Resin composition, method for producing resin composition, composite material, method for producing composite material, and molded body
By integrating aromatic polyether with phosphorus and specific metal elements, along with inorganic metal phosphates and nucleating agents, the resin composition achieves both thermal stability during melting and high-temperature durability, addressing the limitations of conventional PEEK compositions.
Patent Information
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2025-08-20
- Publication Date
- 2026-03-05
AI Technical Summary
Conventional resin compositions, such as those containing polyether ether ketone (PEEK) with additives like sodium dihydrogen orthophosphate and disodium hydrogen phosphate, fail to achieve both excellent thermal stability during melting and high-temperature durability of molded articles effectively.
Incorporating an aromatic polyether with specific components including phosphorus and three or more metal elements, such as sodium, lithium, and aluminum, along with inorganic metal phosphates and nucleating agents, to enhance thermal stability and high-temperature durability.
The resin composition exhibits improved thermal stability during melting and maintains high-temperature durability, preventing deterioration of molded articles under extreme conditions, thereby enhancing the reliability of the molded products.
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Abstract
Description
Resin composition, method for producing resin composition, composite material, method for producing composite material, and molded article
[0001] The present invention relates to a resin composition, a method for producing a resin composition, a composite material, a method for producing a composite material, and a molded article. Specifically, the present invention relates to a resin composition, a method for producing a resin composition, a composite material, a method for producing a composite material, and a molded article that have excellent thermal stability when melted and can improve the high-temperature durability of a molded article.
[0002] Aromatic polyethers have excellent heat resistance and mechanical strength, and because of these characteristics, they are used as metal replacement materials. In recent years, their applications have expanded to include automobiles, aircraft, and the medical field. In particular, polyether ether ketone (abbreviated as "PEEK"), a type of aromatic polyether, is known as a representative resin for engineering plastics. Patent Document 1 attempts to improve thermal stability by incorporating 0.10 to 0.35% by mass of sodium dihydrogen orthophosphate and 0.08 to 0.25% by weight of disodium hydrogen phosphate into PEEK.
[0003] GB Patent Application Publication No. 2536387
[0004] However, it has been found that there is room for further improvement in the conventional techniques including that of Patent Document 1 in terms of achieving both thermal stability during melting and high-temperature durability of the molded article.
[0005] One object of the present invention is to provide a resin composition that has excellent thermal stability when melted and can improve the high-temperature durability of a molded article, a method for producing a resin composition, a composite material, a method for producing a composite material, and a molded article.
[0006] As a result of extensive research, the present inventors have found that a resin composition containing an aromatic polyether and a specific component has excellent thermal stability when melted and can improve the high-temperature durability of a molded product, and have thus completed the present invention. According to the present invention, the following resin compositions and the like can be provided. 1. A resin composition containing an aromatic polyether, phosphorus, and three or more metal elements including sodium. 2. The resin composition according to 1, in which the three or more metal elements include two or more selected from the group consisting of alkaline earth metals and alkali metals. 3. The resin composition according to 1 or 2, in which the three or more metal elements include lithium. 4. The resin composition according to any one of 1 to 3, in which the three or more metal elements include aluminum. 5. The resin composition according to any one of 1 to 4, in which the three or more metal elements include sodium, aluminum, and lithium. 6. The content of the three or more metal elements relative to 100 parts by mass of the aromatic polyether is 1.0 x 10 -4 The resin composition according to any one of 1 to 5, comprising one or more metal elements in an amount of 0.01 to 5.0 parts by mass or more. 7. A resin composition comprising an aromatic polyether, one or more selected from the group consisting of inorganic metal phosphates and decomposition products thereof, and one or more selected from the group consisting of nucleating agents and decomposition products thereof. 8. The resin composition according to 7, wherein the total amount of the one or more selected from the group consisting of inorganic metal phosphates and decomposition products thereof is 0.01 to 5.0 parts by mass per 100 parts by mass of the aromatic polyether. 9. The resin composition according to 7 or 8, wherein the inorganic metal phosphate comprises an alkali metal. 10. The resin composition according to any one of 7 to 9, comprising two or more inorganic metal phosphates. 11. The resin composition according to any one of 7 to 10, wherein the total amount of the one or more selected from the group consisting of nucleating agents and decomposition products thereof is 0.01 to 5.0 parts by mass per 100 parts by mass of the aromatic polyether. 12. 13. The resin composition according to any one of 7 to 11, wherein the nucleating agent is at least one selected from the group consisting of organic nucleating agents and inorganic nucleating agents. 13. The aromatic polyether or the resin composition has a radical amount of 6.5 x 10 at 25°C, measured using TEMPOL as a standard substance and benzene as a solvent for the standard substance. 15~9.0 x 10 17 The resin composition according to any one of 1 to 12, wherein the aromatic polyether is polyarylene ether ketone. 14. The resin composition according to any one of 1 to 13, wherein the aromatic polyether is polyarylene ether ketone. 15. The resin composition according to any one of 1 to 14, wherein the aromatic polyether comprises one or more selected from the group consisting of polyether ether ketone (PEEK), polyether ketone ketone (PEKK), and polyether ketone (PEK). 16. The resin composition according to any one of 1 to 15, wherein the tensile elongation after exposure at 300°C for 100 hours is 10% or more. 17. A method for producing a resin composition, comprising a kneading step of kneading an inorganic metal phosphate and a nucleating agent with an aromatic polyether. 18. A composite material comprising reinforcing fibers and one or more selected from the group consisting of the resin composition according to any one of 1 to 16 and the resin composition obtained by the method for producing a resin composition according to 17. 19. The composite material according to 18, wherein the reinforcing fibers comprise one or more selected from the group consisting of carbon fibers, glass fibers, and aramid fibers. 20. A method for producing a composite material, comprising compounding one or more selected from the group consisting of the resin composition according to any one of 1 to 16, and the resin composition obtained by the method for producing a resin composition according to 17, with reinforcing fibers. 21. The method for producing a composite material according to 20, wherein the reinforcing fibers include one or more selected from the group consisting of carbon fibers, glass fibers, and aramid fibers. 22. A molded product obtained by molding one or more selected from the group consisting of the resin composition according to any one of 1 to 16, the resin composition obtained by the method for producing a resin composition according to 17, the composite material according to 18 or 19, and the composite material obtained by the method for producing a composite material according to 20 or 21.
[0007] According to the present invention, it is possible to provide a resin composition that has excellent thermal stability when melted and can improve the high-temperature durability of a molded article, a method for producing a resin composition, a composite material, a method for producing a composite material, and a molded article.
[0008] The resin composition, method for producing the resin composition, composite material, method for producing the composite material, and molded article of the present invention are described in detail below. In this specification, "x to y" represents a numerical range of "x or more and y or less." The upper and lower limits of the numerical ranges can be combined arbitrarily. Furthermore, among the individual embodiments of the aspects of the present invention described below, two or more embodiments that are not mutually exclusive can be combined, and an embodiment combining two or more embodiments is also an embodiment of the aspects of the present invention.
