Composition for preparing polyether-ether-ketone and insulated cable

Abstract

The invention provides a composition for preparing polyether-ether-ketone and an insulated cable. The composition comprises a copolymer and an organic solvent, and the copolymer is a copolymer of N-phenyl (4, 4 '-difluorodiphenyl) ketoamine and hydroquinone. The copolymer disclosed by the invention has excellent solubility in an organic solvent, the convenience of directly coating a conductor with the composition disclosed by the invention and preparing a polyether-ether-ketone insulating layer is greatly improved, the process difficulty is remarkably reduced, the insulating layer with uniform thickness can be generated through single-time coating and acid treatment, and the service life of the insulating layer is prolonged. The technical problem that the coating is not uniform when polyether-ether-ketone is directly used in the prior art is solved, and the risk of defects caused by extrusion thickness is remarkably reduced.

Description

Technical Field

[0001] The present invention relates to a composition for preparing polyetheretherketone and an insulated cable, belonging to the field of materials. Background Art

[0002] Polyetheretherketone (PEEK) is a new type of semi-crystalline aromatic thermoplastic engineering plastic, which has excellent heat resistance grade, radiation resistance, chemical resistance, wear resistance, fatigue resistance and mechanical properties, etc. It has replaced traditional materials such as metals and ceramics in many fields. At present, it has been widely used in the fields of aerospace, electronics and electrical appliances, automobiles, energy, medical treatment, etc.

[0003] PEEK is widely used as an insulating layer coating material in the field of electromagnetic wires. During the coating process of the PEEK insulating layer on electromagnetic wires, the coating method and the thickness of the coating are often very important, which not only determine the processing method, but also determine the performance of the electromagnetic wires after coating with insulating paint.

[0004] Due to the poor solubility of PEEK polymers, existing processes are difficult to prepare PEEK polymers into coatings and apply them to electromagnetic wires. It can only be extruded and coated on electromagnetic wires after melting PEEK polymers at high temperature. For example, Chinese patent document CN220252858U discloses a coating process for PEEK polymers. The process includes: adding PEEK resin materials into the barrel of a screw extruder, heating the PEEK resin materials to a molten state at a temperature of 380°C - 410°C, and then through the rotation of the screw of the screw extruder, making the PEEK polymers flow uniformly in the barrel. Place the preheated core wire in front of the head of the screw extruder. At the head, through different specifications of dies, the PEEK polymers are uniformly coated on the surface of the core wire and form a PEEK insulating layer after cooling and crystallization. However, in such coating methods, when the thickness of one side of the extrusion is low, more defects will occur, and the thinner the thickness of one side of the extrusion, the more defects will occur.

[0005] Therefore, there is an urgent need to develop coatings suitable for wires or electromagnetic wires and their application methods. Summary of the Invention

[0006] To improve the above technical problems, the present invention provides a composition, which comprises a copolymer and an organic solvent, wherein the copolymer is a copolymer of N-phenyl(4,4'-difluorodiphenyl)ketoneamine and hydroquinone.

[0007] According to an embodiment of the present invention, the organic solvent is selected from at least one or a mixture of two or more of N-methylpyrrolidone (NMP), tetrahydrofuran (THF), N,N-dimethylformamide (DMF) or N,N-dimethylacetamide (DMA), and preferably N-methylpyrrolidone.

[0008] According to an embodiment of the present invention, the weight ratio of the copolymer to the organic solvent in the composition may be 1:1 to 1:9, such as 1:1, 1:1.5, 1:1.6, 1:1.7, 1:1.8, 1:1.9, 1:2, 1:2.1, 1:2.2, 1:2.3, 1:2.4, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5, 1:5, 1:5.5, 1:6, 1:6.5, 1:7, 1:7.5, 1:8, 1:8.5 or 1:9.

[0009] According to an embodiment of the present invention, the solid content in the composition may be 10 wt% to 50 wt%, such as 20 wt% to 40 wt%, and its examples may be 20 wt%, 20.5 wt%, 21 wt%, 21.5 wt%, 22 wt%, 22.5 wt%, 23 wt%, 23.5 wt%, 24 wt%, 24.5 wt%, 25 wt%, 25.5 wt%, 26 wt%, 26.5 wt%, 27 wt%, 27.5 wt%, 28 wt%, 28.5 wt%, 29 wt%, 29.5 wt%, 30 wt%, 30.5 wt%, 31 wt%, 31.5 wt%, 32 wt%, 32.5 wt%, 33 wt%, 33.5 wt%, 34 wt%, 34.5 wt%, 35 wt%, 35.5 wt%, 36 wt%, 36.5 wt%, 37 wt%, 37.5 wt%, 38 wt%, 38.5 wt%, 39 wt%, 39.5 wt% or 40 wt%.

