KR20200071346A - Process for polymerization of polyether ketone ketone and polyether ketone ketone thereof - Google Patents

Abstract

The present invention relates to a method for polymerization of polyether ketone ketone (PEKK) having improved resin flowability through post-addition of a capping agent during the polymerization process, and PEKK polymerized thereby. More specifically, the method includes the steps of: (a) introducing at least one selected from diphenyl oxide (DPO) and 1,4-bis(4-phenoxybenzoyl)benzene (EKKE) to terephthaloyl chloride (TPC), isophthaloyl chloride (IPC) and a liquid reaction medium in a reactor, and dissolving the same at the same time to perform polymerization of the reaction solution; (b) cooling the reaction solution and introducing a catalyst thereto; (c) blowing an inert gas directly into the reaction solution after introducing the catalyst, and carrying out agitation; and (d) adding a first capping agent after introducing the inert gas. Through the post-addition of the capping agent, a chain terminal of PEKK is capped with a benzoyl group strongly resistant to high temperature so that the resultant PEKK may have a controlled molecular weight and improved resin flowability.

Description

Polymerization method of polyether ketone ketone and polyether ketone ketone polymerized thereby {PROCESS FOR POLYMERIZATION OF POLYETHER KETONE KETONE AND POLYETHER KETONE KETONE THEREOF}

The present invention relates to a polymerization method of polyether ketone ketone (hereinafter also referred to as PEKK) and PEKK polymerized thereby, and more specifically, PEKK having improved resin flowability by post-capping agent during polymerization. It relates to a polymerization method and PEKK polymerized thereby.

Polyether ketone is a generic term for a known industrial resin, and includes polyether ketone, polyether ether ketone, polyether ketone ketone, and a copolymer in which a part of polyether ketone and polyether ketone ketone are mixed.

PEKK represented by the following chemical structure 1 is highly used as an engineering plastic because of its high heat resistance and excellent strength. Engineering plastics are used in fields such as automobiles, aircraft, electrical and electronic equipment, and machinery, and their application areas are gradually expanding.

[Chemical structure 1]

As the application area of engineering plastics expands, there is a need for a polyether ketone compound that exhibits improved properties as its use environment becomes more severe. In addition, there is a need for a polymerization process with a high yield in order to reduce costs during polymerization.

The monomer inputted to the polymerization reaction of PEKK is polymerized through a Friedel-Crafts Acylation chain reaction. In order to improve the efficiency of the chain reaction, it is possible to increase the content of the reactants, increase the reaction temperature and time, or increase the amount of the catalyst, but it is possible to have a cost problem, so a method of suppressing oligomer or scale generation is considered.

U.S. Patent No. 4,841,013 relates to the preparation of polyarylene ether ketone, aims to solve the phenomenon of premature precipitation of the polymer and to solve the early inactivation by ignition of the terminal portion of the polymer chain, but the cap of the present invention It is different from the purpose of activating the excipient binding.

U.S. Patent No. 4,918,237 relates to a polymerization process of 1,4-bis(4-phenoxybenzoyl)benzene, which is an intermediate of polyether ketone polymerization, and aims to solve the defect of aluminum chloride used in the polymerization process, but fundamental solution It is hard to say.

U.S. Patent No. 4,987,171 relates to the stabilization of polyether ketone ketones, and for the purpose of thermal stability of polyether ketone ketones, a method of polymerization within a specific temperature range, including organic hydroperoxides and free radicals , It is completely different from the purpose of the present invention.

U.S. Patent No. 5,734,005 relates to the polymerization of polyarylketones, but there is no disclosure about the step of post-adding the capping agent of the present invention.

Therefore, there is a need to develop a polymerization method of PEKK and a polymerization method of PEKK polymerized thereby by improving the resin flowability by adjusting the molecular weight by adding a capping agent.

US 4841013 US 4918237 US 4987171 US 5734005

The present invention aims to solve all of the above-mentioned problems.