[0009] 1. Resin Composition (1) First Aspect The resin composition according to the first aspect of the present invention contains an aromatic polyether, phosphorus, and three or more metal elements including sodium. The resin composition of this aspect exhibits excellent thermal stability during melting and can improve the high-temperature durability of molded articles. "Thermal stability during melting" refers to the stability of the resin structure during molding (during molten retention) under nitrogen. "High-temperature durability" refers to the stability of the physical properties of molded articles exposed to high temperatures in air. For example, even after a molded article is exposed to high temperatures in air for a certain period of time, the strength in tensile tests does not decrease and the molded article exhibits excellent elongation. In conventional resin compositions, it has been thought that the presence of one metal species with nucleating properties is sufficient to form a crystal interface during solidification from a molten state. However, it has been found that when solidified molded articles are exposed to high temperatures, the growth of fine crystals tends to make the articles hard and brittle. In contrast, in this aspect, the inclusion of three or more metal elements including phosphorus and sodium is presumed to inhibit the growth of fine crystals when solidified molded articles are exposed to high temperatures, thereby maintaining toughness. According to this embodiment, in particular, by achieving both thermal stability during melting and high-temperature durability of the molded body, it is possible to prevent deterioration of the resin composition (aromatic polyether) during molding, and also to prevent deterioration of the resin composition (aromatic polyether) when the molded body is used at high temperatures after molding. These effects work synergistically to significantly improve the reliability of the molded body. It was difficult to achieve both thermal stability during melting and high-temperature durability of the molded body in this way with conventional technology.
[0010] In one embodiment, the resin composition includes two or more metal elements selected from the group consisting of alkaline earth metals and alkali metals. Examples of alkaline earth metals include beryllium, magnesium, calcium, strontium, barium, and radium. Examples of alkali metals include lithium, sodium, potassium, rubidium, cesium, and francium. In one embodiment, the resin composition includes one or more metal elements, two or more metal elements, or three or more metal elements selected from the group consisting of alkali metals. In one embodiment, the resin composition includes lithium as the three or more metal elements. In one embodiment, the resin composition includes aluminum as the three or more metal elements. In one embodiment, the resin composition includes potassium as the three or more metal elements. In one embodiment, the resin composition includes sodium, aluminum, and lithium as the three or more metal elements. In one embodiment, the resin composition includes sodium, aluminum, lithium, and potassium as the three or more metal elements. In one embodiment, the resin composition includes four or more metal elements.
[0011] In one embodiment, the resin composition has a content of the three or more metal elements relative to 100 parts by mass of the aromatic polyether of 1.0 × 10 -4 Parts by mass or more, 5.0 x 10 -4 Parts by mass or more, 1.0×10 -3 Parts by mass or more, 1.5 x 10 -3 Parts by mass or more, 2.0×10 -3 parts by mass or more or 2.5 x 10 -3 The resin composition may contain one or more, two or more, or three or more metal elements each having a content of at least 5.0 × 10 parts by mass. -1 In one embodiment, the resin composition may have a content of the three or more metal elements of 1.0 × 10 or less relative to 100 parts by mass of the aromatic polyether. -4 Parts by mass ~5.0×10 -1 Parts by mass, 5.0×10 -4 Parts by mass ~5.0×10-1 Parts by mass, 1.0×10 -3 Parts by mass ~5.0×10 -1 Parts by mass, 1.5 x 10 -3 Parts by mass ~5.0×10 -1 Parts by mass, 2.0×10 -3 Parts by mass ~5.0×10 -1 parts by mass or 2.5 x 10 -3 Parts by mass ~5.0×10 -1 The metal element may include one or more, two or more, or three or more metal elements in an amount of parts by mass.
[0012] In one embodiment, the content of sodium in the resin composition is preferably 1.0 × 10 relative to 100 parts by mass of the aromatic polyether. -4 Parts by mass ~5.0×10 -1 parts by mass, and from the viewpoint of moldability, more preferably 5.0 × 10 -3 Parts by mass ~ 1.5 x 10 -1 From the viewpoint of achieving both moldability and elongation during tensile testing, it is most preferably 1.0 × 10 -2 Parts by mass ~ 1.1×10 -1 In one embodiment, when the resin composition contains lithium as the three or more metal elements, the content thereof relative to 100 parts by mass of the aromatic polyether is preferably 1.0 × 10 -4 Parts by mass ~2.5×10 -2 parts by mass, and from the viewpoint of moldability, more preferably 1.5 × 10 -3 Parts by mass ~ 1.0×10 -2 parts by mass, and from the viewpoint of physical properties after exposure, it is most preferably 2.0 × 10 -3 Parts by mass ~7.0×10 -3 In one embodiment, when the resin composition contains aluminum as the three or more metal elements, the content thereof relative to 100 parts by mass of the aromatic polyether is preferably 1.0 × 10 -4 Parts by mass ~2.5×10 -2 parts by mass, and from the viewpoint of moldability, more preferably 3.0 × 10 -3 Parts by mass ~ 1.0×10 -2 From the viewpoint of achieving both moldability and elongation during tensile testing, it is most preferably 4.0 × 10 -3Parts by mass ~7.0×10 -3 In one embodiment, when the resin composition contains potassium as the three or more metal elements, the content thereof relative to 100 parts by mass of the aromatic polyether is preferably 1.0 × 10 -4 Parts by mass ~ 1.0×10 -1 It is 1.0 × 10 parts by mass from the viewpoint of molding processability. -4 Parts by mass ~ 3.0 x 10 -2 From the viewpoint of achieving both moldability and elongation during tensile testing, it is most preferably 5.0 × 10 -4 Parts by mass ~ 1.1×10 -2 Parts by mass.
[0013] In one embodiment, the total content of metal elements relative to 100 parts by mass of aromatic polyether is 3.0 × 10 -4 Mass parts ~ 6.5×10 -1 Parts by mass, 1.0×10 -3 Parts by mass ~5.0×10 -1 Parts by mass, 1.5 x 10 -3 Parts by mass ~ 3.0 x 10 -1 Parts by mass, 2.0×10 -3 Parts by mass ~ 1.5 x 10 -1 Parts by mass, 3.0×10 -3 Parts by mass ~ 1.2 x 10 -1 Parts by mass, 4.0×10 -3 Parts by mass ~ 1.2 x 10 -1 Parts by mass, 5.0×10 -3 Parts by mass ~ 1.2 x 10 -1 Parts by mass or 1.0 x 10 -2 Parts by mass ~ 1.2 x 10 -1 The total content is 3.0 × 10 -4 When the total content is 6.5×10 or more parts by mass, the above-mentioned high-temperature durability effect and the like are more satisfactorily exhibited, the strength in the tensile test after exposure is not reduced, and the effect of exhibiting excellent elongation is more satisfactorily exhibited. -1 When the content is 100 parts by mass or less, the high temperature durability is better exhibited and the molded article exhibits better physical properties.
