High-temperature-resistant and high-pressure-resistant glass fiber reinforced polyether ketone composite material and preparation method thereof

Abstract

The invention belongs to the technical field of polyether ketone composite materials, and particularly relates to a high-temperature-resistant and high-pressure-resistant glass fiber reinforced polyether ketone composite material and a preparation method thereof. The preparation method comprises the following steps: in the process of synthesizing the phenylethynyl-terminated polyether ketone oligomer, adding the glass fibers into a reaction system to obtain the phenylethynyl-terminated polyether ketone oligomer containing the glass fibers after the reaction is finished, and then carrying out hot-pressing cross-linking molding on the phenylethynyl-terminated polyether ketone oligomer containing the glass fibers to obtain the phenylethynyl-terminated polyether ketone oligomer containing the glass fibers. The high-temperature-resistant and high-pressure-resistant glass fiber reinforced polyether ketone composite material is obtained. The compressive deformation rate of the high-temperature-resistant and high-pressure-resistant glass fiber reinforced polyether ketone composite material disclosed by the invention at 200 DEG C and 100 MPa is as low as 2%, the compressive deformation under high-temperature and high-pressure conditions is small, excellent sealing performance and high-temperature-resistant and high-pressure-resistant performance are shown, and normal use of equipment such as an oil pump and the like in a high-temperature and high-pressure environment is met.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of polyether ketone composite materials, and particularly relates to a glass fiber reinforced polyether ketone composite material resistant to high temperature and high pressure and a preparation method thereof. BACKGROUND

[0002] As a special engineering plastic, polyether ketone has the characteristics of high heat resistance, chemical corrosion resistance, wear resistance, fatigue resistance, hydrolysis resistance, excellent electrical properties, etc. However, in the petrochemical industry, such as the sealing gasket applied to the high-temperature and high-pressure oil pump, the sealing gasket material is required to have high dimensional stability under high temperature and high pressure (for example, 200℃ / 100MPa). In actual use, the existing polyether ketone and the corresponding composite material will produce obvious compression deformation under the environmental conditions of high temperature and high pressure, ultimately leading to sealing failure, thereby affecting the normal operation of the equipment under high temperature and high pressure working conditions. Therefore, it is of great significance to study the polyether ketone composite material resistant to high temperature and high pressure.

[0003] At present, there is no relevant literature report on the polyether ketone composite material resistant to high temperature and high pressure, and only some improvement methods for reinforcing polyether ether ketone with glass fibers are provided in the prior art.

[0004] For example, the patent application with the application publication number CN119264637A provides a preparation method of a low dielectric constant electromagnetic shielding heat-conducting polyether ether ketone composite material, and the specific steps are as follows: S1, uniformly mixing polyether ether ketone resin, low dielectric glass fiber, conductive filler and auxiliary agent to obtain a mixture; S2, adding the mixture from a main feeding port into a double-screw extruder, and adding the low dielectric glass fiber from a side feeding port into the double-screw extruder, uniformly mixing the mixture and the low dielectric glass fiber in the screw cavity of the double-screw extruder to obtain a secondary mixture; S3, after the secondary mixture is subjected to heating melting, extrusion granulation and sieving, the polyether ether ketone composite material is obtained.

[0005] For another example, the patent application with the application publication number CN116328032A provides a preparation method of a glass fiber reinforced polyether ether ketone composite material, which melts and extrudes polyether ether ketone resin and glass fiber to obtain the glass fiber reinforced polyether ether ketone composite material; the melt index of the polyether ether ketone is 89-91g / 10min; the glass fiber is original glass fiber or surface pretreated glass fiber; and the mass ratio of the glass fiber to the polyether ether ketone resin is 3:7-5:5.

[0006] However, the glass fiber reinforced polyether ether ketone composite prepared by the above prior art is usually prepared by first preparing a polyether ether ketone polymer, and then melt blending and granulating the polyether ether ketone polymer with glass fibers. Even if the polyether ether ketone is replaced by polyether ketone, the obtained glass fiber reinforced polyether ketone composite still does not have high temperature and high pressure resistance, and obvious compression deformation occurs under high temperature and high pressure environment conditions, and cannot be applied to sealing work under high temperature and high pressure working conditions.

[0007] Therefore, it is necessary to develop a new type of glass fiber reinforced polyether ketone composite material resistant to high temperature and high pressure, reduce compression deformation under high temperature and high pressure conditions, and be suitable for sealing work under high temperature and high pressure working conditions. SUMMARY

[0008] The purpose of the present application is to solve the problems existing in the prior art, and provide a glass fiber reinforced polyether ketone composite material resistant to high temperature and high pressure and a preparation method thereof.