The objective of the present invention is that the polymerization method of PEKK which post-adds the capping agent so that the capping agent in the initial stage of polymerization is a competitive material through the reaction with the catalyst during the polymerization process and does not play a role, so that the capping agent can function as the original Is to provide PEKK.

Another object of the present invention is to provide a polymerization method of PEKK and a polymerized PEKK thereby improving the resin flowability by adjusting the molecular weight through binding activation of the capping agent by post-adding the capping agent.

In order to achieve the object of the present invention as described above and to realize the characteristic effects of the present invention described later, the characteristic configuration of the present invention is as follows.

Polymerization method of the polyether ketone ketone to obtain high molecular weight polyether ketone ketone according to the present invention, (a) diphenyl oxide (Diphenyl oxide, DPO) and 1,4-bis (4-phenoxy in the reactor) Reaction of at least one selected from benzoyl)benzene (1,4-bis(4-phenoxybenzoyl) benzene, EKKE) with terephthaloyl chloride (TPC) and isophthaloyl chloride (IPC) Polymerizing the reaction solution by dissolving at the same time in a medium; (b) cooling the reaction solution and introducing a catalyst; (c) after the catalyst is introduced, directly blowing and stirring an inert gas into the reaction solution; And (d) adding the first capping agent after introducing the inert gas.

In one preferred example of the present invention, the weight ratio of the second capping agent and the first capping agent may include 1:0.1 to 1:1.

In one preferred embodiment of the present invention, the first capping agent and the second capping agent may include at least one or more of a compound in which an aliphatic or aromatic hydrocarbon is bonded to a benzoyl chloride and benzoyl chloride benzene ring. .

In one preferred embodiment of the present invention, the compound is benzenesulfonyl chloride, 4-chlorobiphenyl, 4-phenoxybenzophenone, 4-(4-phenoxyphenoxy)benzophenone and biphenyl 4-benzenesulfonyl It may include at least one or more selected from phenyl phenyl ether.

In one preferred embodiment of the present invention, the step (c) may disperse the inert gas introduced by rotating a stirrer having a plurality of stirring blades.

In one preferred example of the present invention, at least two agitators may be provided in the reactor to rotate in at least two directions to generate a vortex phenomenon.

In one preferred example of the present invention, a nozzle for blowing the inert gas directly into the reaction solution is formed at the top or bottom of the reactor so that the inert gas may be injected in multiple directions.

In one preferred example of the present invention, the cooling temperature in step (b) may include -10 to -5 °C.

In one preferred example of the present invention, it may include the step of raising the reactor to 80 to 100 ℃ while stirring in step (c).

In one preferred example of the present invention, the temperature of step (d) may be maintained at 70 to 110°C.

In one preferred example of the present invention, after step (d), washing with methanol (CH ₃ OH), hydrochloric acid and sodium hydroxide (NaOH) solution, and may further include washing with deionized water (DI water). .

In one preferred example of the present invention, after the washing step may further include a vacuum drying step at 170 to 190 ℃.

In one preferred example of the present invention, the reaction medium of the liquid phase may include at least one or more solvents selected from ortho-dichlorobenzene (oDCB) and dichloromethane.

In one preferred embodiment of the present invention, the catalyst is at least one selected from aluminum chloride (AlCl ₃ ), potassium carbonate (potassium carbonate, K ₂ CO ₃ ) and iron chloride (iron(III) chloride, FeCl ₃ ). It may include the above.

In one preferred example of the present invention, the inert gas may include at least one selected from nitrogen, helium, neon, argon and krypton.

In one preferred example of the present invention, PEKK polymerized by the polymerization method may be included.

In one preferred example of the present invention, the PEKK may include a component material.

As described above, the polymerization method of PEKK according to the present invention and the PEKK polymerized thereby have an effect that benzoyl groups, which are difficult to form radicals at high temperature processing, are formed at the ends of the PEKK polymer chain.