[0014] In one embodiment, the content of phosphorus element relative to 100 parts by mass of aromatic polyether is preferably 1.0×10-4 Parts by mass ~5.0×10 -1 parts by mass, and from the viewpoint of moldability, more preferably 5.0 × 10 -3 Parts by mass ~ 1.5 x 10 -1 From the viewpoint of achieving both moldability and elongation during tensile testing, it is most preferably 1.0 × 10 -2 Parts by mass ~ 1.2 x 10 -1 The phosphorus content is 1.0 × 10 -4 When the phosphorus content is 5.0×10 or more parts by mass, the effect of high temperature durability described above is more satisfactorily exhibited, the strength in the tensile test after exposure is not reduced, and the effect of exhibiting excellent elongation is more satisfactorily exhibited. -1 When the content is 100 parts by mass or less, the high temperature durability is improved and the molded article exhibits better physical properties.
[0015] In the above description, regarding the content of each metal element, the total content of metal elements, and the content of phosphorus element, the "content per 100 parts by mass of aromatic polyether" A (parts by mass) is calculated by multiplying the "concentration in the resin composition" A by 10 4 It may also be applied as ppm.
[0016] The content of each element in the above description is a value determined by elemental analysis described in Examples. The form of each element (phosphorus element, metal element) described above in the composition is not particularly limited, and each element may be contained as a simple substance or as part of a compound.
[0017] In one embodiment, the resin composition comprises 50% by mass or more, 60% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more, 95% by mass or more, 97% by mass or more, 98% by mass or more, or 99% by mass or more of the aromatic polyether. The upper limit of the content of the aromatic polyether in the resin composition is not particularly limited, and is, for example, less than 100% by mass, 99.999% by mass or less, or 99.99% by mass or less. In one embodiment, the resin composition comprises 50% by mass or more, 60% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more, 95% by mass or more, 97% by mass or more, 98% by mass or more, 99% by mass or more, or substantially 100% by mass of the aromatic polyether, phosphorus element, and the three or more metal elements. Note that "substantially 100% by mass" may contain inevitable impurities.
[0018] In one embodiment, the resin composition has a tensile elongation of 10% or more after exposure for 100 hours at 300° C. The tensile elongation is a value measured by the method described in the examples.
[0019] (2) Second Aspect The resin composition according to the second aspect of the present invention comprises an aromatic polyether, one or more selected from the group consisting of inorganic metal phosphates and their decomposition products, and one or more selected from the group consisting of nucleating agents and their decomposition products. The resin composition of this aspect exhibits excellent thermal stability during melting and can improve the high-temperature durability of molded articles.
[0020] <Inorganic Metal Phosphate> In one embodiment, the total amount of one or more selected from the group consisting of inorganic metal phosphates and decomposition products thereof is preferably 0.01 to 5 parts by mass, more preferably 0.05 to 3 parts by mass from the viewpoint of thermal stability, even more preferably 0.1 to 2 parts by mass from the viewpoint of moldability, and most preferably 0.2 to 1 part by mass from the viewpoint of achieving both moldability and elongation in tensile testing. Note that the "total amount of one or more selected from the group consisting of inorganic metal phosphates and decomposition products thereof" is determined from the blend amount (charge amount) of the inorganic metal phosphate in the composition.
[0021] In one embodiment, the inorganic metal phosphate is LiPO 4 , Na2 HPO 4 、NaH 2 PO 4 、NaH 2 PO 2 、Na 3 PO 4 、Na 4 P 2 O 7 、Na 2 H 2 P 2 O 7 、Na 5 P 3 O 10 、Na 6 P 4 O 13 、K 2 P 2 O 7 、CaHPO 4 、Ca(H 2 PO 4 ) 2 、CaHPO 4 、Ca 3 (PO 4 ) 2 、KH 2 PO 4 、K 2 HPO 4 、K 3 PO 4 、K 4 P 2 O 7 、K 5 P 3 O 10 、Mg 2 P 2 O 7 、Mg(H 2 PO 4 )、MgHPO 4 、Mg 3 (PO 4 ) 2 、Mg(PO 3 ) 2 、Al(H 2 PO 4 )、AlPO 4 、Al(PO 3 ) 3and hydrates thereof. Among these, inorganic metal phosphates containing alkali metals are preferred from the viewpoint of further improving the toughness, heat resistance, and moldability of the resin composition. In one embodiment, the resin composition contains two or more inorganic metal phosphates.
[0022] The "decomposition product" of the inorganic metal phosphate may be a substance produced by thermal decomposition of the inorganic metal phosphate.
[0023] <Nucleating Agent> In one embodiment, the total amount of one or more selected from the group consisting of nucleating agents and decomposition products thereof is preferably 0.01 to 5 parts by mass, more preferably 0.05 to 3 parts by mass from the viewpoint of moldability, even more preferably 0.1 to 2 parts by mass from the viewpoint of thermal stability, and most preferably 0.2 to 1 part by mass from the viewpoint of achieving both thermal stability and elongation in tensile evaluation, relative to 100 parts by mass of the aromatic polyether. Note that the "total amount of one or more selected from the group consisting of nucleating agents and decomposition products thereof" is determined from the blend amount (charge amount) of the nucleating agent in the composition.
[0024] In one embodiment, the nucleating agent is one or more selected from the group consisting of organic nucleating agents and inorganic nucleating agents.
[0025] Examples of organic nucleating agents include aliphatic monocarboxylic acids, metal salts of aliphatic monocarboxylic acids, and metal phosphate salts. Examples of aliphatic monocarboxylic acids include tridecylic acid, myristic acid, pentadecylic acid, palmitic acid, margaric acid, stearic acid, nonadecylic acid, arachidic acid, heneicosylic acid, behenic acid, tricosylic acid, and lignoceric acid. Examples of metals in metal salts of aliphatic monocarboxylic acids include lithium, sodium, magnesium, aluminum, calcium, gallium, strontium, and indium. Examples of metals in phosphate metal salts include lithium, sodium, magnesium, aluminum, calcium, gallium, strontium, and indium. Examples of phosphate acids include phosphorus-containing oxo acids. Examples of phosphate metal salts include phosphate ester metal salts. Examples of the phosphate metal salt include 2,4,8,10-Tetra(tert-butyl)-6-hydroxy-12H-dibenzo[d,g][1,3,2]dioxaphosphocin 6-oxide, sodium salt (available as "ADK STAB NA-11" manufactured by ADEKA Corporation), (Hydroxy aluminum bis(2,4,8,10-tetra-trans-butyl-6-hydroxy-12H-dibenzo[d,g][1.3.2]dioxaphosphocin-6-oxide)) (available as "ADK STAB NA-21" manufactured by ADEKA Corporation), and the like. These organic nucleating agents may be used alone or in combination of two or more.
