Low-energy consumption phenolphthalein polyaryletherketone polymerization reaction process

Abstract

The invention discloses a low-energy consumption phenolphthalein polyaryletherketone polymerization reaction process which comprises the following steps: mixing a phenolphthalein monomer, a 4, 4 '-difluorobenzophenone monomer and a catalyst according to a certain proportion; the preparation method comprises the following steps: firstly, carrying out prepolymerization reaction under low-temperature and normal-pressure conditions to generate a low-molecular-weight prepolymer; transferring the low-molecular-weight prepolymer into a high-temperature reaction kettle, carrying out main polymerization reaction at high temperature and medium pressure, and adding a viscosity reduction additive in the reaction process; and cooling, crushing, washing and drying the product to obtain the phenolphthalein polyaryletherketone product. The invention belongs to the technical field of high polymer material synthesis, and particularly provides a method for solving the problems of impregnation, high energy consumption and low reaction efficiency caused by high melt viscosity in the prior art, the process has the advantages of low melt viscosity, low energy consumption, high reaction efficiency and the like, and the production efficiency and quality of phenolphthalein polyaryletherketone can be remarkably improved.

Description

Technical Field

[0001] The invention belongs to the technical field of polymer material synthesis, and specifically relates to a low-energy consumption phenolphthalein polyaryletherketone polymerization reaction process. Background Art

[0002] Phenolphthalein polyaryletherketone (PEK-C) is a high-performance engineering plastic with excellent heat resistance, chemical corrosion resistance and mechanical properties. It is widely used in aerospace, electronics, automotive industry and other fields. However, the existing PEK-C polymerization process has the following problems:

[0003] 1. The melt viscosity of PEK-C is high during the polymerization process, which results in poor fiber impregnation when preparing composite materials. The high melt viscosity makes it difficult for the resin to fully penetrate between the fibers, resulting in defects inside the prepared composite material, affecting the uniformity and mechanical properties of the material.

[0004] 2. Traditional polymerization reaction processes require high temperature and high pressure conditions, which results in high energy consumption and increases production costs.

[0005] 3. Due to the high melt viscosity and the limitations of reaction conditions, the polymerization efficiency is low and the reaction time is long. Summary of the invention

[0006] The technical problem to be solved by the present invention is the problem in the prior art that high melt viscosity leads to impregnation, high energy consumption and low reaction efficiency.

[0007] To solve the above problems, the technical solution adopted by the present invention is as follows:

[0008] A low-energy consumption phenolphthalein polyaryletherketone polymerization process proposed by the present invention comprises the following steps:

[0009] Step S1, raw material preparation: phenolphthalein monomer, 4,4'-difluorobenzophenone monomer and catalyst are mixed in a certain proportion;

[0010] Step S2, prepolymerization reaction: prepolymerization reaction is first carried out at low temperature and normal pressure to generate a low molecular weight prepolymer; 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;

[0011] Step S3, main polymerization reaction: transferring the low molecular weight prepolymer to a high temperature reactor, carrying out the main polymerization reaction at high temperature and medium pressure, and adding a viscosity reducing agent during the reaction;

[0012] Step S4, post-treatment: cooling, crushing, washing and drying the product to obtain a phenolphthalein polyaryletherketone product.

[0013] Furthermore, in step S1, the molar ratio of the phenolphthalein monomer to the 4,4'-difluorobenzophenone monomer is (0.95-1.05):1, and the amount of the catalyst used is 0.5%-2% of the total mass of the phenolphthalein monomer and the 4,4'-difluorobenzophenone monomer.

[0014] Furthermore, the mixing environment in step S1 is preferably carried out under a nitrogen atmosphere.

[0015] Furthermore, the catalyst in step S1 is an alkaline catalyst, such as sodium hydroxide or potassium hydroxide, which is used to promote the polycondensation reaction.

[0016] Furthermore, the low temperature condition in step S2 is 100-150°C.

[0017] Furthermore, in step S3, the high temperature condition is 200-250° C., and the medium pressure is 1-2 MPa.

[0018] 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%-1% of the total mass of the reaction system.

[0019] Furthermore, the time of the prepolymerization reaction in step S2 is 1-2 hours, and the time of the main polymerization reaction in step S3 is 2-3 hours.

[0020] The beneficial effects achieved by the present invention using the above scheme are as follows:

[0021] 1. The low-energy phenolphthalein polyaryletherketone polymerization process proposed in this scheme reduces the melt viscosity and improves the impregnation effect by optimizing the reaction conditions and adding additives.

[0022] 2. The low-energy consumption phenolphthalein polyaryletherketone polymerization process proposed in this scheme reduces the reaction temperature and pressure and reduces energy consumption through low-temperature prepolymerization and medium-pressure main polymerization.