[0010] According to an embodiment of the present invention, the composition may further contain a filler, such as a wear-resistant filler.

[0011] According to an embodiment of the present invention, the wear-resistant filler is selected from at least one or more than two of the following materials: whisker silicon, alumina, nano-silica, talc powder, mica, kaolin, montmorillonite, illite, boron nitride, titanium dioxide, zinc sulfide, zirconium dioxide, nano-barium sulfate, graphite, nucleating agent, polytetrafluoroethylene, tin disulfide, molybdenum disulfide, silicone, graphene, potassium titanate; preferably talc and / or boron nitride.

[0012] According to an embodiment of the present invention, the wear-resistant filler is in powder form. For example, the particle size of the wear-resistant filler is 1 μm to 30 μm, such as 5 μm, 10 μm, 15 μm, 20 μm, 25 μm.

[0013] According to an embodiment of the present invention, the mass ratio of the copolymer to the filler is 50:50 to 100:0, such as 55:45, 60:40, 65:35, 70:30, 75:25, 80:20, 85:15, 90:10, 95:5.

[0014] According to an embodiment of the present invention, the viscosity of the composition at room temperature (20 - 25 °C) is 2500 cp to 4000 cp, such as 3000 cp to 3500 cp, and examples thereof are 2500 cp, 2600 cp, 2700 cp, 2800 cp, 2900 cp, 3000 cp, 3100 cp, 3200 cp, 3300 cp, 3400 cp, 3500 cp, 3600 cp, 3700 cp, 3800 cp, 3900 cp or 4000 cp.

[0015] The present invention also provides a preparation method of the composition, and the preparation method includes mixing the copolymer with an organic solvent.

[0016] For example, the preparation method includes the following steps:

[0017] (S1-1) Polymerize N-phenyl(4,4'-difluorodiphenyl)ketimine and hydroquinone to obtain a copolymer;

[0018] (S1-2) Mix the product of step (S1-1) with the organic solvent.

[0019] According to an embodiment of the present invention, the polymerization reaction can be carried out in the presence of a carbonate or bicarbonate. For example, the carbonate or bicarbonate can be a salt of an alkali metal, such as a mixture of one or more selected from potassium carbonate, potassium bicarbonate, sodium carbonate, and sodium bicarbonate.

[0020] Preferably, the polymerization reaction can be carried out in an inert atmosphere. The inert atmosphere can be a gas known to those skilled in the art to be inert to the above polymerization reaction, such as a mixture of one or more selected from nitrogen, helium, neon, argon, krypton, and xenon.

[0021] According to an embodiment of the present invention, the polymerization reaction is carried out in the presence of a solvent and / or an azeotropic dehydrating agent. Preferably, the solvent is selected from at least one of sulfolane, diphenyl sulfone, dimethyl sulfoxide, and N-methylpyrrolidone, and the azeotropic dehydrating agent is selected from toluene.

[0022] According to an embodiment of the present invention, before the polymerization reaction, the temperature is first raised to 130 - 180 °C and maintained for 2 - 4 h to remove the water in the reaction.

[0023] According to an embodiment of the present invention, the temperature of the polymerization reaction is 200 - 240 °C, and / or the time of the polymerization reaction is 8 - 13 h.

[0024] The present invention also provides an insulating material, which comprises a cured product, wherein the molecular weight distribution coefficient PD of the cured product is 2.3 - 3.5; the cured product is obtained by acid-treating the copolymer in the composition.

[0025] According to an embodiment of the present invention, the content of the organic solvent in the insulating material is not specifically limited, and those skilled in the art can understand that the insulating material basically does not contain an organic solvent.

[0026] According to an embodiment of the present invention, in the insulating material, the molecular weight distribution coefficient PD of the cured product refers to the ratio of the weight-average molecular weight to the number-average molecular weight, that is, Mw / Mn. Preferably, PD can be 2.4 - 3.5, for example, 2.4 - 3.3, and its examples can be 2.5, 2.6, 2.7, 2.8, 2.9, 3.0, 3.1, 3.2, or 3.3.

[0027] According to an embodiment of the present invention, the insulating material is obtained by removing the solvent from the composition and then acid-treating the copolymer.

[0028] According to an embodiment of the present invention, the acid treatment may include mixing an acid with the copolymer, the copolymer is cured to obtain the cured product, and then further washing with water and ethanol until neutral. Preferably, the acid treatment may include soaking the copolymer with an acid, the copolymer is cured to obtain the cured product, washing the cured product obtained after being soaked with acid with water and ethanol until neutral, and drying the cured product. As an example, the cured product obtained by curing after mixing with an acid is poured into distilled water for washing, dried, washed with ethanol 3 - 5 times, and then washed with distilled water 3 - 10 times and then dried.

