JP2006265393A - Method of manufacturing polyphenylene sulfide resin composition - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method of manufacturing a polyphenylene sulfide resin composition which collects and re-uses wasted fibers created during the process of manufacturing polyphenylene sulfide fibers, wasted fibers created by the process of forming polyphenylene sulfide fibers into a desired shape, and used polyphenylene sulfide fibers. <P>SOLUTION: The method of manufacturing the polyphenylene sulfide resin composition comprises using polyphenylene sulfide fibers (A) as an original material and is characterized by the following steps of: (a) heating and pressing the polyphenylene sulfide fibers (A) to obtain either a massive or a strand form of the heated and compressed product; (b) cutting the above prepared product to form a cut product; and (c) melt kneading the above prepared cut product alone or with an additive to give a polyphenylene sulfide resin composition. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method for producing a polyphenylene sulfide resin composition, and more particularly to a method for producing a polyphenylene sulfide resin composition by recycling polyphenylene sulfide fibers and using this as a starting material.

  Polyphenylene sulfide is an engineering plastic with excellent heat resistance, chemical resistance, flame retardancy, mechanical strength, electrical properties, and dimensional stability. Various types of molding methods such as injection molding, extrusion molding, and compression molding can be used. Since it can be molded into molded articles, films, sheets, fibers, etc., it is used in a wide range of fields such as electric / electronic parts and automobile parts.

  Utilizing the excellent properties of polyphenylene sulfide, polyphenylene sulfide fibers have been actively used in applications such as various acid purification filters and various filters in desulfurization / denitration smoke gas equipment.

  On the other hand, in recent years, studies on recycling of thermoplastic resins have been actively conducted from the viewpoint of resource reuse, environmental problems, and the like. For example, Patent Document 1 discloses that a raw material resin, a resin additive, and a sprue, a runner, and the like generated when a thermoplastic resin containing the raw material resin and the resin additive is molded and then pulverized are disclosed. A composition is described which is compounded with a mixture containing a person. Patent Document 2 describes a resin composition in which polyacrylonitrile fiber is blended with a regenerated thermoplastic resin.

  Regarding the recycling of fibrous materials, when recycling carpet-type structures including polyamide fibers, polyester fibers, and polyolefin resins, a specific copolymer is blended as a compatibilizing agent for each of these resins to make a thermoplastic resin composition. A method for manufacturing a product is disclosed in Patent Document 3.

However, polyphenylene sulfide fibers are difficult to process because they have high heat resistance, and the main applications are various filter applications, and used products are easily contaminated and difficult to reuse. An effective reuse method has not been established.
Japanese Patent Laid-Open No. 2001-26719 (Page 2 (Claims)) JP-A-10-139927 (Page 2 (Claims)) JP 05-287139 A (second page (claims))

  The present invention recycles fiber waste generated in the production process of polyphenylene sulfide fiber, waste generated when polyphenylene sulfide fiber is processed in a later process, and used polyphenylene sulfide fiber, etc. It is an object of the present invention to provide a method for producing a sulfide resin composition.

As a result of intensive studies to solve the above problems, the inventors of the present invention have made the polyphenylene sulfide fiber composition easy to process by heating and compressing, and then using this as a compound raw material, so that the polyphenylene sulfide resin composition can be easily prepared. We found that it can be manufactured. That is, the present invention
(1) In producing a polyphenylene sulfide resin composition using the polyphenylene sulfide fiber (A) as a raw material,
(A) A step of heat-compressing the polyphenylene sulfide fiber (A) to form a block-like or strand-like heat-compressed product (b) a step of cutting the heat-compressed product to obtain a cut product (c) the cut product alone Or a method for producing a polyphenylene sulfide resin composition comprising a step of melt-kneading together with an additive to obtain a polyphenylene sulfide resin composition,
(2) The method for producing a polyphenylene sulfide resin composition according to claim 1, wherein the size of the cut product obtained in step (b) is a size that passes through a punching metal having a hole diameter of 7 mm,
(3) The method for producing a polyphenylene sulfide resin composition according to claim 1 or 2, wherein the additive is 0.1 to 600 parts by mass of filler (B) with respect to 100 parts by mass of the cut product. It is.

