WO2021166461A1 - Method for producing recycled aramid paper - Google Patents

Method for producing recycled aramid paper Download PDF

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Publication number
WO2021166461A1
WO2021166461A1 PCT/JP2020/049089 JP2020049089W WO2021166461A1 WO 2021166461 A1 WO2021166461 A1 WO 2021166461A1 JP 2020049089 W JP2020049089 W JP 2020049089W WO 2021166461 A1 WO2021166461 A1 WO 2021166461A1
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Prior art keywords
aramid
paper
aramid paper
pulp
dried
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PCT/JP2020/049089
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French (fr)
Japanese (ja)
Inventor
竜士 藤森
成瀬　新二
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デュポン帝人アドバンスドペーパー株式会社
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Priority to KR1020227025910A priority Critical patent/KR20220113826A/en
Priority to CN202080097118.4A priority patent/CN115087776A/en
Publication of WO2021166461A1 publication Critical patent/WO2021166461A1/en

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    • 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
    • D21H13/26—Polyamides; Polyimides
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21B—FIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
    • D21B1/00—Fibrous raw materials or their mechanical treatment
    • D21B1/04—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres
    • D21B1/12—Fibrous raw materials or their mechanical treatment by dividing raw materials into small particles, e.g. fibres by wet methods, by the use of steam
    • D21B1/30—Defibrating by other means
    • D21B1/32—Defibrating by other means of waste paper
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/64—Paper recycling

Definitions

  • the present invention relates to a method for producing recycled aramid paper.
  • Aramid paper is a paper manufactured from a material having improved strength and thermal stability.
  • Aramid paper is a synthetic paper made of aromatic polyamide, has excellent heat resistance, flame resistance, electrical insulation, toughness and flexibility, and has been used as an electrical insulating material and a base for aircraft honeycombs.
  • paper containing Nomex® fibers from DuPont (USA) is a slurry in which poly (metaphenylene isophthalamide) flocs and fibrids are mixed in water and mixed. It is manufactured by making paper and processing it on a calendar. This paper has high strength and toughness as well as excellent electrical insulation even at high temperatures.
  • Patent Document 1 describes aramid paper containing aramid paper pulp produced by crushing dried aramid paper to a size that allows it to pass through a 6.4 to 12.7 mm sieve. It is disclosed.
  • Patent Document 1 does not specify the characteristics of aramid paper pulp that can be used as a raw material for paper, and if the micronization treatment for reuse is insufficient, paper pieces can be contained in the aramid paper pulp.
  • the raw material that retains its shape remains, and if paper is produced using the raw material in this state, the appearance and thickness of the paper will be uneven, which is not preferable.
  • An object of the present invention is to provide a method for producing recycled aramid paper, which uses aramid paper pulp made by reusing aramid paper, has sufficient mechanical properties, and has a good appearance.
  • the method for producing recycled aramid paper includes a disintegration step of disintegrating a piece of dried aramid paper formed from aramid short fibers and aramid fibrid in water to obtain aramid paper pulp, and papermaking of the paper pulp. It is characterized in that the aramid paper pulp is disintegrated so that the disintegration degree is 93% or more in the disintegration step including the papermaking process. According to the above-mentioned method for producing recycled aramid paper, in the disintegration step, the aramid paper pulp is disintegrated so that the degree of disintegration is 93% or more, so that the raw material in which the shape of the paper piece remains in the aramid paper pulp can be obtained. It is possible to obtain recycled aramid paper having almost no residue, improved mechanical properties, and a good appearance.
  • a miniaturization treatment step of performing a miniaturization treatment on aramid pulp and paper is further included.
  • the particle size of the piece of aramid paper can be reduced, and high-quality aramid paper can be recycled.
  • the aramid paper in the disintegration step, is dissociated using a disintegrator configured to generate a stirring force in the vertical direction in water.
  • Aramid paper has a low affinity for water, and even if a piece of aramid paper is dropped into water, the piece of paper floats on the surface of the water, and the dissociation does not proceed sufficiently.
  • the disintegration step is performed by a disintegrator configured to generate a stirring force in the vertical direction, so even a piece of aramid paper having a large size can be used.
  • the aramid paper can be disintegrated and reused as a raw material for papermaking. This makes it possible to reuse the dried aramid paper as a raw material for papermaking without crushing it into small pieces.
  • the crushing / cutting step of crushing and / or cutting the dried aramid paper to obtain a piece of paper is further included, and in the crushing / cutting step, the dried aramid paper has a maximum dimension of more than 12.7 mm. Crush and / or cut. Since aramid paper has a low affinity for water, a large piece of paper having a maximum size of more than 12.7 mm floats on the surface of the water, and disintegration does not proceed. On the other hand, according to the above-mentioned method for producing recycled aramid paper, the piece of aramid paper has a maximum size of more than 12.7 mm because the piece of paper sinks into water and circulates due to the stirring force in the vertical direction. However, it can be dissociated.
  • aramid paper pulp is mixed with aramid fibrid and / or aramid short fibers. According to the above-mentioned method for producing recycled aramid paper, recycled aramid paper having further improved mechanical performance can be obtained.
  • a recycled aramid paper having appropriate mechanical properties and a good appearance by using aramid paper pulp obtained by reusing scraps and damaged materials generated during papermaking of aramid paper.
  • a manufacturing method is provided.
  • the aramid means a linear polymer compound in which 60% or more of the amide bonds are directly bonded to the aromatic ring.
  • examples of such an aramid include polymetaphenylene isophthalamide and its copolymer, polyparaphenylene terephthalamide and its copolymer, and copolyparaphenylene 3,4'-diphenyl ether terephthalamide.
  • These aramids are industrially produced by, for example, a solution polymerization method by a condensation reaction with an aromatic acid dichloride and an aromatic diamine, a two-step interfacial polymerization method, etc., and can be obtained as commercial products. , Not limited to this.
  • polymetaphenylene isophthalamide is preferably used because it has properties such as good molding processability, heat adhesion, flame retardancy, and heat resistance.
  • the aramid fibrid is a film-like fine particle composed of aramid, and is sometimes referred to as aramid pulp.
  • Aramid fibrid has paper-making properties like ordinary wood (cellulose) pulp, and can be formed into a sheet by a paper machine after being dispersed in water.
  • a so-called beating process can be performed for the purpose of maintaining the quality suitable for papermaking. This beating process can be performed by a disc refiner, beater, or other papermaking raw material processing device that exerts a mechanical cutting action.
  • the morphological change of the fibrid can be monitored at the drainage degree (freeness) specified in JIS P8121.
  • the drainage degree of the aramid fibrid after the beating treatment is preferably in the range of 10 to 300 cm 3 (Canadian standard freeness). Aramid fibrids with a drainage level greater than 300 cm 3 may reduce the strength of the sheet material formed from it.
  • an aramid binder with a drainage degree smaller than 10 cm 3 is to be obtained, the utilization efficiency of the mechanical power to be input becomes small, the processing amount per unit time is often small, and further, the aramid five Since the lid is miniaturized too much, the so-called binder function is likely to deteriorate.
  • the aramid short fiber is a heat-resistant short fiber obtained by cutting a fiber made from aramid into a predetermined length, and examples of such a fiber include "Teijin Cornex (Teijin Co., Ltd.). Examples include, but are not limited to, those that can be obtained under trade names such as “Registered Trademarks)” and “Nomex (Registered Trademarks)” by DuPont.
  • the length of the aramid short fibers can generally be selected from the range of 1 mm or more and less than 25 mm, preferably 2 mm or more and less than 12 mm. If the length of the short fibers is smaller than 1 mm, the mechanical properties of the sheet material deteriorate, while if the short fibers are 25 mm or more, "entanglement” and “binding” occur during the production of aramid paper by the wet method described later. It is not preferable because it easily causes defects.
  • the fiber diameter of the aramid short fibers can be selected from the range of 0.1 to 40 ⁇ m, preferably 0.5 to 25 ⁇ m, and more preferably 1 to 20 ⁇ m.
  • the dried aramid paper is a sheet-like material mainly composed of the above-mentioned aramid fibrid, aramid short fibers, or a mixture thereof, and is described separately from the "aramid paper” described later.
  • the dried aramid paper generally has a thickness in the range of 20 ⁇ m to 1000 ⁇ m, and the dried aramid paper generally has a thickness in the range of 10 g / m 2 to 1000 g / m 2 , preferably 10 g / m 2 to 500 g / m 2 .
  • Dried aramid paper is generally produced by a method of mixing the above-mentioned aramid fibrid and aramid short fibers, and then forming the mixed aramid fibrid and aramid short fibers into a sheet. Specifically, for example, a method in which aramid fibrid and aramid short fibers are dry-blended and then a sheet is formed using an air flow, aramid fibrid and aramid short fibers are dispersed and mixed in a liquid medium, and then liquid permeable.
  • a method of discharging the material onto a support, for example, a net or a belt to form a sheet, removing the liquid and drying the material can be applied, and among these, a so-called wet method of using water as a medium is preferably selected.
  • the mixing ratio of the aramid fibrid and the aramid short fiber is arbitrary, but the ratio (mass ratio) of the aramid fibrid / aramid short fiber is preferably 1/9 to 9/1, more preferably 2 It is better to set it to / 8 to 8/2.
  • a single or mixed aqueous slurry containing at least aramid fibrid and aramid short fibers is sent to a paper machine to be dispersed, dehydrated, squeezed and dried, and then wound up as a sheet.
  • a paper machine a long net paper machine, a circular net paper machine, an inclined paper machine, a combination paper machine combining these, and the like are used.
  • a composite sheet composed of a plurality of paper layers can be obtained by forming a sheet of slurries having different compounding ratios and coalescing them. Additives such as dispersibility improvers, defoamers, and paper strength enhancers are used during papermaking as needed.
  • thermal pressure processing It is known that the dried aramid paper obtained as described above is subjected to thermal pressure processing at high temperature and high pressure between a pair of rolls to improve density, crystallinity, heat resistance, dimensional stability and other mechanical strength. Has been done.
  • the conditions for thermal pressure processing can be, for example, in the range of a temperature of 100 to 350 ° C. and a linear pressure of 50 to 400 kg / cm when a metal roll is used, but the conditions are not limited thereto. Multiple aramid papers can also be laminated during thermal pressure. Further, the above-mentioned thermal pressure processing can be performed a plurality of times in any order.
  • the aramid paper pulp refers to the above-mentioned dried aramid paper crushed and / or cut into small pieces.
  • the method for producing pulp and paper according to the present embodiment is a disintegration step in which dried aramid paper is put into water and the aramid paper is disintegrated to obtain heat-resistant pulp and paper, and a wet method in which the heat-resistant pulp and paper is subjected to a wet micronization treatment. Manufactured by performing a micronization process. Further, a crushing / cutting step of crushing or cutting the aramid paper to obtain a piece of paper may be performed before the disintegration step, a dust removal step may be performed after the disintegration step, or a dust prevention step may be performed after the wet miniaturization treatment step. A wet sieving step may be performed.
  • the dried aramid paper (hereinafter referred to as “dried aramid paper”) is disintegrated in water using a disintegrator having a stirring force in the vertical direction.
  • a disintegrator having a stirring force in the vertical direction for example, a pulper, a kneader, an intensityer pulper having a rotor arranged on the side surface (wall surface) of the tab, and the like are preferably used, but the present invention is not limited thereto.
  • FIG. 1 is a perspective view showing a configuration of a disintegrator used in the method for producing pulp and paper according to the present embodiment.
  • the disengagement machine 1 is a so-called insulator, and includes a tab 6, a motor 2, and a rotor 4.
  • the tab 6 includes a bottom surface 6A arranged obliquely and a side wall 6B erected upward on the edge of the bottom surface 6A.
  • the tab 6 is supported by connecting the lower surface of the bottom surface 6A to a plurality of leg members 8.
  • the lengths of the plurality of leg members 8 are different, and the legs 4 are supported so that the side on which the rotor 4 is provided is located downward.
  • the bottom surface 6A has an elliptical shape and is inclined downward toward the rotor 4.
  • the side wall 6B extends vertically upward from the edge of the bottom surface 6A, and the tip portion has a tapered shape toward the center.
  • a circular opening is formed in the portion surrounded by the upper end edge of the side wall 6B.