[0026] Examples of inorganic nucleating agents include talc, clay, mica, silica, dolomite powder, quartz powder, diatomaceous earth, etc. These inorganic nucleating agents may be used alone or in combination of two or more.
[0027] The "decomposition product" of the nucleating agent may be a substance produced by thermal decomposition of the nucleating agent.
[0028] In one embodiment, 50% by mass or more, 60% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more, 95% by mass or more, 97% by mass or more, 98% by mass or more, 99% by mass or more, 99.5% by mass or more, 99.7% by mass or more, 99.9% by mass or more, or substantially 100% by mass of the resin composition is one or more selected from the group consisting of an aromatic polyether; an inorganic metal phosphate and decomposition products thereof; and one or more selected from the group consisting of a nucleating agent and decomposition products thereof, or is an aromatic polyether, an inorganic metal phosphate, and a nucleating agent. Note that "substantially 100% by mass" may contain inevitable impurities.
[0029] The resin composition according to the second aspect can be appropriately applied with the configuration described for the resin composition according to the first aspect. Furthermore, the resin composition according to the first aspect can be appropriately applied with the configuration described for the resin composition according to the second aspect. A part or all of the "three or more metal elements" in the resin composition according to the first aspect can be derived from "one or more elements selected from the group consisting of inorganic metal phosphates and decomposition products thereof, and one or more elements selected from the group consisting of nucleating agents and decomposition products thereof" in the resin composition according to the second aspect.
[0030] 2. Manufacturing Method of Resin Composition A manufacturing method of a resin composition according to one aspect of the present invention includes a kneading step of kneading an aromatic polyether with an inorganic metal phosphate and a nucleating agent. According to this aspect, a resin composition can be obtained that has improved thermal stability during melting and also has improved high-temperature durability of a molded article.
[0031] In one embodiment, in the kneading step, the inorganic metal phosphate is preferably used in an amount of 0.01 to 5 parts by mass relative to 100 parts by mass of the aromatic polyether, more preferably 0.05 to 3 parts by mass from the viewpoint of thermal stability, even more preferably 0.1 to 2 parts by mass from the viewpoint of moldability, and most preferably 0.2 to 1 part by mass from the viewpoint of achieving both moldability and elongation in a tensile test. In one embodiment, the inorganic metal phosphate contains an alkali metal. In one embodiment, two or more types of inorganic metal phosphate are used in combination. Note that the explanation given in "1. Resin composition" applies to the inorganic metal phosphate.
[0032] In one embodiment, the amount of the nucleating agent relative to 100 parts by mass of the aromatic polyether is preferably 0.01 to 5 parts by mass, more preferably 0.05 to 3 parts by mass from the viewpoint of moldability, even more preferably 0.1 to 2 parts by mass from the viewpoint of thermal stability, and most preferably 0.2 to 1 part by mass from the viewpoint of achieving both thermal stability and elongation in tensile testing. In one embodiment, the nucleating agent is one or more selected from the group consisting of organic nucleating agents and inorganic nucleating agents. Note that the explanation given in "1. Resin composition" is applicable to the nucleating agent.
[0033] The method for kneading the inorganic metal phosphate and the nucleating agent with the aromatic polyether is not particularly limited, and examples thereof include melt kneading using an extruder or the like. The inorganic metal phosphate and the nucleating agent may be side-fed into the aromatic polyether using a twin-screw kneader. In one embodiment, the inorganic metal phosphate and the nucleating agent are kneaded with the molten aromatic polyether.
[0034] The resin composition obtained by this embodiment can be appropriately applied with the configuration described for the resin composition according to the first embodiment and the configuration described for the resin composition according to the second embodiment.
[0035] 3. Other Preferred embodiments of the resin composition according to the first aspect of the present invention, the resin composition according to the second aspect of the present invention, and the aromatic polyether in the method for producing a resin composition according to one aspect of the present invention will be described below.
[0036] In one embodiment, the aromatic polyether has a radical content of 6.5×10 at 25° C., measured using TEMPOL as a standard and benzene as the solvent for the standard. 15 ~9.0 x 10 17 spin / g.
[0037] In this specification, unless otherwise specified, the "radical amount" of an aromatic polyether means the "radical amount per unit mass (unit: spin / g)" of the aromatic polyether. In this specification, unless otherwise specified, "TEMPOL" means "4-hydroxy-2,2,6,6-tetramethylpiperidine-1-oxyl."
[0038] In one embodiment, the radical content of the aromatic polyether is 6.5×10 15 spin / g or more, 7.0×10 15 spin / g or more, 8.0×10 15 spin / g or more, 8.9×10 15 spin / g or more, 1.0×10 16 spin / g or more, 2.0×10 16 spin / g or more, 3.0×10 16 spin / g or more, or 4.0 x 10 16 spin / g or more, and 17 spin / g or less, 5.0×10 17 spin / g or less, 4.0×10 17 spin / g, 3.7×10 17 spin / g or less, or 1.0 x 10 17 spin / g or less.
[0039] The amount of radicals in the aromatic polyether is 6.5 × 10 15 When the amount of radicals in the aromatic polyether is 9.0×10 or more, the effect of improving the interfacial shear strength with respect to the reinforcing fiber can be obtained when a composite material described later is formed. 17 When the viscosity is not more than spin / g, the thermal stability is improved and the molded article can exhibit good mechanical properties.
[0040] The amount of radicals in the aromatic polyether can be increased to the above-mentioned range, for example, by using a monomer containing a chlorine atom as a reactive group (e.g., 4,4′-dichlorobenzophenone) as a monomer when synthesizing (polymerizing) the aromatic polyether.
[0041] The radical amount of the aromatic polyether explained above can also be applied to the radical amount of the aromatic polyether during preparation of the resin composition (immediately before kneading, etc.).
[0042] Furthermore, the radical amount of the aromatic polyether described above can also be applied to the radical amount per unit mass of the resin composition. In other words, in one embodiment, the resin composition has a radical amount of 6.5 × 10 at 25°C, measured using TEMPOL as a standard substance and benzene as a solvent for the standard substance. 15 ~9.0 x 10 17 spin / g.
[0043] In one embodiment, the aromatic polyether is a polyarylene ether ketone. In one embodiment, the aromatic polyether comprises one or more selected from the group consisting of polyether ether ketone (PEEK), polyether ketone ketone (PEKK), and polyether ketone (PEK). In one embodiment, the aromatic polyether comprises polyether ether ketone (PEEK).
[0044] In one embodiment, 50% by mass or more, 60% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more, 95% by mass or more, 97% by mass or more, 99% by mass or more, 99.5% by mass or more, or substantially 100% by mass of the aromatic polyether is one or more selected from the group consisting of polyetheretherketone (PEEK), polyetherketoneketone (PEKK), and polyetherketone (PEK). In one embodiment, 50% by mass or more, 60% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more, 95% by mass or more, 97% by mass or more, 99% by mass or more, 99.5% by mass or more, or substantially 100% by mass of the aromatic polyether is polyetheretherketone (PEEK). Note that "substantially 100% by mass" may contain inevitable impurities.