  According to the present invention, the fiber waste generated in the production process of the polyphenylene sulfide fiber, the polyphenylene sulfide fiber waste generated when the obtained polyphenylene sulfide fiber is processed into a desired shape in the subsequent process, and the used polyphenylene sulfide fiber are recycled. By utilizing this, a polyphenylene sulfide resin composition having excellent practicality can be produced.

(1) Polyphenylene sulfide fiber The polyphenylene sulfide (hereinafter referred to as PPS) fiber (A) used in the present invention is not particularly limited as long as it is a fiber mainly composed of PPS resin. The PPS resin here is a repeating unit represented by the following structural formula.

を７０モル％以上、好ましくは９０モル％以上を含む重合体である。かかる成分が７０モル％未満では耐熱性が損なわれる傾向にある。また、ＰＰＳ樹脂は、その繰り返し単位の３０モル％以下を、下記の構造式を有する繰り返し単位などで構成することが可能である。

Is a polymer containing 70 mol% or more, preferably 90 mol% or more. If such a component is less than 70 mol%, the heat resistance tends to be impaired. Moreover, PPS resin can comprise 30 mol% or less of the repeating unit with the repeating unit etc. which have the following structural formula.

  As the PPS fiber (A) used in the present invention, PPS fiber waste generated in the PPS fiber manufacturing process, PPS fiber waste generated when processed into a desired shape in the subsequent process, and further used PPS fiber Can be used. If importance is attached to the ease of recovery, fiber waste generated during processing in the fiber manufacturing process or in the subsequent process is preferably used. On the other hand, it is preferable to collect and use PPS fibers used in the market if importance is given to environmental considerations that are increasing in recent years. When using a market-recovered product, if it is considered that the market-recovered product is contaminated by contamination or foreign matter, it is preferable to remove the stain by a suitable method such as washing or separation.

  The viscosity of the PPS fiber (A) used in the present invention is not particularly limited, but when the fiber is melted at 315.5 ° C. and measured under conditions of a residence time of 5 minutes and a load of 5000 g according to JIS K7210. The melt flow rate (MFR) is preferably 20 g / 10 min or more, more preferably 50 to 200 g / 10 min. If the MFR value is too small, when the fiber is melt-kneaded in the extruder using the fiber as a raw material, the load on the extruder motor may become too large, making extrusion difficult.

  In the present invention, the PPS fiber (A) preferably contains 70% by mass or more of the PPS resin, more preferably 95% by mass or more, and the PPS resin alone may be used. When the content of the PPS resin is reduced, heat resistance, mechanical properties, surface properties and the like tend to be impaired. 30 mass% or less of PPS fiber (A) may contain additives, such as a polymer other than PPS resin, an inorganic or organic filler, a lubricant, a coloring agent, antioxidant, and an antistatic agent.

  The PPS fiber (A) in the present invention may be melt-spun unstretched or stretched.

  Furthermore, as the PPS fiber (A) used in the present invention, a resin or a compound such as a release agent or an antistatic agent may be applied to the surface as long as the object of the present invention is not impaired. For example, corona discharge treatment or plasma treatment may be performed.

(Heat compression method)
As a result of intensive studies, the inventors of the present invention have made it easy to cut in the next step if the PPS fiber (A) is reused by heating and compressing the PPS fiber (A) to form a mass or strand of heat-compressed product. Furthermore, it has been found that melt kneading after cutting becomes easy. The heat compression method is not particularly limited as long as the PPS fiber (A) is a mass or a strand-like heat compression product. For example, the following method can be given as a specific example.

  The above heat-compressed product refers to a material that can be handled without causing the PPS fibers to fall apart by heat-compressing the PPS fibers and fusing or pressing the PPS fibers together.

  That is, in a furnace in which the PPS fiber (A) is temperature-controlled at a temperature higher than the glass transition temperature (hereinafter referred to as a heat compression method-1), a furnace in which the PPS fiber (A) is previously temperature-controlled above the glass transition temperature. There is a method in which the temperature is reached by passing through and then compressed with a pressure roller (hereinafter referred to as heat compression method-2).

