WO2012033085A1 - ポリフェニレンサルファイド繊維含有不織布 - Google Patents
ポリフェニレンサルファイド繊維含有不織布 Download PDFInfo
- Publication number
- WO2012033085A1 WO2012033085A1 PCT/JP2011/070239 JP2011070239W WO2012033085A1 WO 2012033085 A1 WO2012033085 A1 WO 2012033085A1 JP 2011070239 W JP2011070239 W JP 2011070239W WO 2012033085 A1 WO2012033085 A1 WO 2012033085A1
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- WIPO (PCT)
- Prior art keywords
- nonwoven fabric
- roll
- contact angle
- fiber
- pps
- Prior art date
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Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H13/00—Other non-woven fabrics
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/10—Organic non-cellulose fibres
- D21H13/20—Organic non-cellulose fibres from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/08—Rearranging applied substances, e.g. metering, smoothing; Removing excess material
- D21H25/12—Rearranging applied substances, e.g. metering, smoothing; Removing excess material with an essentially cylindrical body, e.g. roll or rod
- D21H25/14—Rearranging applied substances, e.g. metering, smoothing; Removing excess material with an essentially cylindrical body, e.g. roll or rod the body being a casting drum, a heated roll or a calender
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/301—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen or carbon in the main chain of the macromolecule, not provided for in group H01B3/302
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/48—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances fibrous materials
- H01B3/485—Other fibrous materials fabric
Definitions
- the present invention relates to a nonwoven fabric containing polyphenylene sulfide fibers and a method for producing the same, and more particularly to a nonwoven fabric suitable for electrical insulation and battery separators and a method for producing the same.
- PPS fibers polyphenylene sulfide fibers
- filters used for high-temperature gas dust collection dryer canvases used in the drying process for industrial products, and roll wipers for office copiers. It is predicted that there will be a wide range of uses in the future.
- Patent Document 1 proposes a heat-resistant electrical insulating material and a battery separator as specific applications.
- Requirement performance for electrical insulation materials used for batteries, motors, inverters, etc. is becoming stricter.
- an insulating material for a motor when the winding and the stator or rotor are insulated, a varnish made of resin may be impregnated to further improve the insulating performance.
- the sheet used for the insulating material is required to have a good impregnation property of the varnish solution when the sheet is impregnated with the varnish.
- secondary batteries with increased energy density are exposed to high temperature environments, and dew may occur due to humidity in the air.
- the insulating material used is required to exhibit a stable moisture-proof effect because the dehydrated water does not penetrate into the insulating material. That is, two performances are required which are high in impregnation of the varnish solution and suppress moisture permeation. Furthermore, in order to make it easy to diffuse the heat generated from the winding of the coil to the surroundings and to suppress the temperature rise of the equipment used, the electrical insulating material is also required to have heat diffusion performance.
- Patent Document 1 discloses that a wet non-woven fabric (non-woven fabric obtained by a papermaking method) made of PPS fibers may contain a binder, and heating and pressurizing through a calendar device.
- the invention of Patent Document 1 is a sufficient solution to the above-mentioned demands and problems, in particular, good wettability of the resin solution to the wet nonwoven fabric (nonwoven fabric obtained by the papermaking method), and moisture penetrates inside. It did not solve the problem of being able to suppress it.
- Patent Document 2 a heat-resistant nonwoven fabric obtained by blending heat-resistant fibers and unstretched polyphenylene sulfide fibers is suitable for a high heat-resistant electrical insulating sheet.
- Patent Document 2 the unstretched polyphenylene sulfide fiber is heat-sealed after a mixing ratio of less than 8%.
- Patent Document 2 The invention of Patent Document 2 is obtained by carding PPS short fibers into a web, and then setting the heat fusion pressure to less than 100 kg / cm so as not to increase the density of the heat-resistant nonwoven fabric. is there.
- the nonwoven fabric obtained by the method of Patent Document 2 has good varnish impregnation properties, it has not been able to sufficiently solve the problem of maintaining the varnish impregnation properties while suppressing the penetration of moisture.
- Patent Document 2 discloses that the nonwoven fabric is a nonwoven fabric obtained by a dry method such as a carding method or an airlay method, and it is preferable that the density is not too high.
- the nonwoven fabric obtained by the carding method or the airlay method generally uses short fibers having a crimped fiber length of 38 mm or more, the resulting web is bulky, and the fiber dispersion state is also a papermaking method. It is inferior to the non-woven fabric obtained. Therefore, the non-woven fabric disclosed in Patent Document 2 does not have uniform formation and thinness, unlike the non-woven fabric obtained by the papermaking method of the present invention, and therefore controls good impregnation with varnish and moisture penetration. It did not solve the problem of combining the performance that can be achieved, and further the problem of lightness required as an electrical insulating material. *
- Patent Document 3 discloses that when calendaring is performed after making paper using pulp, opacity, white glossiness, and smoothness are increased by attaching moisture. Specifically, when calendering is performed using a hot soft nip calender device, the calender device preferably treats at least 6 nips on both sides of the nonwoven fabric.
- the non-woven fabric of PPS fiber obtained by the paper making method known so far has lightness and flexibility peculiar to paper, and further heat resistance, but has high impregnation property with a varnish necessary for an electrically insulating material,
- the dimensional stability in a high temperature environment such as wet heat or dry heat was not excellent.
