WO2019154145A1 - 具有特殊配方的发色膜、压力测试膜及其制备方法 - Google Patents
具有特殊配方的发色膜、压力测试膜及其制备方法 Download PDFInfo
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- WO2019154145A1 WO2019154145A1 PCT/CN2019/073333 CN2019073333W WO2019154145A1 WO 2019154145 A1 WO2019154145 A1 WO 2019154145A1 CN 2019073333 W CN2019073333 W CN 2019073333W WO 2019154145 A1 WO2019154145 A1 WO 2019154145A1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/043—Improving the adhesiveness of the coatings per se, e.g. forming primers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
- B05D3/061—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation using U.V.
- B05D3/065—After-treatment
- B05D3/067—Curing or cross-linking the coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/50—Multilayers
- B05D7/52—Two layers
- B05D7/53—Base coat plus clear coat type
- B05D7/536—Base coat plus clear coat type each layer being cured, at least partially, separately
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0041—Optical brightening agents, organic pigments
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K9/10—Encapsulated ingredients
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
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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
- C09D101/00—Coating compositions based on cellulose, modified cellulose, or cellulose derivatives
- C09D101/08—Cellulose derivatives
- C09D101/26—Cellulose ethers
- C09D101/28—Alkyl ethers
- C09D101/286—Alkyl ethers substituted with acid radicals
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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
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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
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- C09D129/00—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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
- C09D163/10—Epoxy resins modified by unsaturated compounds
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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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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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
- C09D189/00—Coating compositions based on proteins; Coating compositions based on derivatives thereof
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/41—Organic pigments; Organic dyes
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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
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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/02—Measuring force or stress, in general by hydraulic or pneumatic means
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2401/08—Cellulose derivatives
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- C08J2401/28—Alkyl ethers
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2409/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2409/06—Copolymers with styrene
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of 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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
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- C08J2463/10—Epoxy resins modified by unsaturated compounds
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Definitions
- the present disclosure relates to a chromonic film and a pressure test film, and more particularly to a chromonic film having a special formulation, a pressure test film, and a method of preparing the same.
- the pressure test is mainly applied to various production processes such as lamination of printed circuit boards, confirmation and adjustment of pressure between rolls, lamination of liquid crystal glass panels, and assembly of engine cylinders, which have strict requirements on pressure.
- the pressure tester is usually used for stress test, but the pressure test method is complicated in operation, the measurement result is hysteresis, the test accuracy and sensitivity are poor, and it is only applicable to the pressure test in a small area, and is not suitable for online pressure monitoring, and is not applicable. Pressure test with special shaped areas.
- the prior art provides a pressure test film comprising a chromonic film material L containing microcapsules of a dye precursor and a chromogenic film material K containing a chromogenic compound.
- the chromonic film material L and the chromogenic film material K are overlapped in a coating manner relative to each other, placed between the pressure receiving surfaces, and the microcapsules are broken when the pressure is greater than the breaking threshold, releasing the dye.
- the dye is brought into contact with the color developing compound contained in the color developing film material K to cause a color forming reaction, and the pressure test can be completed by observing and measuring the concentration depth of the color forming region.
- the present disclosure is based on the above requirements, improving the formulation of the chromonic layer such that the microcapsules are formed uniformly, and by ensuring a sufficient color development concentration by defining a ratio between the electron-donating leuco dye precursor and the solvent contained in the microcapsules. Under the premise, it is effective to avoid the defects that the color development is weak or even unusable due to the precipitation of the electron-donating leuco dye precursor under low-temperature use conditions.
- a chromonic film comprising: a substrate, an undercoat layer sequentially laminated on the substrate, a textured layer, and a chromonic layer, the chromonic layer comprising the microcapsule
- the microcapsule contains an electron donating leuco dye precursor.
- the microcapsules are coated with a dye solution consisting of an electron-donating leuco dye precursor and a solvent, wherein each 100 parts of the dye solution contains 3 parts to 12 parts of an electron-donating leuco dye precursor.
- a pressure test film comprising: a chromonic film layer comprising a chromonic film; and a chromogenic film layer containing an electron accepting compound Color developing materials.
- a method of preparing a chromonic film comprising: preparing an undercoat layer slurry by dissolving an aqueous resin in water, adding an auxiliary agent and stirring uniformly; and adding a reactive diluent to the UV The resin is stirred evenly, and a photoinitiator or an auxiliary agent is added and stirred to form a slurry of the uneven structure layer; the oil phase is added to the water by a membrane emulsification method by disposing an oil phase and an aqueous phase containing an electron-donating leuco dye precursor.