  For example, when the PPS fiber (A) is a nonwoven fabric or a short fiber, the heat compression method-1 is preferable. The non-woven fabric may be left as it is or may be cut into a size with good handling properties. The temperature is more preferably 200 ° C. or higher, and even more preferably the melting point of the PPS fiber (A) or higher. If the temperature at the time of heating is too low, the PPS fibers will not be fused or pressure-bonded even if they are compressed, so that they do not form a lump or strand. About the upper limit of heating temperature, in order to prevent thermal decomposition and coloring of PPS fiber, it is preferable that it is 400 degrees C or less, and it is more preferable that it is 350 degrees C or less.

  For example, when the PPS fiber (A) is a long fiber, any one of the heat compression method-1, the heat compression method-2, and other methods may be used. However, when the heat compression method-2 is used, continuous processing becomes possible. Therefore, it is preferable. When employing the heat compression method-2, the temperature when the temperature is controlled in advance is preferably not less than the glass transition temperature of the PPS fiber (A) and not more than the melting point, more preferably not less than 200 ° C. and less than the melting point. If the temperature at the time of heating is too low, the PPS fibers will not be fused or pressed together even if they are compressed, so that they will not form a lump or a strand. The fiber (A) is likely to be cut, which may cause difficulty in continuous productivity.

  If the thickness of the heat-compressed product is 1 mm or less, preferably 0.8 mm or less when heat-compressed material is used, heat is easily transmitted during heating, and the fusion property during compression is improved.

  The PPS fiber heat-compressed material thus heat-compressed is fused or pressure-bonded to each other by thermal deformation, so that it becomes a mass-like or strand-like heat-compressed product. The shape of the block-shaped heat-compressed product is preferably a sheet from the viewpoints of fusion property at the time of compression, press-bonding property, pulverization property at the time of cutting, and handling property of the cut product.

(Cutting method)
The heat-compressed product is cut by cutting using a conventionally known pulverizer. Examples of the pulverizer include a shear crusher such as a biaxial rotary shear crusher and a uniaxial rotary shear crusher, an impact crusher such as a hammer mill and an impact crusher, and a shredder.

  When the heat-compressed product is a strand-like heat-compressed product by a method such as the heat-compression method-2, in addition to the method using the pulverizer described above, it is cut using a generally known strand cutter or the like. Also good.

  The size of the cut product thus obtained is not particularly limited as long as there is no problem in supplying the cut product to an extruder for melt-mixing, but from the viewpoint of pulverization productivity and supply stability to the extruder. The size is preferably such that it passes through a punching metal having a hole diameter of 7 mm. More preferably, the size passes through a punching metal having a hole diameter of 5 mm. When the cut product becomes large, the supply to the extruder tends to become unstable.

(2) Additive It is possible to mix | blend an additive other than the said cut material with the PPS resin composition manufactured by this invention. Examples of such other additives include other PPS resins, fillers, other thermoplastic resins, and other additives.

(3) Other PPS resins In the present invention, sufficient physical properties can be obtained even if the total amount of the PPS resin raw material in which the PPS fiber cut product is blended in the composition is used as the PPS fiber cut product. Within a range that does not impair, PPS resin raw materials other than PPS fibers (for example, unmolded (virgin) PPS resin, scraps of molded products other than fibers, etc.) can be added. As the virgin PPS resin, for example, a method for obtaining a polymer having a relatively small molecular weight obtained by a production method represented by Japanese Patent Publication No. 45-3368, or Japanese Patent Publication No. 52-12240 and Japanese Patent Publication No. 61-7332. Examples thereof include a powdery or granular PPS resin produced by a known method such as a method for obtaining a polymer having a relatively large molecular weight described in the publication.

  Further, the powdery or granular PPS resin obtained as described above may be used as it is, and is crosslinked / high molecular weight by heating in air, heat treatment under an inert gas atmosphere such as nitrogen or under reduced pressure, It can also be used after being washed with an organic solvent, hot water, an acid aqueous solution or the like.