[0009] To achieve the above purpose, the technical scheme adopted by the present application is as follows:

[0010] A preparation method of a glass fiber reinforced polyether ketone composite material resistant to high temperature and high pressure, wherein glass fibers are added to the reaction system during the synthesis of phenyl acetylene group terminated polyether ketone oligomers, and the phenyl acetylene group terminated polyether ketone oligomers containing glass fibers are obtained after the reaction is completed. Then, the phenyl acetylene group terminated polyether ketone oligomers containing glass fibers are subjected to hot pressing crosslinking and molding to obtain the glass fiber reinforced polyether ketone composite material resistant to high temperature and high pressure.

[0011] The present application can prepare a glass fiber reinforced polyether ketone composite material resistant to high temperature and high pressure, and the main reasons are as follows:

[0012] ① Physical crosslinking occurs between the molecular chains of glass fibers and polyether ketone, the molecular chains are entangled by the glass fibers, and the movement of the molecular chains is hindered, thereby improving the high temperature and high pressure resistance of the product;

[0013] ② During the hot pressing crosslinking and molding process, chemical crosslinking occurs between the molecular chains of polyether ketone, and the movement of the molecular chains is further hindered, thereby improving the high temperature and high pressure resistance of the product, and the chemical crosslinking reaction equation is as follows:

[0014] ;

[0015] ③ The glass fibers are added early, can be uniformly dispersed in the polyether ketone, and avoid agglomeration in the high viscosity system, so that the glass fibers can fully play a role.

[0016] As a preferred technical scheme:

[0017] The preparation method of the high temperature and high pressure resistant glass fiber reinforced polyetherketone composite material described above, wherein the average length of the glass fiber is 200-3000μm, preferably 3000μm.

[0018] The method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material as described above involves phenylacetylene-terminated polyetherketone oligomers composed of 4,4-hydroxyl groups. ' -Difluorobenzophenone, 4,4 ' -Dihydroxybenzophenone is produced by the reaction of 4-fluoro-4-(phenylethynyl)benzophenone.

[0019] The preparation method of the high temperature and high pressure resistant glass fiber reinforced polyetherketone composite material described above uses a solution polymerization system as the reaction system, wherein the solvent is 3,4-dimethylbenzophenone.

[0020] Existing technologies primarily use diphenyl sulfone as a solvent to synthesize polyetherketones (PEKs). While the high boiling point of this solvent meets the requirements for high-temperature polymerization of PEVs, its high melting point also results in a lengthy subsequent washing process to remove the diphenyl sulfone. Other solvents, such as NMP, while having low melting points, also have low boiling points, making it difficult to polymerize high-molecular-weight PEVs. This invention utilizes 3,4-dimethylbenzophenone, which combines low melting point and high boiling point, meeting the requirements for high-temperature PEV polymerization, and is easily removed during post-processing.

[0021] The preparation method of the high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material described above includes the following steps for preparing phenylacetylene-terminated polyetherketone oligomers containing glass fibers:

[0022] (a) Under nitrogen or inert gas protection conditions, the solvent, 4,4 ' -Difluorobenzophenone, 4,4 ' - Dihydroxybenzophenone and sodium carbonate are mixed at high speed and then undergo a salt formation reaction;

[0023] (b) Increasing the temperature to carry out the polymerization reaction;

[0024] (c) Add 4-fluoro-4-(phenylethynyl)benzophenone for end-capping reaction;

[0025] (d) Add glass fiber and mix.

[0026] (e) Post-processing yields a phenylethynyl-terminated polyetherketone oligomer containing glass fibers.

[0027] The preparation method of the high temperature and high pressure resistant glass fiber reinforced polyetherketone composite material described above, 4,4 ' -Difluorobenzophenone, 4,4 'The molar ratio of 4-dihydroxybenzophenone, sodium carbonate, and 4-fluoro-4-(phenylethynyl)benzophenone is 0.50:0.51:0.52:0.01.

