WO2003054299A1 - Procede de production de papier polytetrafluoroethylene et papier polytetrafluoroethylene - Google Patents

Procede de production de papier polytetrafluoroethylene et papier polytetrafluoroethylene Download PDF

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Publication number
WO2003054299A1
WO2003054299A1 PCT/JP2002/012990 JP0212990W WO03054299A1 WO 2003054299 A1 WO2003054299 A1 WO 2003054299A1 JP 0212990 W JP0212990 W JP 0212990W WO 03054299 A1 WO03054299 A1 WO 03054299A1
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WO
WIPO (PCT)
Prior art keywords
paper
polytetrafluoroethylene
cooling
producing
ptfe
Prior art date
Application number
PCT/JP2002/012990
Other languages
English (en)
Japanese (ja)
Inventor
Tadao Hayashi
Tetsuya Higuchi
Original Assignee
Daikin Industries, Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Daikin Industries, Ltd. filed Critical Daikin Industries, Ltd.
Priority to JP2003554992A priority Critical patent/JP4193696B2/ja
Publication of WO2003054299A1 publication Critical patent/WO2003054299A1/fr

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Classifications

    • 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
    • D21H13/12—Organic non-cellulose fibres from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H13/14—Polyalkenes, e.g. polystyrene polyethylene

Definitions

  • the present invention relates to a paper made of polytetrafluoroethylene and a method for producing paper made of polytetrafluoroethylene. More specifically, it relates to a method for producing thick paper, and further relates to a method for producing a polytetrafluoroethylene vapor paper and a polytetrafluoroethylene paper capable of easily adjusting the paper thickness. . Background art
  • PTFE Polytetrafluoroethylene
  • PTFE fibrous powder having an average fiber length of 100 to 500 m and an aspect ratio of 10 or more, or a filler filled with PTFE fibrous powder.
  • a method has been disclosed in which a composition obtained by mixing in a liquid is dispersed in a liquid to form a paper stock, which is formed on a net-like base material, dried, and then peeled from the base material and fired.
  • a composition obtained by mixing in a liquid is dispersed in a liquid to form a paper stock, which is formed on a net-like base material, dried, and then peeled from the base material and fired.
  • papermaking with a paper thickness of about 0.4 mm can be obtained, but there is no mention of a paper thickness greater than that, and as the paper thickness increases, the surface smoothness decreases and the porosity decreases. Because of its low cost, it was difficult to use for cushioning materials.
  • Conventionally, to change the thickness of the paper to be formed a method of changing the concentration of the stock dispersion in the paper making tank and a method of changing the paper making speed are known. However, these methods have the problems that the paper thickness varies due to the fluctuation of the stock dispersion concentration in the
  • the present invention solves the above-mentioned problems, and a method for producing a polytetrafluoroethylene paper, which can easily adjust the paper thickness and can produce a thick paper, and a polytetrafluoroethylene paper. It provides papermaking.
  • the present invention provides a step of dispersing polytetrafluoroethylene fibrous powder in a liquid, a step of forming a sheet on a substrate having an opening having an opening diameter of 100 to 700 m, a drying step and a firing step.
  • the thickness of the paper formed on the substrate is controlled, and It is preferable that the thickness of the removed paper is 0.2 to 2.0 mm.
  • the polytetrafluoroethylene fibrous powder is preferably dispersed in a liquid by a polyoxyalkylene-based nonionic surfactant. It is preferable that the air permeability of the polytetrafluoroethylene vapor be 1 to 30 seconds / c ⁇ ⁇ 30 OmL.
  • the shrinkage of the polytetrafluoroethylene paper is preferably 1.5% or less.
  • the present invention also relates to a polytetrafluoroethylene vapor produced by the production method.
  • Figure 1 shows an example of a papermaking device.
  • FIG. 2 is an example showing the height of the cylinder 1 with respect to the liquid level of the papermaking tank.
  • FIG. 3 is an example showing the height of the cylinder 1 with respect to the liquid level of the papermaking tank.
  • R f is a perfluoroalkyl group having 1 to 3 carbon atoms
  • PAVE perfluoro (alkyl vinyl ether)
  • a copolymer with 5 mol% (modified PTFE) may be used.
  • fluororefin represented by the above formula (I) examples include hexane Fluoropropylene (hereinafter abbreviated as HFP).
  • the perfluoro (alkyl vinyl ether) represented by the formula (II) includes perfluoro (methyl vinyl ether) (hereinafter abbreviated as PMVE), perfluoro (ethyl vinyl ether) (hereinafter abbreviated as PEVE), perfluoro ( Propyl vinyl ether) (hereinafter abbreviated as PPVE).