  • the rotor 4 is composed of a plurality of blades extending radially outward from the center on the upper surface of a circular disk.
  • the rotor 4 is provided at one end of the tab 6 along the long axis of the bottom surface 6A, and is located at the bottom of the bottom surface 6A.
  • the rotor 4 is connected to the rotation shaft of the motor 2 arranged below the tab 6. The rotor 4 rotates by driving the rotation shaft of the motor 2 to rotate.
  • baffle 10 extending in the vertical direction along the side wall 6B is provided inside the tab 6, a baffle 10 extending in the vertical direction along the side wall 6B is provided.
  • the baffle 10 is provided at the other end of the tab 6 along the long axis of the bottom surface 6A.
  • the baffle 10 has a triangular horizontal cross section, and its width and depth increase upward.
  • the baffle 10 extends in the vertical direction over substantially the entire length of the side wall 6B.
  • the tab 6 of the release machine 1 is filled with water.
  • a swirling flow centered on the rotation axis of the rotor 4 is generated over the entire vertical direction. Since the bottom surface 6A of the tab 6 is inclined downward toward the rotor 4, the swirling flow in the vicinity of the bottom surface 6A of the tab 6 becomes an upward flow. Further, when the swirling flow collides with the baffle 10, a downward flowing flow is generated. As a result, an ascending flow flowing from the bottom to near the surface and a descending flow flowing from near the surface to the bottom are generated in the tab 6, and these ascending and descending flows act as a stirring force for stirring the paper piece in the vertical direction. .. Further, the piece of paper existing at the bottom of the tab 6 is raised by the ascending flow, and the piece of paper existing near the water surface is drawn to the bottom of the tab 6 by the descending flow and cut by the blade of the rotor 4.
  • dried aramid paper has a low affinity for water and does not sink in water simply by contacting it with water. For this reason, in low-concentration pulpers and high-concentration pulpers having a rotor at the center of the bottom surface of a cylindrical tab, which is used for disintegrating pulp fibers made of wood pulp, for example, dry aramid paper and water are difficult to mix and disintegration does not proceed. Therefore, it is difficult to industrially produce aramid pulp and paper.
  • the size (or maximum dimension) of the long side of the dried aramid paper to be put into water in the disintegration step is a size exceeding 12.7 mm, preferably 50 mm or more.
  • the finer the size the higher the specific surface area of the dried aramid paper, which improves the affinity with water as described above, but dust is generated in the crushing / cutting process. It is easy to handle, which is not preferable in terms of the working environment in the crushing / cutting process, and the smaller the size, the lower the crushing efficiency. It is not preferable because it becomes difficult.
  • the dimensions and shape of the dried aramid paper to be put into water are not limited to this, and the dried aramid paper to be put into water may have a continuous sheet shape in the disintegration step.
  • the continuous sheet shape means a sheet having a long side of 1 m or more, and the width is 10 to 3000 mm, preferably 50 to 2000 mm, depending on the size of the tab of the releaser.
  • the concentration of the dried aramid paper in the above-mentioned disintegration step is 1.0 to 7.0% by weight, preferably 1.5 to 6.0% by weight, and more preferably 2.0 to 5.0% by weight.
  • concentration of the dried aramid paper is less than 1.0% by weight, the amount of dissociated aramid paper pulp (hereinafter, sometimes referred to as dissociated aramid paper pulp) obtained is relatively small, and in terms of energy and production efficiency. If it exceeds 7.0% by weight, the viscosity of the slurry becomes too high at the time of disaggregation, and it becomes difficult to proceed with disaggregation.
  • the liquid temperature of the aramid pulp and paper suspension in the disintegration step is 10 to 80 ° C., preferably normal temperature to 70 ° C.
  • an additive such as a dispersibility improver, a defoaming agent, a paper strength enhancer, or a disintegration accelerator which can be added at the time of the above-mentioned papermaking may be used.
  • the dried aramid paper Before the dried aramid paper is put into the disintegrator, if the dried aramid paper is large with respect to the opening of the tab 6, the dried aramid paper is subjected to a crushing / cutting step.
  • the crushed / cutting step the dried aramid paper is crushed and / or cut into pieces having a long side (maximum dimension) of more than 12.7 mm, more preferably a long side of 50 mm or more.
  • the long side (maximum dimension) of the dried aramid paper is preferably 1000 mm or less.
  • the crushing method is not particularly specified, but a method of crushing by a dry method is preferable.
  • a shredder is preferably used because there is little variation in size at the time of cutting and dust is less likely to be generated.
  • the heat-resistant pulp and paper thus obtained can be subjected to a wet miniaturization step of performing a wet miniaturization treatment.
  • Wet miniaturization treatment is a method of impacting aramid paper in an aqueous medium to reduce the particle size, and equipment that efficiently carries out such miniaturization treatment includes high-speed disintegrators, refiners, beaters, etc.
  • the present invention is not limited to these.
  • the degree of disintegration is mentioned as an index of the characteristics of the heat-resistant pulp and paper that can be subjected to the wet micronization treatment, and in the present embodiment, the degree of disintegration is 30% or more, preferably 35% or more. If the size of the piece of dried aramid paper is large, the disintegration is insufficient and there is a possibility that a large piece of paper may remain in the pulp and paper. May cause clogging. Therefore, particularly when the size of the dried aramid paper to be put into water during the disintegration step is 50 mm or more, the disintegration degree is preferably 30% or more.
  • the degree of disintegration is defined as JIS P8232, which is a plate having a slit gap of 150 ⁇ m, which is equivalent to 10 g of absolute dryness of heat-resistant pulp and paper disintegrated using an experimental screen device in which a screen plate is arranged. It is expressed by the absolute dry weight ratio of the heat-resistant pulp and paper that has passed through the screen to the total weight of the charged heat-resistant pulp and paper, and is calculated by the following formula.
  • the degree of disintegration of the aramid paper pulp used for the recycled aramid paper is 93% or more, preferably 94%, more preferably 95% or more.
  • the degree of dissociation is less than 93%, undissociated pieces of paper become apparent on the surface of the sheet when the sheet-like material is formed, resulting in poor appearance and non-uniform thickness of the obtained sheet, which is not preferable.
  • the recycled aramid paper refers to a sheet-like material containing the above-mentioned aramid paper pulp, and generally has a thickness in the range of 20 ⁇ m to 1000 ⁇ m like the above-mentioned dried aramid paper. There is. Further, the recycled aramid paper of the present embodiment generally has a basis weight in the range of 10 g / m 2 to 1000 g / m 2 , preferably 10 g / m 2 to 500 g / m 2.
  • the content of the aramid paper pulp in the total weight of the recycled aramid paper of the present embodiment is not particularly limited as long as it achieves the desired properties, but in order to maintain the process strength during the production of the recycled aramid paper. 1 to 90% by weight is preferable, 1 to 80% by weight is preferable in order to more sufficiently develop the process strength, and 1 to 70% by weight is further preferable to sufficiently develop the electrical insulation characteristic of the aramid paper. Is particularly preferable.
  • the balance may be, but is not limited to, new aramid fibrids, or a combination of these with aramid short fibers.
  • the recycled aramid paper of the present embodiment is produced by the paper pulp obtained by the above-mentioned method for producing paper pulp alone, or by a method of mixing paper pulp with aramid fibrid, aramid short fibers, and the like and then forming a sheet. NS.
  • a method can be applied in which fibers and the like are dispersed and mixed in a liquid medium and then discharged onto a liquid-permeable support, for example, a net or a belt to form a sheet, and the liquid is removed and dried.
  • the so-called wet manufacturing method which uses the above as a medium, is preferable.
  • an aqueous slurry containing at least the above-mentioned aramid pulp and / or aramid fibrid is sent to a paper machine to disperse it, and then dehydrated, squeezed and dried. , It is a method of winding up as a sheet.
  • a paper machine a long net paper machine, a circular net paper machine, an inclined paper machine, a combination paper machine combining these, and the like are used.
  • a composite sheet composed of a plurality of paper layers can be obtained by forming a sheet of slurries having different compounding ratios and coalescing them. Additives such as dispersibility improvers, defoamers, and paper strength enhancers are used during papermaking as needed.
  • fibrous components for example, aramid fiber, polyphenylene sulfide fiber, polyether ether ketone fiber, cellulose fiber, PVA fiber, polyester fiber, allylate fiber, liquid crystal polyester fiber, polyimide fiber and other organic fibers, etc.
  • Inorganic fiber glass fiber such as glass fiber, rock wool, asbestos, and boron fiber
  • the ratio of the aramid short fibers to the total constituent fibers is 80% by weight or more, more preferably 90% by weight or more.
  • the aramid fibrid has excellent properties as a binder, so that fine particles and other additive components can be efficiently captured. Then, in the production of the aramid paper of the present embodiment, the raw material yield is improved, and at the same time, the sheets are stacked in layers in the sheet, the through holes can be reduced, and the electrical insulation property is improved.
  • the recycled aramid paper thus obtained can be heat-pressed at high temperature and high pressure between a pair of flat plates or between metal rolls to improve the density and mechanical strength.
  • the conditions for thermal pressure processing include, but are not limited to, a temperature of 100 to 350 ° C. and a linear pressure of 50 to 400 kg / cm. It is also possible to simply press at room temperature without applying a heating operation. It is also possible to stack a plurality of recycled aramid papers during thermal pressure processing. It is also possible to perform the thermal pressure processing of the above a plurality of times in any order.
  • the following effects are exhibited.
  • the aramid paper pulp in the disintegration step, is disintegrated so that the degree of disintegration is 93% or more, so that almost no paper piece having a shape remains in the aramid paper pulp, and the mechanical properties are improved. It is possible to obtain recycled aramid paper which is improved and has a good appearance.
  • the aramid paper pulp includes the pulverization treatment step of performing the pulverization treatment, the particle size of the paper piece of the aramid paper can be reduced, and the high quality aramid paper can be regenerated. ..
  • aramid paper has a low affinity for water, and even if a piece of aramid paper is dropped into water, the piece of paper will float on the surface of the water and will not be sufficiently dissociated. In particular, when the size of the aramid paper is large, it is difficult to sink in water.
  • the disintegration step is performed by the disintegrator 1 configured to generate a stirring force in the vertical direction, the paper piece is on the water surface even if it is a large piece of aramid paper. Since it sinks into water and circulates, the aramid paper can be dissociated and reused as a raw material for papermaking. This makes it possible to reuse the dried aramid paper as a raw material for papermaking without crushing it into small pieces.
  • the dried aramid paper is crushed and / or cut so that the maximum size exceeds 12.7 mm.
  • aramid paper Since aramid paper has a low affinity for water, a large piece of paper with a maximum size of more than 12.7 mm floats on the surface of the water, and disintegration does not proceed. On the other hand, according to the present embodiment, the piece of paper sinks into the water and circulates due to the stirring force in the vertical direction, so that even a piece of aramid paper having a maximum size exceeding 12.7 mm is dissociated. be able to.
  • the aramid paper pulp is mixed with the aramid fibrid and / or the aramid short fibers, a recycled aramid paper having further improved mechanical performance can be obtained.
  • the absolute dry weights of the aramid pulp and paper that passed through the screen and the aramid pulp and paper remaining on the screen were measured and calculated by the following formula.
  • Sheet basis weight, thickness and density were measured according to JIS C 2300-2, and the density was calculated by (basis weight / thickness).
  • a fibrid of polymethaphenylene isophthalamide was produced by a method using a pulp particle production apparatus (wet precipitator) composed of a combination of a stator and a rotor described in JP-A-52-15621. This was treated with a breaker and a beater to prepare a length-weighted average fiber length of 0.9 mm (aramid fibrid drainage degree: 100 ml (Canadian standard freeness)). On the other hand, a meta-aramid fiber manufactured by DuPont (Nomex (registered trademark), single yarn fineness 2 denier) was cut to a length of 6 mm to obtain an aramid short fiber.
  • a pulp particle production apparatus wet precipitator
  • a breaker and a beater to prepare a length-weighted average fiber length of 0.9 mm (aramid fibrid drainage degree: 100 ml (Canadian standard freeness)
  • a meta-aramid fiber manufactured by DuPont Nomex (registered trademark), single yarn fine
  • Examples 1 to 3 The above disaggregated aramid paper pulp was diluted to a concentration of 1.0% and passed through a refiner (manufactured by Kumagai Riki Kogyo Co., Ltd., disc refiner) at a flow rate of 50 L / min with a minimum clearance to obtain aramid paper pulp.