[0028] The preparation method of the high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material as described above includes the following steps: In step (a), the temperature of the salt formation reaction is 200-230℃, preferably 220℃, and the time is 1-3h, preferably 2h; In step (b), the temperature of the polymerization reaction is 240-260℃, preferably 245℃, and the time is 3-6h, preferably 4h; In step (c), the temperature of the end-capping reaction is 230-270℃, preferably 250℃, and the time is 1-3h, preferably 2h; In step (d), the stirring and mixing time is 2-4h, preferably 1h; In step (e), the post-treatment process is as follows: the reaction mixture is poured into warm water at 45-65℃, preferably 60℃ to precipitate the crude product, and then the crude product is washed with distilled water 5-10 times, preferably 6 times, and then dried under vacuum at 80-100℃, preferably 100℃ for 10-14h, preferably 12h.

[0029] The preparation method of the high temperature and high pressure resistant glass fiber reinforced polyetherketone composite material described above involves a hot-press cross-linking molding temperature of 350-400℃, preferably 360℃, and a time of 1-3h, preferably 1h.

[0030] This invention also provides a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material, which is prepared by the preparation method of a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material as described in any of the preceding claims; the high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material has a glass fiber content of 1wt%-6wt%, a tensile strength of 122-156MPa, a tensile modulus of 4126-5770MPa, a density of 1.30-1.34g / cm³, a compression deformation of 0.08-0.23mm at 200℃ and 100MPa, and a compression deformation rate of 2.0%-5.8% at 200℃ and 100MPa.

[0031] Beneficial effects:

[0032] (1) The preparation method of the present invention adds 1wt%-6wt% glass fiber to the front-end reaction system, which improves the physical cross-linking degree between polymer chains. The resulting high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material has a compression deformation rate of 2.0%-5.8% at 200℃ and 100MPa. The compression deformation under high temperature and high pressure conditions is small, showing excellent sealing performance and high-temperature and high-pressure resistance, which meets the normal use of equipment such as oil pumps in high-temperature and high-pressure environments. In contrast, the conventional PEKGF30 has a glass fiber content of 30%, and its compression deformation rate at 200℃ and 100MPa is 17.8%, which has large compression deformation under high temperature and high pressure conditions and poor high-temperature and high-pressure resistance.

[0033] (2) The preparation method of the present invention uses 3,4-dimethylbenzophenone (melting point 47°C, boiling point 354°C) as the reaction solvent, instead of the traditional diphenyl sulfone (melting point 129°C, boiling point 379°C) solvent. By pouring the solution after the polymerization reaction into warm water at 45-65°C, the solvent and crude product are well separated, avoiding the need for subsequent washing of diphenyl sulfone solvent, simplifying the production process, and facilitating large-scale industrial application. Attached Figure Description

[0034] Figure 1 This is a process flow diagram of the preparation method of the present invention;

[0035] Figure 2 The compression curve of the PEKGF30 sample at 200℃ and 100MPa is shown.

[0036] Figure 3 This is the compression curve of the sample prepared in Comparative Example 1 of the present invention at 200°C and 100MPa.

[0037] Figure 4 The compression curve of the sample obtained in Example 1 of the present invention at 200°C and 100MPa is shown.

[0038] Figure 5 This is the compression curve of the sample obtained in Example 2 of the present invention at 200°C and 100MPa;

[0039] Figure 6 This is the compression curve of the sample obtained in Example 3 of the present invention at 200°C and 100MPa;

[0040] Figure 7 This is the compression curve of the sample obtained in Example 4 of the present invention at 200°C and 100MPa;

[0041] Figure 8 This is the infrared spectrum of the sample obtained in Example 4 of the present invention;

[0042] Figure 9 The sealing gasket is processed using the sample obtained in Example 4 of the present invention (where black is the background and white is the sealing gasket). Detailed Implementation

[0043] The present invention will be further described below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

[0044] The following are the relevant performance testing methods for each embodiment and comparative example:

[0045] (1) Glass fiber content: with glass fiber, 4,4 ' -Difluorobenzophenone, 4,4 ' The total mass of the four raw materials, namely benzophenone, 4-fluoro-4-(phenylethynyl)benzophenone, is used as the basis for the mass percentage of glass fiber.

[0046] (2) Tensile strength: Tested in accordance with standard ISO 527.

[0047] (3) Tensile modulus: Tested in accordance with standard ISO 527.

[0048] (4) Density: Tested according to standard ISO 1183.

[0049] (5) Compression deformation at 200℃ and 100MPa: Place a sample with a length of 10mm, a width of 10mm and a thickness of 4mm in a heating furnace, heat it to 200℃, keep it at a constant temperature for 15min, and then apply positive pressure to the sample. When the pressure reaches 100MPa, record the deformation of the sample at this time.