In addition, the polymerization method of PEKK according to the present invention, and the polymerized PEKK by post-adding the capping agent, forms most of the PEKK polymer chain ends through benzoyl groups through binding activation of the capping agent to control the PEKK molecular weight to improve resin flow and thermal stability. It has the effect of improving.

1 is a view showing the post-capping agent (capping agent) during the polymerization of the PEKK of the present invention.
2 is a H-NMR graph of the benzoyl group at the PEKK chain end of the present invention.
Figure 3 is a H-NMR graph of the benzyol group at the end of the PEKK chain polymerized without post-capping agent.
4 and 5 is a view showing a device capable of simultaneously stirring and flowing nitrogen gas in the reaction solution according to the polymerization method of PEKK of the present invention.

For a detailed description of the present invention, which will be described later, reference is made to the accompanying drawings that illustrate, by way of example, specific embodiments in which the invention may be practiced. These examples are described in detail enough to enable those skilled in the art to practice the present invention. It should be understood that the various embodiments of the invention are different, but need not be mutually exclusive. For example, certain shapes, structures, and characteristics described herein may be implemented in other embodiments without departing from the spirit and scope of the invention in relation to one embodiment. In addition, it should be understood that the location or placement of individual components within each disclosed embodiment can be changed without departing from the spirit and scope of the invention. Therefore, the following detailed description is not intended to be taken in a limiting sense, and the scope of the present invention, if appropriately described, is limited only by the appended claims, along with all ranges equivalent to those claimed. In the drawings, similar reference numerals refer to the same or similar functions throughout several aspects.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings in order to enable those skilled in the art to easily implement the present invention.

As described above, in the past, radicals are generated locally in some PEKK polymer chains or at the ends of the PEKK polymer chains due to high temperatures during processing, so that the radical electrons can bond with adjacent PEKK polymer chains. When a network is formed in the polymer by the interchain linkages generated through this mechanism, the melting viscosity increases as the storage modulus increases. This deteriorates the workability by applying a load to the equipment, which has resulted in deterioration of the work piece density and apparent quality. In order to solve the above problem, a capping agent is added. However, the capping agent, which should prevent the formation of radicals at the end of the PEKK polymer chain, has a problem in that it does not function as a reactant with a reactant by reacting with a catalyst during polymerization. That is, when PEKK polymerization monomers TPC, IPC, and DPO are simultaneously mixed with a capping agent, the polymerization initial capping agent is changed to carbonyl carbocation generated by Al-Cl coordination of AlCl ₃ as a catalyst, such as TPC and IPC. In addition, while heating the polymerization solution, the carbocation of TPC and IPC and the carbocation of the capping agent competed with each other during the electrophile reaction to DPO, and there was a problem that it could not function as a capping agent.

Accordingly, in the present invention, a part of the capping agent input is post-added during the polymerization reaction so that the PEKK chain ends are capped with benzoyl groups resistant to high temperatures, thereby inhibiting crosslinking of the chains and thereby improving the resin flow and thermal stability. Provided is a polymerized PEKK.

In the present invention, the capping agent, which should prevent the occurrence of local radicals at the PEKK chain end during high temperature processing, plays an original role because it competes with the TPC and IPC monomers for the Fridel-crafts acylation reaction when the capping agent is introduced at the initial stage of polymerization. In order to prevent this from being prevented, a polymerization method of PEKK capping the PEKK polymer chain end with a benzoyl group by post-adding the capping agent during polymerization, and PEKK polymerized thereby are presented. Since benzoyl groups are difficult to form radicals at high temperature processing, PEKK with PEKK polymer chain ends capped with benzoyl groups can improve resin flow and thermal stability. That is, by post-adding the capping agent, a significant amount of PEKK polymer chain ends are formed through the binding activation of the capping agent to control the PEKK molecular weight to improve the resin flow and thermal stability.

Specifically, the polymerization method of PEKK according to the present invention will be described below with reference to the drawings.