[0023] 3. The low-energy phenolphthalein polyaryletherketone polymerization process proposed in this scheme improves the polymerization reaction efficiency, shortens the reaction time, and improves the reaction efficiency by optimizing the catalyst and reaction conditions. DETAILED DESCRIPTION

[0024] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments; based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0025] Example 1

[0026] A low-energy consumption phenolphthalein polyaryletherketone polymerization process proposed by the present invention comprises the following steps:

[0027] Step 1, raw material preparation: phenolphthalein monomer, 4,4'-difluorobenzophenone monomer and catalyst are mixed in 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%;

[0028] Step 2, prepolymerization reaction: prepolymerization reaction is carried out at 120° C. and normal pressure for 1.5 hours to generate a low molecular weight prepolymer;

[0029] The prepolymerization reaction is carried out at a relatively low temperature so that the reactants are initially polymerized to 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.

[0030] Step 3, main polymerization reaction: transfer the prepolymer to a high temperature reactor, and carry out the main polymerization reaction at 220°C and 1.5 MPa for 2.5 hours;

[0031] The prepolymer is heated to a higher temperature to cause a further polymerization reaction. The rate and degree of the polymerization reaction can be regulated by controlling the temperature difference, thereby obtaining phenolphthalein polyaryletherketone with a target viscosity and molecular weight.

[0032] Step 4, adding additives: adding silicone oil during the main polymerization reaction, the silicone oil is 0.5% of the total mass of the reaction system, to reduce the melt viscosity;

[0033] Step 5, post-treatment: After the reaction is completed, the product is cooled, crushed, washed and dried to remove impurities, so as to improve the purity of the product and obtain a phenolphthalein polyaryletherketone product.

[0034] Example 2

[0035] A low-energy consumption phenolphthalein polyaryletherketone polymerization process proposed by the present invention comprises the following steps:

[0036] Step 1, raw material preparation: phenolphthalein monomer, 4,4'-difluorobenzophenone monomer and catalyst are mixed in proportion;

[0037] Step 2, prepolymerization reaction: prepolymerization reaction is carried out at 150° C. and normal pressure to generate a low molecular weight prepolymer;

[0038] Step 3, main polymerization reaction: transfer the prepolymer to a high temperature reactor and carry out the main polymerization reaction at 250°C and 2MPa;

[0039] Step 4, adding additives: adding low molecular weight polyether during the main polymerization process to reduce melt viscosity;

[0040] Herein, a formula example of this embodiment is given:

[0041] Phenolphthalein monomer: 100 g (1 mol); 4,4'-difluorobenzophenone monomer: 100 g (1 mol); catalyst (sodium hydroxide): 2 g (1%); auxiliary agent (silicone oil): 0.5 g (0.25%).

[0042] Step 5, post-treatment: After the reaction is completed, the product is cooled, crushed, washed and dried to obtain a phenolphthalein polyaryletherketone product.

[0043] In the above embodiment, 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 raw material ratio can be fine-tuned according to the reaction temperature and pressure to achieve the best reaction effect.

[0044] In this embodiment, low-temperature prepolymerization, medium-pressure main polymerization and the addition of a viscosity-reducing agent solve the problems of poor impregnation effect and high energy consumption caused by high melt viscosity. 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.

[0045] The present invention and its implementation methods are described above, and such description is not restrictive. In short, if ordinary technicians in the field are inspired by it, without departing from the purpose of the invention, they can design structures and embodiments similar to the technical solution without creativity, which should all fall within the protection scope of the present invention.

Claims

1. A low-energy consumption phenolphthalein polyaryletherketone polymerization process, characterized in that: The following steps are involved: Step S1, raw material preparation: phenolphthalein monomer, 4,4'-difluorobenzophenone monomer and catalyst are mixed in a certain proportion; Step S2, prepolymerization reaction: prepolymerization reaction is first carried out at low temperature and normal pressure to generate a low molecular weight prepolymer; Step S3, main polymerization reaction: transferring the low molecular weight prepolymer to a high temperature reactor, carrying out the main polymerization reaction at high temperature and medium pressure, and adding a viscosity reducing agent during the reaction; Step S4, post-treatment: cooling, crushing, washing and drying the product to obtain a phenolphthalein polyaryletherketone product.

2. A low-energy consumption phenolphthalein polyaryletherketone polymerization process according to claim 1, characterized in that: The low temperature condition in step S2 is 100-150° C., and the reaction time is 1-2 hours.

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

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

5. A low-energy consumption phenolphthalein polyaryletherketone polymerization process according to claim 1, characterized in that: The catalyst in step S1 is an alkaline catalyst, and the alkaline catalyst is sodium hydroxide or potassium hydroxide.

6. A low energy consumption phenolphthalein polyaryletherketone 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%-1% of the total mass of the reaction system.

7. A low energy consumption phenolphthalein polyaryletherketone polymerization process according to claim 1, characterized in that: The mixing environment in step S1 is performed under a nitrogen atmosphere.