[0050] (6) Compression deformation rate at 200℃ and 100MPa: The ratio of the compression deformation at 200℃ and 100MPa to the original 4mm thickness is the compression deformation rate of the sample at 200℃ and 100MPa.

[0051] Example 1

[0052] A method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material, such as... Figure 1 As shown, the specific steps are as follows:

[0053] (1) Prepare raw materials;

[0054] Nitrogen;

[0055] Solvent: 3,4-Dimethylbenzophenone;

[0056] 4,4 ' -Difluorobenzophenone;

[0057] 4,4 ' -Dihydroxybenzophenone;

[0058] Sodium carbonate;

[0059] 4-Fluoro-4-(phenylethynyl)benzophenone;

[0060] Glass fiber: average length 3000μm; manufacturer: Taishan Glass Fiber Co., Ltd.; grade: HMG 443R.

[0061] Warm water: Deionized water at 60℃;

[0062] Distilled water;

[0063] (2) The specific steps for preparing phenylacetylene-terminated polyetherketone oligomers containing glass fibers are as follows:

[0064] (a) Under nitrogen or inert gas protection conditions, the solvent, 4,4 ' -Difluorobenzophenone, 4,4 ' - Dihydroxybenzophenone and sodium carbonate were mixed and then subjected to a salt formation reaction at a temperature of 220℃ for 2 hours.

[0065] (b) The polymerization reaction was carried out at a temperature of 245°C for 4 hours.

[0066] (c) A capping reaction was carried out by adding 4-fluoro-4-(phenylethynyl)benzophenone at a temperature of 250°C for 2 hours; solvent, 4,4 ' -Difluorobenzophenone, 4,4 ' The molar ratio of 4-dihydroxybenzophenone, sodium carbonate, and 4-fluoro-4-(phenylethynyl)benzophenone is 2.14:0.50:0.51:0.52:0.01.

[0067] (d) Add glass fiber and stir for 1 hour; using glass fiber, 4,4 ' -Difluorobenzophenone, 4,4 ' Based on the total mass of -dihydroxybenzophenone and 4-fluoro-4-(phenylethynyl)benzophenone, the mass percentage of glass fiber is 1%;

[0068] (e) Pour the reaction mixture into warm water to precipitate the crude product, wash the crude product 6 times with distilled water, and then dry it under vacuum at 100°C for 12 hours to obtain a phenylethynyl-terminated polyetherketone oligomer containing glass fiber.

[0069] (3) The glass fiber-reinforced polyetherketone oligomer with phenyl ethynyl end capping is subjected to hot-press cross-linking molding at a temperature of 360°C for 1 hour to obtain a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material.

[0070] The final high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material has a glass fiber content of 1 wt%, a tensile strength of 122 MPa, a tensile modulus of 4126 MPa, and a density of 1.3 g / cm³. Its compression curve at 200℃ and 100 MPa is shown below. Figure 4As shown, the compression deformation at 200℃ and 100MPa is 0.23mm, and the compression deformation rate at 200℃ and 100MPa is 5.8%.

[0071] Comparative Example 1

[0072] A method for preparing polyetherketone differs from Example 1 only in that glass fiber is not added in step (d).

[0073] The final polyetherketone (PEK) obtained had a tensile strength of 121 MPa, a tensile modulus of 4122 MPa, and a density of 1.29 g / cm³. Its compression curve at 200℃ and 100 MPa is shown below. Figure 3 As shown, the compression deformation at 200℃ and 100MPa is 0.52mm, and the compression deformation rate at 200℃ and 100MPa is 13.0%.

[0074] Compared with Example 1, the tensile strength, tensile modulus and density of the polyetherketone in Comparative Example 1 did not change significantly. The compression deformation at 200°C and 100MPa increased by 126.1%, and the compression deformation rate at 200°C and 100MPa increased by 124.1%. This is because Comparative Example 1 did not add glass fiber, so there was less entanglement between the polyetherketone molecular chains, and the molecular chains still had high mobility.

[0075] Comparative Example 2

[0076] A method for preparing a polyetherketone composite material differs from Example 1 only in that steps (e) and (d) are interchanged, that is, polyetherketone oligomers are precipitated first and then mixed with glass fibers.

[0077] The final polyetherketone composite material has a tensile strength of 89 MPa, a tensile modulus of 3252 MPa, a density of 1.3 g / cm³, a compression deformation of 0.73 mm at 200℃ and 100 MPa, and a compression deformation rate of 18.2% at 200℃ and 100 MPa.