  • the prepared aramid pulp and paper, aramid fibrid, and aramid short fibers were dispersed in water to prepare a slurry. These slurries were mixed so as to have the blending ratio (weight ratio) shown in Table 1, and recycled aramid paper was prepared by a tappy type hand-making machine (cross-sectional area 625 cm 2).
  • the prepared recycled aramid paper was hot-pressed with a metal calendar roll at a temperature of 330 ° C. and a linear pressure of 300 kg / cm to obtain a calendar-processed recycled aramid paper.
  • Table 1 shows the main characteristic values of the aramid pulp and paper thus obtained and the regenerated aramid paper processed by the calendar.
  • the aramid fibrid and aramid short fibers prepared in the above raw material preparation 1 were each dispersed in water to prepare a slurry. These slurries were mixed so that the blending ratio (weight ratio) of aramid fibrid and aramid short fibers was 1/1, and a sheet-like product was prepared by a tappy hand-making machine (cross-sectional area 625 cm 2). .. Next, the sheet-like material was hot-pressed with a metal calendar roll at a temperature of 330 ° C. and a linear pressure of 300 kg / cm to obtain a calendar-processed recycled aramid paper. Table 1 shows the main characteristic values of the calendar-processed recycled aramid paper thus obtained.
  • the calendar-processed recycled aramid papers obtained in Examples 1 to 3 have the same density and tensile strength as the conventional examples, although they contain a high proportion of aramid paper pulp.
  • the appearance is also good, although a few pieces of paper are confirmed, and the appearance after heat treatment does not change, which is useful as an aramid paper for applications such as electrically insulating paper.
  • Example 4 and 5 The disaggregated aramid pulp obtained in the above raw material preparation 2 is diluted to a concentration of 1.0% and passed through a refiner (manufactured by Kumagai Riki Kogyo Co., Ltd., a disc refiner) at a flow rate of 50 L / min with a minimum clearance, and then further.
  • Aramid pulp was obtained by passing through a wet sieve having an opening diameter of 1.4 mm.
  • the prepared aramid pulp and paper, aramid fibrid, and aramid short fibers were dispersed in water to prepare a slurry.
  • the calendar-processed recycled aramid papers obtained in Examples 4 and 5 have the same density and tensile strength as the conventional examples, although they contain a high proportion of aramid paper pulp. , Further, by increasing the degree of disintegration of the mixed aramid pulp and paper, a good appearance was exhibited.
  • the calendar-processed aramid papers of Comparative Examples 1 and 2 have a low degree of separation of the mixed aramid paper pulp, so that the density, thickness unevenness, and tensile strength are inferior to those of the examples, and the sheet appearance is also poor. ..

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Abstract

The present invention provides a method for producing recycled aramid paper having adequate mechanical characteristics and good appearance, said method using aramid paper pulp that is obtained by reusing aramid paper.　This method comprises: a disintegration step wherein aramid paper pulp is obtained by disintegrating pieces of dry aramid paper, which is formed from aramid short fibers and aramid fibrid, in water by means of a disintegration machine 1; and a papermaking step for papermaking the paper pulp. In the disintegration step, the aramid paper pulp is disintegrated so that the degree of disintegration is 93% or more.

Description

再生アラミド紙の製造方法Manufacturing method of recycled aramid paper
　本発明は、再生アラミド紙の製造方法に関する。 The present invention relates to a method for producing recycled aramid paper.
　強度が改善され、かつ、熱安定性を有する材料から製造された紙として、アラミド紙がある。アラミド紙は、芳香族ポリアミドからなる合成紙であり、優れた耐熱性、耐燃性、電気絶縁性、強靱性および可撓性を有し、電気絶縁材料及び航空機ハニカム用ベースとして使用されてきた。これらの材料のうち、デュポン（ＤｕＰｏｎｔ）（米国）のノーメックス（Ｎｏｍｅｘ）（登録商標）繊維を含む紙は、ポリ（メタフェニレンイソフタルアミド）フロックと、ファイブリッドとを水中で混合し、混合したスラリーを抄紙し、カレンダー加工することによって製造されている。この紙は、高温下においても、高い強度および強靱性を有すると共に優れた電気絶縁性を有する。 Aramid paper is a paper manufactured from a material having improved strength and thermal stability. Aramid paper is a synthetic paper made of aromatic polyamide, has excellent heat resistance, flame resistance, electrical insulation, toughness and flexibility, and has been used as an electrical insulating material and a base for aircraft honeycombs. Of these materials, paper containing Nomex® fibers from DuPont (USA) is a slurry in which poly (metaphenylene isophthalamide) flocs and fibrids are mixed in water and mixed. It is manufactured by making paper and processing it on a calendar. This paper has high strength and toughness as well as excellent electrical insulation even at high temperatures.
　このようなアラミド紙の製造工程において発生する端材や破損材を再利用する方法がこれまで検討されている。例えば、特許文献１には、乾燥アラミド紙を６．４－１２.７ｍｍのふるいを通過しうる大きさに粉砕し、この乾燥アラミド紙を用いて製造されたアラミド紙パルプを含有するアラミド紙が開示されている。 A method of reusing scraps and damaged materials generated in the manufacturing process of such aramid paper has been studied so far. For example, Patent Document 1 describes aramid paper containing aramid paper pulp produced by crushing dried aramid paper to a size that allows it to pass through a 6.4 to 12.7 mm sieve. It is disclosed.
特許第３０１２３６５号公報Japanese Patent No. 301265
　しかしながら、特許文献１には、紙の原料として使用可能なアラミド紙パルプの特性については規定されておらず、再利用するための微細化処理が不十分であると、アラミド紙パルプ中に紙片の形状を残したままの原料が残存することとなり、この状態の原料を用いて紙を作製すると、外観や厚みが不均一な紙となるため好ましくない。 However, Patent Document 1 does not specify the characteristics of aramid paper pulp that can be used as a raw material for paper, and if the micronization treatment for reuse is insufficient, paper pieces can be contained in the aramid paper pulp. The raw material that retains its shape remains, and if paper is produced using the raw material in this state, the appearance and thickness of the paper will be uneven, which is not preferable.
　本発明は、アラミド紙を再利用したアラミド紙パルプを使用し、十分な機械的特性を有し、且つ外観も良好な再生アラミド紙の製造方法を提供することを目的とする。 An object of the present invention is to provide a method for producing recycled aramid paper, which uses aramid paper pulp made by reusing aramid paper, has sufficient mechanical properties, and has a good appearance.
　本発明者らはかかる状況に鑑み、抄紙製造されたアラミド紙を再利用したアラミド紙パルプを用いて、機械的特性に優れ、外観良好なアラミド紙を開発すべく鋭意検討を進めた結果、本発明に到達した。 In view of this situation, the present inventors have made diligent studies to develop aramid paper having excellent mechanical properties and good appearance by using aramid paper pulp made by reusing aramid paper produced by papermaking. The invention has been reached.
　本発明の一態様による再生アラミド紙の製造方法は、アラミド短繊維及びアラミドファイブリッドから形成される乾燥アラミド紙の紙片を水中で離解させて、アラミド紙パルプを得る離解工程と、紙パルプを抄紙する抄紙工程と、を含み、離解工程において、離解度が９３％以上となるようにアラミド紙パルプを離解させることを特徴とする。
　上記の再生アラミド紙の製造方法によれば、離解工程において、離解度が９３％以上となるようにアラミド紙パルプを離解させることにより、アラミド紙パルプ中に紙片の形状を残したままの原料がほとんど残存しなくなり、機械的特性が向上され、かつ、外観が良好な再生アラミド紙を得ることができる。 The method for producing recycled aramid paper according to one aspect of the present invention includes a disintegration step of disintegrating a piece of dried aramid paper formed from aramid short fibers and aramid fibrid in water to obtain aramid paper pulp, and papermaking of the paper pulp. It is characterized in that the aramid paper pulp is disintegrated so that the disintegration degree is 93% or more in the disintegration step including the papermaking process.
According to the above-mentioned method for producing recycled aramid paper, in the disintegration step, the aramid paper pulp is disintegrated so that the degree of disintegration is 93% or more, so that the raw material in which the shape of the paper piece remains in the aramid paper pulp can be obtained. It is possible to obtain recycled aramid paper having almost no residue, improved mechanical properties, and a good appearance.
　本発明の一態様において、アラミド紙パルプに微細化処理を行う微細化処理工程をさらに含む。
　上記の再生アラミド紙の製造方法によれば、アラミド紙の紙片の粒度を小さくすることができ、高品質なアラミド紙を再生することができる。 In one aspect of the present invention, a miniaturization treatment step of performing a miniaturization treatment on aramid pulp and paper is further included.
According to the above-mentioned method for producing recycled aramid paper, the particle size of the piece of aramid paper can be reduced, and high-quality aramid paper can be recycled.
　本発明の一態様において、離解工程では、水中で鉛直方向の撹拌力を発生させるように構成された離解機を用いてアラミド紙を離解させる。
　アラミド紙は水との親和性が低く、アラミド紙の紙片を水中に投下しても、紙片が水面に浮遊してしまい、十分に離解が進まない。特に、アラミド紙の寸法が大きい場合には、水中に沈みにくい。これに対して、上記の再生アラミド紙の製造方法によれば、鉛直方向の攪拌力を発生させるように構成された離解機により離解工程を行うため、寸法が大きなアラミド紙の紙片であっても、紙片が水面に留まらずに水中まで沈んで回流するため、アラミド紙を離解させることができ、抄紙用原料としての再利用が可能になる。これにより、乾燥アラミド紙を細かく破砕等することなく、抄紙用原料として再利用することが可能になる。 In one aspect of the present invention, in the disintegration step, the aramid paper is dissociated using a disintegrator configured to generate a stirring force in the vertical direction in water.
Aramid paper has a low affinity for water, and even if a piece of aramid paper is dropped into water, the piece of paper floats on the surface of the water, and the dissociation does not proceed sufficiently. In particular, when the size of the aramid paper is large, it is difficult to sink in water. On the other hand, according to the above-mentioned method for producing recycled aramid paper, the disintegration step is performed by a disintegrator configured to generate a stirring force in the vertical direction, so even a piece of aramid paper having a large size can be used. Since the piece of paper does not stay on the surface of the water but sinks into the water and circulates, the aramid paper can be disintegrated and reused as a raw material for papermaking. This makes it possible to reuse the dried aramid paper as a raw material for papermaking without crushing it into small pieces.
　本発明の一態様において、乾燥アラミド紙を粉砕及び／又は切断して紙片を得る粉砕／切断工程をさらに含み、粉砕／切断工程では、乾燥アラミド紙を、最大寸法が１２．７ｍｍを超えるように粉砕及び／又は切断する。
　アラミド紙は水との親和性が低いため、最大寸法が１２．７ｍｍを超える大きい紙片は水面に浮遊してしまい、離解が進まない。これに対して、上記の再生アラミド紙の製造方法によれば、鉛直方向の攪拌力により、紙片が水中に沈んで回流するため、最大寸法が１２．７ｍｍを超えるようなアラミド紙の紙片であっても、離解させることができる。 In one aspect of the present invention, the crushing / cutting step of crushing and / or cutting the dried aramid paper to obtain a piece of paper is further included, and in the crushing / cutting step, the dried aramid paper has a maximum dimension of more than 12.7 mm. Crush and / or cut.
Since aramid paper has a low affinity for water, a large piece of paper having a maximum size of more than 12.7 mm floats on the surface of the water, and disintegration does not proceed. On the other hand, according to the above-mentioned method for producing recycled aramid paper, the piece of aramid paper has a maximum size of more than 12.7 mm because the piece of paper sinks into water and circulates due to the stirring force in the vertical direction. However, it can be dissociated.
　本発明の一態様において、アラミド紙パルプに、アラミドファイブリッド及び／又はアラミド短繊維を混合する混合処理を行う。
　上記の再生アラミド紙の製造方法によれば、より機械的性能が向上された再生アラミド紙が得られる。 In one aspect of the present invention, aramid paper pulp is mixed with aramid fibrid and / or aramid short fibers.