- a method of preparing a pressure test film comprising: preparing an undercoat layer slurry by dissolving an aqueous resin in water, adding an auxiliary agent and stirring uniformly; and adding a reactive diluent to the UV The resin is stirred evenly, and a photoinitiator or an auxiliary agent is added and stirred to form a slurry of the uneven structure layer; the oil phase is added to the water by a membrane emulsification method by disposing an oil phase and an aqueous phase containing an electron-donating leuco dye precursor.
- the phase forms an emulsion, and then is added with a curing agent and stirred uniformly, and heated to 50 ° C for 4 hours to prepare a microcapsule dispersion, and then added with a binder and water and stirred to form a chromonic layer slurry; by adding activated clay
- the water is stirred and pre-dispersed, and then sanded to form an active white clay aqueous dispersion, and then added with a binder to uniformly form a color developing layer slurry;
- the base coating slurry is coated on the substrate, and then
- the undercoat layer is sequentially coated with the uneven structure layer slurry and the chromonic layer slurry to obtain a chromonic film which can be used for the pressure test film, and the chromogenic layer slurry is coated on the substrate to obtain a display which can be used for the pressure test film.
- Color film and will Said coloring film bonded to the color film to the film stress test.
- the particle size of the microcapsules in the chromonic film material L of the pressure test film provided by the present disclosure is relatively uniform, and the coating is uniformly uniform without agglomeration, effectively avoiding agglomeration caused by large and small particles.
- the critical pressure values between the microcapsules are relatively close, when the pressure value fluctuates very little during the stress test, it can also be displayed with the clearest and most obvious concentration difference, thereby realizing the large-area stress test environment. High sensitivity, high resolution testing.
- the pressure test film provided by the present disclosure can effectively avoid the use condition at low temperature by ensuring a sufficient color development concentration by defining a ratio between the electron-donating leuco dye precursor contained in the microcapsule and the solvent. A defect in which hair color weakening or even unusable due to precipitation of an electron-donating leuco dye precursor.
- FIG. 1 is a schematic structural view of a chromonic film material L according to an embodiment of the present disclosure
- FIG. 2 is a schematic structural view of a pressure test film according to an embodiment of the present disclosure
- FIG. 3 is a flow chart of a method of preparing a chromonic film according to an embodiment of the present disclosure
- FIG. 4 is a flow chart of a method of preparing a pressure test film in accordance with an embodiment of the present disclosure.
- the chromonic film provided by the present disclosure is made of a chromonic film material L, and the chromonic film material L is composed of a chromonic film substrate 213, an undercoat layer 215, a textured layer 217, and a coloring layer 219. composition.
- the undercoat layer 215, the uneven structure layer 217, and the coloring layer 219 are sequentially applied and adhered to the chromonic film substrate 213.
- the structure and function of the undercoat layer 215, the relief structure layer 217, and the coloring layer 219 will be described in more detail below.
- the pressure test film provided by the present disclosure is composed of a chromonic film layer containing a chromonic film material L and a color developing film layer containing a chromogenic film material K.
- the constitution of the color developing film material L is as described above, and the color developing film material K is composed of the color developing film substrate 223 and the color developing layer 225.
- the pressure test film is formed by overlapping the coloring layer 219 of the color developing film so as to face the coloring layer 225 of the color developing film.
- the chromonic film material L and the chromogenic film material K may not be formed into a pressure test film at the time of manufacture, but may be separately manufactured and sold as a separate film, that is, a chromonic film and a chromogenic film, and in application.
- a structure such as a pressure test film is formed (hereinafter, for the sake of explanation, it is still called Test the film for pressure).
- a pressure P is applied between the photographic film pressure receiving surface 211 and the chromizing film pressure receiving surface 221, so that the microcapsules in the chromonic film are released by electron force release.
- the color dye when the electron-donating leuco dye meets with the electron-accepting compound in the color-developing layer, and then determines the pressure P according to the degree of color formation, thereby achieving the purpose of testing the pressure using the pressure test film.
- the substrate described herein includes a substrate 213 of a chromonic film and a substrate 223 of a chromogenic film.
- a substrate suitable for the present disclosure may be selected from a substrate such as a plastic film, paper, synthetic paper, or the like.