Referring to Figure 1, a polymerization method of a polyether ketone ketone to obtain a high yield of polyether ketone ketone of a high molecular weight according to an embodiment of the present invention, (a) diphenyl oxide (Diphenyl oxide, DPO) and At least one selected from 1,4-bis(4-phenoxybenzoyl)benzene (1,4-bis(4-phenoxy benzoyl) benzene, EKKE) is terephthaloyl chloride (TPC) and isophthalo. Polymerizing the reaction solution by simultaneously dissolving it in an aqueous medium (isophthaloyl chloride, IPC) and dissolving it simultaneously; (b) cooling the reaction solution and introducing a catalyst; (c) after the catalyst is introduced, directly blowing and stirring an inert gas into the reaction solution; And (d) adding the first capping agent after the inert gas is introduced.

According to an embodiment of the present invention, a second capping agent may be added to the reaction solution in step (a). Specifically, when dissolving the monomer in a liquid reaction medium, a second capping agent may be simultaneously added to dissolve the monomer.

Further, according to an embodiment of the present invention, the capping agent is added to the polymerization medium to serve to cap the polymer at at least one end of the PEKK polymer chain. This terminates the continuous extension of the PEKK polymer chain and controls the molecular weight of the polymerized polymer.

The molar ratio of the second capping agent and the first capping agent is 1 to 3:1. Preferably a range of 3:1 is provided. For example, when the second capping agent is included at 1.5 mol%, the first capping agent may be included at 0.5 mol%. However, it is not limited thereto.

According to an embodiment of the present invention, when in the above 3:1 range, the present invention can maximize the role as a capping agent to be desired, thereby providing an effect of improving the resin flowability by adjusting the molecular weight do. Also, in this case, the second and first capping agents may or may not be the same type.

According to an embodiment of the present invention, the first capping agent and the second capping agent include all of an aliphatic hydrocarbon or an aromatic hydrocarbon bonded to a benzoyl chloride benzene ring, and may include all of the compounds. Also, preferably in benzoyl chloride and benzenesulfonyl chloride, 4-chlorobiphenyl, 4-phenoxybenzophenone, 4-(4-phenoxyphenoxy)benzophenone and biphenyl 4-benzenesulfonylphenyl phenyl ether Selected at least one or more compounds, more preferably benzoyl chloride.

According to an embodiment of the present invention, the step (c) is characterized in that a stirrer formed with a plurality of stirring blades rotates to disperse the inert gas, and uniformly dissolve the polymerized monomer and the catalyst in the reaction solvent. do.

According to an embodiment of the present invention, the stirrer is provided in at least two or more in the reactor to rotate in at least two directions to generate a vortex phenomenon.

In addition, the rotating shaft of the stirrer may be provided to rotate at a predetermined angle alternately in the forward and reverse directions. In addition, the stirring blade is formed to form a predetermined angle with the rotating shaft can increase the dispersion force of the composition in the reactor.

4 and 5 is a view showing a device capable of simultaneously stirring and flowing nitrogen gas in the reaction solution according to the polymerization method of PEKK of the present invention.

4 and 5, in the polymerization method of PEKK according to the present invention, a nozzle for blowing the inert gas directly into the reaction solution is formed at the top or bottom of the reactor, whereby the inert gas may be injected in multiple directions. This can make the removal of hydrochloric acid by an inert gas more quickly and efficiently.

According to an embodiment of the present invention, the cooling temperature of step (b) may include -10 to -5°C. That is, when the catalyst is added in the polymerization method according to the present invention, the temperature of the reaction solution is lowered before being input, but the temperature may vary depending on the catalyst, but is preferably -10 to -5°C.

According to an embodiment of the present invention, may include the step of raising the reactor to 80 to 110 ℃ while stirring in step (c).

According to an embodiment of the present invention, the temperature of step (d) may include maintaining at 70 to 120°C, preferably 80 to 110°C, and more preferably 100°C. Specifically, benzoyl chloride may be additionally added to PEKK while the temperature of step (d) is maintained at 100°C.

