WO2006035726A1 - Formulation de dispersion aqueuse de polytetrafluoroethylene, film de resine polytetrafluoroethylene, et produits impregnes de resine polytetrafluoroethylene - Google Patents

Formulation de dispersion aqueuse de polytetrafluoroethylene, film de resine polytetrafluoroethylene, et produits impregnes de resine polytetrafluoroethylene Download PDF

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WO2006035726A1
WO2006035726A1 PCT/JP2005/017643 JP2005017643W WO2006035726A1 WO 2006035726 A1 WO2006035726 A1 WO 2006035726A1 JP 2005017643 W JP2005017643 W JP 2005017643W WO 2006035726 A1 WO2006035726 A1 WO 2006035726A1
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Prior art keywords
ptfe
mass
aqueous dispersion
dispersion composition
polytetrafluoroethylene
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PCT/JP2005/017643
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English (en)
Japanese (ja)
Inventor
Yasukazu Nakatani
Toshirou Miura
Yasuhiko Sawada
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Daikin Industries, Ltd.
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Priority to JP2006537730A priority Critical patent/JPWO2006035726A1/ja
Publication of WO2006035726A1 publication Critical patent/WO2006035726A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
    • C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
    • C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C09D127/18—Homopolymers or copolymers of tetrafluoroethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
    • C08L71/02—Polyalkylene oxides

Definitions

  • the present invention relates to a polytetrafluoroethylene aqueous dispersion composition, a polytetrafluoroethylene resin film, and a polytetrafluoroethylene resin impregnated body.
  • Aqueous dispersion compositions containing polytetrafluoroethylene [PTFE] resin particles have heretofore been impregnated into glass fibers, carbon fibers, Kepler fibers, etc., and include roofing materials, etc. of membrane structure buildings. It has been used in the manufacture of immersion bodies, and has been used for film formation by coating and baking on objects to be coated in applications such as high-frequency printed circuit boards, conveyor belts, and packing.
  • PTFE polytetrafluoroethylene
  • a silicone emulsion is blended (for example, see Patent Document 1), a silicone emulsion, and a specific nonionic property.
  • Patent Document 2 A combination of a surfactant and a specific anionic surfactant (see, for example, Patent Document 2), and a thermal decomposition component mainly composed of a nonionic surfactant is 9 to 12% of PTFE
  • Patent Document 3 A blended material (for example, see Patent Document 3) has been proposed.
  • the primary particle diameter is limited to 0.3 to 0.6 m (see, for example, Patent Document 4).
  • a mixture of a PTFE dispersion having an average particle diameter of 180 to 400 nm and a PTFE dispersion having the same particle diameter of 20 to 60 nm (for example, see Patent Document 5) has also been proposed.
  • any of these PTFE aqueous dispersion compositions has a crack limit film thickness. There was still a problem that was not suitable for low thick coating.
  • the roof material of the membrane structure building is required to have high light transmittance.
  • a method for enhancing light transmittance a method of applying an aqueous PTFE dispersion composition to an improved base material (for example, see Patent Documents 6 and 7) has been proposed, but an improvement in the aqueous PTFE dispersion composition has been proposed. It ’s a well-known method.
  • Patent Document 1 Japanese Patent Laid-Open No. 61-34032
  • Patent Document 2 Japanese Patent Laid-Open No. 4-292673
  • Patent Document 3 Japanese Patent Laid-Open No. 2001-89624
  • Patent Document 4 JP-A-5-337439
  • Patent Document 5 JP 2000-53834 A
  • Patent Document 6 Japanese Patent Laid-Open No. 4-300363
  • Patent Document 7 Japanese Patent Laid-Open No. 9-256277
  • the object of the present invention is that the crack limit film thickness is extremely large.
  • a thick film can be formed by a single coating or impregnation, and when modified polytetrafluoroethylene is used. Even so, an object of the present invention is to provide an aqueous PTFE dispersion composition capable of forming a film having excellent crack limit film thickness and transparency.
  • the present invention relates to a polytetrafluoroethylene [PTFE] aqueous dispersion composition
  • PTFE polytetrafluoroethylene
  • the PTFE aqueous dispersion composition has a PTFE rosin solids concentration of 30 to 70% by mass of the PTFE aqueous dispersion composition and a viscosity at 25 ° C of 0.1 lPa's or less.
  • the polyoxyalkylene alkyl ether compound (B) is 9 to 20 parts by mass with respect to 100 parts by mass of the PTFE resin solid content, and constitutes the polytetrafluoroethylene resin particles (A).
  • the polytetrafluoroethylene resin is a PTFE aqueous dispersion composition characterized by being a resin having a modified polytetrafluoroethylene power.
  • the present invention can be obtained by coating the PTFE aqueous dispersion composition on an object to be coated.
  • PTFE resin film characterized by
  • the present invention is a PTFE resin-impregnated body characterized by having an object to be impregnated and a film obtained by impregnating the object to be impregnated with the PTFE aqueous dispersion composition.
  • the PTFE aqueous dispersion composition of the present invention is a composition comprising an aqueous dispersion containing PTFE rosin particles (A) and a specific range of amounts of a polyoxyalkylene alkyl ether compound (B). It has a specific range of PTFE resin solids concentration and a specific range of viscosity.
  • the PTFE aqueous dispersion composition of the present invention is not particularly limited, but is suitable as a coating composition.
  • the PTFE aqueous dispersion composition of the present invention is coated or impregnated on an object to be coated, so that a film made of PTFE resin is coated on the object or the surface of the object to be impregnated. Can be formed on top.
  • “V” is sometimes referred to as “substrate” as a concept that can include both the above-mentioned object to be coated and the object to be impregnated.
  • Coating and impregnation generally involve applying the PTFE aqueous dispersion composition of the present invention onto an object to be coated or immersing the object to be coated (as a concept that can include application and immersion for the purposes of this specification). It may be referred to as “application”), and is an operation consisting of drying by heating, etc., if necessary, and then baking to a temperature above the melting point of PTFE resin.