(4) Filler In the present invention, it is possible to add a filler (B) in order to further improve characteristics such as heat resistance and mechanical strength. Specific examples of the filler (B) to be added include fibrous or plate-like, scale-like, granular, indefinite shape, non-fibrous fillers such as crushed products, and specifically, for example, glass fiber, Glass milled fiber, carbon fiber, wollastonite fiber, stainless steel fiber, metal fiber such as aluminum fiber and brass fiber, organic fiber such as aromatic polyamide fiber, gypsum fiber, ceramic fiber, asbestos fiber, zirconia fiber, alumina fiber, silica fiber , Titanium oxide fiber, silicon carbide fiber, carbon powder, graphite, carbon flake, scaly carbon, carbon nanotube, rock wool, alumina hydrate (whisker / plate), potassium titanate whisker, calcium carbonate whisker, barium titanate Whisker, aluminum borate whisker, silicon nitride Scar, talc, kaolin, silica (crushed / spherical), quartz, calcium carbonate, glass beads, glass flakes, crushed / indeterminate shaped glass, glass microballoon, clay, mica, molybdenum disulfide, wollastonite, aluminum oxide ( Crushed), titanium oxide (crushed), metal oxide such as zinc oxide, metal hydroxide such as aluminum hydroxide, aluminum nitride, calcium polyphosphate, graphite, metal powder, metal flake, metal ribbon, metal oxide, etc. Is mentioned. Specific examples of metal species of metal powder, metal flakes, and metal ribbons include silver, nickel, copper, zinc, aluminum, stainless steel, iron, brass, chromium, and tin. The type of glass fiber or carbon fiber is not particularly limited as long as it is generally used for reinforcing a resin, and can be selected from long fiber type, short fiber type chopped strand, milled fiber, and the like.

  The surface of the filler used in the present invention can be used by treating the surface with a known coupling agent (for example, silane coupling agent, titanate coupling agent, etc.) or other surface treatment agents. .

  Two or more kinds of the fillers (B) described above may be used in combination.

  The blending amount of the filler (B) used in the present invention is 0 to 600 parts by mass of the filler (B) with respect to 100 parts by mass of the PPS fiber (A) from the balance of mechanical strength, heat resistance and fluidity. Yes, preferably 0.1 to 600 parts by mass, more preferably 0.1 to 500 parts by mass. If the amount of the filler (B) is too large, the mechanical strength and fluidity tend to decrease.

(5) Other thermoplastic resins The PPS resin composition of the present invention may contain a thermoplastic resin other than the PPS resin, if desired. Specific examples include polyethylene resin, polypropylene resin, polystyrene resin, ABS resin, polyamide resin, polycarbonate resin, polyethylene terephthalate resin, polybutylene terephthalate resin, polyacetal resin, modified polyphenylene ether resin, polysulfone resin, polyallyl sulfone resin, polyketone. Resin, polyetherimide resin, polyarylate resin, liquid crystal polymer, polyethersulfone resin, polyetherketone resin, polythioetherketone resin, polyetheretherketone resin, polyimide resin, polyamideimide resin, polytetrafluoroethylene resin, heat Plastic polyurethane resin, polyamide elastomer, polyester elastomer, polyester resin, polyphenylene ether resin, SAN resin, active resin Le resin, SBS, SEBS, various elastomers, and the like. These may be used in combination of two or more. These may be used in the form of virgin such as pellets, powders, granules, or may be crushed products such as molded products and films.