According to the above-mentioned method for producing recycled aramid paper, recycled aramid paper having further improved mechanical performance can be obtained.
　本発明によれば、アラミド紙の抄紙製造の際に発生する端材や破損材を再利用したアラミド紙パルプを使用し、適度な機械的特性を有し、且つ外観も良好な再生アラミド紙の製造方法が提供される。 According to the present invention, a recycled aramid paper having appropriate mechanical properties and a good appearance by using aramid paper pulp obtained by reusing scraps and damaged materials generated during papermaking of aramid paper. A manufacturing method is provided.
本発明の一実施形態による紙パルプの製造方法で用いられる離解機の構成を示す斜視図である。It is a perspective view which shows the structure of the disintegrator used in the manufacturing method of pulp and paper by one Embodiment of this invention.
［アラミド］
　本実施形態において、アラミドとは、アミド結合の６０％以上が芳香環に直接結合した線状高分子化合物を意味する。このようなアラミドとしては、例えば、ポリメタフェニレンイソフタルアミドおよびその共重合体、ポリパラフェニレンテレフタルアミドおよびその共重合体、コポリパラフェニレン・３，４’－ジフェニルエーテルテレフタルアミドなどが挙げられる。これらのアラミドは、例えば、芳香族酸二塩化物および芳香族ジアミンとの縮合反応による溶液重合法、二段階界面重合法等により工業的に製造されており、市販品として入手することができるが、これに限定されるものではない。これらのアラミドの中では、ポリメタフェニレンイソフタルアミドが、良好な成型加工性、熱接着性、難燃性、耐熱性などの特性を備えている点で好ましく用いられる。 [Aramid]
In the present embodiment, the aramid means a linear polymer compound in which 60% or more of the amide bonds are directly bonded to the aromatic ring. Examples of such an aramid include polymetaphenylene isophthalamide and its copolymer, polyparaphenylene terephthalamide and its copolymer, and copolyparaphenylene 3,4'-diphenyl ether terephthalamide. These aramids are industrially produced by, for example, a solution polymerization method by a condensation reaction with an aromatic acid dichloride and an aromatic diamine, a two-step interfacial polymerization method, etc., and can be obtained as commercial products. , Not limited to this. Among these aramids, polymetaphenylene isophthalamide is preferably used because it has properties such as good molding processability, heat adhesion, flame retardancy, and heat resistance.
［アラミドファイブリッド］
　本発明においてアラミドファイブリッドとは、アラミドからなるフィルム状微小粒子で、アラミドパルプと称することもある。製造方法は、例えば特公昭３５－１１８５１号、特公昭３７－５７３２号公報等に記載の方法が例示される。アラミドファイブリッドは、通常の木材（セルロース）パルプと同じように抄紙性を有し、水中分散した後、抄紙機にてシート状に成形することができる。この場合、抄紙に適した品質を保つ目的でいわゆる叩解処理を施すことができる。この叩解処理は、ディスクリファイナー、ビーター、その他の機械的切断作用を及ぼす抄紙原料処理機器によって実施することができる。この操作において、ファイブリッドの形態変化は、ＪＩＳ　Ｐ８１２１に規定の濾水度（フリーネス）でモニターすることができる。本発明において、叩解処理を施した後のアラミドファイブリッドの濾水度は、１０～３００ｃｍ3（カナダ標準ろ水度（カナディアンスタンダードフリーネス））の範囲内にあることが好ましい。濾水度が３００ｃｍ3よりも大きいアラミドファイブリッドでは、それから成形されるシート状材料の強度が低下する可能性がある。他方、１０ｃｍ3よりも小さな濾水度のアラミドファイブリッドを得ようとすると、投入する機械動力の利用効率が小さくなり、また、単位時間当たりの処理量が少なくなることが多く、さらに、アラミドファイブリッドの微細化が進行しすぎるため、いわゆるバインダー機能の低下を招きやすい。 [Aramid Five Brid]
In the present invention, the aramid fibrid is a film-like fine particle composed of aramid, and is sometimes referred to as aramid pulp. As the production method, for example, the methods described in Tokukousho 35-11851, Tokukousho 37-5732, and the like are exemplified. Aramid fibrid has paper-making properties like ordinary wood (cellulose) pulp, and can be formed into a sheet by a paper machine after being dispersed in water. In this case, a so-called beating process can be performed for the purpose of maintaining the quality suitable for papermaking. This beating process can be performed by a disc refiner, beater, or other papermaking raw material processing device that exerts a mechanical cutting action. In this operation, the morphological change of the fibrid can be monitored at the drainage degree (freeness) specified in JIS P8121. In the present invention, the drainage degree of the aramid fibrid after the beating treatment is preferably in the range of 10 to 300 cm 3 (Canadian standard freeness). Aramid fibrids with a drainage level greater than 300 cm 3 may reduce the strength of the sheet material formed from it. On the other hand, if an aramid binder with a drainage degree smaller than 10 cm 3 is to be obtained, the utilization efficiency of the mechanical power to be input becomes small, the processing amount per unit time is often small, and further, the aramid five Since the lid is miniaturized too much, the so-called binder function is likely to deteriorate.
［アラミド短繊維］
　本実施形態において、アラミド短繊維とは、アラミドを原料とする繊維を所定の長さに切断した耐熱性短繊維であり、そのような繊維としては、例えば、帝人株式会社の「テイジンコーネックス（登録商標）」、デュポン社の「ノーメックス（登録商標）」等の商品名で入手することができるものが挙げられるが、これらに限定されるものではない。 [Aramid short fiber]
In the present embodiment, the aramid short fiber is a heat-resistant short fiber obtained by cutting a fiber made from aramid into a predetermined length, and examples of such a fiber include "Teijin Cornex (Teijin Co., Ltd.). Examples include, but are not limited to, those that can be obtained under trade names such as "Registered Trademarks)" and "Nomex (Registered Trademarks)" by DuPont.
　アラミド短繊維の長さは、一般に１ｍｍ以上２５ｍｍ未満、好ましくは２ｍｍ以上１２ｍｍ未満の範囲から選ぶことができる。短繊維の長さが１ｍｍよりも小さいと、シート材料の力学特性が低下し、他方、２５ｍｍ以上のものは、後述する湿式法でのアラミド紙の製造に際して「からみ」「結束」などが発生しやすく欠陥の原因となりやすいため好ましくない。
　アラミド短繊維の繊維径は、０．１～４０μｍの範囲から選ぶことができ、好ましくは、０．５～２５μｍ、より好ましくは１～２０μｍである。 The length of the aramid short fibers can generally be selected from the range of 1 mm or more and less than 25 mm, preferably 2 mm or more and less than 12 mm. If the length of the short fibers is smaller than 1 mm, the mechanical properties of the sheet material deteriorate, while if the short fibers are 25 mm or more, "entanglement" and "binding" occur during the production of aramid paper by the wet method described later. It is not preferable because it easily causes defects.
The fiber diameter of the aramid short fibers can be selected from the range of 0.1 to 40 μm, preferably 0.5 to 25 μm, and more preferably 1 to 20 μm.
［乾燥アラミド紙］
　本実施形態において、乾燥アラミド紙とは、上記のアラミドファイブリッド、アラミド短繊維、又はこれらの混合物から主として構成されるシート状物であり、後述の「アラミド紙」と分けて表記する。乾燥アラミド紙は一般に２０μｍ～１０００μｍの範囲内の厚さを有し、さらに、乾燥アラミド紙は、一般に１０ｇ／ｍ2～１０００ｇ／ｍ2、好ましくは１０ｇ／ｍ2～５００ｇ／ｍ2の範囲内の坪量を有している。 [Dried aramid paper]
In the present embodiment, the dried aramid paper is a sheet-like material mainly composed of the above-mentioned aramid fibrid, aramid short fibers, or a mixture thereof, and is described separately from the "aramid paper" described later. The dried aramid paper generally has a thickness in the range of 20 μm to 1000 μm, and the dried aramid paper generally has a thickness in the range of 10 g / m 2 to 1000 g / m 2 , preferably 10 g / m 2 to 500 g / m 2 . Has a basis weight of.
　乾燥アラミド紙は、一般に、上記のアラミドファイブリッドとアラミド短繊維とを混合した後、混合したアラミドファイブリッドとアラミド短繊維をシート化する方法により製造される。具体的には、例えばアラミドファイブリッド及びアラミド短繊維を乾式ブレンドした後に、気流を利用してシートを形成する方法、アラミドファイブリッド及びアラミド短繊維を液体媒体中で分散混合した後、液体透過性の支持体、例えば網またはベルト上に吐出してシート化し、液体を除いて乾燥する方法などが適用できるが、これらのなかでも水を媒体として使用する、いわゆる湿式抄造法が好ましく選択される。ここで、アラミドファイブリッドとアラミド短繊維の混合割合は任意であるが、アラミドファイブリッド／アラミド短繊維の割合（質量比）を１／９～９／１とするのが好ましく、より好ましくは２／８～８／２とするのがよい。 Dried aramid paper is generally produced by a method of mixing the above-mentioned aramid fibrid and aramid short fibers, and then forming the mixed aramid fibrid and aramid short fibers into a sheet. Specifically, for example, a method in which aramid fibrid and aramid short fibers are dry-blended and then a sheet is formed using an air flow, aramid fibrid and aramid short fibers are dispersed and mixed in a liquid medium, and then liquid permeable. A method of discharging the material onto a support, for example, a net or a belt to form a sheet, removing the liquid and drying the material can be applied, and among these, a so-called wet method of using water as a medium is preferably selected. Here, the mixing ratio of the aramid fibrid and the aramid short fiber is arbitrary, but the ratio (mass ratio) of the aramid fibrid / aramid short fiber is preferably 1/9 to 9/1, more preferably 2 It is better to set it to / 8 to 8/2.
　湿式抄造法では、少なくともアラミドファイブリッド、アラミド短繊維を含有する単一または混合物の水性スラリーを、抄紙機に送液し分散した後、脱水、搾水および乾燥した後、シートとして巻き取る方法が知られている。抄紙機としては長網抄紙機、円網抄紙機、傾斜型抄紙機およびこれらを組み合わせたコンビネーション抄紙機などが利用される。コンビネーション抄紙機での製造の場合、配合比率の異なるスラリーをシート成形し合一することで複数の紙層からなる複合体シートを得ることができる。抄造の際に必要に応じて分散性向上剤、消泡剤、紙力増強剤などの添加剤が使用される。 In the wet papermaking method, a single or mixed aqueous slurry containing at least aramid fibrid and aramid short fibers is sent to a paper machine to be dispersed, dehydrated, squeezed and dried, and then wound up as a sheet. Are known. As the paper machine, a long net paper machine, a circular net paper machine, an inclined paper machine, a combination paper machine combining these, and the like are used. In the case of production with a combination paper machine, a composite sheet composed of a plurality of paper layers can be obtained by forming a sheet of slurries having different compounding ratios and coalescing them. Additives such as dispersibility improvers, defoamers, and paper strength enhancers are used during papermaking as needed.
［カレンダー加工］
　上記のようにして得られた乾燥アラミド紙は、一対のロール間にて高温高圧で熱圧加工することにより、密度、結晶化度、耐熱性、寸法安定性ほか機械強度を向上することが知られている。熱圧加工の条件は、例えば、金属製ロールを使用する場合、温度１００～３５０℃ 、線圧５０～４００ｋｇ／ｃｍの範囲内とすることができるが、これらに限定されるものではない。熱圧の際に複数のアラミド紙を積層することもできる。また、上記の熱圧加工を任意の順に複数回行うこともできる。 [Calendar processing]
It is known that the dried aramid paper obtained as described above is subjected to thermal pressure processing at high temperature and high pressure between a pair of rolls to improve density, crystallinity, heat resistance, dimensional stability and other mechanical strength. Has been done. The conditions for thermal pressure processing can be, for example, in the range of a temperature of 100 to 350 ° C. and a linear pressure of 50 to 400 kg / cm when a metal roll is used, but the conditions are not limited thereto. Multiple aramid papers can also be laminated during thermal pressure. Further, the above-mentioned thermal pressure processing can be performed a plurality of times in any order.
［アラミド紙パルプ］
　本実施形態においてアラミド紙パルプとは、上記の乾燥アラミド紙を粉砕及び／又は切断して細かくしたものを示す。 [Aramid Pulp]
In the present embodiment, the aramid paper pulp refers to the above-mentioned dried aramid paper crushed and / or cut into small pieces.
