

Further, in the above-mentioned condensation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer, the diameter of the pipe connected to the glue inlet of each washing condensation and devolatilization kettle is between 50 and 100 mm.

Further, in the above-mentioned coagulation and devolatilization device of the semi-aromatic polyester-polycarbonate copolymer, the hot water at 60-90°C contains 2-5 wt% dispersant.

A condensation and devolatilization method of semi-aromatic polyester-polycarbonate copolymer, using the above-mentioned condensation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer, including the following steps:

A. Add 5~15wt% water into the glue storage tank, stir and mix with the crude product in the glue storage tank to terminate the polymerization reaction;

B. Inject 60-90°C hot water containing 2~5wt% dispersant into the washing coagulation and devolatilization kettle to remove the propylene oxide component in the glue solution; and regulate the amount of hot water injected into the washing coagulation and devolatilization kettle. The flow rate matches the flow rate of the glue pumped into the washing coagulation and devolatilization kettle, so that the mass ratio of water and glue is controlled at 95:5~80:20, and the residence time of the glue in the washing coagulation and devolatilization kettle is greater than 30 minutes. ;

C. The grinding balls added to the horizontal grinder are ceramic balls. The diameter of the grinding balls is 1~5cm. The amount of grinding balls added accounts for 30%~60% of the volume of the horizontal grinder. The particle size of the material after grinding less than 5mm;

D. The decanter separator centrifugally separates the polymer and ethanol to obtain a polymer containing 10~15wt% ethanol. The separated ethanol is returned to the ethanol storage tank for reuse.

The invention provides a condensation devolatilization device and a condensation devolatilization method for a semi-aromatic polyester-polycarbonate copolymer. Since 5 to 15 wt% water is first used to terminate the polymerization reaction, then water containing 60 to 90°C is used. Hot water with 2~5wt% dispersant is used as a washing coagulant to efficiently recover propylene oxide as a reactant and solvent, which can reduce the coagulation and devolatilization time after polymerization, significantly improve the coagulation and devolatilization efficiency, and greatly reduce the cost of PPC products. , significantly reduces the negative impact of small molecule residues on the performance of PPC products, significantly improves the quality of PPC products, and is applicable to all PPC products.

Description of drawings

The drawings described here are for illustrative purposes only and are not intended to limit the scope of the disclosure of the present invention in any way; the shapes and proportional dimensions of each component in the drawings are only schematic and are used to help the understanding of the present invention. The shape and proportional dimensions of each component of the present invention are not specifically limited; those skilled in the art, under the teachings of the present invention, can select various possible shapes and proportional dimensions according to specific circumstances to implement the present invention.

Figure 1 is a schematic structural diagram of an embodiment of a condensation and devolatilization device for semi-aromatic polyester-polycarbonate copolymer of the present invention;

Figure 2 is a nuclear magnetic spectrum of each component of the sample obtained in Example 1 of the condensation devolatilization method of the semi-aromatic polyester-polycarbonate copolymer of the present invention;

Summary of the numbers in the figure: polymerization reactor 1, product outlet 1-1, gas outlet 1-2, glue storage tank 2, product inlet 2-1, gas outlet 2-2, liquid inlet 2-3, glue outlet 2-4. Washing coagulation and devolatilization kettle 3. Glue inlet 3-1, gas outlet 3-2, hot water (washing coagulant) inlet 3-3, product outlet 3-4, vibrating screen 4, horizontal grinder 5 and decanter 6, next processing unit 7, transfer pump 8, pipelines (9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22).

Detailed ways

Specific implementations and examples of the present invention will be described in detail below with reference to the accompanying drawings. The described specific embodiments are only used to explain the present invention and are not intended to limit the specific implementations of the present invention.