According to an embodiment of the present invention, after step (d), washing with methanol (CH ₃ OH), hydrochloric acid and sodium hydroxide (NaOH) solution, and may further include washing with deionized water (DI water). . In detail, the method further includes washing three times with methanol, once with hydrochloric acid and sodium hydroxide (NaOH) solution, and washing three times with deionized water (DI water).

According to an embodiment of the present invention, after the washing step may further include a vacuum drying step at 170 to 190 ℃.

In addition, PEKK powder can be preferably obtained in the vacuum drying step.

According to an embodiment of the present invention, the reaction medium of the liquid phase may include at least one selected from o-dichlorobenzene (oDCB) and dichloromethane, but is not limited thereto, and is generally used as a solvent for Friedel-Crafts Acylation polymerization reaction. If it is used, it is possible.

According to an embodiment of the present invention, the catalyst may include at least one or more selected from aluminum chloride (AlCl ₃ ), potassium carbonate (K ₂ CO ₃ ) and iron(III) chloride (FeCl ₃ ). It is not limited and can be used as long as it is commonly used as a catalyst for the Friedel-Crafts Acylation polymerization reaction.

According to an embodiment of the present invention, the inert gas may include at least one selected from nitrogen, helium, neon, argon, and krypton, but is not limited thereto, and the inert gas may be alone or mixed during the polymerization reaction process. Can be used.

According to an embodiment of the present invention, PEKK polymerized by the polymerization method may be included. PEKK polymerized by the polymerization method exhibits improved physical properties in resin flow compared to PEKK polymerized through the prior art.

According to an embodiment of the present invention, a vehicle material, an electronic device material, an industrial pipe material, a construction civil engineering material, a 3D printer material, a fiber material, including PEKK polymerized by the polymerization method of PEKK according to the present invention, Includes parts material characterized by being selected from the group consisting of coating material, machine tool material, medical material, aviation material, photovoltaic material, battery material, sports material, home appliance material, household material and cosmetic material. can do.

In a specific example, the product containing the component material includes a vehicle air duct, plastic and rubber compound, adhesive, light, polymer optical fiber, fuel filter cap, line system, cable of electronic equipment, reflector, sheath of cable, optical fiber, Wire protection tube, control unit, light, pipe tube, liner, pipe coating, oil field exploration hose, 3D printer, multifilament, spray hose, valve, duct, pulp, gear, medical catheter, aircraft flame retardant, solar cell protection plate, cosmetic , High hardness film, ski boots, headset, glasses frame, toothbrush, water bottle or outsole, but is not limited thereto.

In addition, the polymerization reaction according to the present invention may be performed in various reactors, but may preferably be performed in a continuous stirring reactor (CSTR) or a loop reactor.

Hereinafter, the configuration and operation of the present invention will be described in more detail through preferred embodiments of the present invention. However, this is provided as a preferred example of the present invention and cannot be interpreted as limiting the present invention by any means.

The contents not described herein will be sufficiently technically inferred by those skilled in the art, and thus the description thereof will be omitted.

[Example]

In the reactor, 3 monomers terephthaloyl chloride (TPC), isophthaloyl chloride (IPC) and 1,4-bis(4-phenoxybenzoyl) benzene (EKKE) and capping agent benzoyl chloride 1.5 mol% reaction solvent o-dichlorobenzene (oDCB) were added. After dissolving at the same time, the reactor temperature is lowered to -10 to -5°C, and the catalyst AlCl ₃ is added while maintaining the temperature of the solution constant. After the catalyst is added, N ₂ is blown into the solution and the solution is stirred while the reactor is heated to 100° C. to polymerize PEKK. Thereafter, 0.5 mol% of benzoyl chloride is added to PEKK while maintaining at 100°C. The polymerized PEKK was washed with methanol 3 times, 1M hydrochloric acid and 0.5M NaOH solution, washed with DI water 3 times and vacuum dried at 180°C.