[0078] Compared with Example 1, the density of the polyetherketone composite material in Comparative Example 2 did not change significantly, but the tensile strength decreased by 27.0%, the tensile modulus decreased by 21.2%, the compression deformation at 200℃ and 100MPa increased by 217.4%, and the compression deformation rate at 200℃ and 100MPa increased by 213.8%. This is because the glass fibers in the polyetherketone composite material are unevenly dispersed, making it difficult for the glass fibers to play a full role, resulting in a deterioration in mechanical properties such as tensile strength and tensile modulus, as well as high temperature and high pressure resistance.

[0079] Furthermore, comparing Comparative Example 1 and Comparative Example 2 reveals that the high-temperature and high-pressure resistance of the polyetherketone composite material in Comparative Example 2 is significantly lower than that in Comparative Example 1. This is because no glass fiber was added in Comparative Example 1, resulting in a smaller distance between the end-capping groups of the polyetherketone oligomers. This allows for the formation of a more compact interaction network between the molecular chains. This compact structure significantly inhibits the relative slippage of the molecular chains under high temperature and high pressure, making it difficult for molecular chain segments to move. Consequently, it effectively resists molecular chain relaxation and structural damage caused by high temperature and high pressure, maintaining the material's good mechanical properties and structural stability. In contrast, although glass fiber was added in Comparative Example 2, its addition was too late. Unlike the glass fiber in Example 1, it could not physically cross-link with the polyetherketone molecular chains. Instead, this resulted in a larger distance between the end-capping groups of the polyetherketone oligomers, reducing the high-temperature and high-pressure resistance of the polyetherketone.

[0080] Example 2

[0081] A method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material differs from Example 1 only in that: glass fiber and 4,4-dimethylphenol are used. ' -Difluorobenzophenone, 4,4 ' Based on the total mass of 1-dihydroxybenzophenone and 4-fluoro-4-(phenylethynyl)benzophenone, the mass percentage of glass fiber is 2%.

[0082] The final high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material has a glass fiber content of 2wt%, a tensile strength of 130 MPa, a tensile modulus of 4523 MPa, and a density of 1.3 g / cm³. Its compression curve at 200℃ and 100 MPa is shown below. Figure 5 As shown, the compression deformation at 200℃ and 100MPa is 0.13mm, and the compression deformation rate at 200℃ and 100MPa is 3.2%.

[0083] Example 3

[0084] A method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material differs from Example 1 only in that: glass fiber and 4,4-dimethylphenol are used. ' -Difluorobenzophenone, 4,4 ' Based on the total mass of 1-dihydroxybenzophenone and 4-fluoro-4-(phenylethynyl)benzophenone, the mass percentage of glass fiber is 4%.

[0085] The final high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material has a glass fiber content of 4 wt%, a tensile strength of 142 MPa, a tensile modulus of 5682 MPa, and a density of 1.31 g / cm³. Its compression curve at 200℃ and 100 MPa is shown below. Figure 6As shown, the compressive deformation at 200℃ and 100MPa is 0.11mm, and the compressive deformation rate at 200℃ and 100MPa is 2.8%.

[0086] Example 4

[0087] A method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material differs from Example 1 only in that: glass fiber and 4,4-dimethylphenol are used. ' -Difluorobenzophenone, 4,4 ' Based on the total mass of 1-dihydroxybenzophenone and 4-fluoro-4-(phenylethynyl)benzophenone, the mass percentage of glass fiber is 6%.

[0088] The infrared spectrum of the finally obtained high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material is as follows: Figure 8 As shown, 1647cm -1 The peak at 1595 cm⁻¹ is the stretching vibration peak of C=O. -1 It is an absorption peak within the plane of the Ar-O-Ar benzene ring; 1231 cm⁻¹ -1 It is an aromatic Ar-O-Ar asymmetric stretching absorption peak; 1148 cm⁻¹ -1 It is the absorption peak of the CH bending vibration within the benzene ring; 832 cm⁻¹ -1 and 757cm -1 The absorption peak is the out-of-plane bending vibration of CH in the benzene ring. From this infrared spectrum, it can be seen that the prepared composite material contains polyetherketone with a certain degree of polymerization; the glass fiber content is 6wt%, the tensile strength is 156MPa, the tensile modulus is 5770MPa, and the density is 1.34g / cm³. The compression curve at 200℃ and 100MPa is as follows... Figure 7 As shown, the compression deformation at 200℃ and 100MPa is 0.08mm, and the compression deformation rate at 200℃ and 100MPa is 2%.

