Device and method for stably preparing polyether ketone resin

Abstract

The invention discloses a device and a method for stably preparing polyether ketone resin. The device comprises a reaction kettle, wherein a separation column with a jacket is connected above the reaction kettle; a plurality of filler layers are arranged in the separation column; gas nozzles are arranged in each filler layer. The method comprises the steps of adding reaction monomers into the reaction kettle and performing polymerization reaction under the protection of inert gas in presence of diphenyl sulfone as a solvent, injecting high-temperature high-pressure inert gases regularly in a pulse manner through the gas nozzles, introducing a cooling medium into the jacket of the separation column to change a gas phase of the diphenyl sulfone into a liquid phase, and enabling the diphenyl sulfone to flow back to a polymerization system. The device is capable of effectively discharging water, the diphenyl sulfone can be changed to the liquid phase so as to flow back to the polymerization system, the water is effectively separated from the diphenyl sulfone, and a stable content of solid in the polymerization system is kept so that production stability and quality of products are ensured; the device is also capable of reducing loss of the diphenyl sulfone solvent to a maximum limit, reducing raw material cost and production cost, reducing solid residue in the separation column, avoiding pipeline blockage, prolonging service life of the separation column and reducing manual operation.

Description

technical field [0001] The invention belongs to the field of resin synthesis, and in particular relates to a device and method for stably preparing polyether ketone resins. Background technique [0002] Polyether ketone resins, including PEEK, PEK, PEEKK, PEKEKK, PEDEK, etc., are all produced with diphenyl sulfone as a solvent, and the polymerization temperature is usually above 300°C. In the early stage of polymerization, the salt-forming reaction takes the generated water out of the system. N2 is blown to bring out the moisture, the temperature is between 130-300°C, and the water-carrying time generally takes 3-6 hours. Sulfone will be taken out of the system along with N2, resulting in changes in the concentration or solid content of the polymerization system. If the reflux is unfavorable, at least 10% of diphenyl sulfone will be lost; in addition, since the production process is generally judged by the change of system viscosity At the end of the polymerization reactio...

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Problems solved by technology

[0002] Polyether ketone resins, including PEEK, PEK, PEEKK, PEKEKK, PEDEK, etc., are all produced with diphenyl sulfone as a solvent, and the polymerization temperature is usually above 300°C. In the early stage of polymerization, the salt-forming reaction takes the generated water out of the system. N2 is blown to bring out the moisture, the temperature is between 130-300°C, and the water-carrying time generally takes 3-6 hours. Sulfone will be taken out of the system along with N2, resulting in changes in the concentration or solid content of the polymerization system. If the reflux is unfavorable, at least 10% of diphenyl sulfone will be lost; in addition, since the production process is generally judged by the change of system viscosity At the end of the polymerization reaction and the timing of discharging, if the viscosity is misjudged due to changes in the solid content of the system, it will cause serious fluctuations in the production process and product viscosity stability, affecting product quality

Even, if diphenyl sulfone encounters condensation sublimation, it will generally become flocs. After repeated accumulation, it will scale and harden until the pipes are blocked, resulting in the inability to remove water smoothly, which will further affect the growth of polymerization viscosity, and even lead to polymerization failure.

[0003] The prior art usually adopts a pipe heated with a jacket, and by controlling the temperature of the jacket within a certain range, most of the water vapor is allowed to flow with the N 2 At the same time, most of the diphenyl sulfone is liquefied and returned to the system, but the separation effect of this crude device is very limited

According to the physical characteristics of diphenyl sulfone, its melting point is around 127°C, and when heated above 100°C, a large amount of sublimation will form steam, due to N 2 The flow and velocity are large, and the temperature of the gas phase cannot be controlled. At this time, the gas phase includes N 2 , water vapor and diphenyl sulfone vapor, the diphenyl sulfone vapor cannot fully condense the liquid phase in a short period of time when it passes through the pipeline and reflux, and the water vapor generated by the system is difficult to ensure that it is fully taken out of the system, and The completeness of water vapor carryover seriously affects the success or failure of the polymerization process, that is, the process requirements should be fully carried out of the system, diphenyl sulfone vapor will either be discharged from the system with N2, or the pipeline will be blocked by sublimation, so traditional technology cannot solve the problem. The problem that most of the water vapor is taken out and most of the diphenyl sulfone vapor can return

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