  • the raw material PTFE powder used in the present invention can be obtained by polymerization using a polymerization initiator in the presence of a water-soluble fluorinated dispersant.
  • a polymerization initiator include ammonium persulfate and disuccinic acid peroxide
  • the chain transfer agent include hydrocarbons such as hydrogen, methane, ethane and propane, and water-soluble compounds such as methanol and ethanol.
  • the PTF E powder thus obtained is pulverized with a pulverizer to obtain a fibrous powder.
  • This average fiber length is preferably from 50 to 5000 m. In particular, it is preferably from 100 to 4000 m. If the average fiber length is less than 50 m, it tends to drop off from the net-like base material and cause pinholes. On the other hand, if the average fiber length exceeds 5000 / xm, it tends to be difficult to produce paper having a uniform thickness because the fiber length is long.
  • the aspect ratio is preferably 5 or more. If the aspect ratio is less than 5, it is difficult to peel off from the net-like base material after firing, and the finish tends to be poor.
  • An inorganic filler may be added to the PTFE fibrous powder to impart flexibility, smoothness and the like.
  • the type and amount of the filler used are appropriately determined according to the purpose of use of the PTFE paper.
  • Examples of the dispersion for dispersing the PTFE fibrous powder include aliphatic hydrocarbons such as hexane, heptane, gasoline, and kerosene, and mixtures thereof, aromatic hydrocarbons such as benzene, toluene, and xylene, ethyl alcohol, and methyl alcohol.
  • Alcohols such as alcohol, isopropanol, t-butyl alcohol, aryl alcohol, ethylene glycol, benzyl alcohol, and hexanol; aldehydes such as paraaldehyde, acetal, and acrolein; acetone; cyclohexanone , Methyl ketone, etc., ketones, chloroform form, carbon tetrachloride, aryl iodide, butylene dichloride, chloral, dichloroacetic acid, acetyl chloride, halogenogen derivatives such as monochlorobenzene, benzyl chloride, trichlorotrifluoro, etc.
  • Ruetan mono Fluorotrichloromethane, difluorotetrachloroethane, octafluorosulfone butane, omega monohydroperfluorohexene benzobenzotrifluoride, monobenzotrifluoride, dibromotetrafluoroethane, trichlorobe Fluoro derivatives such as n-fluoropropane and mixtures thereof.
  • fluoro derivatives and mixtures thereof are preferred because they have low surface tension and have an affinity for PTFE.
  • water may be used as the dispersion.
  • a surfactant as a dispersant to lower the surface tension.
  • a surfactant for dispersing the PTFE fibrous powder in the dispersion a surfactant of an aromatic hydrocarbon such as polyoxyethylene alkylphenyl ether, polyoxyethylene alkyl ether, or polyoxyethylene is used. Examples include polyoxyalkylene nonionic surfactants such as alkyl esters. Good dispersion of PTFE fibrous powder even in small amounts Polyoxyalkylene-based nonionic surfactants are preferred in that they do not occur.
  • the surfactant has the formula:
  • R is a linear or branched alkyl group having 5 or more carbon atoms
  • A is a boroxyalkylene chain having 5 to 40 oxyethylene groups and 0 to 6 oxypropylene groups.
  • a boroxyalkylene alkyl ether-based surfactant represented by the following formula is preferable.
  • the alkyl group R include decyl, lauryl, tridecyl, cetyl, stearyl, and the like, and may be linear or branched.
  • the lower limit of the number of carbon atoms of the alkyl group R is 5 because of its excellent surface activity, water solubility, and easy availability. In particular, it preferably has 12 carbon atoms, and more preferably 13 carbon atoms.
  • the upper limit of the number of carbon atoms in the alkyl group R is not particularly limited, but is preferably 18 carbon atoms.
  • the surface tension of the surface active aqueous solution is low because the permeability to the substrate is good.
  • a raw material for producing this surfactant a natural or synthetic higher alcohol may be used, but the minimum condition is that it does not contain any alkylphenols.
  • boroxyethylene lauryl ether average number of oxishylene chains 9
  • boroxyshethylene tridecyl ether average number of oxishylene chains 10
  • polyoxyethylene oxypropylene stearyl ether Average number of oxyethylene chains 11, average number of oxypropylene chains 3).
  • Examples of commercially available products include Nissan Nonion K-206, Nissan Nonion EAD-11, Nissan Nonion S-207 manufactured by NOF Corporation and Emulgen 210P manufactured by Kao Corporation, Emargen 320 P and the like.
  • R 1 is a linear or branched alkyl group having 16 or more carbon atoms
  • R 2 is a hydrogen atom, or a linear or branched alkyl group having 16 or more carbon atoms
  • A is a polyoxyalkylene fatty acid monoester or diester represented by the following formula: (polyoxyalkylene chain having 5 to 40 oxyethylene units and 0 to 6 oxypropylene units).
  • RR 2 is preferably a linear or branched alkyl group having 17 carbon atoms.