［紙パルプの製造方法］
　本実施形態の紙パルプの製造方法は、乾燥状態のアラミド紙を水中に投入し、アラミド紙を離解させて耐熱性紙パルプを得る離解工程と、耐熱性紙パルプに湿式微細化処理を施す湿式微細化処理工程とを行うことにより製造される。また、離解工程の前にアラミド紙を粉砕又は切断して紙片を得る粉砕／切断工程を行ってもよいし、離解工程の後に除じん工程を行ったり、湿式微細化処理工程の後に防じん工程や湿式ふるい分け工程を行ったりしてもよい。 [Pulp manufacturing method]
The method for producing pulp and paper according to the present embodiment is a disintegration step in which dried aramid paper is put into water and the aramid paper is disintegrated to obtain heat-resistant pulp and paper, and a wet method in which the heat-resistant pulp and paper is subjected to a wet micronization treatment. Manufactured by performing a micronization process. Further, a crushing / cutting step of crushing or cutting the aramid paper to obtain a piece of paper may be performed before the disintegration step, a dust removal step may be performed after the disintegration step, or a dust prevention step may be performed after the wet miniaturization treatment step. A wet sieving step may be performed.
［離解工程］
　離解工程は、上記のアラミド紙を乾燥した乾燥状態のアラミド紙（以下「乾燥アラミド紙」という）を鉛直方向に撹拌力を有する離解機を用いて水中で離解させる。鉛直方向に撹拌力を有する離解機としては、例えばタブの側面（壁面）にローターを配したパルパー、ニーダー、インテンサパルパなどが好ましく使用されるが、これらに限定されるものではない。 [Dissociation process]
In the disintegration step, the dried aramid paper (hereinafter referred to as "dried aramid paper") is disintegrated in water using a disintegrator having a stirring force in the vertical direction. As the disassembling machine having a stirring force in the vertical direction, for example, a pulper, a kneader, an intensityer pulper having a rotor arranged on the side surface (wall surface) of the tab, and the like are preferably used, but the present invention is not limited thereto.
　図１は、本実施形態による紙パルプの製造方法で用いられる離解機の構成を示す斜視図である。図１に示すように、離解機１は、いわゆるインテンサパルパであり、タブ６と、モーター２と、ローター４とを備える。
　タブ６は、斜めに配置された底面６Ａと、底面６Ａの縁に上方に向かって立設された側壁６Ｂとを備える。タブ６は、底面６Ａの下面が複数の脚部材８に接続されて、支持されている。複数の脚部材８の長さは異なっており、ローター４が設けられた側が下方に位置するように支持されている。 FIG. 1 is a perspective view showing a configuration of a disintegrator used in the method for producing pulp and paper according to the present embodiment. As shown in FIG. 1, the disengagement machine 1 is a so-called insulator, and includes a tab 6, a motor 2, and a rotor 4.
The tab 6 includes a bottom surface 6A arranged obliquely and a side wall 6B erected upward on the edge of the bottom surface 6A. The tab 6 is supported by connecting the lower surface of the bottom surface 6A to a plurality of leg members 8. The lengths of the plurality of leg members 8 are different, and the legs 4 are supported so that the side on which the rotor 4 is provided is located downward.
　底面６Ａは楕円形であり、ローター４に向かって下方に傾斜している。側壁６Ｂは、底面６Ａの縁から鉛直上方に向かって延び、先端部が中心に向かって先細り形状となっている。側壁６Ｂの上端縁で囲まれた部分には、円形の開口が形成されている。 The bottom surface 6A has an elliptical shape and is inclined downward toward the rotor 4. The side wall 6B extends vertically upward from the edge of the bottom surface 6A, and the tip portion has a tapered shape toward the center. A circular opening is formed in the portion surrounded by the upper end edge of the side wall 6B.
　ローター４は、円形の円板の上面に複数のブレードが中心から半径方向外方に向かって放射状に延びて構成されている。ローター４は、タブ６の底面６Ａの長軸に沿った一方の端部に設けられており、底面６Ａの最下部に位置している。ローター４は、タブ６の下方に配置されたモーター２の回転軸に接続されている。モーター２の回転軸が回転駆動されることにより、ローター４が回転する。 The rotor 4 is composed of a plurality of blades extending radially outward from the center on the upper surface of a circular disk. The rotor 4 is provided at one end of the tab 6 along the long axis of the bottom surface 6A, and is located at the bottom of the bottom surface 6A. The rotor 4 is connected to the rotation shaft of the motor 2 arranged below the tab 6. The rotor 4 rotates by driving the rotation shaft of the motor 2 to rotate.
　タブ６内には、側壁６Ｂに沿って上下方向に延びるようなバッフル１０が設けられている。バッフル１０は、タブ６の底面６Ａの長軸に沿った他方の端部に設けられている。バッフル１０は、水平断面が三角形状であり、上方に向かって幅及び奥行きが大きくなっている。バッフル１０は、鉛直方向に側壁６Ｂの略全長にわたって延びている。 Inside the tab 6, a baffle 10 extending in the vertical direction along the side wall 6B is provided. The baffle 10 is provided at the other end of the tab 6 along the long axis of the bottom surface 6A. The baffle 10 has a triangular horizontal cross section, and its width and depth increase upward. The baffle 10 extends in the vertical direction over substantially the entire length of the side wall 6B.
　離解機１のタブ６には水が充填されている。ローター４が回転するとローター４の回転軸を中心とした旋回流が鉛直方向全域にわたって発生する。タブ６の底面６Ａがローター４に向かって下方に傾斜しているため、タブ６の底面６Ａ近傍の旋回流は上昇流となる。また、旋回流はバッフル１０に衝突すると、下方に向かう下降流が生じる。これにより、タブ６内には、底部から表面近くまで流れる上昇流と、表面近くから底部まで流れる下降流とが生じ、これら上昇流及び下降流が紙片を鉛直方向に攪拌する攪拌力として作用する。さらに、タブ６内の底部に存在する紙片は上昇流により上昇し、水面近くに存在する紙片は下降流によりタブ６の底部まで引き込まれ、ローター４のブレードにより切断される。 The tab 6 of the release machine 1 is filled with water. When the rotor 4 rotates, a swirling flow centered on the rotation axis of the rotor 4 is generated over the entire vertical direction. Since the bottom surface 6A of the tab 6 is inclined downward toward the rotor 4, the swirling flow in the vicinity of the bottom surface 6A of the tab 6 becomes an upward flow. Further, when the swirling flow collides with the baffle 10, a downward flowing flow is generated. As a result, an ascending flow flowing from the bottom to near the surface and a descending flow flowing from near the surface to the bottom are generated in the tab 6, and these ascending and descending flows act as a stirring force for stirring the paper piece in the vertical direction. .. Further, the piece of paper existing at the bottom of the tab 6 is raised by the ascending flow, and the piece of paper existing near the water surface is drawn to the bottom of the tab 6 by the descending flow and cut by the blade of the rotor 4.
　一般的に乾燥アラミド紙は水との親和性が低く、単に水に触れさせるだけでは水中に沈まない。このため、例えば木材パルプからなるパルプ繊維の離解に用いられる、円筒型のタブの底面中心にローターを有する低濃度パルパーや高濃度パルパーでは、乾燥アラミド紙と水が混合しにくく離解が進まない。このため、工業的にアラミド紙パルプを製造することが困難である。 Generally, dried aramid paper has a low affinity for water and does not sink in water simply by contacting it with water. For this reason, in low-concentration pulpers and high-concentration pulpers having a rotor at the center of the bottom surface of a cylindrical tab, which is used for disintegrating pulp fibers made of wood pulp, for example, dry aramid paper and water are difficult to mix and disintegration does not proceed. Therefore, it is difficult to industrially produce aramid pulp and paper.
　本実施形態において、離解工程において、水中に投入する乾燥アラミド紙の長辺のサイズ（又は最大寸法）は１２．７ｍｍを超えるサイズであり、好ましくは５０ｍｍ以上である。１２．７ｍｍ以下の細かいサイズを用いる場合においては、より細かくなる程乾燥アラミド紙の比表面積が増加し、それにより前述の水との親和性が良くなるものの、粉砕／切断工程で粉塵が発生し易くなり、粉砕／切断工程における作業環境上好ましくない上、サイズが小さくなる程粉砕効率も低くなり、更にその後粉砕アラミド紙を離解機に投入する際に粉塵や紙片が舞うなど、取扱いが非常に困難となるため好ましくない。 In the present embodiment, the size (or maximum dimension) of the long side of the dried aramid paper to be put into water in the disintegration step is a size exceeding 12.7 mm, preferably 50 mm or more. When a fine size of 12.7 mm or less is used, the finer the size, the higher the specific surface area of the dried aramid paper, which improves the affinity with water as described above, but dust is generated in the crushing / cutting process. It is easy to handle, which is not preferable in terms of the working environment in the crushing / cutting process, and the smaller the size, the lower the crushing efficiency. It is not preferable because it becomes difficult.
　また、水中に投入する乾燥アラミド紙の寸法及び形状はこれに限らず、離解工程において、水中に投入する乾燥アラミド紙が連続したシート形状を有していてもよい。本実施形態において連続したシート形状とは、長辺が１ｍ以上であるシートのことを示し、幅は離解機のタブのサイズにもよるが、１０～３０００ｍｍ、好ましくは５０～２０００ｍｍである。 Further, the dimensions and shape of the dried aramid paper to be put into water are not limited to this, and the dried aramid paper to be put into water may have a continuous sheet shape in the disintegration step. In the present embodiment, the continuous sheet shape means a sheet having a long side of 1 m or more, and the width is 10 to 3000 mm, preferably 50 to 2000 mm, depending on the size of the tab of the releaser.
　上記の離解工程における乾燥アラミド紙の濃度は、１．０～７．０重量％、好ましくは１．５～６．０重量％、より好ましくは２．０～５．０重量％である。乾燥アラミド紙の濃度が１．０重量％未満の場合は得られる離解処理されたアラミド紙パルプ（以下、離解アラミド紙パルプと称すことがある）が相対的に少なくなり、エネルギーや生産効率の点で好ましくなく、７．０重量％を超えると離解の際にスラリーの粘性が高くなり過ぎ、離解を進めることが困難となる。また離解工程におけるアラミド紙パルプ懸濁液の液温は、１０～８０℃、好ましくは常温～７０℃である。一般的に液温を高めた方が離解処理効率は向上するものの、８０℃を超えるとその効果は飽和するため、エネルギーの無駄になり好ましくない。
　また、離解の際に、前述の抄造の際にも添加可能な分散性向上剤、消泡剤、紙力増強剤、或いは離解促進剤などの添加剤を使用してもよい。 The concentration of the dried aramid paper in the above-mentioned disintegration step is 1.0 to 7.0% by weight, preferably 1.5 to 6.0% by weight, and more preferably 2.0 to 5.0% by weight. When the concentration of the dried aramid paper is less than 1.0% by weight, the amount of dissociated aramid paper pulp (hereinafter, sometimes referred to as dissociated aramid paper pulp) obtained is relatively small, and in terms of energy and production efficiency. If it exceeds 7.0% by weight, the viscosity of the slurry becomes too high at the time of disaggregation, and it becomes difficult to proceed with disaggregation. The liquid temperature of the aramid pulp and paper suspension in the disintegration step is 10 to 80 ° C., preferably normal temperature to 70 ° C. Generally, increasing the liquid temperature improves the dissociation treatment efficiency, but if the temperature exceeds 80 ° C., the effect is saturated, which is not preferable because energy is wasted.
Further, at the time of disintegration, an additive such as a dispersibility improver, a defoaming agent, a paper strength enhancer, or a disintegration accelerator which can be added at the time of the above-mentioned papermaking may be used.