[0045] In one embodiment, the aromatic polyether contains a structural unit represented by the following formula (1) and a structural unit represented by the following formula (2).
[0046] In one embodiment, the aromatic polyether comprises a structural unit represented by the following formula (3):
[0047] The structural unit represented by formula (3) is a bond between the structural unit represented by formula (1) and the structural unit represented by formula (2).
[0048] In one embodiment, the aromatic polyether does not contain any other structure other than the structural units represented by formula (1) and formula (2).
[0049] In one embodiment, the aromatic polyether contains a structure other than the structural units represented by formula (1) and formula (2) within a range that does not impair the effects of the present invention.
[0050] In one embodiment, 50% by mass or more, 60% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more, 95% by mass or more, 97% by mass or more, 99% by mass or more, 99.5% by mass or more, or substantially 100% by mass of the aromatic polyether is a structural unit represented by formula (1) and a structural unit represented by formula (2), or a repeating unit represented by formula (3). Note that when it is "substantially 100% by mass", it may contain inevitable impurities.
[0051] In one embodiment, in the aromatic polyether, the molar ratio of the structural unit represented by formula (1) to the structural unit represented by formula (2) (structural unit represented by formula (1) : structural unit represented by formula (2)) is 47.5:52.5 to 52.5:47.5, 48.0:52.0 to 52.0:48.0, 48.5:51.5 to 51.5:48.5, 49.0:51.0 to 51.0:49.0, or 49.5:50.5 to 50.5:49.5. The number of moles of the structural unit represented by formula (1) may be greater than, smaller than, or the same as the number of moles of the structural unit represented by formula (2).
[0052] The terminal structure of the main chain of the aromatic polyether is not particularly limited. In one embodiment, a structural unit represented by formula (1) is disposed at one or more ends of the main chain of the aromatic polyether. In this case, the terminal structure bonded to the structural unit may be a halogen atom. The halogen atom may be, for example, a chlorine atom (Cl) or a fluorine atom (F). In one embodiment, a structural unit represented by formula (2) is disposed at one or more ends of the main chain of the aromatic polyether. In this case, the terminal structure bonded to the structural unit may be, for example, a hydrogen atom (H) or the like (when the terminal structure is a hydrogen atom (H), a hydroxyl group is formed together with the oxygen atom (O) in the structural unit). The terminal structure of the aromatic polyether may be, for example, a structure in which the above-mentioned halogen atom or hydroxyl group is replaced with a hydrogen atom (H). The terminal structure may have a structure other than those exemplified above. For example, the terminal structure may have a structure derived from a reaction terminator.
[0053] An example of a method for producing the above-mentioned aromatic polyether (particularly PEEK whose radical amount satisfies the above-mentioned condition) will be described. This method involves reacting 4,4'-dichlorobenzophenone and hydroquinone in diphenyl sulfone in the presence of potassium carbonate, where the molar ratio of the 4,4'-dichlorobenzophenone to the hydroquinone is 0.990 to 1.025. This results in a radical amount of 6.5 x 10 15 It is possible to obtain aromatic polyethers having a molecular weight of at least 10 ...
[0054] [4,4'-Dichlorobenzophenone] 4,4'-Dichlorobenzophenone is a monomer for polymerizing aromatic polyethers and corresponds to the structural unit represented by the above formula (1). 4,4'-Dichlorobenzophenone can be easily synthesized and is also commercially available.
[0055] [Hydroquinone] Hydroquinone is a monomer for polymerizing aromatic polyethers and corresponds to the structural unit represented by the above formula (2). Hydroquinone can be easily synthesized and is also commercially available.
[0056] [Potassium Carbonate] Potassium carbonate preferably has a purity of 99% by mass or more and a water content of 0.01% by mass or less. Such potassium carbonate is also commercially available. Potassium carbonate may be of general-purpose reagent grade, general industrial grade, or fine particle grade. When potassium carbonate (or potassium derived from potassium carbonate) remains in the aromatic polyether, it may be considered as "three or more metal elements" in the resin composition described above. The average particle size (D 50 The average particle size (D) is preferably 1000 μm or less, 800 μm or less, 500 μm or less, 300 μm or less, 100 μm or less, or even 50 μm or less. 50 The lower limit of the average particle size (D 50 ) is a value measured by the following method. 50 Measurement method for particle size distribution] Using a CAMSIZER manufactured by Microtrac Bell Co., Ltd., particle size distribution is measured by a dry method. A sample (potassium carbonate) is dropped into the measurement section using a vibrating feeder, and the particles are photographed with a camera to measure the particle diameter. When processing the observed image, the average particle diameter (D 50 ) is calculated.
[0057] In one embodiment, a method for producing an aromatic polyether includes reacting 4,4'-dichlorobenzophenone and hydroquinone in diphenyl sulfone in the presence of potassium carbonate by stirring, and terminating the reaction when the solution viscosity reaches 242 cP or more converted at 300°C after adding a reaction terminator. Terminating the reaction specifically means stopping the stirring and removing the resulting reaction product. The solution viscosity is measured using a process viscometer (XL7-951-HT2-d28-E58, manufactured by Hydramotion Japan Co., Ltd.).
[0058] The solution viscosity at the end of the reaction can be, for example, the value measured in real time with a process viscometer when 4,4'-dichlorobenzophenone and hydroquinone are reacted in diphenyl sulfone in the presence of potassium carbonate, a reaction terminator is added, and the solution viscosity reaches 242 cP or more. Note that the solution viscosity during the reaction may be less than 242 cP.
[0059] In one embodiment, after the addition of the reaction quenching agent, the mixture is stirred while maintaining the temperature before the addition of the reaction quenching agent. In one embodiment, after the addition of the reaction quenching agent, the mixture is stirred while decreasing the temperature from the temperature before the addition of the reaction quenching agent.
[0060] The solution viscosity at the end of the reaction can be adjusted by the temperature conditions of the raw material mixture (maximum temperature, temperature holding time, etc.) and the "reaction concentration" (defined below) of the raw material mixture. In this specification, the maximum temperature during the reaction is the maximum temperature that the reaction mixture reaches from the start of the reaction of the raw material mixture to the completion of the reaction. The "reaction concentration" is defined by the following formula based on the number of moles of OH groups [mol] calculated from the total amount (blended amount) of phenolic monomers (e.g., hydroquinone) to be reacted (blended into the reaction mixture): Reaction concentration [mol / kg] = number of moles of OH groups [mol] / mass of solvent [kg]
[0061] 4. Composite Material and Method for Producing Composite Material A composite material according to one aspect of the present invention includes one or more selected from the group consisting of the resin composition according to one aspect of the present invention and a resin composition obtained by the method for producing a resin composition according to one aspect of the present invention, and reinforcing fibers. A method for producing a composite material according to one aspect of the present invention includes compounding one or more selected from the group consisting of the resin composition according to one aspect of the present invention and a resin composition obtained by the method for producing a resin composition according to one aspect of the present invention with reinforcing fibers. The composite materials according to these aspects have excellent thermal stability when the resin composition is melted, and can improve the high-temperature durability of a molded product.