[0029] According to an embodiment of the present invention, the acid is an inorganic acid, such as hydrochloric acid, sulfuric acid, and preferably hydrochloric acid.

[0030] According to an embodiment of the present invention, the concentration of the acid can be 0.5 mol / L - 12 mol / L, for example, 0.5 mol / L - 5 mol / L, such as, 1 mol / L - 2.5 mol / L, and preferably 1 mol / L - 2 mol / L. The examples of the concentration of the acid can be 0.5 mol / L, 1 mol / L, 1.5 mol / L, 2 mol / L, 2.5 mol / L, 3 mol / L, 3.5 mol / L, 4 mol / L, 4.5 mol / L, or 5 mol / L.

[0031] According to an embodiment of the present invention, the time of the acid treatment may be 0.5 to 12 hours, such as 1 to 8 hours, preferably 2 to 4 hours, and more preferably 3 hours. Examples of the time of the acid treatment may be 1.5, 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5 or 8 hours. It should be understood that the time of the acid treatment can be adjusted by those skilled in the art based on the disclosure of the present invention according to the concentration of the acid used, as long as a copolymer with the molecular weight distribution coefficient PD of the cured product described above can be obtained. For the same purpose, the amount of the acid can also be determined according to the amount of the cured product.

[0032] According to an embodiment of the present invention, the cured product contains a polyetheretherketone compound, and the polyetheretherketone compound is obtained by subjecting the copolymer to the above acid treatment.

[0033] The present invention also provides a method for preparing the insulating material, and the preparation method includes subjecting the copolymer to an acid treatment using an acid.

[0034] According to an embodiment of the present invention, the copolymer is provided by the composition.

[0035] According to an embodiment of the present invention, the preparation method includes the following steps:

[0036] (S2-1) Removing the organic solvent from the composition;

[0037] (S2-2) Subjecting the product of step (S2-1) to an acid treatment.

[0038] In the above method for preparing the insulating material, the acid treatment has the definition described above.

[0039] According to an embodiment of the present invention, the method for removing the organic solvent in step (S2-1) may be to volatilize or evaporate the organic solvent under heating or non-heating conditions.

[0040] According to an embodiment of the present invention, after removing the organic solvent in step (S2-1), a drying treatment may further be performed.

[0041] The present invention also provides a cable, including a conductor and the composition covering the outside of the conductor.

[0042] The present invention also provides a cable, including a conductor and the insulating material covering the outside of the conductor, such as including a conductor and an insulating material layer covering the outside of the conductor.

[0043] According to an embodiment of the present invention, the conductor is an electric wire or an electromagnetic wire.

[0044] According to an embodiment of the present invention, the conductor may be a metal wire (for example, copper).

[0045] According to an embodiment of the present invention, the cross-sectional shape of the conductor may be any shape known in the art, such as selected from a circle, an ellipse, a rectangle, a rectangle with rounded corners, a square with rounded corners, etc.

[0046] According to an embodiment of the present invention, the thickness of the insulating material layer covering the outside of the conductor may be 0.1 to 300 μm, for example, 1 to 100 μm, such as 5 - 60 μm, and examples thereof are 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 56 μm, 57 μm, 58 μm, 59 μm or 60 μm.

[0047] According to an embodiment of the present invention, an adhesive, such as an adhesive layer, may also be included between the conductor and the insulating material layer.

[0048] According to an embodiment of the present invention, other insulating materials, such as other insulating material layers, may also be included between the conductor and the insulating material layer.

[0049] It should be understood that when an adhesive layer and / or other insulating material layers are included between the conductor and the insulating material layer, the insulating layer may form a composite insulating layer with the adhesive layer and / or other insulating material layers.

[0050] According to an embodiment of the present invention, the other insulating material layer may be selected from other insulating materials known in the art, such as polymers, for example, one or a mixture of two or more of polyimide (PI), polyamideimide (PAI), polyethyleneimine (PEI), etc.

[0051] According to an embodiment of the present invention, when the composition contains a filler (such as a wear-resistant filler), the insulating material layer contains: 50 - 100 parts of the cured product, and 0 - 50 parts of the wear-resistant filler.

[0052] According to an exemplary embodiment of the present invention, the insulating material layer contains: 70 - 100 parts of the cured product, 0 - 30 parts of talcum powder.

[0053] According to an exemplary embodiment of the present invention, the insulating material layer contains: 60 - 100 parts of the cured product, 0 - 20 parts of talcum powder, 1 - 10 parts of boron nitride.

[0054] According to an exemplary embodiment of the present invention, the insulating material layer contains: 70 - 100 parts of the cured product, 0 - 15 parts of talcum powder, 1 - 8 parts of boron nitride.

