CN113416305A - Long fiber reinforced polyaryletherketone composite material and preparation method thereof - Google Patents
Long fiber reinforced polyaryletherketone composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a long fiber reinforced polyaryletherketone composite material and a preparation method thereof, wherein sulfonated polyaryletherketone is used for pretreating long fibers in diphenylsulfone, the solubility of the sulfonated polyaryletherketone diphenylsulfone is poor, so that the fibers form micelles, and the fibers are not easy to disperse, the diffusion and adsorption of the long fibers in an in-situ polymerization system are limited, then the micelles are added into a polymerization system formed by a double-halogen monomer and a bisphenol monomer for polymerization, and the long fiber reinforced polyaryletherketone composite material is prepared by in-situ polymerization.
Description
Technical Field
The invention belongs to the field of polymer composite materials, and relates to a long fiber reinforced polyaryletherketone composite material prepared by introducing long carbon fibers into polyaryletherketone in situ and a preparation method thereof.
Background
Polyaryletherketone is a thermoplastic high-performance polymer material with a molecular chain containing benzene rings, ether and ketone as repeating elements, and currently, industrial commodities include polyetheretherketone resin, polyetherketoneetherketoneketone resin and the like. Polyaryletherketones are used as high-performance thermoplastic resins and have many applications in the fields of aviation, aerospace, petroleum, electronics and medical treatment. In order to meet the more demanding service environment, fiber reinforced polyaryletherketone composite materials are developed and have a plurality of applications.
The fiber reinforced polyether-ether-ketone composite material comprises chopped fiber reinforced polyether-ether-ketone, long fiber reinforced polyether-ether-ketone and continuous fiber reinforced polyether-ether-ketone. Wherein the development of the chopped fiber reinforced polyether-ether-ketone is mature, the price is low, and the dosage is large. The fiber content of the chopped fiber reinforced polyether-ether-ketone is increased from 15 percent to 30 percent, and the mechanical property of the chopped fiber reinforced polyether-ether-ketone is gradually changed along with the increase of the fiber content. For example, the tensile strength of the polyether-ether-ketone resin is 90-100 MPa, and the tensile strength of the chopped carbon fiber reinforced polyether-ether-ketone composite material with the content of 30% is 220 MPa. More fibers are added in the composite material, so that the tensile strength of the polyether-ether-ketone fiber reinforced composite material can be improved. Under the condition that the contents of the long-cut fibers and the short-cut fibers are consistent, the long-cut fiber reinforced polyether-ether-ketone composite material can further improve the fiber content compared with the short-cut fiber reinforced polyether-ether-ketone composite material.
The preparation method of the continuous fiber reinforced polyether-ether-ketone comprises the methods of melt extrusion coating, powder electrostatic impregnation, film lamination, solution impregnation, fiber mixed weaving and the like. The continuous fiber reinforced polyether-ether-ketone composite material has good application under a plurality of harsh use environments. Theoretically, the continuous fiber reinforced polyether-ether-ketone composite material can be subjected to fiber shearing to obtain the long fiber reinforced polyether-ether-ketone composite material. However, since the continuous fiber-reinforced polyetheretherketone composite material is difficult to pre-impregnate and expensive, the preparation of a long fiber-reinforced polyetheretherketone composite material using the continuous fiber-reinforced polyetheretherketone composite material as a raw material is not suitable in terms of material properties and cost.
Wu Xinming et al (aeronautical materials Proc., 2009, 6: 98-101) at northwest university report research on processing technology and mechanical properties of injection molding polyetheretherketone composite material reinforced by 30% long glass fiber, but this method usually makes part of the properties of the product insufficient. The preparation of composite materials by in-situ polymerization is a common technique in the field of polymer composite materials. The method solves the problems that the solution of the polyether-ether-ketone resin has high viscosity and the resin is difficult to dissolve in the conventional organic solvent. The resin-based composite material is prepared by in-situ polymerization, and various materials can be selected, such as montmorillonite, graphite sheet (CN201410539991.0), hydroxyapatite and the like. Compared with the composite material prepared by melt blending, the composite material prepared by the in-situ polymerization technology has better dispersibility and better performance.