［粉砕／切断工程］
　乾燥アラミド紙を離解機に投入する前に、乾燥アラミド紙がタブ６の開口に対して大きい場合には、乾燥アラミド紙に対して粉砕／切断工程を行う。粉砕／切断工程では、乾燥アラミド紙を長辺（最大寸法）が１２．７ｍｍを超えるサイズ、より好ましくは、長辺が５０ｍｍ以上のサイズである紙片に粉砕及び／又は切断する。なお、乾燥アラミド紙を長辺（最大寸法）は、１０００ｍｍ以下であることが好ましい。粉砕方法としては、特に指定は無いが、乾式法で粉砕する方法が好ましい。具体的には、シュレッダー、クラッシャー、ボールミル、ジェットミル等を用いて粉砕する方法が挙げられるが、これらに限定されるものではない。本発明においては、裁断時のサイズのバラツキが少なく、且つ粉塵が出にくいという点で、シュレッダーが好ましく使用される。 [Crushing / cutting process]
Before the dried aramid paper is put into the disintegrator, if the dried aramid paper is large with respect to the opening of the tab 6, the dried aramid paper is subjected to a crushing / cutting step. In the crushing / cutting step, the dried aramid paper is crushed and / or cut into pieces having a long side (maximum dimension) of more than 12.7 mm, more preferably a long side of 50 mm or more. The long side (maximum dimension) of the dried aramid paper is preferably 1000 mm or less. The crushing method is not particularly specified, but a method of crushing by a dry method is preferable. Specific examples thereof include, but are not limited to, a method of crushing using a shredder, a crusher, a ball mill, a jet mill, or the like. In the present invention, a shredder is preferably used because there is little variation in size at the time of cutting and dust is less likely to be generated.
［湿式微細化工程］
　このようにして得られた耐熱性紙パルプに、湿式微細化処理を施す湿式微細化工程を行うことができる。湿式微細化処理とは、水媒体中でアラミド紙に衝撃を与えて粒度を小さくする方法であり、そのような微細化処理を効率的に実施する設備としては、高速離解機、リファイナー、ビーター等が例示できるが、これらに限定されるわけではない。 [Wet miniaturization process]
The heat-resistant pulp and paper thus obtained can be subjected to a wet miniaturization step of performing a wet miniaturization treatment. Wet miniaturization treatment is a method of impacting aramid paper in an aqueous medium to reduce the particle size, and equipment that efficiently carries out such miniaturization treatment includes high-speed disintegrators, refiners, beaters, etc. However, the present invention is not limited to these.
　湿式微細化処理を施すことが可能な耐熱性紙パルプの特性の指標として、離解度が挙げられ、本実施形態においては、離解度は３０％以上、好ましくは３５％以上である。
　乾燥アラミド紙の紙片のサイズが大きい場合には、離解が不十分となり、紙パルプ中にサイズの大きい紙片が残存する可能性があり、その場合には湿式微細化処理を行う際に微細化設備が詰まりを起こす可能性がある。このため、特に離解工程の際に水中に投入する乾燥アラミド紙のサイズが５０ｍｍ以上の場合には、離解度が３０％以上であることが好ましい。 The degree of disintegration is mentioned as an index of the characteristics of the heat-resistant pulp and paper that can be subjected to the wet micronization treatment, and in the present embodiment, the degree of disintegration is 30% or more, preferably 35% or more.
If the size of the piece of dried aramid paper is large, the disintegration is insufficient and there is a possibility that a large piece of paper may remain in the pulp and paper. May cause clogging. Therefore, particularly when the size of the dried aramid paper to be put into water during the disintegration step is 50 mm or more, the disintegration degree is preferably 30% or more.
［離解度］
　本実施形態において、離解度とは、ＪＩＳ　Ｐ８２３２に規定される、スクリーン板を配した実験用スクリーン装置を用いて、離解処理した耐熱性紙パルプの絶乾１０ｇ相当分を、スリット間隙１５０μｍの板を備えたスクリーン装置に通し、スクリーンを通過した耐熱性紙パルプの、投入した耐熱性紙パルプの全重量に対する絶乾重量比率で表され、下記の式により計算される。 [Dissolution]
In the present embodiment, the degree of disintegration is defined as JIS P8232, which is a plate having a slit gap of 150 μm, which is equivalent to 10 g of absolute dryness of heat-resistant pulp and paper disintegrated using an experimental screen device in which a screen plate is arranged. It is expressed by the absolute dry weight ratio of the heat-resistant pulp and paper that has passed through the screen to the total weight of the charged heat-resistant pulp and paper, and is calculated by the following formula.
　［スクリーンを通過したアラミド紙パルプの絶乾重量］／（［スクリーン上に残ったアラミド紙パルプの絶乾重量］＋［スクリーンを通過したアラミド紙パルプの絶乾重量］）×１００（％） [Aramid paper pulp that has passed through the screen] / ([Aramid pulp that remains on the screen] + [Aramid pulp that has passed through the screen]) x 100 (%)
　本実施形態において、再生アラミド紙に用いられるアラミド紙パルプの、離解度は９３％以上であり、好ましくは９４％、より好ましくは９５％以上である。離解度が９３％未満の場合、シート状物を形成した時にシート表面に未離解の紙片状物が顕在化し、外観不良はもとより、得られたシートの厚みも不均一となるため好ましくない。 In the present embodiment, the degree of disintegration of the aramid paper pulp used for the recycled aramid paper is 93% or more, preferably 94%, more preferably 95% or more. When the degree of dissociation is less than 93%, undissociated pieces of paper become apparent on the surface of the sheet when the sheet-like material is formed, resulting in poor appearance and non-uniform thickness of the obtained sheet, which is not preferable.
［再生アラミド紙］
　本実施形態において、再生アラミド紙とは、上記のアラミド紙パルプを含有するシート状物のことを示し、上記の乾燥アラミド紙と同様に、一般に２０μｍ～１０００μｍの範囲内の厚さを有している。さらに、本実施形態の再生アラミド紙は、一般に１０ｇ／ｍ2～１０００ｇ／ｍ2、好ましくは１０ｇ／ｍ2～５００ｇ／ｍ2の範囲内の坪量を有している。 [Recycled aramid paper]
In the present embodiment, the recycled aramid paper refers to a sheet-like material containing the above-mentioned aramid paper pulp, and generally has a thickness in the range of 20 μm to 1000 μm like the above-mentioned dried aramid paper. There is. Further, the recycled aramid paper of the present embodiment generally has a basis weight in the range of 10 g / m 2 to 1000 g / m 2 , preferably 10 g / m 2 to 500 g / m 2.
　本実施形態の再生アラミド紙の全重量中に占めるアラミド紙パルプの含有量は、所望の特性を達成するのであれば特に制限はないが、再生アラミド紙の製造中における工程強度を保つためには１～９０重量％が好ましく、より十分に工程強度を発現させるためには１～８０重量％が好ましく、さらにアラミド紙の特徴である電気絶縁性を十分に発現するためには１～７０重量％が特に好ましい。残部は、新たなアラミドファイブリッド、又はこれとアラミド短繊維を併用するのがよいが、これらに限定されるものではない。 The content of the aramid paper pulp in the total weight of the recycled aramid paper of the present embodiment is not particularly limited as long as it achieves the desired properties, but in order to maintain the process strength during the production of the recycled aramid paper. 1 to 90% by weight is preferable, 1 to 80% by weight is preferable in order to more sufficiently develop the process strength, and 1 to 70% by weight is further preferable to sufficiently develop the electrical insulation characteristic of the aramid paper. Is particularly preferable. The balance may be, but is not limited to, new aramid fibrids, or a combination of these with aramid short fibers.
［再生アラミド紙の製造方法］
　本実施形態の再生アラミド紙は、上記の紙パルプの製造方法により得られた紙パルプ単独で、或いは紙パルプとアラミドファイブリッドやアラミド短繊維などとを混合した後、シート化する方法により製造される。 [Manufacturing method of recycled aramid paper]
The recycled aramid paper of the present embodiment is produced by the paper pulp obtained by the above-mentioned method for producing paper pulp alone, or by a method of mixing paper pulp with aramid fibrid, aramid short fibers, and the like and then forming a sheet. NS.
　シート製造にあたっては、例えば上記のアラミド紙パルプとアラミドファイブリッドやアラミド短繊維などとを乾式ブレンドした後に、気流を利用してシートを形成する方法、上記のアラミド紙パルプとアラミドファイブリッドやアラミド短繊維などとを液体媒体中で分散混合した後、液体透過性の支持体、例えば網またはベルト上に吐出してシート化し、液体を除いて乾燥する方法などを適用できるが、これらのなかでも水を媒体として使用する、いわゆる湿式抄造法が好ましい。 In sheet production, for example, a method of forming a sheet by dry blending the above-mentioned aramid paper pulp with aramid fibrid or aramid short fiber and then using an air flow, the above-mentioned aramid paper pulp and aramid fibrid or aramid short fiber. A method can be applied in which fibers and the like are dispersed and mixed in a liquid medium and then discharged onto a liquid-permeable support, for example, a net or a belt to form a sheet, and the liquid is removed and dried. The so-called wet manufacturing method, which uses the above as a medium, is preferable.
　湿式抄造法では、少なくとも上記のアラミド紙パルプ、及び／又はアラミドファイブリッドを含有する単一または混合物の水性スラリーを、抄紙機に送液し分散した後、脱水、搾水および乾燥操作することによって、シートとして巻き取る方法である。抄紙機としては長網抄紙機、円網抄紙機、傾斜型抄紙機およびこれらを組み合わせたコンビネーション抄紙機などが利用される。コンビネーション抄紙機での製造の場合、配合比率の異なるスラリーをシート成形し合一することで複数の紙層からなる複合体シートを得ることができる。抄造の際に必要に応じて分散性向上剤、消泡剤、紙力増強剤などの添加剤が使用される。 In the wet papermaking method, an aqueous slurry containing at least the above-mentioned aramid pulp and / or aramid fibrid is sent to a paper machine to disperse it, and then dehydrated, squeezed and dried. , It is a method of winding up as a sheet. As the paper machine, a long net paper machine, a circular net paper machine, an inclined paper machine, a combination paper machine combining these, and the like are used. In the case of production with a combination paper machine, a composite sheet composed of a plurality of paper layers can be obtained by forming a sheet of slurries having different compounding ratios and coalescing them. Additives such as dispersibility improvers, defoamers, and paper strength enhancers are used during papermaking as needed.
　また、これ以外にその他の繊維状成分（例えばアラミド繊維、ポリフェニレンスルフィド繊維、ポリエーテルエーテルケトン繊維、セルロース系繊維、ＰＶＡ系繊維、ポリエステル繊維、アリレート繊維、液晶ポリエステル繊維、ポリイミド繊維などの有機繊維、ガラス繊維、ロックウール、アスベスト、ボロン繊維などの無機繊維ガラス繊維）を添加することが出来る。この場合、全構成繊維中に占めるアラミド短繊維の割合は、８０重量％以上、より好ましくは９０重量％以上である。 In addition to this, other fibrous components (for example, aramid fiber, polyphenylene sulfide fiber, polyether ether ketone fiber, cellulose fiber, PVA fiber, polyester fiber, allylate fiber, liquid crystal polyester fiber, polyimide fiber and other organic fibers, etc. Inorganic fiber glass fiber such as glass fiber, rock wool, asbestos, and boron fiber) can be added. In this case, the ratio of the aramid short fibers to the total constituent fibers is 80% by weight or more, more preferably 90% by weight or more.
　本実施形態の再生アラミド紙において、アラミドファイブリッドは、バインダーとして優れた特性を有しているため微粒子および他の添加成分を効率的に捕捉できる。そして、本実施形態のアラミド紙の製造において原料歩留まりが良好となると同時にシート内で層状に重なり、貫通孔を減少させることが可能で、電気絶縁性が向上する。 In the recycled aramid paper of the present embodiment, the aramid fibrid has excellent properties as a binder, so that fine particles and other additive components can be efficiently captured. Then, in the production of the aramid paper of the present embodiment, the raw material yield is improved, and at the same time, the sheets are stacked in layers in the sheet, the through holes can be reduced, and the electrical insulation property is improved.