- an object of the present invention is to provide a nonwoven fabric containing PPS fibers and having a high varnish impregnation property. Furthermore, when the dimensional stability in a high temperature and high humidity environment is requested
- the present invention is intended to achieve the above object.
- the nonwoven fabric of the present invention is obtained by a papermaking method comprising PPS fibers, and the contact angle of water on the nonwoven fabric surface (Otemen) is 5 ° or more larger than the contact angle of water on the back surface of the nonwoven fabric. It is a feature.
- the contact angle between the nonwoven fabric surface and the nonwoven fabric back surface is within the range of 70 ° to 110 °.
- unstretched PPS fibers are included in a part of the PPS fibers, and the unstretched PPS fibers are fused to form a nonwoven fabric. Is selectively present on the surface of the nonwoven fabric.
- the non-woven fabric production method disclosed in the present invention is a suitable method for producing any of the above non-woven fabrics. That is, unstretched PPS fiber is dispersed in water, rolled up on a wire (papermaking net), dried and removed, and then heated and pressurized in a calender device. It is manufactured by treating the surface temperature at a temperature different by 10 ° C. or more.
- a nonwoven fabric having both varnish impregnation properties and dimensional stability in a high temperature environment can be obtained.
- the non-stretched PPS fiber is included in a part of the PPS fiber, the unstretched PPS fiber is fused to form a nonwoven fabric, and the fusion is selectively present on the nonwoven fabric surface. It has excellent impregnation properties, excellent dimensional stability in a high-temperature environment, and high insulation performance.
- the varnish impregnation property is improved by increasing the contact angle of the nonwoven fabric surface by 5 ° or more than the contact angle of the nonwoven fabric back surface, and at a high temperature. It was found that the dimensional change can be reduced.
- the present inventors have further paid attention to the problem that the insulating material changes in size due to the dew phenomenon in a high humidity such as a pump motor, and the contact angle between the nonwoven fabric surface and the back surface is 70 °. It has been found that by being within the range of ⁇ 110 °, the prevention of dimensional change in a high temperature and high humidity environment can be solved, and the present invention has been achieved.
- the contact angle specified in the present invention is a contact angle with water, and is measured by a method in accordance with JIS R 3257 (1999) “6 Still Drop Method”. That the contact angle of the nonwoven fabric surface is 5 ° or more larger than the contact angle of the nonwoven fabric back surface means that the nonwoven fabric surface side repels droplets more than the nonwoven fabric back surface side.
- the surface with the larger contact angle is defined as the surface.
- the nonwoven fabric surface side is arranged on the winding side and sandwiched between the winding and the stator, so that it is possible to prevent the winding from being exposed and degrading the winding, and
- the varnish impregnation property is selectively high on the back surface of the nonwoven fabric on the stator side, the insulation durability can be improved and the heat diffusion performance can be provided.
- the contact angle on the nonwoven fabric surface is more preferably 9 ° or more than the contact angle on the nonwoven fabric back surface.
- the contact angle between the nonwoven fabric surface and the nonwoven fabric back surface is preferably in the range of 70 ° to 110 °, and more preferably in the range of 70 ° to 100 °. This is because when the contact angle is 70 ° or more, moisture (water droplets) from the air is particularly easily repelled, and the dimensional stability in a high humidity and high temperature environment is excellent. Further, it is preferable that the contact angle is not more than the above angle because the varnish impregnation property, in particular, the varnish impregnation property using water as a medium becomes good.
- a non-woven fabric having a contact angle in the range of 80 ° to 100 ° is more preferable because it is less deteriorated due to adhesion of water droplets and has sufficient varnish impregnation properties.
- the contact angle of water on the non-woven fabric surface is 5 ° or more larger than the contact angle on the back surface of the non-woven fabric, the contact angle of the surface (Omenen) must be in the range of 75 ° to 110 °, and moreover 75 ° to 100 °. Is preferred.
- the contact angle on the back surface is preferably in the range of 70 to 105 °, more preferably 70 to 95 °.
- the surface of the nonwoven fabric refers to the surface of the nonwoven fabric that has a larger contact angle
- the back surface of the nonwoven fabric refers to the other surface.
- the nonwoven fabric of the present invention is obtained by a papermaking method.
- raw material fibers are dispersed in water, and a papermaking stock solution to which a dispersant, an antifoaming agent, etc. are added as necessary is prepared.
- the paper stock solution is passed through a paper machine to make paper.
- the paper machine may be any of a circular net, a long net, and a short net.
- the obtained wet paper is placed on a belt, dried and rolled up while squeezing water, and a nonwoven fabric obtained by a papermaking method can be obtained.
- the PPS fiber used in the present invention has a polymer structural unit of-(C 6 H 4 -S)- Is a synthetic fiber made of a polymer having a main structural unit.
- Typical examples of these PPS polymers include polyphenylene sulfide, polyphenylene sulfide sulfone, polyphenylene sulfide ketone, random copolymers thereof, block copolymers, and mixtures thereof.
- polyphenylene sulfide containing a p-phenylene unit represented by — (C 6 H 4 —S) —, preferably 90 mol% or more, as the main structural unit of the polymer is desirable.