[0055] According to an exemplary embodiment of the present invention, the insulating material layer comprises: 88 parts of the cured product, 10 parts of talcum powder, and 2 parts of boron nitride.

[0056] The present invention also provides a method for preparing the above-mentioned cable, the method comprising: coating the above-mentioned composition on the outside of the conductor, and forming a coating layer after shaping; optionally, subjecting the coating layer to acid treatment to obtain the cable.

[0057] According to an embodiment of the present invention, the acid treatment has the definition described above.

[0058] According to an embodiment of the present invention, the shaping is to remove the organic solvent in the composition, and the specific operation can be carried out by using the method of the above-mentioned step (S2-1).

[0059] According to an embodiment of the present invention, after the coating layer is subjected to acid treatment, the copolymer in the coating layer forms the above-mentioned insulating material, that is, an insulating material layer is obtained.

[0060] According to an embodiment of the present invention, before the above-mentioned composition is coated on the outside of the conductor, the surface of the conductor may optionally further comprise other insulating materials, such as other insulating material layers.

[0061] The present invention also provides the use of the insulating material, which is used for insulating the conductor, especially for insulating the conductor in the fields of aerospace, electronic appliances, automobiles, energy, medical treatment, etc.

[0062] Beneficial effects

[0063] The inventors surprisingly found that the copolymer provided by the present invention has excellent solubility in organic solvents, greatly improving the convenience of directly coating the composition of the present invention on the conductor and preparing the insulating layer, significantly reducing the process difficulty, and a uniform-thickness insulating layer can be produced through single coating and acid treatment, solving the technical problem of uneven coating when directly using polyether ether ketone in the prior art, and significantly reducing the risk of defects caused by the extrusion thickness.

[0064] The insulating material of the present invention increases the bonding ability on the surface of the conductor (such as copper) through in-situ curing. Moreover, the insulating layer of the present invention is processed under low-temperature conditions, reducing the uneven stress caused by uneven temperature during the cooling of polyether ether ketone, resulting in the peeling off of the insulating layer.

[0065] In addition, the method of the present invention can be realized by using a traditional enameling machine, without incurring additional costs due to replacing the processing equipment. Description of the drawings

[0066] Figure 1 Two-layer structure diagram of the insulated wire.

[0067] Figure 2 Diagram of the three-layer structure of insulated wire.

[0068] Figure 3 Diagram of the multi-layer structure of insulated wire.

[0069] Figure 4 Schematic diagram of the U-bend test of an insulated wire.

[0070] Figure 5 Schematic diagram of a wire wrap test for an insulated wire.

[0071] Description of reference numerals:

[0072] 1. Conductor bare wire; 2. PEEK resin insulation layer; 3. Adhesive layer; 4. Second insulation layer; 5. First insulation layer. DETAILED DESCRIPTION

[0073] The technical scheme of the present invention will be further described in detail below in conjunction with specific embodiments. It should be understood that the following embodiments are only exemplary descriptions and explanations of the present invention and should not be construed as limiting the scope of protection of the present invention. All technologies implemented based on the above content of the present invention are included in the scope that the present invention is intended to protect.

[0074] Unless otherwise specified, the raw materials and reagents used in the following examples are commercially available or can be prepared by known methods.

[0075] The performance testing method of the present invention is as follows:

[0076] 1. Adhesion test

[0077] Take 300mm of the insulated wire obtained in the embodiment and the comparative example as a sample, place the sample between two clamps, place the sample and the clamp on the same axis, clamp both ends, stretch 20% at a rate of 300mm / min, and check the length of the sample paint film losing adhesion. In this test method, if the length of the paint film losing adhesion is less than 2mm, it means that the paint film has excellent adhesion.

[0078] 2. Bending processability test

[0079] U-bend test: Figure 4 As shown, two straight insulated wires with a length of 500 mm are taken and bent 180±2° around a polished test shaft core respectively. One is wound flat (shaft core diameter = 2 times wire thickness) and the other is wound vertically (shaft core diameter = 2 times wire width). Figure 3 In the figure, "B" and "D" represent the wire width and thickness of the insulated wire respectively.

[0080] In this test, after flat winding and vertical winding, if the surface of the product is smooth and free of cracks, it is recorded as "qualified"; if the surface has cracks, it is recorded as "unqualified".

[0081] 3. Coiling Test

[0082] As Figure 5 shown, take two insulated wires with a length of 500 mm in a straight line and wind coils around a polished test mandrel. The number of turns of the coil is 6. One is wound flat (mandrel diameter = 2 times the wire thickness), and the other is wound vertically (mandrel diameter = 2 times the wire width). And each single coil should be wound tightly and in contact with each other, with the maximum gap ≤ 2 mm.