[0062] In one embodiment, the content of the reinforcing fibers in the composite material is 0.01 parts by mass or more, 0.1 parts by mass or more, 1 part by mass or more, or 10 parts by mass or more, and 500 parts by mass or less, 300 parts by mass or less, 200 parts by mass or less, or 100 parts by mass or less, relative to 100 parts by mass of the resin composition.
[0063] In one embodiment, the reinforcing fibers include one or more selected from the group consisting of carbon fibers, glass fibers, and aramid fibers. In one embodiment, 50 mass% or more, 60 mass% or more, 70 mass% or more, 80 mass% or more, 90 mass% or more, 95 mass% or more, 97 mass% or more, 99 mass% or more, 99.5 mass% or more, or substantially 100 mass% of the reinforcing fibers are one or more selected from the group consisting of carbon fibers, glass fibers, and aramid fibers.
[0064] In one embodiment, the carbon fiber comprises one or more selected from the group consisting of PAN-based carbon fiber, pitch-based carbon fiber, thermosetting carbon fiber, phenolic carbon fiber, vapor-grown carbon fiber, and recycled carbon fiber (RCF). In one embodiment, 50 mass% or more, 60 mass% or more, 70 mass% or more, 80 mass% or more, 90 mass% or more, 95 mass% or more, 97 mass% or more, 99 mass% or more, 99.5 mass% or more, or substantially 100 mass% of the carbon fiber is one or more selected from the group consisting of PAN-based carbon fiber, pitch-based carbon fiber, thermosetting carbon fiber, phenolic carbon fiber, vapor-grown carbon fiber, and recycled carbon fiber (RCF).
[0065] The type of glass fiber or aramid fiber is not particularly limited, and glass fibers of various compositions, such as E-glass, low dielectric glass, and silica glass, can be selected and used depending on the purpose and application.
[0066] In one embodiment, the average fiber length of the reinforcing fibers in the composite material is 5 mm or more. When the average fiber length of the reinforcing fibers is 5 mm or more, the fibers are also called "continuous fibers." The average fiber length is determined by the arithmetic mean of values measured with a vernier caliper.
[0067] In one embodiment, at least 50%, at least 60%, at least 70%, at least 80%, at least 90%, at least 95%, at least 97%, at least 99%, at least 99.5%, or substantially 100% by weight of the composite material is the resin composition and reinforcing fibers.
[0068] The method for producing the composite material (composite method) is not particularly limited. For example, a method of melt-kneading a resin composition with reinforcing fibers, or a method of melting and impregnating an aggregate of reinforcing fibers with one or more resin compositions in a powder, film, or pellet form may be used. A twin-screw kneader may be used to side-feed the reinforcing fibers into the resin composition. The aggregate of reinforcing fibers may be in one or more forms selected from the group consisting of woven fabric, nonwoven fabric, and unidirectional material (also called "UD material"). In these forms, the average fiber length of the reinforcing fibers may be 5 mm or more. That is, the reinforcing fibers may be continuous fibers. This further improves the strength of the composite material.
[0069] Pellets of the composite material may be produced. The pellets can be used as a raw material for producing a molded body, which will be described later. In one embodiment, the method for producing pellets includes cutting reinforcing fibers short to form chopped strands, and then adding a resin composition to the reinforcing fibers. Pellets (also referred to as "short fiber pellets") can be produced by mixing the short fibers and the resin composition and granulating them. In one embodiment, the method for producing pellets involves immersing a roving of reinforcing fibers in a molten resin composition, pultrusion molding the mixture, and then cutting the roving into a desired pellet length to produce pellets (also referred to as "long fiber pellets"). When long fiber pellets are produced as described above, breakage of the reinforcing fibers can be suppressed.
[0070] 5. Molded Article A molded article according to one aspect of the present invention is obtained by molding one or more selected from the group consisting of the resin composition according to one aspect of the present invention, the resin composition obtained by the method for producing a resin composition according to one aspect of the present invention, the composite material according to one aspect of the present invention, and the composite material obtained by the method for producing a composite material according to one aspect of the present invention. The molded article according to these aspects can provide excellent thermal stability of the resin composition when melted, and can improve the high-temperature durability of the molded article.
[0071] The form of the molded article according to this embodiment is not particularly limited. In one embodiment, the molded article is an injection molded article, an extrusion molded article, or a compression molded article.
[0072] The uses of the resin composition, composite material, and molded article described above are not particularly limited and can be widely applied to various uses, for example, as a metal replacement material, particularly for uses requiring heat resistance, solvent resistance, and durability, etc. Specific uses include, but are not limited to, bearings, gaskets, gears, structural materials, automotive parts, battery-related parts, semiconductor manufacturing parts, aviation structural members, medical instruments, 3D printer filaments, semiconductor manufacturing equipment members, etc.
[0073] Examples of the present invention will be described below, but the present invention is not limited to these examples.
[0074] (Preparation Example 1) Synthesis of Aromatic Polyether Nitrogen gas was circulated through a 240 L reactor equipped with a stirrer, thermometer, nitrogen inlet tube, and a water collection container connected to a condenser. 132.47 kg of diphenyl sulfone (manufactured by Sino-High Corporation) was added stepwise, and the temperature was raised to 160°C. Once melting was confirmed, 39.00 kg (155 mol) of 4,4'-dichlorobenzophenone (manufactured by Sino-High Corporation), 16.85 kg (153 mol) of hydroquinone, and 21.78 kg (158 mol) of potassium carbonate (AGC Corporation, fine powder) were added in that order. The reaction concentration at this time was 2.31 mol / kg.
[0075] The reaction mixture was reacted under the following temperature control, and then 6.15 kg (25 moles) of 4,4'-dichlorobenzophenone was added as a reaction terminator. <Temperature control> (1) At a stirring speed of 100 rpm, the temperature was raised from 160°C to 200°C over 90 minutes. (2) The temperature was maintained at 200°C for 60 minutes. (3) The temperature was raised from 200°C to 250°C over 80 minutes. (4) The temperature was maintained at 250°C for 60 minutes. (5) The temperature was raised from 250°C to 300°C over 150 minutes. (6) The temperature was maintained at 300°C for 263 minutes. (7) The reaction terminator was added, and the temperature was maintained at 300°C. The reaction was terminated when the solution viscosity reached 295 cP.