  • Specific examples include, for example, boroxyethylene glycol monosoleate, polyethylene glycol monostearate and the like.
  • Examples of commercially available products include NONION 0-4, NONION S-4, and NONION S-10 manufactured by NOF Corporation, and EMANOL 319 and EMANOL 3299 manufactured by Kao Corporation. is there.
  • R is a linear or branched alkyl group having 16 or more carbon atoms
  • a and B are the same or different and each has 5 to 30 oxyethylene units, and oxypropylene (A polyoxyalkylene chain having 0 to 6 units).
  • R is a linear or branched alkyl group having 18 carbon atoms.
  • Specific examples include polyethylene glycol stearylamine, polyethylene glycol oleylamine and the like.
  • Nymeen S—210 manufactured by NOF Corporation
  • Nimin S-215, Nimin S-220 and Esomin 0/20 manufactured by Kao Corporation are commercially available products, for example, Nymeen S—210, manufactured by NOF Corporation.
  • Nimin S-220 Nimin S-220
  • Esomin 0/20 manufactured by Kao Corporation.
  • R is a linear or branched alkyl group having 16 or more carbon atoms
  • a and B are the same or different, and each includes 530 ethylene oxide units and oxypropylene units.
  • R is a linear or branched alkyl group having 18 carbon atoms.
  • polyethylene glycol stearylamide is used.
  • polyoxyalkylene chain contains 540, preferably 530, more preferably 102, oxoxyethylene units, and if necessary, oxypropylene units. Are preferred.
  • the amount of carbon remaining on the substrate 4 generated in the subsequent firing step can be reduced. Therefore, the subsequent step of washing the base material is facilitated, and the contamination of the paper to be subsequently formed is reduced, which is also preferable in this respect.
  • the concentration of the PTFE fibrous powder dispersion is preferably adjusted to 0.1 to 5%. If the concentration of the dispersion is less than 0.1%, it tends to be impossible to obtain a thick paper. When the concentration of the dispersion exceeds 5%, the paper tends to have poor surface smoothness.
  • the production method of the present invention can be carried out, for example, by the paper machine shown in FIG.
  • the PTF E dispersion prepared as described above is supplied from the head tank 1 to the paper making tank 2.
  • the papermaking tank 2 is provided with a rotating cylinder 3 on which a base material 4 is stretched. By the rotation of the cylinder 3, the dispersion is formed on a continuous base material 4 while being appropriately dehydrated.
  • the paper thickness is determined by the amount of the PTF E fibrous powder on the substrate 4.
  • the present invention controls the paper thickness by adjusting the amount of the PTFE fibrous powder to be formed on the base material 4 by changing the liquid level of the papermaking tank (hereinafter, referred to as the liquid level). is there. In other words, increasing the liquid level as shown in Fig. 2 increases the paper thickness, and decreasing the liquid level as shown in Fig. 3 decreases the paper thickness.
  • the liquid level (liquid level) of the papermaking tank is changed in a range from the height of the central portion of the round net to the highest position of the round net.
  • the liquid level may be adjusted by increasing or decreasing the amount of the dispersion in the papermaking layer 2, as shown in FIGS. 2 and 3.
  • the adjustment may be made by raising and lowering one to three.
  • the base material 4 include a metal mesh, a glass cloth, and a plastic mesh having a hole portion so that the air permeability and the porosity of the PTFE paper to be produced can be adjusted.
  • a metal mesh is preferred because of the ease of removing deposits from the net-like substrate after the paper is peeled off.
  • the base material 4 has an opening having an opening diameter of 100 to 700 xm. More preferably, it is 150 to 650 m.
  • the opening diameter of the base material 4 is 100 to 700 m, generation of paper dust when the PTFE paper is peeled from the base material 4 after firing is suppressed. Therefore, paper powder is not mixed into the PTFE paper to be manufactured subsequently, and paper with a smooth surface can be stably manufactured.
  • the opening diameter is smaller than 100 m, the air permeability is low, resulting in poor cushioning paper. If the opening diameter exceeds 700 m, some of the mesh-like base material drops off from the eyes of the net-like base material, resulting in a rough surface. ⁇ It will be one par.
  • the papermaking speed is preferably 0.5 to 5. OmZ. More preferably, it is 0.8 to 1. Om / min. If the papermaking speed is lower than 0.5 mZ, productivity tends to decrease and cost tends to be unacceptable. If the papermaking speed exceeds 5.Om/min, foaming in the papermaking tank tends to result in poorly finished paper containing bubbles.
  • the paper formed on the base material 4 is dried by a drying device 5 at a temperature of 130 to 180 ° (preferably 145 to 155 ° C) for 5 to 20 minutes.