- the fiber length is preferably in the range of 2 to 38 mm. If the fiber length is in the range of 2 to 38 mm, it can be uniformly dispersed in the stock solution for papermaking, and has the tensile strength necessary to pass through the drying process in a wet state (wet paper) immediately after papermaking.
- the thickness of the PPS fiber is preferably in the range of 0.1 to 10 dtex because the fiber can be uniformly dispersed without agglomerating in the stock solution for papermaking.
- the method for producing the PPS fiber used in the present invention is preferably a method in which the polymer having the phenylene sulfide structural unit described above is melted at a melting point or higher and spun from a spinneret to form a fiber.
- the spun fiber is an unstretched PPS fiber as it is.
- Most of the unstretched PPS fibers have an amorphous structure and can act as a binder for bonding the fibers to each other by applying heat.
- stretched yarns are commercially available in which the fiber is stretched and oriented following spinning to improve the strength and thermal dimensional stability of the fibers.
- a plurality of PPS fibers such as “Torcon” (registered trademark) (manufactured by Toray) and “Procon” (registered trademark) (manufactured by Toyobo) are in circulation.
- the nonwoven fabric of the present invention preferably has a basis weight of 10 to 800 g / m 2 and a thickness of 10 to 800 ⁇ m, and is appropriately selected depending on required insulation performance.
- moderate flexibility may be required because they are inserted between the winding and the stator or rotor.
- the basis weight it is preferably in the range of 40 to 300 g / m 2 .
- the thickness is preferably 40 to 300 ⁇ m. More preferably, the thickness is 40 to 230 ⁇ m. This is because if the basis weight is 40 g / m 2 or more, the insulation performance can be satisfied.
- the basis weight is 300 g / m 2 or less, it has flexibility when incorporated in a motor.
- the nonwoven fabric of the present invention is a nonwoven fabric containing PPS fibers. Further, as the nonwoven fabric, unstretched PPS fibers are included in a part of the PPS fibers, and the unstretched PPS fibers are fused to form a nonwoven fabric. It is preferable that there are many in the direction. Heating by using unstretched PPS fibers as a part of the PPS fibers is preferable because the fibers constituting the nonwoven fabric can be fixed to each other, and the tensile breaking strength of the nonwoven fabric can be improved. Furthermore, the fused portion is generally formed by heating and pressurizing the nonwoven fabric with two smooth rolls.
- the fact that unstretched PPS fibers are fused to form a non-woven fabric as in the present invention makes it easy to repel water because some of the PPS fibers change from the fiber state and become smooth. As a result, there is a reduction in performance due to dew and a change in dimensions due to moisture absorption.
- the surface (hymen) temperature of the two smooth rolls is set to a temperature different by 10 ° C. or more to perform heating / pressurizing treatment, so that a large amount of fusion is selectively performed on the nonwoven fabric surface side.
- a portion is present, and water is easily selectively repelled on the surface, while the back surface of the nonwoven fabric is more hydrophilic with water than the nonwoven fabric surface and exhibits varnish impregnation, which is preferable.
- a polyester component having a low melting point can be used in place of the PPS undrawn yarn, but the PPS undrawn yarn can be selectively heat-sealed at a lower heating / pressurizing temperature.
- the component to be attached is preferably an undrawn PPS yarn.
- the fusion part is present on the surface of the nonwoven fabric in a large amount and the back surface of the nonwoven fabric is less in the fusion part.
- the nonwoven fabric of the present invention can suppress dew condensation due to moisture in the atmosphere, and also has high varnish impregnation properties. Therefore, when used for electrical insulation, the insulation durability is improved and the thermal diffusion performance is also improved. Since it can be combined, it can be used suitably for electrical insulation.
- the material in which the nonwoven fabric of the present invention is impregnated with varnish can be suitably used as an electrical insulating material because it has a high dielectric breakdown voltage and excellent wet heat dimensional stability.
- various thermosetting resins and thermoplastic resins such as epoxy resin, phenol resin, polyimide, and polyamideimide resin can be used.
- the nonwoven fabric of this invention can be manufactured, for example with the following method.
- a material containing unstretched PPS fibers is dispersed in water, rolled up on a wire (papermaking net), and moisture is removed by drying (the process so far is the papermaking method).
- a heating / pressurizing process is performed with a calendar device.
- the two roll surface (hymen) temperatures of the calendar apparatus are processed at a temperature different by 10 ° C. or more.
- a stretched yarn of PPS fiber may be added.
- a dispersant or an antifoaming agent may be added to uniformly disperse the PPS fiber.
- the unstretched PPS fiber used is preferably 20% by mass or more of the whole nonwoven fabric. Further, from the viewpoint of compatibility between prevention of dew suitable for use in electrical insulation and varnish impregnation, unstretched PPS fibers are more preferably 30% by mass or more and 70% by mass or less of the whole nonwoven fabric.
- a paper machine and a dryer part attached to it can be used.
- the dryer part it is possible to use a process in which the wet paper rolled up by the paper machine in the previous process is transferred onto a belt, the water is squeezed between two belts, and dried on a rotating drum.
- the drying temperature of the rotating drum is preferably 90 to 120 ° C. This is because at this temperature, moisture can be efficiently removed, and the amorphous component contained in the unstretched PPS fiber remains without being softened, and fusion is caused by subsequent heating and pressurization with a calender device. This is because it occurs sufficiently.