(6) Other various additives Furthermore, the PPS resin composition of the present invention is a coupling agent such as an isocyanate compound, an organic titanate compound, an organic borane compound, or an epoxy compound within a range that does not impair the effects of the present invention. , Plasticizers such as alkylene oxide oligomeric compounds, thioether compounds, ester compounds, organic phosphorus compounds, inorganic fine particles, organic phosphorus compounds, metal oxides, crystal nucleating agents such as polyetheretherketone, polyethylene, polypropylene, etc. Metal soap such as polyolefin, montanic acid wax, lithium stearate, aluminum stearate, release agent such as ethylenediamine / stearic acid / sebacic acid polycondensate, silicone compound, anti-coloring agent such as hypophosphite, Hindered phenolic antioxidants Antioxidants, antioxidants such as sulfur antioxidants, weathering agents and ultraviolet light inhibitors (resorcinol-based, salicylate-based, benzotriazole-based, benzophenone-based, hindered amine-based, etc.), heat stabilizer, lubricant (montanic acid) And metal salts thereof, esters thereof, half esters thereof, stearyl alcohol, stearamide, various bisamides, bisureas, and polyethylene waxes), foaming agents, pigments (cadmium sulfide, phthalocyanine, carbon black, metallic pigments, etc.), dyes (nigrosin, etc.) ), Antistatic agents (alkyl sulfate type anionic antistatic agents, quaternary ammonium salt type cationic antistatic agents, nonionic antistatic agents such as polyoxyethylene sorbitan monostearate, betaine amphoteric antistatic agents, etc. ), Ordinary additives such as flame retardants Agent can be added.

(7) Melt-kneading method of PPS resin composition The PPS resin composition produced in the present invention is a cut product of PPS fiber (A) alone or an additive as an optional component ((B) The component and / or other compounding components) are obtained by melt-kneading and then pelletizing. Specifically, the mixture of raw materials is supplied to a generally known melt mixer such as a single or twin screw extruder, Banbury mixer, kneader, or mixin gall, and kneaded at a temperature of 210 to 450 ° C. The method of doing can be given as an example. In addition, there is no particular limitation on the mixing order of the raw materials, a method in which all the raw materials are blended and then melt-kneaded by the above method, a part of the raw materials are melted and kneaded by the above method, and the remaining raw materials are blended and melted Any method may be used, such as a method of kneading, or a method of mixing a part of raw materials and mixing the remaining raw materials using a side feeder during melt-kneading with a single or twin screw extruder. As for a small amount of additive component, other components can be kneaded and pelletized by the above-described method and then added before molding and used for molding.

  The PPS resin composition obtained by the present invention can be applied to various moldings such as injection molding, extrusion molding, blow molding, transfer molding and film molding.

  Hereinafter, although an Example and a comparative example demonstrate concretely, these are described as an illustration and this invention is not limited to these.

  In addition, the performances of the PPS polymer products, PPS fiber cut products, melt-kneaded products, etc. obtained in the reference examples, examples and comparative examples described below are evaluated by the measuring methods described in the following (1) to (4). did.

(1) Measurement of melt flow rate (MFR) MFR of PPS polymerized products, PPS fibers, cut products of heat-compressed products, etc. is 315.5 ° C. for 5 minutes according to JIS K7210, load 5000 g (orifice diameter 2.095 mm) And a length of 8.00 mm) using a melt indexer.

(2) Tensile properties Tensile specimens (1/8 inch (3.2 mm) thick) were injection molded according to ASTM D638 and measured under a temperature condition of 23 ° C.

(3) Impact properties Impact test pieces (1/8 inch (3.2 mm) thick, with notches) were injection molded in accordance with ASTM D256 and measured under a temperature condition of 23 ° C.

(4) Glass transition temperature and melting point of PPS resin Using DSC-7 manufactured by PERKIN ELMER, the temperature was increased at a rate of temperature increase of 20 ° C./min.