  • the drying temperature is 130. If the temperature is lower than ° C, moisture will remain in the paper and drying will be insufficient. If the temperature is higher than 180 ° C, the water in the vapor will evaporate rapidly and the surface of the paper will become rough.
  • pre-cooling is performed at 10 to 25 ° C for 1 to 20 seconds by pre-cooling 8 by air cooling. If the air temperature is lower than 10 ° C, it will cause cracking of the vapor, and if it is higher than 25, the cooling will be insufficient.
  • a spot cooler is used for pre-cooling.
  • the cooling drum 13 After being pre-cooled, it is subsequently cooled for 0.5 to 2.0 minutes by the cooling drum 13 cooled at a drum surface temperature of 5 to 20. If the drum surface temperature is lower than 5 ° C, the surface of the cooling drum will condense and water will tend to adhere to the paper.If it is higher than 20 ° C, the paper will not easily peel off from the base material, and paper dust will form on the base material. Tends to stick.
  • the PTFE paper is peeled from the base material and wound up by the winder 7.
  • the paper is easy to peel off from the substrate, and paper powder hardly adheres to the release surface.
  • the papermaking step, the drying step, the baking step, the pre-cooling step by air cooling, the step of cooling with a cooling drum, and the step of peeling off from the base material be performed in a series of steps, since tension is not easily applied to the paper.
  • the base material 4 passes through the tension roll 9 and the drive roll 10, passes through the washing process using the washing nozzle 11, the dewatering process using the dehydrator 12, and then returns to the papermaking tank 2 again. be introduced.
  • the paper thickness is preferably from 0.4 to 1.0 mm. If the paper thickness is less than 0.2 mm, it is unsuitable for cushioning applications. If the paper thickness exceeds 2. Omm, it is unsuitable for filter applications.
  • the basis weight is preferably 200 to 800 g / m 2 . When the grammage is less than 100 g / m 2 , the paper thickness is small and the paper strength is low. If the grammage exceeds 1000 g / m 2 , the paper thickness will increase, making it difficult to dry after making the paper, resulting in a paper with low air permeability.
  • the PTFE paper preferably has an air permeability of 1 to 30 seconds (Zcmci) ⁇ 30 OmL and a porosity of 50 to 85%.
  • the air permeability is more preferably 3 to 10 seconds / cm ⁇ i) ⁇ 300 mL, and the porosity is more preferably 72 to 82%.
  • the air permeability is more preferably 8 to 20 seconds Zcmc /) ⁇ 30 OmL, and the porosity is more preferably 70 to 80%. If the air permeability is less than 1 second / ⁇ ⁇ 30 OmL, the strength of the paper is weak and the paper tends to have low durability.
  • the shrinkage of the PTFE paper is preferably 1.5% or less. More preferably, it is 1.0% or less. If the shrinkage ratio is more than 1.5%, defective products tend to be generated in the liquid crystal panel bonding Z sealing step.
  • the PTFE vapor obtained according to the present invention is used as a chemical-resistant filter, a gas vent cap, a cushion material used in a liquid crystal panel laminating Z sealing step and a printed board forming step, and the like.
  • the PTFE paper is measured using a dial gauge H type (pressure 200 g or less). Using the PTFE paper, the time required for 30 OmL of air to pass through the 1 c ⁇ orifice is measured by a gull tester.
  • the arithmetic average roughness of the PTFE paper is measured using a stylus type surface roughness meter.
  • the PTFE paper of 20 Omm square is heated at 150 ° C for 1 hour, then naturally cooled, and can be obtained by the following equation.
  • Shrinkage () ((dimension before heating)-(dimension after heating)) / (dimension before heating) X 100
  • Raw material PTFE powder consisting of a polymer obtained by emulsion polymerization of a polymer component consisting of 100% by mole of tetrafluoroethylene is subjected to a parverizer (manufactured by Hosokawa Micron, ACM-10) at a temperature of 70 ° C. This was ground to obtain a PTFE fibrous powder having an average fiber length of 1500 zm.
  • a polyoxyalkylene-based nonionic surfactant (Nonion EAD-11, manufactured by NOF Corporation) and 1,000 parts by weight of water were mixed as a dispersant.
  • the stock was made with a round mesh paper machine having an opening having an opening diameter of 250 m as a base material. Table 1 shows the liquid level at this time. The papermaking speed was 1.0 m / min.
  • a PTFE paper was obtained in the same manner as in Example 1, except that the PTFE fibrous powder was changed to 15 parts by weight. table 1
  • a polytetrafluoroethylene paper having a large paper thickness can be manufactured, and the paper thickness can be easily changed by adjusting the liquid level.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Paper (AREA)