- a preferred method for producing the nonwoven fabric of the present invention is to treat the two roll surface temperatures of the calender device at temperatures different by 10 ° C. or more when the calender device is heated and pressurized after the moisture is dried and removed.
- the calender device may be any one as long as it has two pairs of rolls and has heating and pressurizing means.
- Metal, paper, rubber or the like can be appropriately selected and used as the material of the roll.
- a roll of metal such as iron is preferably used in order to reduce fine fluff on the nonwoven fabric surface.
- Another preferred aspect of the material of the roll is that one of the two is made of metal and the other is made of paper.
- the metal roll By setting the metal roll to a high surface temperature, while setting the paper roll to the low surface temperature side, it is possible to have a more remarkable difference in the surface state between the front and back of the resulting nonwoven fabric, which is preferable. .
- voids between the fibers remain and the water and varnish are well-suited, and excellent varnish impregnation can be exhibited.
- the occurrence of wrinkles in the width direction of the resulting nonwoven fabric can be reduced and thickness unevenness is less likely to occur than when only a metal roll is used.
- the features of the present invention are provided on the front and back surfaces of the two rolls by heating and pressurizing in a state where the surface temperatures of the two rolls are different by 10 ° C. or more.
- a large number of fused portions are selectively present and can be smoothed. Presence and smoothing of the fused portion makes it easy to repel water, and can also increase the tensile strength of the entire nonwoven fabric.
- the non-woven fabric surface on the side where the roll surface temperature is low since the gaps between the fibers remain, the familiarity with water and varnish is good and the varnish impregnation property is excellent.
- a preferable temperature when processing with two rolls of metal is such that one is in the range of 150 to 190 ° C. and the other is in the range of 190 to 220 ° C., and the surface temperature of the two rolls is different by 10 ° C. or more. By doing so, the obtained nonwoven fabric is preferable because it has both the wet heat dimensional stability and the varnish impregnation performance more remarkably.
- the two rolls are a paper roll and a metal roll
- the preferable roll temperature is such that the metal roll is in the range of 150 to 190 ° C. and the paper roll is in the range of 105 to 130 ° C. It is preferable that the temperature is different by 20 ° C.
- the heating / pressurizing treatment can be carried out without problems and the obtained nonwoven fabric is excellent in both wet heat dimensional stability and varnish impregnation performance.
- the surface temperature of the two rolls is preferably different by 15 ° C. or more because both the hygroscopic dimensional stability and the water absorption can be achieved with excellent performance.
- a linear pressure range of 100 to 8,000 N / cm can be preferably employed. By adopting a linear pressure of 100 to 8,000 N / cm, unstretched PPS fibers are sufficiently fused to express the strength of the nonwoven fabric, and have both the performances of prevention of dew condensation and varnish impregnation. A nonwoven fabric can be obtained.
- Thickness In accordance with JIS L 1096 (1999) applied mutatis mutandis according to JIS L 1906 (2000), under a pressure of 2 kPa with a pressurizer having a diameter of 22 mm, using a thickness measuring machine at 10 different points of the sample. Then, after waiting for 10 seconds to calm down the thickness, the thickness was measured and the average value was calculated.
- Varnish impregnation Two test pieces of 5 cm ⁇ 5 cm were collected, and polyamide imide resin, “Viromax” HR-11NN manufactured by Toyobo Co., Ltd. was used as the varnish, and the test piece was placed in a plastic vat at room temperature. After impregnating for 30 seconds and squeezing lightly, it was dried at 150 ° C. for 20 minutes with a hot air dryer, and the mass was measured. The amount of varnish impregnation was calculated by the following formula.
- Varnish impregnation amount (g / m 2 ) (mass after drying ⁇ mass before impregnation) /0.0025
- Varnish impregnation amount (%) (varnish impregnation amount (g / m 2 ) / non-woven fabric basis weight (g / m 2 ) ⁇ 100 (5)
- Dielectric breakdown voltage Two test pieces of 5 cm ⁇ 5 cm impregnated with varnish were used and measured according to JIS K 6911 (1995).
- a test piece is sandwiched between disc-shaped electrodes having a diameter of 25 mm and a mass of 250 g, air is used as a test medium, an AC voltage with a frequency of 60 Hz is applied while increasing the voltage at 0.25 kV / sec, and the voltage when dielectric breakdown occurs. It was measured.
- a dielectric breakdown voltage tester manufactured by Yasuda Seiki Seisakusho was used for the measurement.
- Shrinkage rate (%) (length before test ⁇ length after test) / (length before test) ⁇ 100 (Undrawn yarn of PPS fiber)
- “Torucon” registered trademark manufactured by Toray with a single fiber fineness of 3.0 dtex (diameter: 17 ⁇ m) and a cut length of 6 mm, product number S111 was used.
- PPS fiber drawn yarn As the stretched PPS fiber, “Torucon” (registered trademark) manufactured by Toray with a single fiber fineness of 1.0 dtex (diameter: 10 ⁇ m) and a cut length of 6 mm, product number S301 was used.
- TETORON (registered trademark) manufactured by Toray with a single fiber fineness of 2.2 dtex (diameter: 14 ⁇ m), product number T9615 was cut into 6 mm and used.