  • the PTFE aqueous dispersion composition of the present invention reduces both mud cracks that have conventionally occurred during drying after application, and shrinkage cracks that have conventionally occurred due to the shrinkage of the grease accompanying cooling after firing. Also, the crack limit film thickness by one coating or impregnation is extremely large. Thick film can be formed by one coating or impregnation (thick coating property).
  • film-forming property the property that can form a film while reducing the occurrence of the above-mentioned cracks is sometimes referred to as “film-forming property”.
  • the PTFE aqueous dispersion composition of the present invention contains PTFE rosin particles (A).
  • the PTFE resin particles (A) are particles made of PTFE resin.
  • PTFE resin includes a resin made of modified polytetrafluoroethylene [modified PTFE]. If the PTFE resin contains a resin that also has a modified PTFE power, it may be a tetrafluoroethylene [TFE] homopolymer or a modified PTFE card. Fat may be sufficient.
  • the PTFE resin constituting the PTFE resin particles (A) is a resin made of a modified PTFE cartridge.
  • the aqueous PTFE dispersion composition of the present invention can improve the light transmittance of the resulting coating, particularly when the resin made of modified PTFE is used as the PTFE resin. Therefore, the processed article having a coating film having the composition power of the PTFE aqueous dispersion of the present invention can be suitably used as a roofing material for a membrane structure building.
  • the modified PTFE is a copolymer of TFE and a small amount of monomer copolymerizable with TFE.
  • examples of the trace amount of monomer include fluoroolefin, fluorinated (alkyl vinyl ether), cyclic fluorinated monomer, and perfluoroalkylethylene.
  • fluorination examples include perfluoro (alkyl butyl ether) [PAVE], and examples of the PAVE include perfluoro (methyl vinyl ether) [PMVE], perfluoro (ethyl butyl ether) [ PEVE], perfluoro (propyl butyl ether) [PPVE] and the like.
  • trace amounts of monomers include PAVE, hexafluoropropylene, black trifluoride. PP is more preferred. PVE is more preferred.
  • the trace monomer unit derived from the above trace monomer is preferably in the range of 0.001 to 2% by mass of the entire polymer chain of the modified PTFE, and is in the range of 0.01 to 1% by mass. It is more preferable.
  • the content of the trace monomer unit derived from the trace monomer is determined by using an infrared absorption scan using a powder obtained by coagulating, washing and drying the PTFE aqueous dispersion. It is the value obtained by measuring the petal, or the value obtained by measuring the residual amount in the reaction system by gas chromatography and calculating the consumption power consumption.
  • “monomer unit” such as the above-mentioned trace monomer unit means a part of the molecular structure of the modified PTFE and derived from the corresponding monomer.
  • the PP VE unit is a part of the molecular structure of modified PTFE, which is derived from PPVE. Yes, represented by [CF—CF (OCF;)] —.
  • the PTFE resin preferably has a number average molecular weight of 2 ⁇ 10 4 to 1 ⁇ 10 7 , more preferably 2 ⁇ 10 5 to 8 ⁇ 10 6 .
  • the coating film tends to be brittle, and when it exceeds 1 ⁇ 10 7 , the melt viscosity tends to be too high and the particles tend not to be fused.
  • the number average molecular weight can be determined by measurement by the method described in “Journal of Applied Polymer Science”, Vol. 17, pages 3253-3257 (1973).
  • the PTFE resin particles (A) have an average particle diameter of S200 to 500 nm.
  • a more preferable lower limit of the average particle diameter is 300 nm, and a more preferable upper limit is 400 nm. If it is 200 nm or more, the force that dramatically increases the crack limit film thickness exceeds 500 nm, the particles tend to settle, and the stability of the aqueous dispersion composition decreases.
  • the PTFE aqueous dispersion composition of the present invention enables a large particle size of 300 nm or more, which is not generally achieved with modified PTFE.
  • the average particle size is large in this way, it is easy to increase the film thickness by a single application. Therefore, even when the film is finally made thick, the number of applications can be reduced, and the work becomes easier. It can also suppress mud cracks that are more likely to occur than conventional TFE homopolymers.
  • the average particle size is defined as the transmittance of 550 nm projection light with respect to the unit length of the PTF E aqueous dispersion prepared at a solid content concentration of 0.22% by mass, and the unidirectional diameter in the transmission electron micrograph. Based on the calibration curve with the average particle diameter determined by measuring the above, the transmittance was determined from the above.
  • PTFE aqueous dispersion composition of the present invention is PTFE ⁇ solid concentration is 30 to 70 mass 0/0 aqueous PTFE dispersion composition.
  • the PTFE rosin solid content concentration is preferably U, the lower limit is 40% by mass of the PTFE aqueous dispersion composition, and the upper limit is preferably 65% by mass of the PTFE aqueous dispersion composition.
  • the PTFE aqueous dispersion composition of the present invention has the above-mentioned PTFE rosin solid content concentration within the above range, it is excellent in film forming property and can be easily formed into a thick film.
  • the concentration of the solid content of PTFE resin is the mass of the residue obtained by drying 10 g of the PTFE aqueous dispersion composition described later at a temperature of 380 ° C. for 45 minutes. Determined as a percentage of the mass of the PTFE aqueous dispersion composition
  • the PTFE rosin particles (A) are obtained by polymerizing TFE and the above-mentioned trace amount of monomers in the presence of an aqueous medium by a known polymerization method such as emulsion polymerization or suspension polymerization. Supplied PTFE aqueous dispersion.
  • the polymerization is preferably performed by emulsion polymerization.
  • aqueous medium used in the polymerization examples include water and a mixed liquid of water and a known water-soluble solvent.
  • the above polymerization can be carried out by appropriately setting conditions according to the type and amount of PTFE resin used and the type of emulsifier.