[0083] In this test, after flat winding and vertical winding, if the surface of the product is smooth and free of cracks, it is recorded as "qualified"; if the surface has cracks, it is recorded as "unqualified".

[0084] 4. Test of Molecular Weight Distribution Coefficient:

[0085] Take 20 mg of PEEK (polyetheretherketone) sample and place it in a 10 ml vial. Use a pipette to add 3.15 ml of α-chloronaphthalene, and place it in an oscillator at 150 °C for 1.5 h. The sample is completely dissolved in α-chloronaphthalene. After cooling, add 4.20 ml of 1,2,4-trichlorobenzene to the vial, shake well, take 2 ml of the sample from the vial with a filtered pipette and add it to an ampoule, seal it with an aluminum cap, place the ampoule on the sample tray of a PL-220 gel permeation chromatograph (GPC), at a column temperature of 115 °C, with a mobile phase flow rate of 1 ml / min, an injection volume of 200 μl, and under the conditions of taking k value as 14.1 and Alpha value as 0.7, measure the molecular weight distribution coefficient of the sample.

[0086] 5. Test of Tensile Strength:

[0087] After injection molding into standard test specimens by an injection molding machine, use a Shimadzu AG-Xplus universal testing machine to detect the tensile strength of the samples according to the standard of ISO 527. Test method: First, cut the samples injection molded into standard test specimens by an injection molding machine into sample strips with a size of 50 × 4 mm using a mold, fix both ends of the samples on the tensile mold of the universal testing machine, with a tensile speed of 2 mm / min, and repeat the test three times for each sample and take the average value.

[0088] 6. Friction and Wear Test

[0089] Carry out friction and wear tests on PEEK composite materials according to the national standard GB / T3960-2016. Use a 45# steel ring (radius 20 mm, hardness HRC48 - 50, surface roughness Ra of the outer circle not greater than 0.4) as the counter-material, and calculate the friction coefficient (μ) through the following formula: μ = M / r·Fn

[0090] Wherein: M represents the frictional torque (N·mm), r represents the radius of the steel ring (mm), and Fn is the load applied to the specimen (N).

[0091] Preparation Example 1

[0092] Synthesis process of N-phenyl(4,4'-difluorobenzophenone)amine: 21.82 g (0.10 mol) of difluorobenzophenone, 13.70 mL (0.15 mol) of aniline, and 50.00 g of molecular sieve 80 mL of toluene was charged into a 250 mL three-necked round-bottom flask equipped with an argon inlet / outlet, a water separator, a mechanical stirrer, and a reflux condenser. The above reaction was heated at 160 °C for 24 h and then cooled to room temperature. After filtering off the molecular sieve, the mixture was evaporated using a rotary evaporator to obtain a crude product. The crude product was recrystallized from methanol three times to obtain yellow N-phenyl(4,4'-difluorobenzophenone)amine monomer.

[0093] Example 1:

[0094] (1) Preparation of polyetheretherketone intermediate (copolymer)

[0095] In a three-necked flask equipped with a stirrer, a thermometer and a high-purity nitrogen inlet were connected to one side port through a three-way joint, and a spherical condenser was connected to the other side port for exhaust. The three-necked flask was placed in an electric heating mantle, and 60.0 mL of toluene, 99.0 mL of sulfolane, 11.0 g (0.1 mol) of hydroquinone, 26.4 g (0.09 mol) of N-phenyl(4,4'-difluorobenzophenone)amine, 13.8 g (0.1 mol) of potassium carbonate, and 2.12 g (0.02 mol) of sodium carbonate were added to the flask. High-purity nitrogen was introduced at a flow rate of 100 mL / min. Under continuous stirring (stirring rate: 80 rpm), the temperature was raised to 150 °C and maintained for 3 h to remove the water in the reaction. Subsequently, the temperature was raised to 220 °C and maintained for 11 h to finally obtain a viscous light green liquid of polyetheretherketone intermediate.

[0096] Finally, the light green liquid was poured into distilled water and continuously stirred to form fibrous solids. The obtained solids were crushed and washed with distilled water five times at room temperature to obtain a light green polyetheretherketone intermediate for use after drying.

[0097] (2) After the polyetheretherketone intermediate was dried, it was soaked in hydrochloric acid at different concentrations for a certain period of time to convert the polyetheretherketone intermediate into polyetheretherketone PEEK (i.e., the cured product). Subsequently, it was washed five times with distilled water to remove hydrochloric acid. The corresponding polyetheretherketone samples were denoted as A1 - A5 respectively.