- Heating / pressurizing process A heating / pressurizing step was performed using a hydraulic three-roll calender processing machine (manufactured by Yuri Roll, model IH type H3RCM) composed of an iron roll and a paper roll.
- Example 1 An undrawn yarn of PPS fiber and a drawn yarn of PPS fiber were prepared so as to have a mass ratio shown in Table 1, and they were dispersed in water to prepare a dispersion.
- Wet paper was made from the dispersion with a handmade paper machine. The wet paper was heated and dried at 110 ° C. for 70 seconds using a rotary dryer, and then the temperature on the iron roll side and the paper roll side was changed to 45 ° C. as shown in Table 1, and the linear pressure was 490 N / cm, A non-woven fabric was obtained by heating and pressing twice with the same surface facing the iron roll at a roll rotation speed of 5 m / min. The obtained non-woven fabric was excellent in wet heat dimensional stability and had sufficient varnish impregnation performance.
- the sample after impregnating the varnish had a high dielectric breakdown voltage and had excellent performance as an insulating material.
- Example 2 An undrawn yarn of PPS fiber and a drawn yarn of PPS fiber were prepared so as to have a mass ratio shown in Table 1, and they were dispersed in water to prepare a dispersion.
- Wet paper was made from the dispersion with a handmade paper machine. The wet paper was heated and dried at 110 ° C. for 70 seconds using a rotary dryer, and then the temperature on the iron roll side and the paper roll side was changed to 55 ° C. as shown in Table 1, and the linear pressure was 490 N / cm, A non-woven fabric was obtained by heating and pressing twice with the same surface facing the iron roll at a roll rotation speed of 5 m / min.
- Example 1 A drawn fiber of polyester fiber and a drawn yarn of PPS fiber were prepared so as to have a mass ratio shown in Table 1, and they were dispersed in water to prepare a dispersion.
- Wet paper was made from the dispersion with a handmade paper machine. The wet paper was heated and dried at 110 ° C. for 70 seconds using a rotary dryer. Subsequently, the temperature on the iron roll side and the paper roll side was changed to 55 ° C. as shown in Table 1, and an attempt was made to heat and press at a linear pressure of 490 N / cm and a roll rotation speed of 5 m / min.
- Example 3 Similarly to the reference example, a drawn fiber of polyester fiber and a drawn yarn of PPS fiber were prepared so as to have a mass ratio shown in Table 1, and they were dispersed in water to prepare a dispersion.
- a wet paper was prepared from the dispersion with a handmade paper machine, and heated and dried at 110 ° C. for 70 seconds using a rotary dryer. Subsequently, the temperature on the iron roll side and the paper roll side was changed to 60 ° C. as shown in Table 1, and the nonwoven fabric was obtained by heating and pressurizing only once at a linear pressure of 490 N / cm and a roll rotation speed of 5 m / min.
- the varnish impregnation performance of the obtained nonwoven fabric was sufficient as in Example 2. Although the dielectric breakdown voltage was lower than that of Example 1, it was good.
- Example 4 An undrawn yarn of PPS fiber and a drawn yarn of PPS fiber were prepared so as to have a mass ratio shown in Table 2, and they were dispersed in water to prepare a dispersion.
- Wet paper was made from the dispersion with a handmade paper machine. The wet paper was dried at 110 ° C. for 70 seconds using a rotary dryer, and then the temperature on the iron roll side and the paper roll side was changed to 35 ° C. as shown in Table 1, with a linear pressure of 490 N / cm and roll rotation.
- the nonwoven fabric was obtained by heating and pressurizing only once at a speed of 5 m / min. The obtained nonwoven fabric was excellent in wet heat dimensional stability and had high varnish impregnation performance as in Example 3.
- the wet paper was heated and dried at 110 ° C. for 70 seconds using a rotary dryer. Subsequently, the temperature on the iron roll side and the paper roll side was set as shown in Table 1, and each time the linear pressure was 490 N / cm and the roll rotation speed was 5 m / min. The mixture was heated and pressurized to obtain a nonwoven fabric.
- the obtained non-woven fabric was one in which unstretched PPS fibers were fused on both the front surface and the back surface of the non-woven fabric, and the varnish impregnation performance and wet heat dimensional stability were greatly inferior.
- the sample after impregnating the varnish also had a low dielectric breakdown voltage.
- Example 4 is a paper composed only of PPS fibers, and since the absolute value of the contact angle of the surface is higher than those of Example 1 and Example 2 having the same structure, it is easy to repel moisture from the air, and varnish. The impregnation property was high. Further, in Reference Example 2 having the same configuration, the contact angle could be increased, but varnish impregnation was impossible due to weak nonwoven fabric strength.