  • the PTFE aqueous dispersion composition of the present invention contains a polyoxyalkylene alkyl ether compound (B) in addition to the PTFE rosin particles (A).
  • the gap between the PTFE rosin particles (A) in the coating is formed into a polyoxyalkylene alkyl ether.
  • the compound (B) is buried and can act as a binder during drying after application to suppress the generation of cracks and improve the film-forming property.
  • the polyoxyalkylene alkyl ether compound (B) suppresses shrinkage cracks that have conventionally occurred due to grease shrinkage by some action even during cooling after firing the coating.
  • the polyoxyalkylene alkyl ether compound (B) is considered to contribute to the dispersion stability of the PTFE resin particles (A).
  • polyoxyalkylene alkyl ether compound (B) examples include those represented by the formula (I): R—O—A 1 —H (I)
  • R is a linear or branched alkyl group having 8 to 19, and preferably 10 to 16 carbon atoms;
  • a 1 is a polyoxyalkylene chain having 8 to 58 carbon atoms
  • the polyoxyalkylene alkyl ether represented by these is preferable.
  • A polyoxyalkylene chain preferably having 4 to 20 amino Okishiechiren units and 0-6 O carboxymethyl propylene Unit.
  • x is an integer of 1 or more
  • y is an integer of 1 or more
  • n is an integer from 4 to 20
  • a polyoxyalkylene alkyl ether represented by
  • a 2 is preferably a polyoxyalkylene chain having 5 to 20 oxyethylene units and 1 to 2 oxypropylene units.
  • the polyoxyalkylene alkyl ether compound (B) further includes the following formula (IV):
  • R 4 is a linear or branched alkyl group having 4 to 12 carbon atoms, and A 3 is a polyoxyalkylene chain having 8 to 58 carbon atoms). Examples thereof include oxyethylene alkyl ether.
  • a 3 is preferably a polyoxyalkylene chain having 5 to 20 oxyethylene units and 0 to 12 oxypropylene units, and 5 to 20 oxyshethylene units and 1 to More preferred is a polyoxyalkylene chain having 12 oxypropylene units.
  • the polyoxyalkylene alkyl ether compound (B) exceeds 12 parts by mass with respect to 100 parts by mass of PTFE rosin solids, and 20 parts by mass. It may be 9 to 12 parts by mass with respect to 100 parts by mass of PTFE resin solid content.
  • the film-forming property is insufficient.
  • Kirene alkyl ether compound (B) strength When the content exceeds 20 parts by mass with respect to 100 parts by mass of the solid content of PTFE resin, the physical properties of the PTFE film may deteriorate, for example, the film may be colored.
  • the content of the polyoxyalkylene alkyl ether compound (B) with respect to 100 parts by mass of the PTFE rosin solid content is preferably 12 parts by mass, more preferably 12.1 parts by mass, and preferably 16 parts by mass. is there.
  • the amount of the polyoxyalkylene alkyl ether compound (B) is determined based on the solid content concentration of the PTFE resin and the amount blended when preparing the PTFE aqueous dispersion composition of the present invention ( (Including the blending amount at the time of preparation of the PTFE aqueous dispersion), and can be obtained as a mass with respect to 100 parts by mass of the PTFE resin solids, or 10 g of the PTFE aqueous dispersion composition at a temperature of 100 ° C.
  • the residue obtained by drying for 60 minutes is extracted with hexane, and then the mass of the residue obtained by volatilizing the hexane is expressed as a percentage of the mass of the PTFE resin solid before drying. You can ask for it.
  • the crack limit film thickness is a force evaluated by baking a film on an aluminum plate at 380 ° C for 15 minutes, which is a practical processing condition.
  • PTFE resin solid content 10 0 Cracks do not occur even when the polyoxyalkylene alkyl ether compound (B) is 9 parts by mass or more with respect to parts by mass. If cracks do not occur under these conditions, there will be no major problems in practical use.
  • the firing time can be shortened according to practical use.
  • a PTFE aqueous dispersion composition is fired for a long time, the actual thermal decomposition amount increases and cracks are likely to occur. .
  • the force depending on the heat capacity of the substrate For example, in the case of glass cloth impregnation, the coating is exposed to an atmosphere of 380 ° C. for about 5 minutes or less. After that, it takes about 15 to 20 minutes for the film to be exposed to an atmosphere of 380 ° C when applied to kitchen equipment.
  • the polyoxyalkylene alkyl ether compound (B) is 9 to 20 parts by mass with respect to 100 parts by mass of the PTFE resin solid content
  • the polyoxyalkylene alkyl ether compound (B) is: It is preferable that the average HLB contains a polyoxyalkylene alkyl ether compound of 12 or more, preferably 12-14.
  • the polyoxyalkylene alkyl ether compound (B) exceeds 12 parts by mass with respect to 100 parts by mass of the PTFE resin solid content, and 20 parts by mass.
  • the polyoxyalkylene alkyl ether compound (B1) having an average HLB of 14 or more is preferred! / ,.
  • the polyoxyalkylene alkyl ether compound (B) is more than 12 parts by mass and less than 20 parts by mass with respect to 100 parts by mass of the PTFE resin solid content, and
  • the polyoxyalkylene alkyl ether compound (B) includes the polyoxyalkylene alkyl ether compound (B1), the film-forming property is particularly excellent.
  • the average HLB is a value calculated based on the Griffin equation.
  • the polyoxyalkylene alkyl ether compound (B1) is more than 12 parts by mass and less than 20 parts by mass with respect to 100 parts by mass of the PTFE resin solid content. In some cases, it is preferably 1 to 99% by mass of the polyoxyalkylene alkyl ether compound (B).
  • the content of the polyoxyalkylene alkyl ether compound (B1) is such that the polyoxyalkylene alkyl ether compound (B) exceeds 12 parts by mass and 20 parts by mass or less based on 100 parts by mass of the PTFE resin solid content.