[0076] After the reaction was completed, the contents were transferred to a SUS tray, cooled to room temperature, and solidified. The product was coarsely pulverized and crushed in a pin mill (160UPZ manufactured by Hosokawa Micron Corporation), washed with acetone, an aqueous oxalic acid solution, and water in that order, and then vacuum dried to obtain a powdery aromatic polyether (PEEK (A1)).
[0077] Example 1 1. Production of Resin Composition 100 parts by mass of the aromatic polyether (PEEK (A1)) obtained in Production Example 1 was mixed with 100 parts by mass of water. Thereafter, an inorganic metal phosphate ("Na" manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) was added. 2 HPO 4 " and Fujifilm Wako Pure Chemical Industries, Ltd. "NaH 2 P.O. 4 0.25 parts by mass of a nucleating agent ("ADEKA STAB NA-21" manufactured by ADEKA Corporation) was added and mixed at 25°C for 30 minutes. After mixing, the mixture was dried at 140°C for 24 hours. The dry-blended raw material obtained by dry-blending 0.25 parts by mass of a nucleating agent ("ADEKA STAB NA-21" manufactured by ADEKA Corporation) was then melt-kneaded using a twin-screw extruder ("Process-11" manufactured by Thermo Fisher Scientific, cylinder volume 20cc) with an 11 mm cylinder diameter at a screw rotation speed of 250 rpm and a set temperature of 380°C. The dry-blended raw material was fed from the base of the twin-screw extruder (upstream of the screw) at a rate of 6 g per minute. The residence time in the twin-screw extruder was 3.5 minutes. The strands discharged from the twin-screw extruder were cooled in water and then pelletized using a pelletizer to obtain a resin composition.
[0078] 2. Measurement of radical concentration of resin composition The radical concentration of the obtained resin composition (radical concentration at 25°C measured using TEMPOL as the standard substance and benzene as the solvent for the standard substance) was measured by ESR (electron spin resonance) under the following conditions and procedures.
[0079] [ESR measurement conditions] ESR apparatus: JESFA200 model manufactured by JEOL Ltd. ESR sample tube diameter: 5 mm Microwave output: 0.5 mW Modulation magnetic field: 0.3 mT Time constant: 0.03 seconds Magnetic field range: 328 to 344 mT Measurement time: 60 seconds Mn intensity: 650 Measurement temperature: 25°C
[0080] [Procedure] TEMPOL (4-hydroxy-2,2,6,6-tetramethylpiperidine-1-oxyl) was dissolved in benzene to a concentration of 5 μM, and 400 μL of this solution was added to an ESR sample tube. ESR was measured under the above-mentioned measurement conditions. The integral of the obtained peak derived from TEMPOL was divided by the integral of the peak of Mn for normalization (integral value A). Thereafter, the measurement sample (here, a resin composition) was weighed (weighed value B), filled into an ESR sample tube, and ESR was measured under the above-mentioned measurement conditions. The integral of the obtained peak derived from the sample was divided by the integral of the peak of Mn for normalization (integral value C). The obtained values of A, B, and C were used to calculate the amount of radicals per unit mass of the sample (radical concentration) according to the following formula: Radical concentration [spin / g]=(5×10 -6 x400 x 10 -6 x 6.02 x 10 23 × C) / (A × B)
[0081] 3. Thermal Stability (Thickening Rate) During Melting The thermal stability (thickening rate) of the resin composition during melting was evaluated based on the complex viscosity (Pa s). The complex viscosity was measured using a viscoelasticity measuring device under the following conditions and procedures. The quotient obtained by dividing the value at 60 minutes from the start of measurement by the value at 1 minute from the start of measurement was determined as the thickening rate due to melt retention.
[0082] [Measurement conditions] Viscoelasticity measuring device: MCR302 (manufactured by Anton Paar) Jig: SHAFT FOR DISPOSABLE MEASUREMENT SYSTEM D-CP / PP25 Disposable dish: Φ41 mm Disposable parallel plate: Φ25 mm Temperature: 420°C Preheating time: 3 min Gap: 0.8 mm Time: 300 min Shear strain: 1% Angular frequency: 2.76 rad / s
[0083] [Procedure] A disk-shaped resin composition was placed on a disposable dish and measured under the conditions described above. Before the measurement, the disk was sandwiched between the disposable dish and a disposable parallel plate with a gap of 0.8 mm, and then preheated and trimmed to a diameter of 25 mm.
[0084] The "disc" was obtained by the following method: The resin composition was filled into a mold and pressed at a temperature of 380°C using a vacuum press (IMC-6215 manufactured by Imoto Machinery Co., Ltd.). After pressing, it was quenched at 25°C to form a disk with a diameter of 25 mm and a thickness of 1.0 mm.
[0085] 4. Elemental Analysis Measurement by ICP The contents of Al (aluminum), Li (lithium), Na (sodium), and P (phosphorus) in the resin composition were dissolved under the following pretreatment conditions and measured by inductively coupled plasma atomic emission spectroscopy. Quantitative values were determined using a calibration curve derived from a reference of known concentration. <Pretreatment Conditions> 0.1 g of the resin composition was weighed into a quartz container as a sample. Next, nitric acid was added and the container was sealed. The container was then placed in a microwave decomposition device (Milestone General's "UltraWAVE" or equivalent) and subjected to pressure acid decomposition by microwave irradiation. After pressure acid decomposition, ultrapure water was added to the container to obtain a constant volume. <Measurement conditions> ICP optical emission spectrometer (Agilent Technologies, "Agilent 5100") Al measurement wavelength: 396.152 nm Li measurement wavelength: 670.783 nm Na measurement wavelength: 589.592 nm P measurement wavelength: 213.618 nm
[0086] The detection limit (lower detection limit) of the elemental analysis is 1 ppm. In Table 1 shown later, "ND" (Not Detected) means less than the detection limit (i.e., less than 1 ppm). The obtained measured value (the value shown in Table 1) corresponds to the "concentration in the resin composition," and when this value is designated as B (ppm), the "content relative to 100 parts by mass of aromatic polyether" is substantially B x 10 -4 (parts by mass) (because the content of phosphorus and metal elements is relatively small compared to the content of aromatic polyether).
[0087] 5. Preparation of Tensile Test Pieces (Injection Molded Articles) The pellets of the resin composition obtained in Example 1 were injection molded using an injection molding machine ("Mini Jet Pro" manufactured by Thermo Fisher Scientific) under the following conditions to obtain ISO 527-2-1BA tensile test pieces. <Injection conditions> (1) Cylinder temperature: 400°C (2) Mold temperature: 210°C (3) Preheating time: 3 min (4) Pressure holding time: 10 s
[0088] 6. Exposure Test The obtained test piece was exposed to air at 300°C for 100 hours.
[0089] 7. Tensile Test A tensile test was carried out on the obtained test specimen (the test specimen subjected to the above exposure test) under the following conditions to measure the elongation (tensile elongation): <Tensile conditions> Temperature: 23°C Speed: 20 mm / min Chuck distance: 50 mm
[0090] The results are shown in Table 1.