[Reference example]
(Manufacturing of PPS)
An autoclave with a stirrer was charged with 6.005 kg (25 mol) of sodium sulfide 9 hydrate, 0.787 kg (9.6 mol) of sodium acetate and 5 kg of NMP, and gradually heated to 205 ° C. through nitrogen, and 3.6 liters of water Distilled. Next, after cooling the reaction vessel to 180 ° C, 3.712 kg (25.25 mol) of 1,4-dichlorobenzene and 2.4 kg of NMP were added, sealed under nitrogen, heated to 270 ° C, heated at 270 ° C. Reacted for 2.5 hours. Next, the mixture was put into 10 kg of NMP heated to 100 ° C., stirred for about 1 hour, filtered, and further washed with hot water at 80 ° C. for 30 minutes three times. This was filtered, poured into 25 liters of an aqueous solution containing 10.4 g of calcium acetate, stirred for about 1 hour at 192 ° C. in a sealed autoclave, filtered, and the pH of the filtrate reached 7. After washing with ion-exchanged water at about 90 ° C. and drying under reduced pressure at 80 ° C. for 24 hours, the temperature-falling crystallization temperature is 180 ° C., the amount of chloroform extracted is 0.30% by mass, MFR is 100 g / 10 minutes, the glass transition temperature is 87 ° C., the melting point is 279 ° C. Of PPS-1. The same operation was repeated and used for the following examples. The MFR was determined after drying 5 g of PPS resin powder at 130 ° C. for 3 hours.

(Manufacture of PPS fibers)
PPS-1 was supplied to a twin-screw extruder (PCM-30 manufactured by Ikegai Kogyo Co., Ltd.) set at 320 ° C., and the gut discharged from the die was immediately cooled with water and pelletized using a strand cutter. After drying the pellets at 180 ° C. for 3 hours, the pellets were melted again with an extruder-type spinning machine under a vacuum of 1.3 KPa (10 torr) so that the polymer temperature was 315 ° C. After filtration through a metal filter having 5 μm pores, spinning is performed through a spinneret having 50 holes with a hole diameter of 0.30 mm and a hole depth / hole diameter ratio of 4, and the discharge amount is 220 dtex for the wound yarn. The spinning conditions were adjusted as follows. Pass the chimney with the ambient temperature of 10cm below the base surface set to 220 ° C (chimney passing time: 1 second), immediately cool the yarn with cold air of 25 ° C, and then rotate at a speed of 600m / min The film was taken up by a take-up roll heated to 50 ° C., and the undrawn yarn was temporarily wound up and temporarily stretched 1.10 times with a feed roll heated to 90 ° C. continuously. Subsequently, 3.0-fold secondary stretching was performed between the feed roll and the first stretching roll at 105 ° C. Further, the yarn was subjected to a relaxation treatment of 0.98 times between the second drawing roll at 200 ° C. and the relaxation roll, and wound with a winder to obtain PPS fibers. This PPS fiber is designated as PPS-A.

(PPS fiber heat compression-1)
PPS-A was sandwiched in a press adjusted to 260 ° C. and left for 10 minutes. Subsequently, it compressed with the hydraulic jack of 1 ton pressure for 10 minutes, and obtained the block-shaped heat compression thing which is a sheet shape of thickness 0.5mm. This operation was repeated and used for the following examples. This PPS fiber heat compression product is referred to as PPS-B.

  In addition, when PPS-A was compressed without heating, it did not become a lump.

(PPS fiber heat compression-2)
PPS-A was sandwiched in a press adjusted to 300 ° C. and left for 10 minutes. Subsequently, it compressed with the hydraulic jack of 1 ton pressure for 10 minutes, and obtained the block-shaped heat compression thing which is a sheet form of thickness 0.4mm. This operation was repeated and used for the following examples. This PPS fiber heat compression product is designated as PPS-C.

(PPS fiber heat compression-3)
PPS-A was sandwiched in a press adjusted to 260 ° C. and left for 10 minutes. Immediately after taking out, it was sandwiched between pressure rollers having a metal roller portion heated to 260 ° C. in advance, and the pressure roller was rotated with a hydraulic jack with a pressure of 1 ton to obtain a strand-like heat compression product having a thickness of 0.5 mm. . Since the front end portion of the strand-like heat-compressed material was not pressurized, it was cut and discarded. This operation was repeated and used for the following examples. This PPS fiber heat compression product is designated as PPS-D.

(PPS fiber heat compression-4)
PPS-A was sandwiched in a press adjusted to 300 ° C. and left for 10 minutes. When it was taken out as it was and sandwiched between pressure rollers and the roller was rotated, the PPS-A melt was broken by tension, and no strand-like material was obtained.