The long fiber is introduced by solution in-situ polymerization to prepare the long fiber reinforced polyaryletherketone composite material, and a series of problems exist, such as small diameter and large specific surface area of the long fiber, when a large amount of the long fiber exists in a polymerization system, the fiber adsorbs a solvent and a polymerization monomer to influence the reaction system, so that the polymerization reaction system basically has no solvent, the molecular collision is difficult, and the reaction molecular weight is difficult to control. Meanwhile, the solution viscosity is too high due to the introduction of high content of long fiber, and the solution is difficult to mix, thereby influencing the polymerization reaction. If the solution at the end of the polymerization is used to add long fibers for compounding, it is difficult to prepare a fiber-reinforced composite material having a high content of the long fibers due to the dispersing effect of the long fibers. The problems exist in the preparation of the long fiber reinforced polyaryletherketone resin matrix composite material by utilizing the in-situ polymerization technology; the price of the long fiber reinforced composite material prepared by shearing the continuous fiber prepreg polyaryletherketone resin is too high, so that no commercialized long fiber reinforced polyaryletherketone composite material exists at present.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a long fiber reinforced polyaryletherketone composite material, which specifically comprises the following steps:
s1: dissolving sulfonated polyaryletherketone in an organic solvent, adding long fibers after uniformly stirring, stirring to obtain a mixed solution, adding an aqueous solution containing 5% of carbonate into the mixed solution, filtering, and drying to obtain treated long fibers;
s2: heating and uniformly mixing diphenyl sulfone, a double-halogen monomer, a bisphenol monomer and an acid binding agent, reacting to obtain a polyaryletherketone polymer, adding the long fiber treated in the step S1, reacting for a period of time to obtain a composite material, adding the composite material into deionized water, crushing, filtering, purifying and drying the solid to obtain the long fiber reinforced polyaryletherketone composite material.
According to the technical scheme of the invention, the sulfonation degree of the sulfonated polyaryletherketone is that the proportion of the repeating unit containing the sulfonic acid group in the total repeating unit is 40-70%, preferably 50%.
According to the technical scheme of the invention, the mass percentage concentration of the sulfonated polyaryletherketone solution is 0.5-20%, and the mass ratio of the sulfonated polyaryletherketone to the long fiber is 1: 50-200.
According to the technical scheme of the invention, the long fiber accounts for 10-60% of the total weight of the composite material, and preferably 20-40%.
According to the technical scheme of the invention, the polymerization degree of the polyaryletherketone polymer is 80-400.
According to the technical scheme of the invention, the organic solvent is at least one of dimethyl sulfoxide, N, N-dimethylformamide, N, N-dimethylacetamide, sulfolane and N-methylpyrrolidone.
According to the technical scheme of the invention, the molar ratio of the bisphenol monomer, the double-halogen monomer and the acid-binding agent is 1.0-1.01: 1: 1.05-1.5; the long fiber accounts for 10-60% of the total weight of the composite material, the weight ratio of the initial diphenyl sulfone to the polyaryletherketone polymer is 1: 0.1-0.3, and the weight ratio of the dosage of the diphenyl sulfone serving as a dilution effect to the initial diphenyl sulfone is 1: 0.5 to 2. Wherein the inert gas includes, but is not particularly limited to, nitrogen and argon.
According to the technical scheme of the invention, the sulfonated polyaryletherketone has the following structure, wherein the repeating unit of sulfonic acid in the sulfonated polyaryletherketone comprises but is not limited to the following molecular structure,
wherein Ar is one of the following figures:
m is one of sodium ion, potassium ion and cesium ion.
According to the technical scheme of the invention, the bisphenol monomer is a bisphenol monomer with phenolic hydroxyl groups at two ends, can be subjected to polymerization reaction with a double-halogen monomer, and comprises one of the following molecular structures, but is not particularly limited to the following molecular structure:
the double-halogen monomer is characterized in that the end group is halogen and can perform nucleophilic substitution reaction with the bisphenol monomer, and comprises one of the following molecular structures, but is not particularly limited to the following molecular structure:
according to the technical scheme of the invention, the acid-binding agent is carbonate and comprises at least one of sodium carbonate, potassium carbonate, cesium carbonate and calcium carbonate, and preferably sodium carbonate.
Further, the long fiber has a length of 0.5mm to 5 mm; the long fiber type is at least one selected from glass fiber, carbon fiber and basalt fiber.
Further, the specific process of step S2 is: adding diphenyl sulfone into a reaction kettle under the protection of inert gas in a melting way, keeping the temperature of a reaction system at 130-170 ℃, and sequentially and continuously adding a double-halogen monomer, a bisphenol monomer and an acid-binding agent; keeping the reaction system in a stirring state, continuously heating to 190 ℃ for 30 min-1 h, continuously heating to 220 ℃ for 30 min-1 h, continuously heating to 250 ℃ for 30 min-1 h, continuously heating to 280 ℃ for 30 min-1 h, and continuously heating to 320 ℃ for 2-5 h; adding a diphenyl sulfone solvent with the temperature of 220-250 ℃ into a reaction system, diluting a polymerization solution, adding the treated long fiber into the reaction system when the temperature of the reaction system is maintained at 250 ℃, stirring for 10min, adding a reaction material into distilled water, crushing, drying, extracting the reaction material to constant weight by using ethanol or acetone, and extracting the material to constant weight by using the distilled water.