Abstract

La présente invention concerne un procédé de production de papier polytétrafluoroéthylène qui consiste en une étape de dispersion d'une poudre de fibre polytétrafluoroéthylène dans un liquide, une étape de fabrication d'un papier sur un substrat possédant des pores ouverts d'un diamètre compris entre 100 et 700 νm, une étape de traitement de séchage et de traitement de chauffe, une étape de prérefroidissement à l'air, une étape de refroidissements successifs au moyen d'un tambour de refroidissement et enfin en un décollage d'un papier du substrat. Ce procédé permet de produire un papier de grande épaisseur, laquelle peut être facilement réglée.
PCT/JP2002/012990 2001-12-13 2002-12-12 Procede de production de papier polytetrafluoroethylene et papier polytetrafluoroethylene WO2003054299A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2003554992A JP4193696B2 (ja) 2001-12-13 2002-12-12 ポリテトラフルオロエチレン製ペーパーの製造方法

Applications Claiming Priority (2)

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JP2001380194 2001-12-13
JP2001-380194 2001-12-13

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012081444A1 (fr) * 2010-12-17 2012-06-21 デュプロ精工株式会社 Dispositif de recyclage de déchets de papier
CN102877374A (zh) * 2012-09-25 2013-01-16 蚌埠凤凰滤清器有限责任公司 一种聚四氟乙烯纤维阻燃滤纸
CN105030343A (zh) * 2015-06-11 2015-11-11 郭岚 外出便携体检箱
CN114471759A (zh) * 2022-01-27 2022-05-13 盖秩舶 一种基于聚四氟乙烯和玻璃的微流控芯片及其制备方法

Citations (3)

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Publication number Priority date Publication date Assignee Title
US5216068A (en) * 1989-12-15 1993-06-01 Hoechst Aktiengesellschaft Process for producing an agglomerated molding powder composed of polytetrafluoroethylene and hydrophobic fillers
JPH06176750A (ja) * 1992-12-10 1994-06-24 Tomoegawa Paper Co Ltd 電池セパレータ用基材シートの製造方法
JPH11188812A (ja) * 1997-12-26 1999-07-13 Tomoegawa Paper Co Ltd ポリ四フッ化エチレン複合紙状物及びその製造方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3295684B2 (ja) * 1998-03-20 2002-06-24 株式会社巴川製紙所 ポリ四フッ化エチレン紙状物及びその製造方法
CN1081260C (zh) * 1998-04-01 2002-03-20 陕西省档案馆 一种对生宣纸的处理液

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5216068A (en) * 1989-12-15 1993-06-01 Hoechst Aktiengesellschaft Process for producing an agglomerated molding powder composed of polytetrafluoroethylene and hydrophobic fillers
JPH06176750A (ja) * 1992-12-10 1994-06-24 Tomoegawa Paper Co Ltd 電池セパレータ用基材シートの製造方法
JPH11188812A (ja) * 1997-12-26 1999-07-13 Tomoegawa Paper Co Ltd ポリ四フッ化エチレン複合紙状物及びその製造方法

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012081444A1 (fr) * 2010-12-17 2012-06-21 デュプロ精工株式会社 Dispositif de recyclage de déchets de papier
JP2012140738A (ja) * 2010-12-17 2012-07-26 Duplo Seiko Corp 古紙再生処理装置
CN102877374A (zh) * 2012-09-25 2013-01-16 蚌埠凤凰滤清器有限责任公司 一种聚四氟乙烯纤维阻燃滤纸
CN105030343A (zh) * 2015-06-11 2015-11-11 郭岚 外出便携体检箱
CN114471759A (zh) * 2022-01-27 2022-05-13 盖秩舶 一种基于聚四氟乙烯和玻璃的微流控芯片及其制备方法
CN114471759B (zh) * 2022-01-27 2023-06-06 盖秩舶 一种基于聚四氟乙烯和玻璃的微流控芯片及其制备方法

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CN1589349A (zh) 2005-03-02
CN1294325C (zh) 2007-01-10
JPWO2003054299A1 (ja) 2005-04-28
JP4193696B2 (ja) 2008-12-10

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