[0098] Table 1

[0099] Example 1 Concentration of hydrochloric acid (mol / l) Immersion time of polyetheretherketone intermediate state in hydrochloric acid (h) A1 0.5 7 A2 1 4 A3 1.5 5 A4 1.5 3.5 A5 1.5 2 A6 2 3.2 A7 2.5 2.8

[0100] Comparative Example 1

[0101] In a three-necked flask equipped with a stirrer, one side is connected to a three-way connection for placing a thermometer and a high-purity nitrogen inlet, and the other side is connected to a spherical condenser for exhaust. The three-necked flask is placed in an electric heating mantle, 550.00 g of diphenyl sulfone, 98.19 g of 4,4'-difluorobenzophenone, and 49.55 g of hydroquinone are added into the flask, and high-purity nitrogen at a flow rate of 100 ml / min is introduced. Under continuous stirring (stirring rate: 80 rpm), the temperature is raised to 160 degrees Celsius, 47.70 g of Na2CO3 powder is slowly added, and the reaction is continued at this temperature for 30 minutes, the temperature is raised to 200 degrees Celsius, and the temperature is maintained for 1 hour, and the temperature is raised to 310 degrees Celsius for 2 hours, and the material is poured into cold distilled water to obtain a blocky loose material.

[0102] After the loose block material was crushed into the required powder by a pounder, it was refluxed and boiled with a large excess of ethanol for 2 hours, and then the ethanol was poured out, pure water was added and refluxed and boiled for 1 hour, and this was repeated 5 times to remove the diphenyl sulfone solvent and inorganic salt in the system. The sample was placed in a vacuum drying oven, evacuated and heated to 120 degrees Celsius for 12 hours to obtain a pure polyetheretherketone (PEEK) sample C1.

[0103] Testing the properties of prepared PEEK

[0104] The molecular weight distribution coefficient and tensile strength of polyetheretherketone A1-A7 prepared in Example 1 and polyetheretherketone C1 produced by conventional polymerization in Comparative Example 1 were tested respectively, and the test results are as follows:

[0105] Table 2

[0106] Polyetheretherketone Molecular weight distribution coefficient PD Tensile strength Ts (MPa) A1 2.215 85 A2 2.437 89 A3 2.376 88 A4 2.424 96 A5 3.155 90 A6 2.569 95 A7 3.076 92 C1 2.341 94

[0107] It can be seen from Table 2 that when preparing polyetheretherketone in Example 1:

[0108] 1) With the increase of immersion time in hydrochloric acid, the molecular weight distribution coefficient PD shows a trend of gradually decreasing. This is because during the immersion process, small molecular weight polymers will gradually precipitate with the increase of immersion time, and the molecular weight distribution coefficient will become smaller.

[0109] 2) When low concentration hydrochloric acid (e.g., concentration less than 1.5 mol / l) is used for immersion, the molecular chains in the polymer will be excessively rearranged due to the long immersion time, thus affecting its tensile strength. Therefore, increasing the hydrochloric acid concentration and reducing the immersion time can improve the tensile strength of polyetheretherketone. However, when the immersion time is too short (e.g., less than 2 hours), the intermediate state of polyetheretherketone has not been completely converted into polyetheretherketone, so too short an immersion time has a certain impact on the tensile strength.

[0110] It can be seen from the comparison of Samples A2 - A7 and C1 that the polyetheretherketone obtained by converting the polyetheretherketone intermediate state using the method of the present invention has a molecular weight distribution coefficient and a tensile strength that are almost the same as those of conventionally commercially available polyetheretherketone.

[0111] Example 2:

[0112] Prepare an electromagnetic wire with a PEEK insulating layer as Figure 1 shown:

[0113] (1) Dissolve the polyetheretherketone intermediate prepared in A4 of Example 1 in NMP to form insulating layer coatings (i.e., compositions) B1 - B5 with different solid contents. The specific solid contents and viscosities at room temperature are shown in Table 3, and let it stand for defoaming; (2) Take the above-mentioned insulating layer coatings B1 - B5 respectively, and use a vertical enameling machine to coat the insulating layer coating on the outside of the bare conductor 1 (copper wire). During the coating process, the organic solvents in the insulating layer coating volatilize, and the insulating layer coating cures to form a 30 - μm - thick coating covering the bare conductor 1.

[0114] After the coating is dried, soak it in 1.5 mol / l hydrochloric acid for 3.5 h to convert the polyetheretherketone intermediate into PEEK, forming a PEEK resin insulating layer 2, as Figure 1 shown. Then wash the residual hydrochloric acid on the surface of the electromagnetic wire with distilled water and dry it.