- the plastic film include polyethylene terephthalate (PET), polyethylene (PE), polypropylene (PP), and polyvinyl chloride (PVC).
- Specific examples of the paper include high quality paper, coated paper, art paper, and the like.
- Specific examples of the synthetic paper include synthetic papers formed of synthetic fibers such as polyethylene, polyamide, and polyethylene terephthalate, or synthetic papers formed by laminating them on one or both sides of paper. Paper, etc.
- the present disclosure preferably has a PET of 50-125 [mu]m.
- the undercoat layer 215 functions to improve adhesion of the textured structure layer 217 on the chromonic film substrate 213.
- the undercoat layer 215 is usually composed of one or more aqueous resins including styrene-butadiene copolymer latex (SBR), acrylate latex, polyvinyl alcohol (PVA), gelatin, carboxymethyl group.
- SBR styrene-butadiene copolymer latex
- PVA polyvinyl alcohol
- gelatin carboxymethyl group.
- a synthetic or natural polymeric substance such as cellulose (CMC).
- the present disclosure is preferably PVA and SBR.
- the relief structure layer 217 functions to apply pressure to the microcapsules in the chromonic layer 219 after the pressure applied to the surface of the pressure test film is converted by area.
- the textured structure layer 217 is composed of a UV resin, a reactive diluent, and a photoinitiator.
- the UV resin in the uneven structure layer 217 is composed of two or more of the following UV resins, and the UV resin suitable for the present disclosure includes, but is not limited to, urethane acrylate, ring Oxy acrylate, aliphatic urethane acrylate, and the like.
- the reactive diluent in the textured structure layer 217 is composed of two or more of the following reactive diluents, including but not limited to difunctional monomers such as tripropylene glycol diacrylate (TPGDA), dipropylene glycol double Acrylate (DPGDA), trifunctional monomers such as pentaerythritol triacrylate (PET3A), trimethylolpropane triacrylate (TMPTA), polyfunctional monomers such as dipentaerythritol hexaacrylate (DPHA), pentaerythritol tetraacrylate Ester (PET4A) and the like.
- difunctional monomers such as tripropylene glycol diacrylate (TPGDA), dipropylene glycol double Acrylate (DPGDA), trifunctional monomers such as pentaerythritol triacrylate (PET3A), trimethylolpropane triacrylate (TMPTA), polyfunctional monomers such as dipentaerythritol
- Photoinitiators include, but are not limited to, 1-hydroxycyclohexyl phenyl ketone (184), 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO), 2-methyl-1-[ 4-Methylthiophenyl]-2-morphinyl-1-propanone (907) and the like.
- the uneven structure layer 217 is disposed on the undercoat layer 215, and the uneven portion of the uneven structure layer 217 has at least two convex portions, and two adjacent convex portions
- the linear distance L between them satisfies D50X0.2 ⁇ L ⁇ D50X0.8.
- L ⁇ D50X0.2 because the spacing between adjacent convex portions is too small, the force area of the microcapsules cannot be effectively concentrated, and the pressure distribution under micro-pressure conditions cannot be measured.
- L>D50X0.8 most of the microcapsules The pressure distribution measurement cannot be achieved because it is trapped in the gap between the adjacent convex portions and cannot be broken when the pressure is applied.
- the shape of the protrusion in the relief structure layer 217 includes, but is not limited to, a shape of a cylinder, a cone, a cuboid, a cube, or the like.
- the chromonic layer 219 comprises microcapsules, a binder, and an adjuvant comprising an electron donating leuco dye precursor.
- the microcapsules of the present disclosure comprise at least two portions of an electron donating leuco dye precursor solution and a microcapsule wall.
- the electron donating leuco dye precursor solution comprises at least one electron donating leuco dye precursor and at least one solvent.
- the role of the electron donating leuco dye precursor is the primary coupler.
- the electron-donating leuco dye precursor a known one can be used, such as a fluoran compound, a mercaptopeptide ketone compound, a rhodamine lactam compound, a spiropyran compound, or a phenothiazine compound.
- Electron-donating leuco dye precursors suitable for use in the present disclosure include, but are not limited to, crystal violet lactone (CVL), leuco methylene blue (BLMB).
- the solvent mainly serves to dissolve the electron-donating leuco dye precursor, and a known one can be used.