As shown in Figure 1, Figure 1 is a schematic structural diagram of an embodiment of the condensation and devolatilization device of the semi-aromatic polyester-polycarbonate copolymer of the present invention. The device includes a polymerization reaction kettle 1, a glue storage tank 2, a washing, coagulation and devolatilization kettle 3, a transfer pump 8, a vibrating screen 4, a horizontal grinder 5 and a decanter separator 6; among them, the lower part of the polymerization reaction kettle 1 is provided with The product outlet 1-1 is provided with a gas outlet 1-2 on the upper part. Under abnormal circumstances, the gas outlet 1-2 is used for venting; the upper part of the glue storage tank 2 is provided with a product inlet 2-1 and a gas outlet 2- 2. There is a glue outlet 2-4 in the lower part; the product inlet 2-1 of the glue storage tank 2 is connected to the product outlet 1-1 of the polymerization reactor 1 through the corresponding pipeline 9; the washing, condensation and devolatilization kettle 3 is provided in the lower part. The glue inlet 3-1 and the hot water inlet 3-3 are provided with a product outlet 3-4 and a gas outlet 3-2 on the upper part; the glue inlet 3-1 of the washing, condensation and devolatilization kettle 3 is connected to the glue through the corresponding pipeline 12 The glue liquid outlet 2-4 of the liquid storage tank 2; hot water enters the washing, condensation and devolatilization kettle 3 from the hot water inlet 3-3 through the pipe 13, and the delivery pump 8 is installed in the glue liquid outlet 2-4 of the glue liquid storage tank 2 on the pipeline 12 between the glue liquid inlet 3-1 of the washing, condensation and devolatilization kettle 3; the product outlet 3-4 of the washing, condensation and devolatilization kettle 3 is connected to the inlet end of the vibrating screen 4 via corresponding pipes (15 and 16) , the outlet end of the vibrating screen 4 is connected to the inlet end of the horizontal grinder 5 , the outlet end of the horizontal grinder 5 is connected to the inlet end of the decanter separator 6 , and the outlet end of the decanter separator 6 is connected to the next processing unit 7 .

Preferably, the polymerization reactor 1, the glue storage tank 2 and the washing, coagulation and devolatization kettle 3 are each provided with their own stirring devices, so as to facilitate the realization of the polymerization reaction kettle 1, the glue storage tank 2 and the washing, coagulation and devolatization. Volatile kettle 3 has better volatilization function.

Different from the condensation and devolatilization device in the prior art, the improvement points of the condensation and devolatilization device of the semi-aromatic polyester-polycarbonate copolymer of the present invention are: on the one hand, a liquid is arranged in the middle of the glue storage tank 2 Inlet 2-3 is used to add water equivalent to 5~15wt% of the total amount of glue into the glue storage tank 2 through the corresponding pipeline 11, and stir and mix with the crude product in the glue storage tank 2 to terminate the polymerization reaction , part of the monomer solvent such as propylene oxide monomer volatilizes into gas and enters the corresponding pipeline 10 from the gas outlet 2-2. The glue obtained thereby passes from the glue outlet 2-4 through the corresponding pipe under the action of the delivery pump 8. The pipeline (12) is sprayed from the glue inlet 3-1 into the washing coagulation and devolatilization kettle 3; on the other hand, it is composed of at least two washing coagulation and devolatilization kettles 3 (for example, the three washing coagulation and devolatilization kettles shown in the embodiment of Figure 1 3) Connected in parallel between the glue storage tank 2 and the vibrating screen 4, the glue inlet 3-1 of each washing, condensation and devolatilization kettle 3 is collected through parallel pipelines to the corresponding pipeline 12 and then connected to the delivery pump 8 , and the product outlets 3-4 of each washing, condensation and devolatilization tank 3 are collected to the corresponding pipeline 16 through the parallel pipeline 15, and then connected to the inlet end of the decanter separator 6 through the vibrating screen 4 and the horizontal grinder 5 and the lower part of each washing coagulation and devolatilization kettle 3 is provided with a washing coagulant inlet 3-3, which is used to inject 60-90°C dispersion containing 2-5wt% into the washing coagulation and devolatilization kettle 3 through the corresponding pipeline. The hot water of the agent is used to volatilize the remaining propylene oxide in the glue into gas to the greatest extent and enter the corresponding pipe 14 from the gas outlet 3-2, while the components such as the catalyst and cyclic carbonate are washed out, and the The obtained semi-aromatic polyester-polycarbonate copolymer block solid suspension is first separated from the hot water and the polymer by using the vibrating screen 5, and then ethanol is added to the horizontal grinder 5 to wash down the water and polymerize at the same time. The material is ground into smaller particles, and then the ethanol and polymer are separated by a decanter 6, and finally a powdery solid of semi-aromatic polyester-polycarbonate copolymer is obtained.

According to the physical properties of the semi-aromatic polyester-polycarbonate copolymer, the condensation and devolatilization device of the semi-aromatic polyester-polycarbonate copolymer of the present invention creatively adopts the method of first mixing 5 to 15 wt% water and glue. The glue liquid in the storage tank 2 is stirred and mixed to terminate the polymerization reaction, and then hot water at 60 to 90°C containing 2 to 5 wt% dispersant is used as a washing coagulant to remove as much glue as possible in the washing, coagulation and devolatilization tank 3 The remaining low boiling point monomer propylene oxide (34°C), catalyst, cyclic carbonate and other components in the liquid are simultaneously combined with a parallel structure composed of at least two washing condensation and devolatilization kettles 3, which can greatly shorten the condensation and devolatilization time. , significantly improve the condensation devolatilization efficiency, significantly improve the quality of PPC products, and is applicable to all PPC products.