  • a more preferable lower limit is 10% by mass of the polyoxyalkylene alkyl ether compound (B)
  • a further preferable lower limit is 20% by mass
  • a more preferable upper limit is 95% by mass
  • a further preferable upper limit is 90% by mass.
  • the PTFE aqueous dispersion composition of the present invention has the polyoxyalkylene alkyl ether compound (B1) in an amount within the above range, it has an appropriate viscosity, and further has excellent film-forming properties. It will be a thing.
  • the polyoxyalkylene alkyl ether compound (B) is 9 to 12 parts by mass with respect to 100 parts by mass of the PTFE resin solid content
  • the polyoxyalkylene alkyl ether compound (B) is: It is preferred that the polyoxyalkylene alkyl ether compound (B2) has an average HLB of 12 or more and less than 14.
  • the aqueous PTFE dispersion composition of the present invention comprises the above polyoxyalkylene alkyl ether.
  • Compound (B) is 9 to 12 parts by mass with respect to 100 parts by mass of the PTFE resin solid content, and the polyoxyalkylene alkyl ether compound (B2) is used as the polyoxyalkylene alkyl ether compound (B). )
  • the polyoxyalkylene alkyl ether compound (B2) exhibiting particularly excellent film-forming properties is preferably those having an average HLB of 12.5 to 13.7 in terms of film-forming properties.
  • the polyoxyalkylene alkyl ether compound (B2) is a polyoxyalkylene alkyl ether compound (B2) when the polyoxyalkylene alkyl ether compound (B) is 9 to 12 parts by mass with respect to 100 parts by mass of the PTFE resin solid content. It is preferably 1 to 99% by mass of the alkylene alkyl ether compound (B).
  • the content of the polyoxyalkylene alkyl ether compound (B2) is more when the polyoxyalkylene alkyl ether compound (B) is 9 to 12 parts by mass with respect to 100 parts by mass of the PTFE resin solid content.
  • a preferable lower limit is 10% by mass of the polyoxyalkylene alkyl ether compound (B), a further preferable lower limit is 20% by mass, a more preferable upper limit is 95% by mass, and a further preferable upper limit is 90% by mass.
  • the PTFE aqueous dispersion composition of the present invention has the polyoxyalkylene alkyl ether compound (B2) in an amount within the above range, it has an appropriate viscosity, and further has excellent film-forming properties. It becomes.
  • the PTFE aqueous dispersion composition of the present invention can be adjusted to an appropriate value for the surface tension by adding a trace amount of a fluorosurfactant, a silicone surfactant, or the like. . Since the addition amount of these surfactants is very small, the viscosity of the aqueous PTFE dispersion composition does not change greatly.
  • the aqueous PTFE dispersion composition of the present invention further contains a film-forming improver (C).
  • the film-forming modifier (C) is a polyoxyalkylene alkyl ether compound (B) in which PTFE It is considered that the film forming property is improved by supplementing the filling of the gaps between the resin particles.
  • the PTFE aqueous dispersion composition of the present invention uses, in particular, a resin made of a modified PTFE resin as the PTFE resin, cracks are more likely to occur than a TFE homopolymer.
  • C) is also preferably included.
  • the PTFE aqueous dispersion composition of the present invention also has a polyoxyalkylene alkyl ether compound (B) strength. Since it is 9 to 20 parts by mass with respect to 100 parts by mass of the solid content of PTFE resin, the crack generation inhibiting power is improved. In view of this, it is preferable that the film-forming improver (C) is included.
  • the film-forming improver (C) depends on the type of film-forming improver (C) to be used, but it is 10 parts by mass or less with respect to 100 parts by mass of PTFE oil solid content. If it is in the above-mentioned range, it is more preferable that it is 0.1 part by mass or more, and it is more preferable that it is 1 part by mass or more.
  • the film-forming improver (C) is not particularly limited, but is a nonionic surfactant having an acrylic resin, a silicone-based surfactant, and a decomposition residue at 5% or more at 380 ° C.
  • a nonionic surfactant having an acrylic resin, a silicone-based surfactant, and a decomposition residue at 5% or more at 380 ° C.
  • acrylic resin, silicone surfactant, nonionic surfactant having a decomposition residue at 5% or more at 380 ° C. and Z or drying retarder refers to these four types. Of these, one or two or more can be used.
  • the acrylic polymer constituting the acrylic resin is not particularly limited, but a polymer obtained by polymerizing a methacrylate monomer is preferred.
  • metatalylate monomer examples include methyl metatalylate, ethyl methacrylate, propyl methacrylate, dimethylpropyl methacrylate, butyl methacrylate, and pentyl methacrylate.
  • the acrylic resin can be prepared as a stable aqueous dispersion even if it is a homopolymer.
  • the polymer is a polymer having a monomer having a ru group as appropriate as a comonomer.
  • a nonionic surfactant may be added to the aqueous dispersion as necessary in order to further enhance the stability.
  • the above-mentioned acrylic resin remains in a temperature range of 300 to 320 ° C, approximately 25 to 50% by mass before heating, and a temperature range of 330 to 345 ° C. It is preferable that 10 to 20% by mass before heating remains.
  • the acrylic resin when acrylic resin is used as the film-forming improver (C), the acrylic resin is 10 parts by mass with respect to 100 parts by mass of PTFE resin solids. It is preferable that
  • a more preferable upper limit of the above-mentioned acrylic resin relative to 100 parts by mass of PTFE resin is 8 parts by mass, and the lower limit is not particularly limited, but is preferable in that it obtains an effect by blending the above-mentioned acrylic resin.
  • the lower limit is 1 part by mass.
  • silicone surfactant examples include the following general formula:
  • R 1 may be the same or different and has 1 to 30 carbon atoms.
  • R 2 is a formula —R 3 — (CHO)
  • R 3 represents a substituent represented by r.
  • q and r are the same or different and represent an integer of 0 to 20, and q + r> l. ).