　このようにして得られた再生アラミド紙は、一対の平板間または金属製ロール間にて高温高圧で熱圧加工することで密度、機械強度を向上することができる。熱圧加工の条件は、たとえば金属製ロール使用の場合、温度１００～３５０℃、線圧５０～４００ｋｇ／ｃｍが例示できるが、これらに限定されるものではない。加熱操作を加えずに常温で単にプレスだけを行うこともできる。熱圧加工の際に複数の再生アラミド紙を積層することもできる。の熱圧加工を任意の順に複数回行うこともできる。 The recycled aramid paper thus obtained can be heat-pressed at high temperature and high pressure between a pair of flat plates or between metal rolls to improve the density and mechanical strength. For example, in the case of using a metal roll, the conditions for thermal pressure processing include, but are not limited to, a temperature of 100 to 350 ° C. and a linear pressure of 50 to 400 kg / cm. It is also possible to simply press at room temperature without applying a heating operation. It is also possible to stack a plurality of recycled aramid papers during thermal pressure processing. It is also possible to perform the thermal pressure processing of the above a plurality of times in any order.
［作用効果］
　本実施形態によれば、以下の作用効果が奏される。
　本実施形態によれば、離解工程において、離解度が９３％以上となるようにアラミド紙パルプを離解させることにより、アラミド紙パルプ中に形状を残した紙片がほとんど残存しなくなり、機械的特性が向上され、かつ、外観が良好な再生アラミド紙を得ることができる。 [Action effect]
According to this embodiment, the following effects are exhibited.
According to the present embodiment, in the disintegration step, the aramid paper pulp is disintegrated so that the degree of disintegration is 93% or more, so that almost no paper piece having a shape remains in the aramid paper pulp, and the mechanical properties are improved. It is possible to obtain recycled aramid paper which is improved and has a good appearance.
　また、本実施形態によれば、アラミド紙パルプに微細化処理を行う微細化処理工程を含むため、アラミド紙の紙片の粒度を小さくすることができ、高品質なアラミド紙を再生することができる。 Further, according to the present embodiment, since the aramid paper pulp includes the pulverization treatment step of performing the pulverization treatment, the particle size of the paper piece of the aramid paper can be reduced, and the high quality aramid paper can be regenerated. ..
　また、アラミド紙は水との親和性が低く、アラミド紙の紙片を水中に投下しても、紙片が水面に浮遊してしまい、十分に離解が進まない。特に、アラミド紙の寸法が大きい場合には、水中に沈みにくい。これに対して、本実施形態によれば、鉛直方向の攪拌力を発生させるように構成された離解機１により離解工程を行うため、寸法が大きなアラミド紙の紙片であっても、紙片が水面に留まらずに水中まで沈んで回流するため、アラミド紙を離解させることができ、抄紙用原料としての再利用が可能になる。これにより、乾燥アラミド紙を細かく破砕等することなく、抄紙用原料として再利用することが可能になる。 Also, aramid paper has a low affinity for water, and even if a piece of aramid paper is dropped into water, the piece of paper will float on the surface of the water and will not be sufficiently dissociated. In particular, when the size of the aramid paper is large, it is difficult to sink in water. On the other hand, according to the present embodiment, since the disintegration step is performed by the disintegrator 1 configured to generate a stirring force in the vertical direction, the paper piece is on the water surface even if it is a large piece of aramid paper. Since it sinks into water and circulates, the aramid paper can be dissociated and reused as a raw material for papermaking. This makes it possible to reuse the dried aramid paper as a raw material for papermaking without crushing it into small pieces.
　また、本実施形態によれば、粉砕／切断工程では、乾燥アラミド紙を、最大寸法が１２．７ｍｍを超えるように粉砕及び／又は切断する。 Further, according to the present embodiment, in the crushing / cutting step, the dried aramid paper is crushed and / or cut so that the maximum size exceeds 12.7 mm.
　アラミド紙は水との親和性が低いため、最大寸法が１２．７ｍｍを超える大きい紙片は水面に浮遊してしまい、離解が進まない。これに対して、本実施形態によれば、鉛直方向の攪拌力により、紙片が水中に沈んで回流するため、最大寸法が１２．７ｍｍを超えるようなアラミド紙の紙片であっても、離解させることができる。 Since aramid paper has a low affinity for water, a large piece of paper with a maximum size of more than 12.7 mm floats on the surface of the water, and disintegration does not proceed. On the other hand, according to the present embodiment, the piece of paper sinks into the water and circulates due to the stirring force in the vertical direction, so that even a piece of aramid paper having a maximum size exceeding 12.7 mm is dissociated. be able to.
　また、本実施形態によれば、アラミド紙パルプに、アラミドファイブリッド及び／又はアラミド短繊維を混合する混合処理を行うため、より機械的性能が向上された再生アラミド紙が得られる。 Further, according to the present embodiment, since the aramid paper pulp is mixed with the aramid fibrid and / or the aramid short fibers, a recycled aramid paper having further improved mechanical performance can be obtained.
　以下、本発明について実施例を挙げて説明する。なお、これらの実施例は、本発明の内容を例示するためのものであり、本発明の内容を何ら限定するためのものではない。
［測定方法］
（１）離解度
　ＪＩＳ　Ｐ８２３２に準じて、アラミド紙パルプからなるスラリーの絶乾１０ｇ相当分を、スリット間隙１５０μｍの板を備えた試験用フラットスクリーン（熊谷理機工業株式会社製）に投入し、スクリーンを通過するアラミド紙パルプがなくなるまで十分に通過させた後、スクリーンを通過したアラミド紙パルプ、及びスクリーン上に残ったアラミド紙パルプの絶乾重量を測定し、下記の式で計算した。 Hereinafter, the present invention will be described with reference to examples. It should be noted that these examples are for exemplifying the contents of the present invention, and are not for limiting the contents of the present invention at all.
[Measuring method]
(1) Degree of Separation According to JIS P8232, 10 g of absolute dryness of a slurry made of aramid pulp and paper was put into a test flat screen (manufactured by Kumagai Riki Kogyo Co., Ltd.) equipped with a plate with a slit gap of 150 μm. After passing the aramid pulp and paper sufficiently until there was no aramid pulp and paper passing through the screen, the absolute dry weights of the aramid pulp and paper that passed through the screen and the aramid pulp and paper remaining on the screen were measured and calculated by the following formula.
［スクリーンを通過したアラミド紙パルプの絶乾重量］／（［スクリーン上に残ったアラミド紙パルプの絶乾重量］＋［スクリーンを通過したアラミド紙パルプの絶乾重量］）×１００（％） [Aramid pulp dry weight that has passed through the screen] / ([Aramid pulp dry weight remaining on the screen] + [Aramid pulp dry weight that has passed through the screen]) x 100 (%)
（２）長さ加重平均繊維長
　メッツォオートメーション社製ファイバーサイズアナライザーを用い、約１００００個の原料繊維についての長さ加重平均繊維長を測定した。 (2) Length-weighted average fiber length Using a fiber size analyzer manufactured by Mezzo Automation Co., Ltd., the length-weighted average fiber lengths of about 10,000 raw material fibers were measured.
（３）シートの坪量、厚み、密度
　シートの坪量及び厚みはＪＩＳ　Ｃ　２３００－２に準じて測定し、密度は（坪量／厚み）により算出した。 (3) Sheet basis weight, thickness and density The sheet basis weight and thickness were measured according to JIS C 2300-2, and the density was calculated by (basis weight / thickness).
（４）シートの厚みむら
　上記の（３）の厚み測定で用いた方法にて、連続した４０点の厚みを測定し、その標準偏差を厚みむらとした。 (4) Sheet thickness unevenness The thickness of 40 consecutive points was measured by the method used in the thickness measurement of (3) above, and the standard deviation was defined as the thickness unevenness.
（５）引張強度
　ＡＳＴＭ　Ｄ－８２８に準じて、縦方向と横方向について実施し、両者の平均値を引張強度として算出した。 (5) Tensile strength According to ASTM D-828, it was carried out in the vertical direction and the horizontal direction, and the average value of both was calculated as the tensile strength.
（６）シート外観
　２０ｃｍ角のシート各５枚の外観を目視で観察し、未離解の紙片状物が無く均一に見えるものを「○」、わずかに未離解の紙片状物が残存している（長辺サイズが１０ｍｍを超える紙片状物が合計５個以下）ものを「△」、未離解の紙片状物がはっきりと確認できる（「△」よりも多い）ものを「×」とした。 (6) Appearance of sheets The appearance of each of the five 20 cm square sheets was visually observed, and those that looked uniform without undissolved pieces of paper were marked with "○", and slightly undissolved pieces of paper remained. (A total of 5 or less pieces of paper with a long side size exceeding 10 mm) are marked with "△", and undissolved pieces of paper can be clearly confirmed (more than "△") with "×". ".
［原料調成１］
　特開昭５２－１５６２１号公報に記載のステーターとローターの組み合わせで構成されるパルプ粒子の製造装置（湿式沈殿機）を用いる方法によって、ポリメタフェニレンイソフタルアミドのファイブリッドを製造した。これを、離解機、叩解機で処理して長さ加重平均繊維長を０．９ｍｍに調製した（アラミドファイブリッドの濾水度：１００ｍｌ（カナディアンスタンダードフリーネス））。一方、デュポン社製メタアラミド繊維（ノーメックス（登録商標）、単糸繊度２デニール）を長さ６ｍｍに切断し、アラミド短繊維を得た。 [Ingredient preparation 1]
A fibrid of polymethaphenylene isophthalamide was produced by a method using a pulp particle production apparatus (wet precipitator) composed of a combination of a stator and a rotor described in JP-A-52-15621. This was treated with a breaker and a beater to prepare a length-weighted average fiber length of 0.9 mm (aramid fibrid drainage degree: 100 ml (Canadian standard freeness)). On the other hand, a meta-aramid fiber manufactured by DuPont (Nomex (registered trademark), single yarn fineness 2 denier) was cut to a length of 6 mm to obtain an aramid short fiber.
［乾燥アラミド紙の製造］
　調製したアラミドファイブリッドとアラミド短繊維をおのおの水中で分散しスラリーを作成した。これらのスラリーを、アラミドファイブリッドとアラミド短繊維が１／１の配合比率（重量比）となるように混合した後、フォードリニヤー型抄紙機へ送液し、脱水、搾水の後、１５０℃で乾燥して巻取り、乾燥アラミド紙を作製した。 [Manufacturing of dried aramid paper]
The prepared aramid fibrid and aramid short fibers were each dispersed in water to prepare a slurry. These slurries are mixed so that the blending ratio (weight ratio) of aramid fibrid and aramid short fibers is 1/1, and then the liquid is sent to a Fordliner type paper machine, dehydrated and squeezed, and then 150. It was dried at ° C. and rolled up to prepare dried aramid paper.
［原料調成２］
　上記の乾燥アラミド紙を粉砕又は切断し、表１及び表２に示すサイズに調整した。このサイズ調整した乾燥アラミド紙３重量部と水９７重量部とを、図１に示すような、インテンサパルパ（株式会社ＩＨＩフォイトペーパーテクノロジー製）に投入し、温度５０℃で４０分間離解し、離解アラミド紙パルプを調製した。 [Ingredient preparation 2]
The above dried aramid paper was pulverized or cut to adjust the size shown in Tables 1 and 2. 3 parts by weight of the size-adjusted dried aramid paper and 97 parts by weight of water were put into Intensa Pulp (manufactured by IHI Voith Paper Technology Co., Ltd.) as shown in FIG. Dissolved aramid paper pulp was prepared.
［実施例１～３］
　上記の離解アラミド紙パルプを濃度１．０％に希釈し、リファイナー（熊谷理機工業株式会社製、ディスクレファイナー）に流量５０Ｌ／ｍｉｎ、クリアランス最小で通し、アラミド紙パルプを得た。この調製したアラミド紙パルプ、アラミドファイブリッド、及びアラミド短繊維を、水に分散させてスラリーを作製した。これらのスラリーを、表１に示す配合比率（重量比）となるように混合し、タッピー式手抄き機（断面積６２５ｃｍ2）にて再生アラミド紙を作製した。次いで、作成した再生アラミド紙を金属製カレンダーロールにより温度３３０℃、線圧３００ｋｇ／ｃｍで熱圧加工し、カレンダー加工された再生アラミド紙を得た。このようにして得られたアラミド紙パルプ及びカレンダー加工された再生アラミド紙の主要特性値を表１に示す。 [Examples 1 to 3]
The above disaggregated aramid paper pulp was diluted to a concentration of 1.0% and passed through a refiner (manufactured by Kumagai Riki Kogyo Co., Ltd., disc refiner) at a flow rate of 50 L / min with a minimum clearance to obtain aramid paper pulp. The prepared aramid pulp and paper, aramid fibrid, and aramid short fibers were dispersed in water to prepare a slurry. These slurries were mixed so as to have the blending ratio (weight ratio) shown in Table 1, and recycled aramid paper was prepared by a tappy type hand-making machine (cross-sectional area 625 cm 2). Next, the prepared recycled aramid paper was hot-pressed with a metal calendar roll at a temperature of 330 ° C. and a linear pressure of 300 kg / cm to obtain a calendar-processed recycled aramid paper. Table 1 shows the main characteristic values of the aramid pulp and paper thus obtained and the regenerated aramid paper processed by the calendar.