Preferably, 60-90°C hot water equivalent to 5-15wt% of the total amount of glue is added into the glue storage tank 2 from the liquid inlet 2-3 of the glue storage tank 2 through the corresponding pipeline 11, and the glue is used. When the pressure of the liquid storage tank 2 increases, more propylene oxide monomer volatilizes into gas and enters the corresponding pipeline 10 from the gas outlet 2-2, so that the glue liquid can be obtained more quickly.

The glue in the glue storage tank 2 includes semi-aromatic polyester-polycarbonate copolymer, propylene oxide, cyclic carbonate, catalyst, co-catalyst and branching agent, wherein the catalyst, co-catalyst and branching agent Chemical agents are well known in the art and will not be described in detail here.

Preferably, the horizontal grinder 5 is a ball grinder, and the grinding medium is ethanol with a temperature of 30±10°C. When the semi-aromatic polyester-polycarbonate copolymer enters the horizontal grinder, the bulk polymer It hardens when cooled, thus making it easier to grind the semi-aromatic polyester-polycarbonate copolymer into a powdery solid.

Preferably, the diameter of the pipe 12 connected to the glue inlet 3-1 of each washing condensation and devolatilization kettle 3 is between 50 and 100 mm, and the regulation is from the hot water inlet 3-3 to the washing condensation and devolatilization kettle 3. The flow rate of 60-90°C hot water injected into the kettle 3 matches the flow rate of the glue liquid pumped into the washing, condensation and devolatilization kettle 3 through the transfer pump 8, and the semi-aromatic polyester-polycarbonate copolymer block solid obtained thereby The suspended solids have better fluidity and greater apparent density, which is more conducive to solid-liquid separation by the vibrating screen 4 and grinding by the horizontal grinder 5.

Based on the above-mentioned condensation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer, the present invention also proposes a condensation and devolatilization method of semi-aromatic polyester-polycarbonate copolymer, which mainly includes the following steps:

A. Add 5~15wt% water into the glue storage tank, stir and mix with the crude product in the glue storage tank to terminate the polymerization reaction;

B. Inject 60-90°C hot water containing 2~5wt% dispersant into the washing coagulation and devolatilization kettle to remove the propylene oxide component in the glue solution; and regulate the amount of hot water injected into the washing coagulation and devolatilization kettle. The flow rate matches the flow rate of the glue pumped into the washing coagulation and devolatilization kettle, so that the mass ratio of water and glue is controlled at 95:5~80:20, and the residence time of the glue in the washing coagulation and devolatilization kettle is greater than 30 minutes. ;

C. The grinding balls added to the horizontal grinder are ceramic balls. The diameter of the grinding balls is 1~5cm. The amount of grinding balls added accounts for 30%~60% of the volume of the horizontal grinder. The particle size of the material after grinding less than 5mm;

D. The decanter separator centrifugally separates the polymer and ethanol to obtain a polymer containing 10~15wt% ethanol. The separated ethanol is returned to the ethanol storage tank for reuse.

The condensation and devolatilization method of the semi-aromatic polyester-polycarbonate copolymer of the present invention greatly reduces the cost of PPC products, significantly reduces the negative impact of small molecule residues on the performance of PPC products, and significantly improves the quality of PPC products. , and is applicable to all PPC products; the production process is simpler, more suitable for automatic control, can continuously carry out condensation and devolatilization operations, and can make full use of material energy; and the condensation and devolatilization device used is basically a closed and pressurized one. Containers and pipelines are not in contact with the surrounding air at all. There is basically no gas phase evacuation (i.e. collection through the condensation system) during the operation, and no cleaning is required. The product is completely dedusted and devolatilized, producing very little solid and liquid waste, which meets the requirements It meets the raw material usage requirements in related fields; at the same time, the cost of industrialized production is lower, and the industrialization process basically meets the requirements of green chemistry.