  • a compound having such a general formula is sold as a modified silicone oil, but in this application, it is treated as a silicone surfactant.
  • the silicone-based surfactant when a silicone-based surfactant is used as the film-forming improver (C), the silicone-based surfactant is used with respect to 100 parts by mass of the solid content of PTFE resin. It is preferable that the amount is 10 parts by mass or less.
  • the upper limit of the silicone-based surfactant is 100 parts by weight based on PTFE rosin solid content, and the lower limit is not particularly limited.
  • a preferable lower limit is 0.1 part by mass in terms of obtaining the effect of the above.
  • Examples of the nonionic surfactant whose decomposition residue at 380 ° C is 5% or more include various polyoxyethylene derivatives.
  • the decomposition residue at 380 ° C. is 5% or more
  • the residue after heating at 380 ° C. for at least 10 minutes is 5% by mass or more before the heating. Means that.
  • the PTFE aqueous dispersion composition of the present invention uses the nonionic surfactant when the nonionic surfactant whose decomposition residue at 380 ° C is 5% or more is used as the film-forming improver (C).
  • the agent is preferably 10 parts by mass or less with respect to 100 parts by mass of the solid content of PTFE resin.
  • the decomposition residue at 380 ° C is 5% or more with respect to 100 parts by mass of PTFE resin solid content.
  • a more preferable upper limit of the nonionic surfactant is 5 parts by mass, and the lower limit is not particularly limited.
  • a preferable lower limit is 0.1 part by mass in that an effect is obtained by adding a nonionic surfactant whose decomposition residue at 380 ° C is 5% or more.
  • drying retardant examples include those having a boiling point of about 200 to 300 ° C, as long as they are normally recognized by those skilled in the art as “drying retardants”.
  • a solvent a water-soluble solvent is preferable.
  • water-soluble solvent examples include glycerin, diethylene glycol monoethyl ether (ethyl carbitol), diethylene glycol monobutyl ether (butyl carbitol), triethylene glycol, ethylene glycol, 1,3 propanediol, 1,3 butanediol, 1 1,4-butanediol, 1,5-pentanediol, 2-butene-1,4-diol, 2-ethyl-2-hydroxymethyl-1,3-propanediol and the like are preferred.
  • the drying retardant is obtained by reducing or removing water, polyoxyalkylene alkyl ether compound (B), etc. by drying or heating from a coating obtained by applying the PTFE aqueous dispersion composition of the present invention to a substrate.
  • the film-forming property is improved by remaining in the coating and acting to fill the gaps between the PTFE resin particles.
  • the amount of the drying retarder is appropriately set according to the type of the drying retarder. It is possible The strength is preferably 10 parts by mass or less with respect to 100 parts by mass of the solid content of PTFE resin.
  • diethylene glycol monoalkyl ether has a function of dissolving acrylic resin, so that the film forming property can be further improved by using it together with acrylic resin.
  • the PTFE aqueous dispersion composition of the present invention has, as the film-forming improver (C), an allyl resin, a silicone-based surfactant, or a decomposition residue at 380 ° C of 5% or more. It is more preferable to include an acrylic resin which preferably includes a certain nonionic surfactant.
  • the acrylic resin used as the film-forming modifier (C) in the present invention maintains the binder effect on the PTFE resin particles (A) when the PTFE aqueous dispersion composition of the present invention is applied and dried and then fired. Since it gradually decomposes, the occurrence of shrinkage cracks can be effectively prevented.
  • the PTFE aqueous dispersion composition of the present invention can be blended with various known additives as long as the effects of the present invention are not impaired.
  • the additive include pigments, fillers, antifoaming agents, drying agents, thickeners, leveling agents, repellency inhibitors, and the like.
  • the pigment is not particularly limited, and examples thereof include known pigments such as titanium oxide, carbon black, and bengara.
  • antifoaming agent examples include toluene, xylene, non-polar solvents such as hydrocarbons having 9 to 11 carbon atoms, and silicone oil.
  • Examples of the desiccant include acid cobalt.
  • thickener examples include methyl cellulose, polybulal alcohol, carboxylated bulle polymer, and the like.
  • the PTFE aqueous dispersion composition of the present invention has a viscosity at 25 ° C of 0.1 Pa's or less.
  • the PTFE aqueous dispersion composition of the present invention preferably has a viscosity of 0.06 Pa's or less, and may be 0.0 OlPa's or more as long as it is within the above range.
  • the viscosity is measured at a temperature of 25 ° C. according to JIS K6893 using a B-type rotational viscometer (manufactured by Tokyo Keiki Co., Ltd.).
  • the PTFE aqueous dispersion composition of the present invention is not particularly limited. For example, while stirring the PTFE aqueous dispersion obtained by polymerization, the polyoxyalkylene alkyl ether compound (B), and as necessary, Depending on the situation, the film-forming improver (C) and other additives can be added and mixed.
  • the polyoxyalkylene alkyl ether compound (B) can be added when preparing an aqueous PTFE dispersion, and has been conventionally used, for example, for concentrating an aqueous dispersion that is a polymerization product. Although it may be added as a dispersant, it is usually preferable to add after the preparation of the PTFE aqueous dispersion to adjust to the target viscosity.
  • the conditions for the above-mentioned stirring, addition and mixing operations are preferably performed at a force of 5 to 30 ° C., which can be appropriately set according to the type and amount of the composition to be used.
  • the PTFE aqueous dispersion composition of the present invention has the above-described configuration, it improves the crack resistance and thick coatability as described above, and also has an extremely large crack limit film thickness by one application.
  • the crack limit film thickness by one application can be achieved only up to about 2 m in the past, especially when using a PTFE resin particle (A) as a modified PTFE resin.
  • it can be about 20 m or more.
  • the crack limit film thickness is determined by dropping a PTFE aqueous dispersion composition (5 ml) on an aluminum plate of 20 cm ⁇ 10 cm ⁇ l. 5 mm and using a coating applicator (manufactured by Yasuda Seiki Co., Ltd.).