(Cut of heat-compressed PPS fiber)
PPS-B was cut with a uniaxial rotary shearing pulverizer provided with a punching metal having a hole diameter (D) of 7 mm. Let the obtained cut material be PPS-2 (B). Moreover, PPS-C was cut | disconnected by the same method. This is PPS-2 (C). Furthermore, PPS-D was cut by the same method. This is PPS-2 (D).

  Moreover, what cut | disconnected PPS-B with the uniaxial rotation shearing-type grinder provided with the punching metal of 5 mm of hole diameters (D) is set to PPS-3 (B).

  PPS-4 (B) is obtained by cutting PPS-B with a uniaxial rotary shear crusher provided with a punching metal having a hole diameter (D) of 10 mm.

  Further, a part of the used PPS bag filter recovered from the market was cut after being heated and compressed in the same manner as described in the section of PPS fiber heated compressed product-1 using a 260 ° C. press. For cutting, a uniaxial rotary shear pulverizer provided with a punching metal having a hole diameter (D) of 7 mm was used. Let the obtained cut product be PPS-5 (B). The used PPS bag filter collected from the market had an MFR of 120 g / 10 min, and was washed and dried before heat compression.

[Compositions used in Examples and Comparative Examples]
PPS
PPS-1: PPS polymerized product PPS-2 (B): PPS-A heated and compressed with a press machine at 260 ° C. (passed through punching metal with a hole diameter (D) of 7 mm)
PPS-2 (C): PPS-A heated and compressed with a 300 ° C press (cut through a punching metal with a hole diameter (D) of 7 mm)
PPS-2 (D): PPS-A heated to 260 ° C, compressed with a pressure roller and cut (passed through punching metal with a hole diameter (D) of 7 mm)
PPS-3 (B): PPS-A heated and compressed with a press machine at 260 ° C. and cut (through a punching metal with a hole diameter (D) of 5 mm)
PPS-4 (B): PPS-A heated and compressed with a press machine at 260 ° C. and cut (passed through punching metal with a hole diameter (D) of 10 mm)
PPS-5 (B): A PPS bag filter collected from the market, washed with water and dried, then heated and compressed with a press machine at 260 ° C. (passed through a punching metal with a hole diameter (D) of 7 mm)
PPS-A: PPS fiber produced from PPS-1 PPS-B: Heat-compressed product of PPS-A (using a press machine at 260 ° C.)
PPS-C: PPS-A heat compression product (using a press machine at 300 ° C.)
PPS-D: Heat-compressed product of PPS-A (heated to 260 ° C. and then compressed with a pressure roller)
Filler
Filler-1: Glass fiber: “T-717” average fiber diameter 13 μm (manufactured by Nippon Electric Glass)
Filler-2: Calcium carbonate: “KSS-1000” Average particle size 2 μm (manufactured by Dowa Calfin)
Additive Additive-1: Ethylenediamine / stearic acid / sebacic acid polycondensate “Lightamide WH-255” (manufactured by Kyoeisha Chemical).

Examples 1-8, Comparative Examples 1-4
Each compounding agent prepared as described above was dry-blended at the ratio shown in Table 1, and then melt-kneaded and pelletized by a single-screw extruder having a diameter of 90 mm set at an extrusion condition of 320 ° C. Extrusion was stable in all examples, but in Example 5, the discharge amount was slightly lower than in the other examples. In all of Comparative Examples 1 to 4, the dry blended product was caught in the extruder and could not be extruded.

The obtained pellets were dried at 130 ° C. for 3 hours, and then on a Toshiba Machine IS80 type injection molding machine, cylinder temperature: 320 ° C., mold temperature: 130 ° C., injection / cooling time: 13/15 seconds, injection speed: 75 %, Injection pressure: injection molding under the setting conditions of filling lower limit pressure + 10 kg / cm ² (G) to obtain a predetermined test piece for characteristic evaluation. About the obtained test piece, the tensile characteristic and the impact characteristic were evaluated by the method mentioned above. The results are shown in Table 1.

  As is apparent from Table 1, according to the method of the present invention, fiber waste generated in the PPS fiber production process, PPS fiber waste generated when the obtained PPS fiber is processed into a desired shape in a subsequent process, and used A PPS resin composition can be obtained by reusing PPS fibers by applying the production method of the present invention.