Example 1, taking a 30L polymerization reactor 1, a 40L glue storage tank 2 and three parallel 30L washing, condensation and devolatilization kettles 3 as an example, the glue inlet 3-1 of each washing, condensation and devolatilization kettle 3 is connected. The diameters of the pipes 13 are all 50mm. The content of propylene oxide in the reaction liquid after the completion of the polymerization reaction in the polymerization reactor 1 is 40wt%, and the content of cyclic carbonate is 10wt%. The reaction liquid is injected into the glue storage tank 2 , while adding 85°C hot water equivalent to 10wt% of the reaction solution to terminate the reaction to obtain glue liquid, and then inject the glue liquid into the washing coagulation devolatilization kettle 3 through the glue liquid pump 8, and at the same time inject 85°C hot water; using the semi-aromatic liquid of the present invention After the condensation and devolatilization device of the polyester-polycarbonate copolymer performs condensation and devolatilization, the content of propylene oxide in the obtained semi-aromatic polyester-polycarbonate copolymer powdery solid is reduced to 0.2wt%. The content of cyclic carbonate is reduced to 1.2wt%; it is dried and then dissolved in methylene chloride. There is no turbidity when extracted and washed with ethanol, that is, no obvious residue (oligomers and catalysts) is seen to precipitate.

At the same time, the present invention also uses Nuclear Magnetic Resonance Spectroscopy (NMR) to study the absorption of radio-frequency radiation (Radio-frequency Radiation) by atomic nuclei to analyze the semi-aromatic polyester-polycarbonate copolymer obtained in Example 1. The composition and structure of the powder were analyzed and verified, as shown in Figure 2. Figure 2 is the nuclear magnetic resonance spectrum of the material obtained after condensation and devolatilization in Example 1 of the present invention, where D represents semi-aromatic polyester-polycarbonate. Copolymer, E represents cyclic carbonate, F represents propylene oxide; it can also be seen from the verification results in Figure 2 that the condensation devolatilization device of the semi-aromatic polyester-polycarbonate copolymer of the present invention is used for condensation devolatilization. After that, the contents of the propylene oxide component and the cyclic carbonate component were significantly reduced, especially the propylene oxide component as a monomer and solvent has been basically removed from the PPC product.

Example 2 is different from Example 1 in that the content of propylene oxide in the reaction liquid after the completion of the polymerization reaction in the polymerization reactor 1 is 45wt%, and the content of cyclic carbonate is 9wt%; using the semi-aromatic solution of the present invention After the condensation and devolatilization device of the semi-aromatic polyester-polycarbonate copolymer is used for condensation and devolatilization, the content of propylene oxide in the obtained semi-aromatic polyester-polycarbonate copolymer powder solid is reduced to 0.3wt%. , the content of cyclic carbonate is reduced to 1.0wt%; after drying, it is dissolved in methylene chloride, and there is no turbidity when extracted and washed with ethanol, that is, no obvious residue (oligomers and catalysts) is visible. .

Embodiment 3 is different from Embodiment 1 in that the content of propylene oxide in the reaction liquid after the completion of the polymerization reaction in polymerization reactor 1 is 50wt%, and the content of cyclic carbonate is 11wt%; using the semi-aromatic solution of the present invention After the condensation and devolatilization device of the semi-aromatic polyester-polycarbonate copolymer is used for condensation and devolatilization, the content of propylene oxide in the obtained semi-aromatic polyester-polycarbonate copolymer powder solid is reduced to 0.4wt%. , the content of cyclic carbonate was reduced to 1.3wt%; after drying, it was dissolved in methylene chloride, and when extracted and washed with ethanol, there was no turbidity, that is, no obvious (oligomers and catalysts) were visible. The residue precipitates.

It can be seen from the data results of the above three examples that as the propylene oxide content and the cyclic carbonate content in the reaction liquid of the polymerization reactor 1 gradually increase, the use of the semi-aromatic polyester-polycarbonate of the present invention After condensation and devolatilization of the copolymer, in the obtained semi-aromatic polyester-polycarbonate copolymer powdery solid, the content of propylene oxide and the content of cyclic carbonate did not increase significantly. , which illustrates that the coagulation devolatilization device and method of the semi-aromatic polyester-polycarbonate copolymer of the present invention is effective for the propylene oxide component and the cyclic carbonate group in the semi-aromatic polyester-polycarbonate copolymer. All have efficient removal effects.

It should be understood that the above descriptions are only preferred embodiments of the present invention and are not sufficient to limit the technical solutions of the present invention. For those of ordinary skill in the art, within the spirit and principles of the present invention, they can be based on the above Additions, deletions, substitutions, transformations or improvements may be made to the description, and all technical solutions after these additions, deletions, substitutions, transformations or improvements shall fall within the protection scope of the appended claims of the present invention.