- diarylalkanes such as 1-phenyl-1-dimethylphenylethane, diaryl olefins, alkylnaphthalenes such as diisopropylnaphthalene, aliphatic hydrocarbons such as isoalkanes, and corn oil
- Natural animal and vegetable oils such as castor oil and rapeseed oil, mineral oil, etc.
- the electron-donating leuco dye precursor solution contains 3 parts to 12 parts of an electron-donating leuco dye precursor per 100 parts of the dye solution, if given If the electronic leuco dye precursor is less than 3 parts, the coloring concentration is insufficient. If the electron-donating leuco dye precursor is higher than 12 parts, the electron-donating leuco dye precursor crystallizes in a low temperature environment, resulting in effective development. The color component is reduced.
- a solvent having a lower boiling point may be added as a co-solvent as needed to better dissolve the electron-donating leuco dye precursor in a solvent.
- Low boiling solvents suitable for use in the present disclosure include, but are not limited to, ketones such as acetone, methyl ethyl ketone, esters such as methyl acetate and ethyl acetate.
- the wall material of the microcapsule may be a well-known water-insoluble and oil-insoluble substance such as polyurethaneurea, gelatin, melamine-formaldehyde resin, etc., and the present disclosure is preferably a polyurethaneurea.
- the wall material of the microcapsules may be formed by a known method such as an interfacial polymerization method, an in-situ polymerization method, a coacervation method, or the like.
- the wall material is preferably formed by interfacial polymerization.
- the wall material consists at least of a reactive monomer and a curing agent.
- Suitable reactive monomers for the microcapsule wall material include, but are not limited to, dicyclohexylmethane diisocyanate (HDI), hexamethylene diisocyanate (HMDI), trimethylolpropane adduct of hexamethylene diisocyanate, benzene A polyisocyanate oligomer such as a trimethylolpropane adduct of dimethic acid diisocyanate.
- Curing agents suitable for the preparation of the microcapsule wall material include, but are not limited to, polyhydric hydroxy compounds such as aliphatic or aromatic polyols, polyamines such as triethylenetetramine, hexamethylenediamine, aliphatic polyamines, epoxy An alkane adduct such as a butylene oxide adduct of ethylenediamine may be used as long as it contains two or more -NH groups or -NH2 groups in the molecule.
- the curing agent is preferably dissolved in water before use.
- the span is less than 0.5, the manufacturing cost of the microcapsules increases sharply; if the span is larger than 1.2, the phenomenon of agglomeration of the size particles in the microcapsule system due to the difference in surface energy is prominent, which causes the pressure test film to cause coloration due to agglomeration during application. The density is uneven, resulting in reduced measurement accuracy.
- the binder in the coloring layer may be a water-soluble polymer such as starch, CMC, or PVA.
- the adjuvant includes at least an emulsifier including, but not limited to, an amphiphilic polymer such as PVA, CMC, starch, gelatin, etc., and PVA is preferred in the present disclosure.
- an emulsifier including, but not limited to, an amphiphilic polymer such as PVA, CMC, starch, gelatin, etc., and PVA is preferred in the present disclosure.
- the color developing layer 225 includes an electron accepting compound and a binder.
- the electron-accepting compound is a main color developing agent, and the electron-accepting compound may be a known electron-accepting compound including an inorganic compound such as activated clay, kaolin, clay, or the like.
- organic compounds such as: aromatic carboxylic acid metal salts, carboxylated terpene phenolic resin metal salts, phenolic resins, salicylates and derivatives thereof.
- the function of the binder of the color developing layer 225 is to improve the adhesion of the electron-accepting compound to the color developing film substrate 223.
- the adhesive to which the color developing layer 225 of the present disclosure is applied is composed of one or more of the following water-soluble adhesives including, but not limited to, SBR, acrylate latex, PVA, gum arabic, gelatin, CMC, and the like.
- step S310 various pastes used for producing a coloring film, that is, a coloring film material L, are prepared.
- the slurry includes at least an undercoat layer paste, a textured layer slurry, and a chromonic layer slurry.
- the step S310 comprises preparing an undercoat slurry to be used by dissolving the aqueous resin in water, adding an auxiliary agent and stirring uniformly.
- the step S310 further comprises forming a relief structure layer slurry to be used by adding a reactive diluent to the UV resin and stirring uniformly, adding a photoinitiator or an auxiliary agent and stirring.
- the step S310 further includes preparing the microcapsules and formulating the chromonic layer slurry, wherein the preparing the microcapsules comprises emulsification of the water-oil mixture and forming the microcapsule wall material.
