A low energy phenolphthalein polyaryletherketone polymerization process

Abstract

The application discloses a low-energy- consumption phenolphthalein polyaryletherketone polymerization process, comprising the following steps: mixing phenolphthalein monomer, 4,4'-difluorobenzophenone monomer and a catalyst in a certain proportion; performing a prepolymerization reaction under low temperature and normal pressure to generate a low-molecular-weight prepolymer; transferring the low-molecular-weight prepolymer into a high-temperature reaction kettle, performing a main polymerization reaction under high temperature and medium pressure, and adding a viscosity-reducing additive in the reaction process; and cooling, crushing, washing and drying the product to obtain a phenolphthalein polyaryletherketone product. The application belongs to the technical field of high polymer material synthesis, and specifically provides a process for solving the problems of high melt viscosity, high energy consumption and low reaction efficiency in the prior art; the process has the advantages of low melt viscosity, low energy consumption, high reaction efficiency and the like, and can significantly improve the production efficiency and quality of the phenolphthalein polyaryletherketone.

Description

Technical Field

[0001] This invention belongs to the field of polymer material synthesis technology, specifically referring to a low-energy-consumption phenolphthalein polyarylether ketone polymerization process. Background Technology

[0002] Phenolic phthalate polyaryletherketone (PEK-C) is a high-performance engineering plastic with excellent heat resistance, chemical resistance, and mechanical properties, and is widely used in aerospace, electronics, and automotive industries. However, existing PEK-C polymerization processes have the following problems: 1. PEK-C exhibits high melt viscosity during polymerization, which leads to poor fiber impregnation during composite material preparation. The high melt viscosity makes it difficult for the resin to fully penetrate between the fibers, resulting in internal defects in the prepared composite material and affecting its uniformity and mechanical properties.

[0003] 2. Traditional polymerization processes require high temperature and high pressure conditions, resulting in high energy consumption and increased production costs.

[0004] 3. Due to the high melt viscosity and limitations of the reaction conditions, the polymerization reaction efficiency is low and the reaction time is long. Summary of the Invention

[0005] The technical problem to be solved by the present invention is that the high melt viscosity in the prior art leads to impregnation, high energy consumption and low reaction efficiency.

[0006] To solve the above problems, the technical solution adopted by the present invention is as follows: The present invention proposes a low-energy-consumption phenolphthalein polyarylether ketone polymerization process, comprising the following steps: Step S1, Raw material preparation: Mix phenolphthalein monomer, 4,4'-difluorobenzophenone monomer and catalyst in a certain proportion; Step S2, Prepolymerization reaction: A prepolymerization reaction is carried out under low temperature and normal pressure conditions to generate a low molecular weight prepolymer; at this time, the product is a low viscosity polymer, the purpose of which is to reduce the viscosity of the initial reactants, improve the impregnation effect, and reduce energy consumption; Step S3, Main polymerization reaction: The low molecular weight prepolymer is transferred to a high-temperature reactor and the main polymerization reaction is carried out under high temperature and medium pressure. A viscosity reducer is added during the reaction. Step S4, Post-processing: Cool, pulverize, wash and dry the product to obtain the phenolphthalein polyarylether ketone product.

[0007] Further, in step S1, the molar ratio of phenolphthalein monomer to 4,4'-difluorobenzophenone monomer is (0.95-1.05):1, and the amount of catalyst used is 0.5%-2% of the total mass of phenolphthalein monomer and 4,4'-difluorobenzophenone monomer.

[0008] Furthermore, the mixing environment in step S1 is preferably carried out under a nitrogen atmosphere.

[0009] Furthermore, in step S1, the catalyst is an alkaline catalyst, such as sodium hydroxide or potassium hydroxide, used to promote the polycondensation reaction.

[0010] Furthermore, the low temperature condition in step S2 is 100-150℃.

[0011] Furthermore, in step S3, the high temperature condition is 200-250℃, and the medium pressure is 1-2MPa.

[0012] Furthermore, in step S3, the viscosity reducing agent is silicone oil or low molecular weight polyether, and the viscosity reducing agent accounts for 0.1% to 1% of the total mass of the reaction system.

[0013] Furthermore, the prepolymerization reaction in step S2 takes 1-2 hours, and the main polymerization reaction in step S3 takes 2-3 hours.

[0014] The beneficial effects achieved by the present invention using the above solution are as follows: 1. The low-energy phenolphthalein polyarylether ketone polymerization process proposed in this scheme reduces melt viscosity and improves impregnation effect by optimizing reaction conditions and adding additives.

[0015] 2. The low-energy phenolphthalein polyarylether ketone polymerization process proposed in this scheme reduces reaction temperature and pressure and energy consumption through low-temperature prepolymerization and medium-pressure main polymerization.

[0016] 3. The low-energy phenolphthalein polyarylether ketone polymerization process proposed in this scheme improves polymerization efficiency, shortens reaction time, and enhances reaction efficiency by optimizing catalysts and reaction conditions. Detailed Implementation

[0017] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Example

[0018] The present invention proposes a low-energy-consumption phenolphthalein polyarylether ketone polymerization process, comprising the following steps: Step 1, Raw material preparation: Mix phenolphthalein monomer, 4,4'-difluorobenzophenone monomer and catalyst in a certain proportion. The molar ratio of phenolphthalein monomer to 4,4'-difluorobenzophenone monomer is 1:1. The amount of catalyst is 2% of the total mass of phenolphthalein monomer and 4,4'-difluorobenzophenone monomer, of which sodium hydroxide accounts for 1% and potassium hydroxide accounts for 1%. Step 2, Prepolymerization reaction: The prepolymerization reaction is carried out at 120℃ and normal pressure for 1.5 hours to generate a low molecular weight prepolymer; The prepolymerization reaction is carried out at a lower temperature, which allows the reactants to initially polymerize and form a low-viscosity prepolymer. The purpose of this step is to reduce the viscosity of the initial reactants, improve the impregnation effect, and reduce energy consumption.