Further, in step S1, the carbonate is sodium carbonate.
The invention also aims to obtain the long fiber reinforced polyaryletherketone composite material by adopting the preparation method.
The invention has the beneficial effects that:
(1) the invention utilizes a high molecular polymerization technology, and the sulfonated polyaryletherketone is used for pretreating long fibers in the diphenylsulfone, so that the sulfonated polyetheretherketone diphenylsulfone has poor solubility, the fibers form micelles, and the fibers are not easy to disperse, the diffusion and the adsorption of the long fibers in an in-situ polymerization system are limited, then the micelles are added into a polymerization system formed by a double-halogen monomer and a bisphenol monomer for polymerization, and the in-situ polymerization is used for preparing the long fiber reinforced polyaryletherketone composite material, thereby solving the problems that in the in-situ polymerization, the reaction cannot be carried out, the fibers are excessively dispersed and entangled after the reaction, and the fibers are not beneficial to crushing due to large specific surface area of the long fibers.
(2) Due to the introduction of the sulfonated polyaryletherketone pretreatment long fiber system, fibers can not be completely dispersed in the polymerization process due to the problem of molecular polarity of a sulfonated material in diphenylsulfone, the specific surface area of the whole fibers is reduced, the polyaryletherketone can be reinforced by high-content long fibers, a composite material with excellent mechanical properties is prepared, and the problem that high-content long fibers are difficult to disperse uniformly is avoided. Because sulfonic acid groups are difficult to bear the high temperature of 320 ℃ of polyether-ether-ketone polymerization, the invention dilutes the mother liquor after the polymerization of the polyaryletherketone at high temperature, reduces the polymerization mother liquor to the temperature below 250 ℃, still keeps the solution state, and then adds the treated long fiber to prepare the long fiber reinforced polyaryletherketone composite material.
(3) The mechanical property of the long fiber reinforced polyaryletherketone composite material prepared by the invention is far higher than that of the commercial chopped fiber reinforced composite material, the manufacturing cost is not greatly increased, and the notch impact strength of the long glass fiber reinforced polyaryletherketone composite material with the content of 30 percent is up to 22kJ/m2Much higher than commercially available chopped fiber reinforced polyetheretherketone products of the same fiber content (Victrex, UK, product of PEEK450GL30 with a notched impact strength of 8kJ/m2)。
Drawings
FIG. 1: SEM image of the composite material containing long carbon fiber reinforced polyaryletherketone in example 1.
Detailed Description
The compounds of the general formula and the preparation and use thereof according to the present invention will be described in further detail with reference to the following examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1
S1: the fiber pretreatment process can be carried out according to the following examples:
1.5g of polyether ether ketone resin (wherein Ar is benzene-ketone-benzene and M is sodium ion) with the sulfonation degree of 50% is weighed, 150ml of DMF is added, and uniform solution is obtained after stirring and dissolving. Adding 90g of 2mm long-cut glass fiber into the solution, stirring for 15min, adding the reaction system into 500mL of 5% sodium carbonate solution, soaking for 12 h, filtering, and drying at 120 ℃ for 12 h to obtain the treated long fiber.
S2: the polyetheretherketone polymerization process and compounding can be carried out according to the following examples:
adding 115g of molten diphenyl sulfone into a reaction bottle filled with nitrogen, adding 43.82g of 4, 4' -difluorodiphenyl ketone into a three-neck flask provided with a mechanical stirrer and a thermometer, heating to 160 ℃ under the protection of nitrogen, adding 25.44g of anhydrous sodium carbonate, heating to 165 ℃, adding 22.00g of hydroquinone, continuously heating to 190 ℃, controlling the temperature for 1 hour, heating to 220 ℃, reacting for 1 hour, gradually heating to 250 ℃, reacting for 35 minutes, heating to 280 ℃, controlling the temperature for 1 hour, finally heating to 320 ℃, reacting for 3 hours, adding 100g of molten diphenyl sulfone, reacting at the temperature of below 250 ℃ to obtain a polyether-ether-ketone polymer, adding 23.04g of treated glass fiber, reacting for 10 minutes to obtain a composite material, pouring the product into water, crushing by a crusher, filtering, directly extracting the solid by acetone for 48 hours, filtering, extracting by distilled water for 48 hours, drying in an oven, obtaining the long fiber reinforced polyaryletherketone composite material.
Example 2
The glass fiber in example 1 was replaced with carbon fiber T700.
Example 3
The amount of the added treated glass fiber in example 1 was 17.3 g.
Example 4
The length of the glass fiber in example 1 was set to 0.5 mm.