[Comparative example]

PEKK was polymerized in the same manner as in Example, except that benzoyl chloride was not additionally post-added in the middle of the polymerization.

[Experimental Example]

<Experimental Example 1>

H-NMR analysis (benzoyl group analysis)

Whether the increase of the benzoyl group at the ends of the PEKK chains of Examples and Comparative Examples was confirmed by H-NMR, and the results are shown in the graphs of FIGS. 2 and 3. In addition, the area of H-NMR of hydrogen atoms A and B excluding hydrogen atom C among the three bonded to the benzoyl group is shown in Table 1 below. Hydrogen atom C is difficult to read due to overlapping peaks with other hydrogen atoms bound to the PEKK back bone.

H-NMR analysis peak area Hydrogen atom A (7.80 ppm) Hydrogen atom B (7.65 ppm) Example 0.5300 0.0600 Comparative example 0.3437 0.0276

2 and 3, it can be seen that there are more benzoyl groups at the chain ends of the PEKK of the Examples than the benzoyl groups at the PEKK chain ends of the comparative example polymerized without post-addition of benzoyl chloride. That is, it can be seen from the H-NMR graph that the chain end of the PEKK polymerized by the polymerization method of PEKK of the present invention is capped with a strong benzoyl group. In addition, as shown in Table 1, it can be seen that the area of the hydrogen atoms in the example is smaller than that of the comparative example.

As a result, when the polymerization method of the existing PEKK is used, the capping agent benzoyl chloride competes in the Friedel-Crafts Acylation reaction with the polymerization monomers TPC and IPC. It can be seen that it was not generated. On the other hand, PEKK polymerized by the polymerization method comprising the step of post-adding the capping agent according to the present invention is resin flow and thermal stability because the chain ends are capped with a benzoyl group that is stable at high temperatures, so that radicals are not well formed during high temperature processing of the resin. It can be improved.

<Experimental Example 2>

Measurement of Inherent Viscosity and Melt Index

Inherent Viscosity and Melt Index of Examples and Comparative Examples were measured, and the results are shown in Table 2 below. Inherent Viscosity is the value obtained by dividing the viscosity of a thin polymer solution by the viscosity of a pure solvent. The Melt Index is a measure of the outflow of molten resin according to a certain pressure and temperature using an extruded plasticity meter, and is expressed in units of g/10min.

Inherent Viscosity (dL/g) Melt Index(g/10min) Example 1.0 20 Comparative example 1.3 One

As shown in Table 2, the Inherent Viscosity of the Examples of the present invention was 1.0, and the Melt Index was measured as 20. On the other hand, the Inherent Viscosity of the comparative example was 1.3, and the Melt Index was measured as 1, and in the case of the Melt Index, a difference of almost 20 times was observed.

In the case of Examples, the benzoyl chloride, a capping agent, is combined with DPO or EKKE by adding a capping agent to form a number of benzoyl groups at the ends of the PEKK polymer chain, and these benzoyl group ends inhibit the Friedel-Crafts Acylation reaction of TPC and IPC. It can be seen that the molecular weight is controlled by being controlled.

On the other hand, as shown in the result of the comparative example, the step of post-adding the capping agent is not included, so that the initial polymerization capping agent is changed to carbonyl carbocation produced by Al-Cl coordination of AlCl ₃ as a catalyst as in TPC and IPC. In addition, it can be seen that while heating the polymerization solution, the carbocation of TPC and IPC and the carbocation of the capping agent competed in the electrophile reaction to DPO, so that the problem of not functioning as a capping agent was not solved. have.

In the above, the present invention has been described by specific matters such as specific components and limited embodiments and drawings, but this is provided only to help a more comprehensive understanding of the present invention, and the present invention is not limited to the above embodiments , Those skilled in the art to which the present invention pertains can make various modifications and variations from these descriptions.