[0115] Table 3

[0116] Insulating layer coating Solid content (%) Viscosity (cp) B1 20 2503 B2 25 2649 B3 30 2779 B4 35 3198 B5 40 3732

[0117] Comparative Example 2

[0118] Add the polyetheretherketone resin material C1 prepared in Comparative Example 1 into the barrel of the screw extruder. At a temperature of 380°C - 410°C, heat the PEEK resin material to the molten state, and then through the rotation of the screw of the screw extruder, make the PEEK resin material flow uniformly in the barrel. Place the pre - heated bare conductor 1 in front of the head of the screw extruder, and at the head, use different - sized molds to uniformly wrap the PEEK resin material on the surface of the bare conductor 1. After cooling and crystallization, a 30 - μm - thick polyetheretherketone insulating layer 2 is formed. This sample is marked as C2.

[0119] Conduct adhesion test, U - shaped bending test and winding test on the insulated wires prepared in Example 2 and Comparative Example 2. The test results are shown in Table 4 below.

[0120] Table 4

[0121]

[0122]

[0123] It can be seen from Table 4 that:

[0124] 1) It can be seen from the adhesion test that the insulated wires prepared in Example 2 all have relatively excellent adhesion properties, while the insulated wires prepared in Comparative Example 2 had a relatively large peel length during the stretching process. Thus, it can be known that when using the polyether ether ketone intermediate state obtained by the method of the present invention to prepare insulated wires, the adhesion property of polyether ether ketone is better than that of Comparative Example 2.

[0125] 2) Although when the solid content of the insulating layer coating is low (less than 30%), a small amount of defects will occur on the insulating layer of the insulated wire surface, resulting in a small number of cracks during the winding test, causing the product to be unqualified; when the solid content of the insulating layer coating is increased to more than 30%, this problem can be improved. However, for the insulated wire obtained by directly coating the commercially available polyether ether ketone in Comparative Example 2, it can only pass the U-shaped bending test and is unqualified in the winding test.

[0126] To ensure the thickness uniformity of the insulating layer prepared in Example 2, the insulating layers of the insulated wires prepared in Example 2 and Comparative Example 2 were respectively tested: the insulating layers of the insulated wires in Example 2 and Comparative Example 2 were respectively peeled off, the maximum and minimum values of the thickness on the insulating layer were measured, and the ratio of the maximum value / minimum value was calculated. A ratio between 1 and 1.1 was considered qualified, otherwise it was unqualified. The test results are shown in Table 5 below:

[0127] Table 5

[0128] Insulating layer Judgment (qualified / unqualified) B4 Qualified C2 Unqualified

[0129] Example 3

[0130] Prepare an electromagnetic wire with a PEEK insulating layer as Figure 1 shown:

[0131] This example refers to the preparation method of Example 2, except that: an insulating layer coating with a solid content of 35% and a viscosity of 3198 cp was used, and a 45-μm-thick coating covering the bare conductor 1 was cured; the remaining steps were the same as in Example 2, and this sample was labeled B6.

[0132] Insulating layer coating Solid content (%) Viscosity (cp) B6 35 3198

[0133] Comparative Example 3

[0134] (1) Dissolve the polyamide-imide resin in an organic solvent, heat and stir to dissolve it, and then add the organic solvent NMP again to adjust the viscosity to 3100 cp to obtain an adhesive. Use an enameling machine to coat the adhesive on the outside of the bare wire 1. During the coating process, the organic solvent in the adhesive volatilizes, and the adhesive cures to form an adhesive layer 3 covering the bare wire 1, and the thickness of the adhesive layer 3 is 15 μm to obtain a core wire;

[0135] (2) Add the polyetheretherketone resin material prepared in Comparative Example 1 into the barrel of the screw extruder. At a temperature of 380°C - 410°C, heat the PEEK resin material to the molten state. Then, through the rotation of the screw of the screw extruder, make the PEEK resin material flow uniformly in the barrel. Place the preheated core wire in front of the head of the screw extruder. At the head, through different specifications of molds, the PEEK resin material is uniformly wrapped on the surface of the core wire in step (1). After cooling and crystallization, a 30-μm polyetheretherketone insulating layer 2 is formed. The structure is as Figure 2 shown, and this sample is marked as C3.

[0136] Table 6

[0137]

[0138] As can be seen from Table 6, through testing, it is found that the adhesiveness, U-shaped bending test, and winding test of B6 and C3 are all qualified. This shows that all aspects of the performance of the single-layer insulated electromagnetic wire prepared by the method of the present invention are the same as those of the double-layer insulated electromagnetic wire with polyamideimide added as the bonding layer.

[0139] Example 4

[0140] The present invention can also prepare an electromagnetic wire with the structure as Figure 3 shown. The specific steps refer to Example 2, except that a first insulating layer 5 and a second insulating layer 4 are sequentially coated on the outside of the bare conductor 1 (copper wire). Among them, the materials used for the first insulating layer 5 and the second insulating layer 4 can be the same or different, and are independently selected from the bonding layer of polyimide, the polyamideimide bonding layer, the polyetherimide bonding layer, and the polyetheretherketone insulating layer.