[0089] The conventional PEKGF30 sample has a glass fiber content of 30wt%, a tensile strength of 185MPa, a tensile modulus of 13200MPa, and a density of 1.51g / cm³. The compression curve of the conventional PEKGF30 sample at 200℃ and 100MPa is shown below. Figure 2As shown, the compression deformation at 200℃ and 100MPa was 0.71mm, and the compression deformation rate at 200℃ and 100MPa was 17.8%. This large deformation is the main reason for the sealing failure of conventional PEKGF30 gaskets under high temperature and high pressure conditions. The samples prepared in Examples 1-4 of this invention had a glass fiber content of 1wt%-6wt%, and their compression deformation rates at 200℃ and 100MPa were all within 6%. The samples prepared in Examples 3 and 4 had compression deformation rates within 3% at 200℃ and 100MPa. In particular, the sample prepared in Example 4 had a glass fiber content of 6wt%, and its compression deformation rate at 200℃ and 100MPa was 2%. The sample prepared in Example 4 was processed into... Figure 9 The sealing gasket shown was tested on an oil pump. The machine operated continuously for 168 hours without any leakage, indicating that the glass fiber reinforced polyetherketone composite material prepared in Example 4 can meet the long-term use requirements of sealing products under high temperature and high pressure conditions.

Claims

1. A method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material, characterized in that, In the process of synthesizing phenylacetylene-terminated polyetherketone oligomers, glass fibers are added to the reaction system. After the reaction is completed, phenylacetylene-terminated polyetherketone oligomers containing glass fibers are obtained. Then, the phenylacetylene-terminated polyetherketone oligomers containing glass fibers are subjected to hot-press cross-linking molding to obtain a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material.

2. The method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material according to claim 1, characterized in that, The average length of the glass fiber is 200-3000 μm.

3. The method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material according to claim 1, characterized in that, Phenylacetyl-terminated polyetherketone oligomers are composed of 4,4- ' -Difluorobenzophenone, 4,4 ' -Dihydroxybenzophenone is produced by the reaction of 4-fluoro-4-(phenylethynyl)benzophenone.

4. The method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material according to claim 3, characterized in that, The reaction system is a solution polymerization system, in which the solvent is 3,4-dimethylbenzophenone.

5. The method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material according to claim 4, characterized in that, The steps for preparing phenylacetylene-terminated polyetherketone oligomers containing glass fibers are as follows: (a) Under nitrogen or inert gas protection conditions, the solvent, 4,4 ' -Difluorobenzophenone, 4,4 ' - Dihydroxybenzophenone and sodium carbonate are mixed and then undergo a salt formation reaction; (b) Increasing the temperature to carry out the polymerization reaction; (c) Add 4-fluoro-4-(phenylethynyl)benzophenone for end-capping reaction; (d) Add glass fiber and mix. (e) Post-processing yields a phenylethynyl-terminated polyetherketone oligomer containing glass fibers.

6. The method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material according to claim 5, characterized in that, 4,4 ' -Difluorobenzophenone, 4,4 ' The molar ratio of 4-dihydroxybenzophenone, sodium carbonate, and 4-fluoro-4-(phenylethynyl)benzophenone is 0.50:0.51:0.52:0.

01.

7. The method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material according to claim 5, characterized in that, In step (a), the temperature of the salt formation reaction is 200-230℃ and the time is 1-3h; in step (b), the temperature of the polymerization reaction is 240-260℃ and the time is 3-6h; in step (c), the temperature of the end-capping reaction is 230-270℃ and the time is 1-3h; in step (d), the stirring and mixing time is 2-4h.

8. The method for preparing a high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material according to claim 1, characterized in that, The temperature for hot-press cross-linking molding is 350-400℃, and the time is 1-3 hours.

9. A high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material, characterized in that, The high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material is prepared by the preparation method described in any one of claims 1-8; the high-temperature and high-pressure resistant glass fiber reinforced polyetherketone composite material has a glass fiber content of 1wt%-6wt%, a tensile strength of 122-156MPa, a tensile modulus of 4126-5770MPa, a density of 1.30-1.34g / cm³, a compression deformation of 0.08-0.23mm at 200℃ and 100MPa, and a compression deformation rate of 2.0%-5.8% at 200℃ and 100MPa.

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