[0091] (Example 2) A resin composition was obtained in the same manner as in "1. Production of resin composition" in Example 1, except that the amount of inorganic metal phosphate was changed to 0.50 parts by mass. The obtained resin composition was evaluated in the same manner as in Example 1, and the results are shown in Table 1.
[0092] (Example 3) A dry blend raw material obtained by dry blending 0.5 parts by mass of a nucleating agent (ADEKA Corporation "ADK STAB NA-21") with commercially available aromatic polyether (PEEK, manufactured by Victrex, 151G) (PEEK (A2)) was melt-kneaded using a twin-screw extruder (Thermo Fisher Scientific "Process-11", cylinder volume 20 cc) having a cylinder diameter of 11 mm at a screw rotation speed of 250 rpm and a set temperature of 380 ° C. Here, the dry blend raw material was fed from the base of the twin-screw extruder (upstream side of the screw) at a rate of 6 g per minute. The residence time in the twin-screw extruder was 3.5 minutes. The strands discharged from the twin-screw extruder were cooled in water and then pelletized using a pelletizer to obtain a resin composition. The obtained resin composition was evaluated in the same manner as in Example 1, and the results are shown in Table 1.
[0093] Comparative Example 1 A resin composition was obtained in the same manner as in "1. Production of resin composition" in Example 1, except that the blending of the nucleating agent was omitted. The obtained resin composition was evaluated in the same manner as in Example 1, and the results are shown in Table 1.
[0094] Comparative Example 2 A resin composition was obtained in the same manner as in Example 1, except that the amount of inorganic metal phosphate was changed to 0.50 parts by mass and the addition of the nucleating agent was omitted in "1. Production of resin composition." The obtained resin composition was evaluated in the same manner as in Example 1, and the results are shown in Table 1.
[0095] Comparative Example 3 A resin composition was obtained in the same manner as in Example 1, except that the step of adding the inorganic metal phosphate was omitted, and 0.25 parts by mass of an organic metal phosphate (Ultranox 626, (2,4-di-tert-butyl-phenyl)-phosphiterythritol diphosphate, manufactured by ADEKA Corporation) was added as an antioxidant in the dry blending step, and the amount of nucleating agent blended was changed to 1.0 part by mass. The obtained resin composition was evaluated in the same manner as in Example 1, and the results are shown in Table 1.
[0096] Comparative Example 4 A commercially available aromatic polyether (PEEK, manufactured by Victrex, 151G) (PEEK (A2)) was used as a resin composition. This resin composition was evaluated in the same manner as in Example 1, and the results are shown in Table 1.
[0097]
[0098] From Table 1, it can be seen that the Examples are superior in thermal stability during melting compared to the Comparative Examples, and are capable of improving the high-temperature durability of the molded article.
[0099] Although several embodiments and / or examples of the present invention have been described in detail above, those skilled in the art will readily be able to make numerous modifications to these exemplary embodiments and / or examples without substantially departing from the novel teachings and advantages of the present invention. Accordingly, these numerous modifications are within the scope of the present invention. The contents of all documents cited in this specification and of the applications from which this application claims priority under the Paris Convention are incorporated by reference in their entirety.
Claims
1. A resin composition comprising an aromatic polyether, phosphorus, and three or more metal elements including sodium.
2. The resin composition according to claim 1, wherein the three or more metal elements include two or more selected from the group consisting of alkaline earth metals and alkali metals.
3. The resin composition according to claim 1 or 2, wherein the three or more metal elements include lithium.
4. The resin composition according to any one of claims 1 to 3, wherein the three or more metal elements include aluminum.
5. The resin composition according to any one of claims 1 to 4, wherein the three or more metal elements include sodium, aluminum, and lithium.
6. The content of the three or more metal elements relative to 100 parts by mass of the aromatic polyether is 1.0 × 10 -4 The resin composition according to any one of claims 1 to 5, comprising one or more metal elements in an amount of at least 100 parts by mass.
7. A resin composition comprising: an aromatic polyether; one or more members selected from the group consisting of inorganic metal phosphates and decomposition products thereof; and one or more members selected from the group consisting of nucleating agents and decomposition products thereof.
8. The resin composition according to claim 7, wherein the total amount of one or more selected from the group consisting of inorganic metal phosphates and decomposition products thereof is 0.01 to 5.0 parts by mass per 100 parts by mass of the aromatic polyether.
9. The resin composition according to claim 7 or 8, wherein the inorganic metal phosphate contains an alkali metal.
10. The resin composition according to any one of claims 7 to 9, which contains two or more types of inorganic metal phosphates.
11. A resin composition according to any one of claims 7 to 10, wherein the total amount of one or more selected from the group consisting of the nucleating agent and its decomposition products is 0.01 to 5.0 parts by mass per 100 parts by mass of the aromatic polyether.
12. The resin composition according to any one of claims 7 to 11, wherein the nucleating agent is at least one selected from the group consisting of organic nucleating agents and inorganic nucleating agents.
13. The aromatic polyether or the resin composition has a radical amount of 6.5 x 10 at 25°C, measured using TEMPOL as a standard substance and benzene as the solvent for the standard substance. 15 ~9.0 x 10 17 The resin composition according to any one of claims 1 to 12, wherein the viscosity is 1000 kJ / g.
14. The resin composition according to any one of claims 1 to 13, wherein the aromatic polyether is a polyarylene ether ketone.
15. A resin composition according to any one of claims 1 to 14, wherein the aromatic polyether comprises at least one selected from the group consisting of polyether ether ketone (PEEK), polyether ketone ketone (PEKK), and polyether ketone (PEK).
16. The resin composition according to any one of claims 1 to 15, which has a tensile elongation of 10% or more after exposure at 300°C for 100 hours.
17. A method for producing a resin composition, comprising a kneading step of kneading an aromatic polyether with an inorganic metal phosphate and a nucleating agent.
18. A composite material comprising at least one resin composition selected from the group consisting of the resin composition according to any one of claims 1 to 16 and the resin composition obtained by the method for producing a resin composition according to claim 17, and reinforcing fibers.
19. The composite material of claim 18, wherein the reinforcing fibers comprise one or more selected from the group consisting of carbon fibers, glass fibers, and aramid fibers.
20. A method for producing a composite material, comprising compounding one or more selected from the group consisting of the resin composition according to any one of claims 1 to 16 and the resin composition obtained by the method for producing a resin composition according to claim 17 with reinforcing fibers.
21. The method for producing a composite material according to claim 20, wherein the reinforcing fibers include at least one selected from the group consisting of carbon fibers, glass fibers, and aramid fibers.
22. A molded article obtained by molding one or more selected from the group consisting of the resin composition according to any one of claims 1 to 16, the resin composition obtained by the method for producing a resin composition according to claim 17, the composite material according to claim 18 or 19, and the composite material obtained by the method for producing a composite material according to claim 20 or 21.
Citation Information
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