  • a coating applicator manufactured by Yasuda Seiki Co., Ltd.
  • the coating thickness is greater than O / zm and continuously changes between 200 m and below, when dried at 100 ° C for 10 minutes and then baked at 380 ° C for 15 minutes, no cracks occur. The film thickness was measured.
  • modified PTFE can provide a coating with better transparency than a TFE homopolymer, but the aqueous PTFE dispersion composition of the present invention has a modified PTFE strength as a PTFE resin.
  • the resin is used, it is possible to obtain a thick film with high light transmittance despite the extremely large crack limit film thickness.
  • the PTFE resin film of the present invention is obtained by coating the above-mentioned PTFE aqueous dispersion composition of the present invention on an object to be coated.
  • the material to be coated is not particularly limited, and examples thereof include various metals, enamel, glass, various ceramics, and various heat-resistant resin molded products.
  • the object to be coated may have any shape.
  • the coating can usually be performed by applying the PTFE aqueous dispersion composition of the present invention, drying, and then firing.
  • aqueous PTFE dispersion composition of the present invention may be directly applied to a substrate, but in order to improve the adhesion to the substrate, a primer layer may be provided and formed as an overcoat layer.
  • the application is not particularly limited, and can be performed by a known coating method such as a dating method, a spray method, a roll coating method, a doctor blade method, a flow coating method, or the like.
  • the drying can be appropriately set according to the type of polyoxyalkylene alkyl ether compound (B), film-forming improver (C), etc. to be used, but it is room temperature to 150 ° C, preferably 80 to 150 °. It is preferably performed at a temperature of C for 5 to 20 minutes.
  • the firing can be performed for 5 to 60 minutes at a temperature equal to or higher than the melting temperature of the PTFE resin to be used, usually 340 to 415 ° C, and is performed at 360 to 400 ° C for 10 to 30 minutes. That power S is preferable.
  • the PTFE resin film of the present invention may be peeled off from the object to be coated after the above-mentioned firing depending on the type of object to be coated. It may be in contact with the coated product via a primer layer or the like.
  • the PTFE resin film of the present invention is formed by coating the PTFE aqueous dispersion composition of the present invention described above, it is usually about 5 to: LOO ⁇ m, preferably about 10 to: It has a thickness of LOO ⁇ m.
  • the PTFE resin film of the present invention can be obtained without particular limitation as long as the object to be coated does not substantially deteriorate upon firing, it can be obtained, for example, metal cooking utensils, bearings, valves, etc. , Electric wire, metal foil, boiler, pipe, ship bottom, oven lining, iron bottom plate, ice tray, snow shovel, plow, chute, conveyor, roll, mold, die, saw, file, cutting tool, knife, Scissors, hoppers, other industrial containers (especially for the semiconductor industry), and scissors can be used.
  • metal cooking utensils, bearings, valves, etc. Electric wire, metal foil, boiler, pipe, ship bottom, oven lining, iron bottom plate, ice tray, snow shovel, plow, chute, conveyor, roll, mold, die, saw, file, cutting tool, knife, Scissors, hoppers, other industrial containers (especially for the semiconductor industry), and scissors can be used.
  • the PTFE resin film of the present invention can be suitably used as a coating material for high-frequency printed circuit boards, conveyor belts, packings and the like.
  • the PTFE resin-impregnated body of the present invention has an impregnated body and a film obtained by impregnating the above-mentioned impregnated body with the above-mentioned PTFE aqueous dispersion composition of the present invention.
  • the impregnated body is not particularly limited, and examples thereof include a fiber base material, a woven fabric and a non-woven fabric.
  • the fiber substrate is not particularly limited, and examples thereof include glass fiber, carbon fiber, and aramid fiber (Kepler fiber, etc.).
  • Examples of the woven fabric'nonwoven fabric include a roof material (tent membrane) of a membrane structure building. When light transmission is required as the roofing material, it is preferable to use a modified PTFE resin as the PTFE resin.
  • the impregnation can be performed by a known method.
  • the coating film is formed by impregnating the above-mentioned PTFE aqueous dispersion composition of the present invention, it usually depends on the shape and thickness of the substrate, but is usually about 5 to: LOO ⁇ m, preferably About 10 ⁇ : having a thickness of LOO ⁇ m.
  • the PTFE aqueous dispersion composition of the present invention has the above-mentioned constitution, it can be suitably used as a coating yarn and composition that does not cause cracks despite being a thick film. Togashi.
  • the PTFE resin film of the present invention has the above-described configuration, it can be easily formed into a thick film free from defects such as cracks.
  • the PTFE resin impregnated body of the present invention has the above-mentioned constitution, it can be a thick film without cracks and the like.
  • aqueous PTFE dispersion composition of the present invention contains a resin made of modified PTFE, the resulting coating is highly light transmissive.
  • the mass of the residue obtained by drying 10 g of the PTFE aqueous dispersion at a temperature of 380 ° C. for 45 minutes was determined as a percentage of the mass of the PTFE aqueous dispersion before the drying.
  • PTFE rosin solid concentration determined in (3) above and the amount to be blended when preparing the PTFE aqueous dispersion composition of the present invention (including the blending amount at the time of preparing the PTFE aqueous dispersion), PT FE It calculated
  • composition concentrations other than (3) and (4) are values in which mass force at the time of addition is also converted.
  • PC 71.2% by mass polyoxy A PTFE aqueous dispersion concentrate A having an ethylene alkyl ether concentration [NC] of 2.9% by mass of PTFE rosin solids was prepared.
  • NC force SPTFE Kitsuki PTFE aqueous dispersion concentrated product B is 1.9% by weight of the fact solids.
  • a PTFE aqueous dispersion composition in which “(Bl) Z (B)” and “)” were 54 mass% was obtained.