Abstract
Description
PPS繊維からなる紙をロール拭き取り材として採用するコピー機が増加している。このPPS繊維からなる紙は、PPS繊維として捲縮を有する繊維を採用することで低目付でもシート強力が高く、かつ緻密で均一な紙とすることができたと言われている(特許文献1参照)。特許文献1では、具体的な用途として耐熱性電気絶縁材料や電池セパレータを提案している。
本発明の不織布は抄紙法で得られるものである。抄紙法とは原料となる繊維を水に分散し、必要に応じて分散剤や消泡剤等を加えた抄紙原液を調整する。その後に、抄紙原液を抄紙機に通じて漉きあげ抄紙とするものである。抄紙機は、一般的な構造のものであれば問題なく採用することができる。抄紙機としては、円網、長網および短網のいずれでも良い。得られた湿紙をベルト上に載せて、水を絞りつつ乾燥して巻き取ることにより抄紙法で得られた不織布とすることができる。
-(C6H4-S)-
を主な構造単位とする重合体からなる合成繊維である。これらPPS重合体の代表例としては、ポリフェニレンスルフィド、ポリフェニレンスルフィドスルホン、ポリフェニレンスルフィドケトン、これらのランダム共重合体、ブロック共重合体およびそれらの混合物などが挙げられる。特に好ましいPPS重合体としては、ポリマーの主要構造単位として、-(C6H4-S)-で表されるp-フェニレン単位を、好ましくは90モル%以上含有するポリフェニレンスルフィドが望ましい。質量の観点からは、p-フェニレン単位を80質量%、さらには90質量%以上含有するポリフェニレンスルフィドが望ましい。また本発明で用いられるPPS繊維は、抄紙法に用いることから、その繊維長が2~38mmの範囲内にあることが好ましい。繊維長が2~38mmの範囲内であれば、抄紙用の原液に均一に分散が可能となり、抄紙直後の濡れた状態(湿紙)で乾燥工程を通過させるのに必要な引張強力を有する。また、PPS繊維の太さについても、抄紙用の原液に繊維が凝集せずに均一分散できることから、単繊維繊度は0.1~10dtexの範囲内にあるものが好ましい。
未延伸のPPS繊維を水に分散する際、PPS繊維の延伸糸を加えても良く、必要に応じて分散剤や消泡剤を添加して、PPS繊維を均一に分散させることもできる。PPS繊維の延伸糸を加えることで、得られる不織布の引張強度が向上するので好ましい。ただし未延伸のPPS繊維が少なくなるとカレンダー装置で加熱・加圧処理を施した時に、融着部分が十分に発生しないため、露つき予防の効果が低下する傾向がある。そのため用いる未延伸のPPS繊維は不織布全体の20質量%以上が良い。さらに電気絶縁用途に用いる際に好適な露付き予防とワニス含浸性の両立という点から、未延伸のPPS繊維は不織布全体の30質量%以上、一方70質量%以下のものがより好ましい。
2本のロールをペーパーロールと金属ロールとする場合、好ましいロールの温度は、金属ロールを150~190℃の範囲内とし、ペーパーロールを105~130℃の範囲内にして、2本のロール表面温度を20℃以上異なる温度にすることが、加熱・加圧処理を問題なく実施でき、かつ、得られた不織布が湿熱寸法安定性とワニス含浸性の両方の性能に優れることから好ましい。より好ましくは2本のロール表面温度は15℃以上異なることが、吸湿寸法安定性と吸水性をいずれも優れた性能で両立できるので好ましい。ロール間の圧力については100~8,000N/cmの線圧範囲が好ましく採用できる。100~8,000N/cmの線圧を採用することで、未延伸のPPS繊維が十分に融着して不織布の強力を発現しつつ、露付き予防とワニス含浸性という2つの性能を兼備する不織布を得ることが可能となる。
(1)目付
JIS L 1913(2010)に準じて、25cm×25cmの試験片を3枚採取し、標準状態(20℃±2℃、65±4%RH)におけるそれぞれの質量(g)を量り、1m2当たりの質量(g/m2)で表した。
JIS L 1906(2000)で準用するJIS L 1096(1999)に準じて、試料の異なる10か所について、厚さ測定機を用いて、直径22mmの加圧子による2kPaの加圧下、厚さを落ち着かせるために10秒間待った後に厚さを測定し、平均値を算出した。
接触角の測定は、20℃、65%RHの環境でおこなった。JIS R 3257(1999)の「 6.」の静滴法に準じて、8cm×3.5cmの試験片を1枚採取し、両面テープを使ってプレパラート上に貼り付けて固定した。タイプ22Gの針を有する注射筒を用意し、液滴量2.0μlにて液滴を作成した。液滴作成には400msの負荷時間、2000mVの負荷電圧とした。液滴には蒸留水を使用した。また液滴が試験片上に静置してから1秒経過した時に接触角を測定した。液滴の接触角は協和界面科学(株)製DropMaster700を用い、協和界面科学(株)のFAMAS接触角測定[液滴法]アドインソフトウェアを用いてθ/2法で解析し、10点の平均値を算出した。
5cm×5cmの試験片を2枚採取し、ワニスとしてポリアミドイミド系樹脂、東洋紡績社製の“バイロマックス”HR-11NNを用い、プラスチック製のバット内で試験片に室温で30秒の間含浸して軽く絞った後、150℃で20分、熱風乾燥機で乾燥して質量を測定した。ワニス含浸量は以下の式で算出した。
ワニス含浸量(%)=(ワニス含浸量(g/m2)/カレンダー後の不織布目付け(g/m2)×100
(5)絶縁破壊電圧
ワニスを含浸した5cm×5cmの試験片を2枚用い、JIS K 6911(1995)に準じて測定した。直径25mm、質量250gの円盤状の電極で試験片を挟み、試験媒体には空気を用い、0.25kV/秒で電圧を上昇させながら周波数60Hzの交流電圧をかけ、絶縁破壊したときの電圧を測定した。測定には、絶縁破壊耐電圧試験機(安田精機製作所製)を使用した。