[0141] Example 5

[0142] Disperse talcum powder with a particle size of 5 microns evenly in NMP by ultrasonic treatment to form a suspension;

[0143] And dissolve the polyetheretherketone intermediate state A4 prepared in Example 1 in the above suspension to form different insulating layer coatings E1 - E3. The solid content and viscosity at room temperature are specifically shown in Table 7. The mass ratio of the polyetheretherketone intermediate state A4 to the filler talcum powder in different insulating layer coatings is shown in Table 7; let it stand for defoaming, and use a vertical enameling machine to coat the insulating layer coating on the outside of the bare conductor 1. During the coating process, the organic solvent in the insulating layer coating volatilizes, and the insulating layer coating cures to form a 30-μm thick coating covering the bare conductor 1;

[0144] After the coating is dried, soak it in 1.5 mol / l hydrochloric acid for 3.5 h to convert the polyetheretherketone intermediate state into PEEK, forming a PEEK resin insulating layer 2. Then, wash the residual hydrochloric acid on the surface of the electromagnetic wire with distilled water and dry it. The obtained samples are respectively marked as E1, E2, and E3.

[0145] The insulating wire prepared in Example 5 was subjected to friction coefficient, adhesion, U-bend test and winding test, and the test results are shown in Table 7 below.

[0146] Table 7

[0147]

[0148] As can be seen from Table 7, the insulating layer coating after adding the wear-resistant filler talcum powder still has excellent adhesion properties for the prepared insulating wire, and when a certain amount of wear-resistant filler is added, the friction coefficient of the insulating wire is also increased.

[0149] The exemplary embodiments of the present invention have been described above. However, the protection scope of this application is not limited to the above embodiments. Any modifications, equivalent replacements, improvements, etc. made by those skilled in the art within the spirit and principles of the present invention shall be included within the protection scope of the present invention.

Claims

1. A composition, characterized in that The composition comprises a copolymer and an organic solvent, wherein the copolymer is a copolymer of N-phenyl(4,4′-difluorodiphenyl)ketoneamine and hydroquinone.

2. The composition according to claim 1, characterized in that The organic solvent is selected from at least one of N-methylpyrrolidone, tetrahydrofuran, N,N-dimethylformamide, N,N-dimethylacetamide (DMA) or a mixture of two or more thereof; and / or, the weight ratio of the copolymer to the organic solvent in the composition is 1:1 to 1:9; And / or, the solid content of the composition is 10wt% to 50wt%; and / or, the composition further comprises a wear-resistant filler; And / or, the wear-resistant filler is selected from at least one or more of the following materials: whisker silicon, alumina, nano silicon dioxide, talc, mica, kaolin, montmorillonite, illite, boron nitride, titanium dioxide, zinc sulfide, zirconium dioxide, nano barium sulfate, graphite, nucleating agent, polytetrafluoroethylene, tin disulfide, molybdenum disulfide, silicone, graphene, potassium titanate; And / or, the mass ratio of the copolymer to the wear-resistant filler is 50:50 to 100:0; And / or, the viscosity of the composition at room temperature is 2500cp to 4000cp.

3. The method for preparing the composition according to claim 1 or 2, characterized in that: The preparation method includes mixing the copolymer with an organic solvent.

4. An insulating material, characterized in that: The insulating material comprises a cured product, wherein the molecular weight distribution coefficient PD of the cured product is 2.3 to 3.5; the cured product is obtained by subjecting the copolymer in the composition to acid treatment.

5. The insulating material according to claim 4, characterized in that In the insulating material, the molecular weight distribution coefficient PD of the cured product is 2.4 to 3.5; And / or, the insulating material is obtained by removing the solvent from the composition and then subjecting the copolymer to acid treatment; And / or, the acid treatment comprises mixing an acid with the copolymer, curing the copolymer to obtain the solidified product, and further washing with water and ethanol to neutrality; and / or, the acid is an inorganic acid; and / or, the concentration of the acid is 0.5 mol / L to 12 mol / L; And / or, the acid treatment time is 0.5 to 12 hours.

6. The method for preparing the insulating material according to claim 4 or 5, characterized in that: The preparation method includes subjecting the copolymer to an acid treatment using an acid.

7. A cable, characterized in that: The cable comprises a conductor and the composition according to claim 1 or 2 covering the outside of the conductor.

8. A cable, characterized in that: The cable comprises a conductor and the insulating material according to claim 4 or 5 covering the outside of the conductor.

9. A method for preparing the cable according to claim 7 or 8, characterized in that: The method comprises: coating the composition according to claim 2 on the outside of a conductor to form a coating after shaping; and optionally subjecting the coating to an acid treatment to obtain the cable.

10. Use of the insulating material according to claim 4 or 5 in the insulation of a conductor.

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