  • the obtained PTFE aqueous dispersion composition had a viscosity of 2.05 X 10 " 2 Pa-s and a crack limit film thickness force SlO / zm.
  • the obtained PTFE aqueous dispersion composition had a viscosity of 5.80 ⁇ 10 ” 2 Pa-s, crack limit film thickness force ⁇ 4; ⁇ ⁇ .
  • PTFE aqueous dispersion concentrate A 300 g, TDS-120 21.6 g, acrylic resin aqueous dispersion (Nihon Shokubai Co., Ltd., solid concentration 40% by mass) 16. Og, ethyl carbitol (Nippon Shokubai Co., Ltd.) (Boiling point: 202 ° C) 8.
  • the obtained PTFE aqueous dispersion composition had a viscosity of 4.80 ⁇ 10 ” 2 Pa-s and a crack limit film thickness of 20 / zm.
  • PTFE aqueous dispersion concentrate A 300 g, TDS-120 19.4 g, acrylic resin aqueous dispersion (Nippon Shokubai Co., Ltd., solid concentration 40% by mass) 16. Og, Emargen A-60 (manufactured by Kao Corporation) Polyoxyethylene derivatives) 2. lg, ethyl carbitol 4.
  • the obtained PTFE aqueous dispersion composition had a viscosity of 3.55 ⁇ 10 ” 2 Pa-s and a crack limit film thickness of 20 / zm.
  • PTFE aqueous dispersion concentrate A 300 g, TDS-120 21.6 g, acrylic resin aqueous dispersion (Nippon Shokubai Co., Ltd., solid content 40% by mass) 16.0 g, ethyl carbitol 8.0 g, g glycerin 2. lg and pure water 55. 2 g of ⁇ Ka ⁇ , PC 53 mass 0/0, NC force 13 mass% of PTFE ⁇ solids, 3% by weight of acrylic ⁇ is PTFE ⁇ solids, Ethylcarbitol is 50% by mass of the aqueous dispersion of acrylic resin, and glycerin is a part of the solid content of PTFE resin.
  • the obtained PTFE aqueous dispersion composition had a viscosity of 5.70 ⁇ 10 ” 2 Pa-s, a crack limit film thickness force of 8; ⁇ .
  • PTFE aqueous dispersion concentrate A 300 g, TDS-120 21.6 g, Silwet L-77 (manufactured by Nippon Carker, silicone surfactant) 2. Add Ig and 79.3 g of pure water, .53% by mass, NC is 13% by mass of PTFE resin solids, Silicone surfactant is 1% by mass of PTFE resin solids, (Bl) Z (B)
  • the obtained PTFE aqueous dispersion composition had a viscosity of 5.70 ⁇ 10 ” 2 Pa-s, crack limit film thickness force ⁇ 2; ⁇ .
  • the resulting PTFE aqueous dispersion composition had a viscosity of 4.40 ⁇ 10 ” 2 Pa-s and a crack limit film thickness of 12 / zm.
  • the obtained PTFE aqueous dispersion composition had a viscosity of 4.90 ⁇ 10 ” 2 Pa-s and a crack limit film thickness force m.
  • the obtained PTFE aqueous dispersion composition had a viscosity of 5.70 ⁇ 10 ” 2 Pa-s and a crack limit film thickness force SlO / zm.
  • the obtained PTFE aqueous dispersion composition had a viscosity of 4.95 ⁇ 10 ” 2 Pa-s and a crack limit film thickness of 29 / zm.
  • PTFE aqueous dispersion concentrate A 300g coconut, TDS-80 13. Add Og and pure water 90.Og, PC 53% by mass, NC is 9% by mass of PTFE oil solids, (Bl) Z ( B) A 0% by mass PTFE aqueous dispersion was obtained.
  • the obtained aqueous dispersion composition had a viscosity of 1.80 ⁇ 10 ” 2 Pa ′s and a crack limit film thickness of 5 ⁇ m.
  • the obtained aqueous dispersion composition had a viscosity of 7.45 ⁇ 10_2 Pa's and a crack limit film thickness of 5 m.
  • the resulting aqueous dispersion composition has a viscosity of 2.00 X 10 _2 Pa's and a crack limit film thickness of 8 m.
  • the obtained aqueous dispersion composition had a viscosity of 2.00 ⁇ 10 ” 2 Pa-s and a crack limit film thickness of 29 ⁇ m.
  • the resulting aqueous dispersion composition had a viscosity of 0.60 ⁇ 10 ” 2 Pa-s and a crack limit film thickness of 1 ⁇ m.
  • the resulting aqueous dispersion composition had a viscosity of 13.90 ⁇ 10 ” 2 Pa-s and a crack limit film thickness of 6 ⁇ m.
  • the resulting aqueous dispersion composition had a viscosity of 15.05 ⁇ 10 ” 2 Pa-s and a crack limit film thickness of 5 ⁇ m.
  • PTFE aqueous dispersion concentrate C 300g, TDS-80 7.lg, TDS-120 15.lg, acrylic resin aqueous dispersion (Nippon Shokubai Co., Ltd., solid content concentration 40% by mass) 16.2g, Ethylcal Bitoru 8. added lg and pure water 60.
  • the obtained aqueous dispersion composition had a viscosity of 3.05 X 10 " 2 Pa-s and a crack limit film thickness of 41 ⁇ m.
  • PTFE aqueous dispersion concentrated product A 300g, TDS-808.8g and pure water 94.2g added, 53% PC by weight, NC 7% by weight PTFE solids, (Bl) Z (B) A PTFE aqueous dispersion with 0 mass% was obtained.
  • the obtained aqueous dispersion composition had a viscosity of 1.55 ⁇ 10 ” 2 Pa-s and a crack limit film thickness of 2 m.