  Since the polyphenylene sulfide resin composition obtained by the present invention is excellent in the properties inherent to polyphenylene sulfide, examples of its use include lamp cases, lamp boxes, lamp housings, lamp sockets, lamp reflectors, lens holders, Lighting parts such as lamp units, optical chassis, lens units, reflection mirrors, and liquid crystal frames, and sensors, LED lamps, connectors, sockets, resistors, relay cases, switches, coil bobbins, capacitors, variable capacitor cases, optical pickups, oscillators, etc. Various terminal boards, transformers, plugs, printed circuit boards, tuners, speakers, microphones, headphones, small motors, magnetic headspaces, power modules, semiconductors, liquid crystals, FDD carriages, FDD systems -Electric, electronic parts such as motor brush holders, parabolic antennas, computer-related parts; generators, motors, transformers, current transformers, voltage regulators, rectifiers, inverters, relays, power contacts, switching Applications: Electrical equipment parts such as ovens, circuit breakers, knife switches, other pole rods, electrical parts cabinets; VTR parts, TV parts, irons, hair dryers, rice cooker parts, microwave oven parts, acoustic parts, audio laser discs Audio equipment parts such as compact discs, lighting parts, refrigerator parts, air conditioner parts, typewriter parts, word processor parts, home appliances, office electrical parts, office computer-related parts, telephone-related parts, facsimile-related parts, copying Machine-related parts, cleaning jigs, motor parts, Mechanical parts such as iter and typewriters; Optical equipment such as microscopes, binoculars, cameras, and watches, precision machine parts; water faucet tops, mixing faucets, pump parts, pipe joints, water volume control valves Water supply parts such as relief valves, hot water temperature sensors, water volume sensors, water meter housings; alternator terminals, alternator connectors, IC regulators, light meter potentiometer bases, various valves such as exhaust gas valves, fuel-related / exhaust systems・ Various intake pipes, air intake nozzle snorkel, intake manifold, fuel pump, engine coolant joint, carburetor main body, carburetor spacer, exhaust gas sensor, coolant sensor, oil temperature sensor, brake pad wear sensor , Throttle position sensor, crankshaft position sensor, air flow meter, brake pad wear sensor, thermostat base for air conditioner, heating hot air flow control valve, brush holder for radiator motor, water hump impeller, turbine vane, wiper motor related parts, du Distributor, starter switch, starter relay, transmission wire harness, window washer nozzle, air conditioner panel switch board, coil for fuel related electromagnetic valve, fuse connector, horn terminal, electrical component insulation plate, step motor rotor, lamp socket, lamp Reflector, lamp housing, brake piston, solenoid bobbin, engine oil fill Automotive / vehicle-related parts such as motors, ignition device cases, film capacitor dielectrics, variable capacitor dielectrics, aluminum electrolytic capacitor dielectrics, aluminum electrolytic capacitor element fastening tape, motor / transformer electrical insulation, lithium ion secondary battery insulation, Examples include circuit board applications, liquid crystal film release, high functional polymer film release, ceramic film release, and other various uses.

Claims (3)

In producing a polyphenylene sulfide resin composition using the polyphenylene sulfide fiber (A) as a raw material,
(A) A step of heat-compressing the polyphenylene sulfide fiber (A) to obtain a block-shaped or strand-shaped heat-compressed product (b) a step of cutting the heat-compressed product to obtain a cut product (c) the above-mentioned cut product alone Or a method for producing a polyphenylene sulfide resin composition, comprising a step of melt-kneading together with an additive to obtain a polyphenylene sulfide resin composition. The method for producing a polyphenylene sulfide resin composition according to claim 1, wherein the size of the cut product obtained in the step (b) is a size passing through a punching metal having a hole diameter of 7 mm. The method for producing a polyphenylene sulfide resin composition according to claim 1 or 2, wherein the additive is 0.1 to 600 parts by mass of the filler (B) with respect to 100 parts by mass of the cut product.