Example 5
The length of the glass fiber in example 1 was changed to 3mm, and the amount of the glass fiber added after the treatment was 25.37 g.
Application example
Taking the long carbon fiber reinforced polyaryletherketone composite material in example 1 as an example, SEM test is performed to obtain an SEM image shown in fig. 1.
The long fiber reinforced polyaryletherketone composite materials prepared in the examples and the comparative examples are molded at 390 ℃, and the tensile and impact properties of the materials are measured, and the test results are shown in table 1.
TABLE 1
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the long fiber reinforced polyaryletherketone composite material is characterized by comprising the following steps:
s1: dissolving sulfonated polyaryletherketone in an organic solvent, adding long fibers after uniformly stirring, stirring to obtain a mixed solution, adding an aqueous solution containing 5% of carbonate into the mixed solution, filtering, and drying to obtain treated long fibers;
s2: heating and uniformly mixing diphenyl sulfone, a double-halogen monomer, a bisphenol monomer and an acid binding agent, reacting to obtain a polyaryletherketone polymer, adding the long fiber treated in the step S1, reacting for a period of time to obtain a composite material, adding the composite material into deionized water, crushing, filtering, purifying and drying the solid to obtain the long fiber reinforced polyaryletherketone composite material.
2. The method of claim 1, wherein the sulfonated polyaryletherketone has a sulfonation degree of 40-70% of the total weight of the repeating units containing sulfonic acid groups.
3. The preparation method of the long fiber reinforced polyaryletherketone composite material of claim 1, wherein the mass percentage concentration of the sulfonated polyaryletherketone solution is 0.5-20%, the mass ratio of the sulfonated polyaryletherketone to the long fiber is 1: 50-200, and the long fiber accounts for 10-60% of the total weight of the composite material.
4. The method of claim 1, wherein the organic solvent is at least one of dimethyl sulfoxide, N, N-dimethylformamide, N, N-dimethylacetamide, sulfolane, and N-methylpyrrolidone.
5. The preparation method of the long fiber reinforced polyaryletherketone composite material of claim 1, wherein the molar ratio of the bisphenol monomer, the double-halogen monomer and the acid-binding agent is 1.0-1.01: 1: 1.05-1.5; the weight ratio of the initial diphenyl sulfone to the polyaryletherketone polymer is 1: 0.1-0.3; the weight ratio of the amount of diphenyl sulfone used as dilution to the initial diphenyl sulfone is 1; 0.5 to 2.
6. The method of claim 1, wherein the sulfonated polyaryletherketone has a structure as shown in the following figure, and the repeating units of the sulfonic acid in the sulfonated polyaryletherketone include but are not limited to the following molecular structures,
wherein Ar is one of the following figures:
m is one of sodium ion, potassium ion and cesium ion;
the bisphenol monomer is a bisphenol monomer with phenolic hydroxyl groups at two ends, can be subjected to polymerization reaction with a double-halogen monomer, and comprises one of the following molecular structures, but is not particularly limited to the following molecular structure:
the double-halogen monomer is characterized in that the end group is halogen and can perform nucleophilic substitution reaction with the bisphenol monomer, and comprises one of the following molecular structures, but is not particularly limited to the following molecular structure:
7. the method of claim 1, wherein in step S2, the acid scavenger is a carbonate comprising at least one of sodium carbonate, potassium carbonate, cesium carbonate, and calcium carbonate.
8. The method of claim 1, wherein the long fiber has a length of 0.5mm to 5 mm; the long fiber type is at least one selected from glass fiber, carbon fiber and basalt fiber.
9. The method of claim 1, wherein the carbonate salt is sodium carbonate in step S1.
10. The long fiber reinforced polyaryletherketone composite material prepared by the preparation method of any one of claims 1 to 9.
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Cited By (3)
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| CN114685971A (en) * | 2022-04-18 | 2022-07-01 | 东华大学 | Short carbon fiber/polyether ketone composite powder material and preparation method thereof |
| CN117384463A (en) * | 2023-12-12 | 2024-01-12 | 季华实验室 | Carbon fiber reinforced sulfonated PEEK composite material and preparation method thereof |
| CN117603473A (en) * | 2023-11-29 | 2024-02-27 | 江苏君华特种高分子材料股份有限公司 | High-bioactivity chopped carbon fiber reinforced polyether-ether-ketone composite material and preparation method thereof |
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| CN117384463A (en) * | 2023-12-12 | 2024-01-12 | 季华实验室 | Carbon fiber reinforced sulfonated PEEK composite material and preparation method thereof |
| CN117384463B (en) * | 2023-12-12 | 2024-03-08 | 季华实验室 | Carbon fiber reinforced sulfonated PEEK composite material and preparation method thereof |
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