  • the PTFE aqueous dispersion composition obtained from Example 3 and the aqueous dispersion compositions obtained from Comparative Example 1 and Comparative Example 5 were coated on an aluminum plate (20 cm ⁇ 15 cm ⁇ l.5 mm) with a film thickness of 10 Apply to ⁇ 20 m, dry at 100 ° C for 10 minutes, peel off the film obtained by baking at 380 ° C for 15 minutes, and use a direct reading haze meter (Toyo Seiki Seisakusho) Then, the total light transmittance and haze value of the portion having a film thickness of 15 m were measured.
  • the total light transmittance indicates the light transmission ratio, and the larger the value, the better the light transmittance.
  • the haze value indicates the ratio of diffused light in the transmitted light, and the smaller the value, the better the transparency.
  • Table 1 shows the total light transmittance and haze value of the coatings obtained in Example 3, Comparative Example 1 and Comparative Example 5.
  • Example 3 9 4 .9% 8.0% Comparative Example 1 9 2.5% 2 3.7% Comparative Example 5 9 3 .5% 1 9 .4%
  • Example 3 PPVE-modified PTFE is used, while in Comparative Examples 1 and 5, PTFE homopolymer (Homo PTFE) is used! It can be seen that the coating containing the modified PTFE-strengthened resin is superior in light transmission, and has a low ratio of diffused light, and thus excellent in transparency.
  • PTFE homopolymer Homo PTFE
  • the PTFE aqueous dispersion composition of the present invention also has the above-mentioned constitutional power, it is suitable as a coating yarn and composition that does not cause cracks despite being easy to form a thick film. Can be used.
  • the PTFE resin film of the present invention has the above-described configuration, it can be easily formed into a thick film free from defects such as cracks.
  • the PTFE resin impregnated body of the present invention has the above-mentioned constitution, it can be a thick film without cracks and the like.
  • aqueous PTFE dispersion composition of the present invention contains a resin made of modified PTFE, the resulting coating is highly light transmissive.

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Abstract

La présente invention a pour objet une formulation de dispersion aqueuse de polytétrafluoroéthylène (PTFE) dont l'épaisseur au seuil de rupture de film est élevée et qui permet la formation d'un film épais par application ou imprégnation unique. Ladite formulation permet d’obtenir un film dont les propriétés d'épaisseur au seuil de rupture et de transparence sont excellentes, et ce alors qu’un PTFE modifié est employé. La formulation de la dispersion comprend des particules de résine PTFE (A) et un dérivé de polyoxyalkylène alkyléther (B), et est caractérisée en ce que la concentration de résine PTFE solide est comprise entre 30 et 70 % en masse vis-à-vis de la masse totale de la dispersion, en ce que la viscosité de ladite formulation à 25 °C est inférieure à 0,1 Pa.s, en ce que le dérivé de polyoxyalkylène alkyléther (B) est inclus dans une proportion de 9 à 20 parts en masse pour 100 parts en masse de PTFE solide, et en ce que la résine PTFE qui constitue les particules (A) est une résine PTFE modifiée.
PCT/JP2005/017643 2004-09-27 2005-09-26 Formulation de dispersion aqueuse de polytetrafluoroethylene, film de resine polytetrafluoroethylene, et produits impregnes de resine polytetrafluoroethylene WO2006035726A1 (fr)

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JP2006175732A (ja) * 2004-12-22 2006-07-06 Matsushita Electric Works Ltd プリント配線板用シート材、プリント配線板用積層板、多層プリント配線板用積層板
WO2009022579A1 (fr) * 2007-08-10 2009-02-19 Daikin Industries, Ltd. Composition de revêtement
JPWO2007074901A1 (ja) * 2005-12-28 2009-06-04 ダイキン工業株式会社 フルオロポリマー水性分散液
JP2010512429A (ja) * 2006-12-08 2010-04-22 アーケマ・インコーポレイテッド 安定な含フッ素ポリマー分散液を製造するための水系方法
JP2018011033A (ja) * 2016-07-15 2018-01-18 住友電工ファインポリマー株式会社 プリプレグ及び多層基板
US10030163B2 (en) 2014-10-01 2018-07-24 Nok Corporation Coating agent aqueous dispersion
JP2019043134A (ja) * 2017-08-31 2019-03-22 スターライト工業株式会社 非粘着シート
CN111918922A (zh) * 2018-04-05 2020-11-10 三菱铅笔株式会社 聚四氟乙烯水性分散体
CN113061311A (zh) * 2021-04-21 2021-07-02 山东森荣新材料股份有限公司 高频覆铜板用ptfe改性膜

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JP2006175732A (ja) * 2004-12-22 2006-07-06 Matsushita Electric Works Ltd プリント配線板用シート材、プリント配線板用積層板、多層プリント配線板用積層板
JP4985399B2 (ja) * 2005-12-28 2012-07-25 ダイキン工業株式会社 フルオロポリマー水性分散液
JPWO2007074901A1 (ja) * 2005-12-28 2009-06-04 ダイキン工業株式会社 フルオロポリマー水性分散液
JP2010512429A (ja) * 2006-12-08 2010-04-22 アーケマ・インコーポレイテッド 安定な含フッ素ポリマー分散液を製造するための水系方法
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WO2009022579A1 (fr) * 2007-08-10 2009-02-19 Daikin Industries, Ltd. Composition de revêtement
US10030163B2 (en) 2014-10-01 2018-07-24 Nok Corporation Coating agent aqueous dispersion
JP2018011033A (ja) * 2016-07-15 2018-01-18 住友電工ファインポリマー株式会社 プリプレグ及び多層基板
JP2019043134A (ja) * 2017-08-31 2019-03-22 スターライト工業株式会社 非粘着シート
CN111918922A (zh) * 2018-04-05 2020-11-10 三菱铅笔株式会社 聚四氟乙烯水性分散体
CN111918922B (zh) * 2018-04-05 2022-12-30 三菱铅笔株式会社 聚四氟乙烯水性分散体
CN113061311A (zh) * 2021-04-21 2021-07-02 山东森荣新材料股份有限公司 高频覆铜板用ptfe改性膜

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