ワニスを含浸していない20cm×20cmの試験片を5枚採取し、温度20℃、湿度65%RHの室内でデシケータ中に24時間保管した。しかる後に温度25℃、湿度80%RHに調整した恒温恒湿室中に6時間、静置した後、試験片の大きさを測定し、次式でタテ方向とヨコ方向の収縮率を計算した。恒温恒湿室はTABAI ESPEC社製を使用した。
収縮率(%)=(試験前の長さ-試験後の長さ)/(試験前の長さ)×100
(PPS繊維の未延伸糸)
未延伸のPPS繊維として、単繊維繊度3.0dtex(直径17μm)、カット長6mmの東レ製“トルコン”(登録商標)、品番S111を用いた。
延伸されたPPS繊維として、単繊維繊度1.0dtex(直径10μm)、カット長6mmの東レ製“トルコン”(登録商標)、品番S301を用いた。
延伸されたポリエステル繊維として、単繊維繊度2.2dtex(直径14μm)、の東レ製“テトロン”(登録商標)、品番T9615を6mmにカットして用いた。
延伸されたパラ系アラミド繊維として、単繊維繊度1.7dtex(直径12μm)、カット長6mmの東レ・デュポン製“ケブラー”(登録商標)を用いた。
底に140メッシュの手漉き抄紙網を設置した大きさ25cm×25cm、高さ40cmの手すき抄紙機(熊谷理機工業製)を用いた。
手すき抄紙した後の乾燥には回転型乾燥機(熊谷理機工業製ROTARY DRYER DR-200)を用いた。
鉄ロールとペーパーロールとからなる油圧式3本ロールカレンダー加工機(由利ロール製、型式IH式H3RCM)を使用して加熱・加圧工程を施した。
PPS繊維の未延伸糸とPPS繊維の延伸糸とを表1の質量比率になるように準備し、それらを水に分散し分散液を作成した。分散液から手漉きの抄紙機で湿紙を作成した。湿紙を、回転型乾燥機を用いて110℃で70秒間加熱、乾燥し、続いて鉄ロール側とペーパーロール側の温度を表1のとおりに45℃異なる条件とし、線圧490N/cm、ロール回転速度5m/分で同じ面を鉄ロール側にして2回、加熱・加圧し、不織布を得た。得られた不織布は湿熱寸法安定性に優れるとともに、十分なワニス含浸性能を有するものであった。
PPS繊維の未延伸糸とPPS繊維の延伸糸とを表1の質量比率になるように準備し、それらを水に分散し分散液を作成した。分散液から手漉きの抄紙機で湿紙を作成した。湿紙を、回転型乾燥機を用いて110℃で70秒間加熱、乾燥し、続いて鉄ロール側とペーパーロール側の温度を表1のとおりに55℃異なる条件とし、線圧490N/cm、ロール回転速度5m/分で同じ面を鉄ロール側にして2回、加熱・加圧し、不織布を得た。得られた不織布は湿熱寸法安定性に優れるとともに、実施例1と同様に高いワニス含浸性能を有するものであった。
[参考例1]
ポリエステル繊維の延伸糸とPPS繊維の延伸糸とを表1の質量比率になるように準備し、それらを水に分散し分散液を作成した。分散液から手漉きの抄紙機で湿紙を作成した。湿紙を、回転乾燥機を用いて110℃で70秒間加熱、乾燥した。得られたものを、続いて鉄ロール側とペーパーロール側の温度を表1のとおりに55℃異なる条件とし、線圧490N/cm、ロール回転速度5m/分で加熱・加圧しようとしたが、ロール面に貼り付きが発生し、良好な不織布を得ることができなかった。
[実施例3]
参考例と同様にポリエステル繊維の延伸糸とPPS繊維の延伸糸とを表1の質量比率になるように準備し、それらを水に分散、分散液を作成した。分散液から手漉きの抄紙機で湿紙を作成し、回転乾燥機を用いて110℃で70秒間加熱・乾燥した。続いて鉄ロール側とペーパーロール側の温度を表1のとおりに60℃異なる条件とし、線圧490N/cm、ロール回転速度5m/分で1回のみ加熱・加圧し、不織布を得た。得られた不織布のワニス含浸性能は実施例2と同様、十分なものであった。絶縁破壊電圧は実施例1よりは低いものの良好なものであった。
PPS繊維の未延伸糸とPPS繊維の延伸糸とを表2の質量比率になるように準備し、それらを水に分散し、分散液を作成した。分散液から手漉きの抄紙機で湿紙を作成した。湿紙を、回転型乾燥機を用いて110℃で70秒間乾燥し、続いて鉄ロール側とペーパーロール側の温度を表1のとおりに35℃異なる条件とし、線圧490N/cm、ロール回転速度5m/分で1回のみ加熱・加圧し、不織布を得た。得られた不織布は湿熱寸法安定性に優れるとともに、実施例3と同様に高いワニス含浸性能を有するものであった。
[比較例1]
PPS繊維の未延伸糸とPPS繊維の延伸糸とを表2の質量比率になるように準備した。それらを水に分散して分散液を作成した。分散液から手漉きの抄紙機で湿紙を作成した。湿紙を、回転型乾燥機を用いて110℃で70秒間加熱、乾燥した。得られたものを、続いて鉄ロール側とペーパーロール側の温度を表1のとおりとし、線圧490N/cm、ロール回転速度5m/分で同じ面を鉄ロール側にして、2回、加熱・加圧処理した。カレンダー加工の温度が高かったため、表面(おもてめん)同様に裏面のPPS繊維の未延伸糸も融着が進み、得られた不織布は表面(おもてめん)と裏面とで表面状態に違いが無く、ワニス含浸性能の低いものであった。
またワニスを含浸した後のサンプルも絶縁破壊電圧が低いものであった。
[比較例2]
PPS繊維の未延伸糸とパラ系アラミド繊維の延伸糸とを表2の質量比率になるように準備した。それらを水に分散し分散液を作成した。分散液から手漉きの抄紙機で湿紙を作成した。湿紙を、回転型乾燥機を用いて110℃で70秒間加熱、乾燥した。得られたものを、続いて鉄ロール側とペーパーロール側の温度を表1のとおりにし、線圧490N/cm、ロール回転速度5m/分で異なる面が鉄ロール側になるよう、1回ずつ、加熱・加圧し、不織布を得た。得られた不織布は不織布の表面(おもてめん)、裏面ともにPPS繊維の未延伸糸が融着して存在するものであり、ワニス含浸性能と湿熱寸法安定性が大きく劣るものであった。