Therefore, the spirit of the present invention is not limited to the above-described embodiment, and should not be determined, and all claims that are equally or equivalently modified as well as the claims below will fall within the scope of the spirit of the present invention. Would say

Claims (18)

In the polymerization method of polyether ketone ketone to obtain high molecular weight polyether ketone ketone in high yield,
(a) At least one selected from diphenyl oxide (DPO) and 1,4-bis(4-phenoxybenzoyl)benzene (1,4-bis(4-phenoxybenzoyl) benzene, EKKE) in the reactor. Putting terephthaloyl chloride (TPC) and isophthaloyl chloride (IPC) into a liquid reaction medium and simultaneously dissolving to polymerize the reaction solution;
(b) cooling the reaction solution and introducing a catalyst;
(c) after the catalyst is introduced, directly blowing and stirring an inert gas into the reaction solution; And
(D) a step of adding a first capping agent (capping agent) after the inert gas input; polymerization method of a polyether ketone ketone comprising a.
According to claim 1,
Polymerization method of a polyether ketone ketone, characterized in that a second capping agent is added to the reaction solution in step (a).
According to claim 2,
The polyether ketone ketone polymerization method, characterized in that the molar ratio of the second capping agent and the first capping agent is 1 to 3: 1.
According to claim 2,
The first capping agent and the second capping agent is a polymerization method of polyether ketone ketone, characterized in that it comprises at least one or more of a compound in which an aliphatic or aromatic hydrocarbon is attached to a benzoyl chloride and benzoyl chloride benzene ring. .
The method of claim 4,
The compound is at least one selected from benzenesulfonyl chloride, 4-chlorobiphenyl, 4-phenoxybenzophenone, 4-(4-phenoxyphenoxy)benzophenone and biphenyl 4-benzenesulfonylphenyl phenyl ether. Polymerization method of a polyether ketone ketone comprising a.
According to claim 1,
The step (c) is a polymerization method of a polyether ketone ketone, characterized in that a stirrer with a plurality of stirring blades is rotated to disperse the inert gas.
The method of claim 6,
The stirrer is provided in at least two or more in the reactor to rotate in at least two directions to generate a vortex phenomenon, characterized in that the polymerization method of the polyether ketone ketone.
According to claim 1,
A method for polymerizing a polyether ketone ketone, characterized in that a nozzle for blowing the inert gas directly into the reaction solution is formed at the top or bottom of the reactor and injected in multiple directions.
According to claim 1,
Cooling temperature in the step (b) is -10 to -5 ℃ polymerization method of a polyether ketone ketone, characterized in that.
According to claim 1,
The method of polymerization of a polyether ketone ketone, comprising; raising the reactor to 80 to 110°C while stirring in step (c).
According to claim 1,
Polymerization method of the polyether ketone ketone, characterized in that the temperature of the step (d) is maintained at 70 to 120 ℃.
According to claim 1,
After the step (d), washing with methanol (CH ₃ OH), hydrochloric acid and sodium hydroxide (NaOH) solution, and a method of polymerization of polyether ketone ketone, comprising the step of washing with deionized water (DI water).
The method of claim 12,
After the washing step, the polymerization method of polyether ketone ketone further comprising the step of vacuum drying at 170 to 190 ℃.
According to claim 1,
The liquid reaction medium is a method of polymerizing polyether ketone ketone, characterized in that it is at least one or more solvents selected from ortho-dichlorobenzene (oDCB) and dichloromethane.
According to claim 1,
The catalyst is a polyether ketone ketone, characterized in that at least one selected from aluminum chloride (aluminum chloride, AlCl ₃ ), potassium carbonate (potassium carbonate, K ₂ CO ₃ ) and iron (III) chloride, FeCl ₃ ) Polymerization method.
According to claim 1,
The inert gas is a polymerization method of polyether ketone ketone, characterized in that at least one selected from nitrogen, helium, neon, argon and krypton.
A polyether ketone ketone polymerized by the polymerization method according to any one of claims 1 to 16.
Part material comprising a polyether ketone ketone according to claim 17.

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