[0019] Step 3, main polymerization reaction: The prepolymer is transferred to a high-temperature reactor and the main polymerization reaction is carried out at 220°C and 1.5 MPa for 2.5 hours. The prepolymer is heated to a higher temperature to induce further polymerization. By controlling the temperature difference, the rate and extent of the polymerization reaction can be controlled, thereby obtaining phenolphthalein polyarylether ketone with the target viscosity and molecular weight.

[0020] Step 4, Additive addition: Silicone oil is added during the main polymerization reaction. The amount of silicone oil is 0.5% of the total mass of the reaction system, which is used to reduce the melt viscosity. Step 5, Post-processing: After the reaction is complete, the product is cooled, pulverized, washed and dried to remove impurities and improve the purity of the product, thus obtaining the phenolphthalein polyarylether ketone product. Example

[0021] The present invention proposes a low-energy-consumption phenolphthalein polyarylether ketone polymerization process, comprising the following steps: Step 1, Raw material preparation: Mix phenolphthalein monomer, 4,4'-difluorobenzophenone monomer and catalyst in a certain proportion; Step 2, Prepolymerization reaction: A prepolymerization reaction is carried out at 150°C and normal pressure to generate a low molecular weight prepolymer; Step 3, Main polymerization reaction: The prepolymer is transferred to a high-temperature reactor and the main polymerization reaction is carried out at 250°C and 2 MPa; Step 4, Additives: Add low molecular weight polyether during the main polymerization reaction to reduce melt viscosity; The following is a sample recipe for this embodiment: Phenolphthalein monomer: 100 g (1 mol); 4,4'-difluorobenzophenone monomer: 100 g (1 mol); Catalyst (sodium hydroxide): 2 g (1%); Additive (silicone oil): 0.5 g (0.25%).

[0022] Step 5, Post-processing: After the reaction is complete, the product is cooled, pulverized, washed and dried to obtain the phenolphthalein polyarylether ketone product.

[0023] In the above embodiments, the purity of phenolphthalein monomer and 4,4'-difluorobenzophenone monomer is ensured to be high (≥99%) to avoid the influence of impurities on the reaction. In actual operation, the ratio of raw materials can be fine-tuned according to the reaction temperature and pressure to achieve the best reaction effect.

[0024] In this embodiment, the problems of poor impregnation effect and high energy consumption caused by high melt viscosity are solved by low-temperature prepolymerization, medium-pressure main polymerization, and the addition of viscosity-reducing agents. This process has the advantages of low melt viscosity, low energy consumption, and high reaction efficiency, and can significantly improve the production efficiency and quality of phenolphthalein polyaryletherketone.

[0025] The present invention and its embodiments have been described above, and such description is not restrictive. In conclusion, if those skilled in the art are inspired by this description and design similar structures and embodiments without departing from the spirit of the invention, such designs should fall within the protection scope of the present invention.

Claims

1. A low-energy-consumption phenolphthalein polyaryletherketone polymerization process, characterized in that, Includes the following steps: Step S1, Raw material preparation: Mix phenolphthalein monomer, 4,4'-difluorobenzophenone monomer and catalyst in a certain proportion; Step S2, Prepolymerization reaction: A prepolymerization reaction is carried out under low temperature and normal pressure conditions to generate a low molecular weight prepolymer; Step S3, Main polymerization reaction: The low molecular weight prepolymer is transferred to a high-temperature reactor and the main polymerization reaction is carried out under high temperature and medium pressure. A viscosity reducer is added during the reaction. Step S4, Post-processing: Cool, pulverize, wash and dry the product to obtain the phenolphthalein polyarylether ketone product.

2. The low-energy phenolphthalein polyarylether ketone polymerization process according to claim 1, characterized in that: In step S2, the low temperature condition is 100-150℃, and the reaction time is 1-2 hours.

3. The low-energy phenolphthalein polyaryletherketone polymerization process according to claim 1 or 2, characterized in that: In step S3, the high temperature conditions are 200-250℃, the medium pressure is 1-2MPa, and the reaction time is 2-3 hours.

4. The low-energy phenolphthalein polyarylether ketone polymerization process according to claim 1, characterized in that: In step S1, the molar ratio of phenolphthalein monomer to 4,4'-difluorobenzophenone monomer is (0.95-1.05):1, and the amount of catalyst used is 0.5%-2% of the total mass of phenolphthalein monomer and 4,4'-difluorobenzophenone monomer.

5. The low-energy phenolphthalein polyarylether ketone polymerization process according to claim 1, characterized in that: In step S1, the catalyst is an alkaline catalyst, which may be sodium hydroxide or potassium hydroxide.

6. The low-energy-consumption phenolphthalein polyarylether ketone polymerization process according to claim 1 or 4, characterized in that: In step S3, the viscosity reducing agent is silicone oil or low molecular weight polyether, and the viscosity reducing agent accounts for 0.1% to 1% of the total mass of the reaction system.

7. The low-energy phenolphthalein polyarylether ketone polymerization process according to claim 1, characterized in that: The mixing process in step S1 is carried out under a nitrogen atmosphere.