ワニスを含浸した後のサンプルも絶縁破壊電圧が低いものであった。
[参考例2]
PPS繊維の未延伸糸とPPS繊維の延伸糸とを表2の質量比率になるように準備した。それらを水に分散し分散液を作成した。分散液から手漉きの抄紙機で湿紙を作成した。得られた湿紙を回転乾燥機を用いずに室内で乾燥して不織布を得た。得られた不織布は表面(おもてめん)と裏面で接触角に差が無かった。また不織布強度が弱いため、ワニス含浸加工をすることができなかった。
Claims (8)
- ポリフェニレンサルファイド繊維を含んでなる不織布であり、該不織布が抄紙法で得られたもので、かつ、不織布表面(おもてめん)の水の接触角が不織布裏面の接触角よりも5°以上大きいことを特徴とする不織布。
- 不織布表面と不織布裏面の接触角が、いずれも70°~110°の範囲内であることを特徴とする請求項1記載の不織布。
- ポリフェニレンサルファイド繊維の一部に未延伸のポリフェニレンサルファイド繊維を含み、該未延伸のポリフェニレンサルファイド繊維が融着して不織布を構成しており、更に該融着が不織布表面に選択的に存在することを特徴とする請求項1または2記載の不織布。
- 電気絶縁用途に用いることを特徴とする請求項1~3のいずれかに記載の不織布。
- 上記請求項1~3のいずれかの不織布を使った電気絶縁材料。
- 未延伸のポリフェニレンサルファイド繊維を水に分散して抄紙網に漉き上げて水分を乾燥除去した後、カレンダー装置で加熱・加圧処理を行うことを特徴とする請求項1~4いずれかの不織布の製造方法であって、カレンダー装置の2本のロール表面(ひょうめん)温度を10℃以上異なる温度とすることを特徴とする不織布の製造方法。
- カレンダー装置が有する第1のロールの表面温度が、105~130℃、第2のロールの表面温度が150~190℃であることを特徴とする請求項6記載の不織布の製造方法。
- カレンダー装置が有する第1のロールの材質がペーパーであって、表面温度が、105~130℃、第2のロールの材質が金属であって、表面温度が150~190℃であることを特徴とする請求項6記載の不織布の製造方法。
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BRPI0920472B1 (pt) * | 2008-09-26 | 2019-09-17 | Whitford Corporation | Composição de fluoropolímero compreendendo politetrafluoroetileno de alto peso molecular (hptfe), politetrafluoroetileno de baixo peso molecular (lptfe) e fluoropolímero processável por fusão (mpf), revestimento aplicado a um substrato e película contendo tal composição |
CN101532212A (zh) * | 2009-04-23 | 2009-09-16 | 华南理工大学 | Pps纺粘非织造布及其复合产品以及制备方法 |
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- 2011-09-06 EP EP11823560.5A patent/EP2615206A4/en not_active Withdrawn
- 2011-09-06 US US13/819,263 patent/US8900413B2/en active Active
- 2011-09-06 CN CN201180042839.6A patent/CN103080418B/zh active Active
- 2011-09-06 JP JP2011542383A patent/JP5640993B2/ja active Active
- 2011-09-06 WO PCT/JP2011/070239 patent/WO2012033085A1/ja active Application Filing
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JP2020051004A (ja) * | 2018-09-28 | 2020-04-02 | 三菱製紙株式会社 | ポリフェニレンサルファイド繊維含有湿式不織布 |
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Also Published As
Publication number | Publication date |
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JP5640993B2 (ja) | 2014-12-17 |
JPWO2012033085A1 (ja) | 2014-01-20 |
EP2615206A1 (en) | 2013-07-17 |
CN103080418B (zh) | 2014-04-02 |
US20140144599A1 (en) | 2014-05-29 |
US8900413B2 (en) | 2014-12-02 |
CN103080418A (zh) | 2013-05-01 |
EP2615206A4 (en) | 2015-04-01 |
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