Claims (10)

1. A condensation and devolatilization device for semi-aromatic polyester-polycarbonate copolymer, which is characterized in that it includes a polymerization reaction kettle, a glue storage tank, a washing coagulation and devolatilization kettle, a transfer pump, a vibrating screen, and a horizontal grinder and decanter separator; the lower part of the polymerization reactor is provided with a product outlet, and the upper part is provided with a gas outlet; the upper part of the glue storage tank is provided with a product inlet and a gas outlet, and the lower part is provided with a glue outlet; the product inlet of the glue storage tank It is connected to the product outlet of the polymerization reactor through corresponding pipelines; the lower part of the washing and condensation devolatilization kettle is provided with a glue inlet and a hot water inlet, and the upper part is provided with a product outlet and a gas outlet; the glue inlet of the washing and condensation devolatilization kettle is connected through the corresponding The pipeline is connected to the glue outlet of the glue storage tank; the transfer pump is arranged on the pipeline between the glue outlet of the glue storage tank and the glue inlet of the washing condensation and devolatilization kettle; the product outlet of the washing condensation and devolatilization kettle The vibrating screen is connected through corresponding pipes, the vibrating screen is connected to the horizontal grinder through corresponding pipes, and the horizontal grinding machine is connected to the inlet end of the decanter separator through corresponding pipes; There is a liquid inlet in the middle of the glue storage tank, which is used to add 5 to 15wt% water into the glue storage tank through the corresponding pipeline, and mix it with the glue in the glue storage tank to terminate the polymerization reaction; At least two washing, condensation and devolatilization kettles are connected in parallel between the glue storage tank and the vibrating screen. The glue inlet of each washing, condensation and devolatilization kettle is collected through parallel pipelines to the corresponding pipeline and then connected to the transfer pump. The product outlet of each washing, condensation and devolatilization kettle is collected through parallel pipelines to the corresponding pipeline and then connected to the inlet end of the vibrating screen; And the lower part of each washing, condensation and devolatilization kettle is provided with a hot water inlet, which is used to inject 60-90°C hot water into the washing, condensation and devolatilization kettle through corresponding pipelines to remove the propylene oxide component in the glue solution. ; The polycarbonate is PPC. 2. The coagulation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: there are three washing coagulation and devolatilization kettles in parallel between the glue storage tank and the vibrating screen. . 3. The condensation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: the capacity of the polymerization reactor is 30L, and the capacity of the glue storage tank is 40L. The capacity of each washing condensation and devolatilization kettle is 30L. 4. The coagulation and devolatilization device for semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: a stirring device is provided in the polymerization reaction kettle. 5. The coagulation and devolatilization device for semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: a stirring device is provided in the glue storage tank. 6. The coagulation and devolatilization device for semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: a stirring device is provided in the washing coagulation and devolatilization kettle. 7. The condensation and devolatilization device for semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: the grinding medium used in the horizontal grinder is ethanol with a temperature of 30±10°C. 8. The condensation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: the diameter of the pipes connected to the glue inlet of each washing condensation and devolatilization kettle is within Between 50~100mm. 9. The coagulation and devolatilization device for semi-aromatic polyester-polycarbonate copolymer according to claim 1, characterized in that: the hot water at 60-90°C contains 2-5 wt% dispersant. 10. A method for condensation and devolatilization of semi-aromatic polyester-polycarbonate copolymer, using the condensation and devolatilization device of semi-aromatic polyester-polycarbonate copolymer according to any one of claims 1 to 9 , which is characterized by including the following steps: A. Add 5-15wt% water into the glue storage tank, stir and mix with the crude product in the glue storage tank to terminate the polymerization reaction; B. Inject 60-90°C hot water containing 2-5wt% dispersant into the washing coagulation and devolatilization kettle to remove the propylene oxide component in the glue solution; and regulate the injection of hot water into the washing coagulation and devolatilization kettle. The flow rate matches the flow rate of glue pumped into the washing coagulation and devolatilization kettle, so that the mass ratio of water and glue is controlled at 95:5 ~ 80:20, and the residence time of the glue in the washing coagulation and devolatilization kettle is greater than 30 minutes. ; C. The grinding balls added to the horizontal grinder are ceramic balls. The diameter of the grinding balls is 1 to 5 cm. The amount of grinding balls added accounts for 30% to 60% of the volume of the horizontal grinder. The particle size of the material after grinding less than 5mm; D. The decanter separator centrifugally separates the polymer and ethanol to obtain a polymer containing 10 to 15 wt% ethanol. The separated ethanol is returned to the ethanol storage tank for reuse.