［従来例］
　上記の原料調成１で調製したアラミドファイブリッドとアラミド短繊維をおのおの水中で分散しスラリーを作成した。これらのスラリーを、アラミドファイブリッドとアラミド短繊維が１／１の配合比率（重量比）となるように混合し、タッピー式手抄き機（断面積６２５ｃｍ2）にてシート状物を作製した。次いで、シート状物を金属製カレンダーロールにより温度３３０℃、線圧３００ｋｇ／ｃｍで熱圧加工し、カレンダー加工された再生アラミド紙を得た。このようにして得られた、カレンダー加工された再生アラミド紙の主要特性値を表１に示す。 [Conventional example]
The aramid fibrid and aramid short fibers prepared in the above raw material preparation 1 were each dispersed in water to prepare a slurry. These slurries were mixed so that the blending ratio (weight ratio) of aramid fibrid and aramid short fibers was 1/1, and a sheet-like product was prepared by a tappy hand-making machine (cross-sectional area 625 cm 2). .. Next, the sheet-like material was hot-pressed with a metal calendar roll at a temperature of 330 ° C. and a linear pressure of 300 kg / cm to obtain a calendar-processed recycled aramid paper. Table 1 shows the main characteristic values of the calendar-processed recycled aramid paper thus obtained.
Figure JPOXMLDOC01-appb-T000001
 ※連続：裁断されていない状態（ロール状）から乾燥アラミド紙を引き出しながら連続的に離解機に投入した
Figure JPOXMLDOC01-appb-T000001
 * Continuous: While pulling out the dried aramid paper from the uncut state (roll shape), it was continuously put into the disintegrator.
　表１の結果から、実施例１～３で得られた、カレンダー加工された再生アラミド紙は、アラミド紙パルプを高い比率で配合しているものの、従来例と同等の密度、引張強度を有し、外観もわずかに紙片が確認されたものの良好で、更に熱処理後の外観も変化が無く、アラミド紙として電気絶縁紙等の用途向けに有用である。 From the results in Table 1, the calendar-processed recycled aramid papers obtained in Examples 1 to 3 have the same density and tensile strength as the conventional examples, although they contain a high proportion of aramid paper pulp. The appearance is also good, although a few pieces of paper are confirmed, and the appearance after heat treatment does not change, which is useful as an aramid paper for applications such as electrically insulating paper.
［実施例４、５］
　上記の原料調成２で得た離解アラミド紙パルプを濃度１．０％に希釈し、リファイナー（熊谷理機工業株式会社製、ディスクレファイナー）に流量５０Ｌ／ｍｉｎ、クリアランス最小で通し、その後更に開口径１．４ｍｍの湿式ふるいに通し、アラミド紙パルプを得た。この調製したアラミド紙パルプ、アラミドファイブリッド、及びアラミド短繊維を、水に分散させてスラリーを作製した。これらのスラリーを、表２に示す配合比率（重量比）となるように混合し、タッピー式手抄き機（断面積６２５ｃｍ2）にて再生アラミド紙を作製した。次いで、これを金属製カレンダーロールにより温度３３０℃、線圧３００ｋｇ／ｃｍで熱圧加工し、カレンダー加工された再生アラミド紙を得た。このようにして得られたアラミド紙パルプ及びカレンダー加工された再生アラミド紙の主要特性値を表２に示す。 [Examples 4 and 5]
The disaggregated aramid pulp obtained in the above raw material preparation 2 is diluted to a concentration of 1.0% and passed through a refiner (manufactured by Kumagai Riki Kogyo Co., Ltd., a disc refiner) at a flow rate of 50 L / min with a minimum clearance, and then further. Aramid pulp was obtained by passing through a wet sieve having an opening diameter of 1.4 mm. The prepared aramid pulp and paper, aramid fibrid, and aramid short fibers were dispersed in water to prepare a slurry. These slurries were mixed so as to have the blending ratio (weight ratio) shown in Table 2, and recycled aramid paper was prepared by a tappy type hand-making machine (cross-sectional area 625 cm 2). Next, this was thermally pressure-processed with a metal calendar roll at a temperature of 330 ° C. and a linear pressure of 300 kg / cm to obtain a calendar-processed recycled aramid paper. Table 2 shows the main characteristic values of the aramid pulp and paper thus obtained and the regenerated aramid paper processed by the calendar.
［比較例１］
　上記の原料調成２で得た離解アラミド紙パルプ、調製したアラミドファイブリッド、及びアラミド短繊維を、水に分散させてスラリーを作製した。これらのスラリーを、表２に示す配合比率（重量比）となるように混合し、タッピー式手抄き機（断面積６２５ｃｍ2）にて再生アラミド紙を作製した。次いで、これを金属製カレンダーロールにより温度３３０℃、線圧３００ｋｇ／ｃｍで熱圧加工し、カレンダー加工された再生アラミド紙を得た。このようにして得られたアラミド紙パルプ及びカレンダー加工された再生アラミド紙の主要特性値を表２に示す。 [Comparative Example 1]
The disaggregated aramid paper pulp obtained in the above raw material preparation 2, the prepared aramid fibrid, and the aramid short fibers were dispersed in water to prepare a slurry. These slurries were mixed so as to have the blending ratio (weight ratio) shown in Table 2, and recycled aramid paper was prepared by a tappy type hand-making machine (cross-sectional area 625 cm 2). Next, this was thermally pressure-processed with a metal calendar roll at a temperature of 330 ° C. and a linear pressure of 300 kg / cm to obtain a calendar-processed recycled aramid paper. Table 2 shows the main characteristic values of the aramid pulp and paper thus obtained and the regenerated aramid paper processed by the calendar.
［比較例２］
　上記の原料調成２で得た離解アラミド紙パルプを濃度１．０％に希釈し、高速離解機（株式会社新浜ポンプ製作所製、ＶＦ）に流量５０Ｌ／ｍｉｎで通し、アラミド紙パルプを得た。この調製したアラミド紙パルプ、アラミドファイブリッド、及びアラミド短繊維を、水に分散させてスラリーを作製した。これらのスラリーを、表２に示す配合比率（重量比）となるように混合し、タッピー式手抄き機（断面積６２５ｃｍ2）にて再生アラミド紙を作製した。次いで、これを金属製カレンダーロールにより温度３３０℃、線圧３００ｋｇ／ｃｍで熱圧加工し、カレンダー加工された再生アラミド紙を得た。このようにして得られたアラミド紙パルプ及びカレンダー加工された再生アラミド紙の主要特性値を表２に示す。 [Comparative Example 2]
The disaggregated aramid pulp obtained in the above raw material preparation 2 was diluted to a concentration of 1.0% and passed through a high-speed disintegrator (manufactured by Shinhama Pump Mfg. Co., Ltd., VF) at a flow rate of 50 L / min to obtain aramid pulp. .. The prepared aramid pulp and paper, aramid fibrid, and aramid short fibers were dispersed in water to prepare a slurry. These slurries were mixed so as to have the blending ratio (weight ratio) shown in Table 2, and recycled aramid paper was prepared by a tappy type hand-making machine (cross-sectional area 625 cm 2). Next, this was thermally pressure-processed with a metal calendar roll at a temperature of 330 ° C. and a linear pressure of 300 kg / cm to obtain a calendar-processed recycled aramid paper. Table 2 shows the main characteristic values of the aramid pulp and paper thus obtained and the regenerated aramid paper processed by the calendar.
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
　表２の結果から、実施例４、５で得られた、カレンダー加工された再生アラミド紙は、アラミド紙パルプを高い比率で配合しているものの、従来例と同等の密度、引張強度を有し、さらに混合するアラミド紙パルプの離解度を高めたことにより、良好な外観を示した。一方で、比較例１、２のカレンダー加工されたアラミド紙は、混合するアラミド紙パルプの離解度が低いため、密度、厚みむら、引張強度が実施例よりも劣り、更にシート外観も不良である。したがって、アラミド紙の抄紙製造の際に発生する端材や破損材を再利用したアラミド紙パルプを使用し、従来のアラミド紙に匹敵する機械的特性を有し、外観も良好なアラミド紙を得るためには、上記実施例で例示した条件が有効であることが判明した。 From the results in Table 2, the calendar-processed recycled aramid papers obtained in Examples 4 and 5 have the same density and tensile strength as the conventional examples, although they contain a high proportion of aramid paper pulp. , Further, by increasing the degree of disintegration of the mixed aramid pulp and paper, a good appearance was exhibited. On the other hand, the calendar-processed aramid papers of Comparative Examples 1 and 2 have a low degree of separation of the mixed aramid paper pulp, so that the density, thickness unevenness, and tensile strength are inferior to those of the examples, and the sheet appearance is also poor. .. Therefore, by using aramid paper pulp that reuses scraps and damaged materials generated during papermaking of aramid paper, it is possible to obtain aramid paper having mechanical properties comparable to those of conventional aramid paper and having a good appearance. Therefore, it was found that the conditions illustrated in the above examples are effective.
１　　　離解機
２　　　モーター
４　　　ローター
６　　　タブ
６Ａ　　底面
６Ｂ　　側壁
８　　　脚部材
１０　　バッフル 1 Dissociator 2 Motor 4 Rotor 6 Tab 6A Bottom 6B Side wall 8 Leg member 10 Baffle

Claims (5)

  1. 　アラミド短繊維及びアラミドファイブリッドから形成される乾燥アラミド紙の紙片を水中で離解させて、アラミド紙パルプを得る離解工程と、
    　前記紙パルプを抄紙する抄紙工程と、を含み、
    　前記離解工程において、離解度が９３％以上となるように前記アラミド紙パルプを離解させることを特徴とする再生アラミド紙の製造方法。     A decoupling step of obtaining aramid paper pulp by disintegrating a piece of dried aramid paper formed from aramid short fibers and aramid fibrid in water.
    Includes a papermaking process for making the pulp and paper.
    A method for producing recycled aramid paper, which comprises dissociating the aramid paper pulp so that the degree of disintegration is 93% or more in the dissociation step.
  2. 　前記アラミド紙パルプに微細化処理を行う微細化処理工程をさらに含む、
    　請求項１に記載の再生アラミド紙の製造方法。     The aramid paper pulp further includes a miniaturization treatment step of performing the miniaturization treatment.
    The method for producing recycled aramid paper according to claim 1.
  3. 　前記離解工程では、水中で鉛直方向の撹拌力を発生させるように構成された離解機を用いて前記アラミド紙を離解させる、
    　請求項１又は２に記載の再生アラミド紙の製造方法。     In the disintegration step, the aramid paper is dissociated using an disintegrator configured to generate a stirring force in the vertical direction in water.
    The method for producing recycled aramid paper according to claim 1 or 2.
  4. 　前記乾燥アラミド紙を粉砕及び／又は切断して紙片を得る粉砕／切断工程をさらに含み、
    　前記粉砕／切断工程では、前記乾燥アラミド紙を、最大寸法が１２．７ｍｍを超えるように粉砕及び／又は切断する、
    　請求項３に記載の再生アラミド紙の製造方法。     Further comprising a crushing / cutting step of crushing and / or cutting the dried aramid paper to obtain a piece of paper.
    In the crushing / cutting step, the dried aramid paper is crushed and / or cut so that the maximum size exceeds 12.7 mm.
    The method for producing recycled aramid paper according to claim 3.
  5. 　前記アラミド紙パルプに、アラミドファイブリッド及び／又はアラミド短繊維を混合する混合処理を行う、
    　請求項１～４のいずれか一項に記載の再生アラミド紙の製造方法。     The aramid paper pulp is subjected to a mixing treatment in which aramid fibrid and / or aramid short fibers are mixed.
    The method for producing recycled aramid paper according to any one of claims 1 to 4.
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