- the oil phase is composed at least of the above-mentioned electron donating leuco dye precursor solution, a reaction monomer for synthesizing the microcapsule wall material, and the aqueous phase is composed of at least an emulsifier and water.
- the emulsification process may employ a known emulsification method such as a mechanical stirring emulsification method, a homogeneous emulsification method, a phacoemulsification method, a membrane emulsification method, or the like.
- the emulsion is preferably prepared by a membrane emulsification method, and the aqueous solution of the curing agent is added and stirred uniformly, and the temperature is raised to 50 ° C for 4 hours to prepare a microcapsule dispersion, and the preparation color is prepared.
- the layer slurry comprises adding a binder and water to the microcapsule dispersion and stirring to form a chromonic layer slurry for use.
- step S320 the undercoat layer is applied onto the substrate by a known coating method such as wire bar, gravure coating, extrusion coating, reverse roll coating or the like and dried.
- step S330 the wet coating of the uneven structure layer is applied on the undercoat layer by a known coating method such as wire bar, gravure coating, extrusion coating, reverse roll coating or the like to obtain a textured structure layer.
- step S340 the coloring layer is applied onto the uneven structure layer by a known coating method such as slope coating or curtain coating, and dried to obtain a coloring film material according to the present disclosure.
- FIG. 4 is a flow chart of a method of preparing a pressure test film in accordance with an embodiment of the present disclosure.
- the preparation method of the pressure test film is basically the same as the preparation method of the chromonic film as shown in FIG. 3 except for the steps S410, S450 and S460, and therefore the same part will be referred to the description of FIG.
- the step S410 in the pressure test film preparing method shown in FIG. 4 includes the content in step S310 shown in FIG.
- a slurry for forming a chromogenic film material is prepared in step S410, the paste comprising at least a chromogenic layer slurry, and the chromogenic layer slurry is passed
- the activated clay is added to water and stirred for pre-dispersion, and then sanded to obtain an aqueous dispersion of activated clay, and added with a binder to uniformly form a coloring layer slurry for use.
- step S450 the coloring layer is applied onto the substrate by a known coating method such as wire bar, gravure coating, extrusion coating, reverse roll coating or the like, and dried to obtain the color developing film material. .
- step S460 the obtained chromonic film material and chromogenic film material are bonded together or temporarily bonded together when they are used to form the pressure test film.
- step S410 as shown in FIG. 4 with respect to step S310 shown in FIG. 3, and the content of step S450 shown in FIG. Together, a method for preparing a chromogenic film material can be formed.
- the microcapsule emulsion is obtained by the membrane emulsification method, and then the curing agent aqueous solution is added to the obtained emulsion, and the temperature is raised to 50 ° C under stirring. After continuing to react for 4 hours, it was cooled to room temperature and water was added to adjust the solid content to 30%, thereby obtaining a microcapsule dispersion containing an electron-donating leuco dye precursor.
- a 0.5 micron undercoat layer and a textured layer were sequentially coated with a wire bar, and a 12 micron chromonic layer was coated with a slope coater, dried, and wound to obtain the pressure of the present disclosure.
- a 13 micron chromogenic layer was coated on a 75 micron PET substrate using a wire bar, and after drying, the chromogenic film material of the pressure test film of the present disclosure was obtained.
- the resulting chromonic film material was overlaid with the chromogenic film material in a manner opposite to the coating to test its properties.
- the aqueous phase solution was used as a continuous mobile phase of a membrane emulsifier, and the oil phase solution was used as a dispersed phase to obtain a microcapsule emulsion by a membrane emulsification method. Then, an aqueous solution of a curing agent was added to the obtained emulsion, and the temperature was raised to 50 ° C under stirring, and the reaction was continued for 4 hours, and then cooled to room temperature and water was added to adjust the solid content to 30%, thereby obtaining an electron-donating leuco dye precursor. Microcapsule dispersion.
- a 0.5 micron undercoat layer and a textured layer were sequentially coated with a wire bar, and a 12 micron chromonic layer was coated with a slope coater, dried, and wound to obtain the pressure of the present disclosure.
- a 13 micron chromogenic layer was coated on a 75 micron PET substrate using a wire bar, and after drying, the chromogenic film material of the pressure test film of the present disclosure was obtained.
- the resulting chromonic film material was overlaid with the chromogenic film material in a manner opposite to the coating to test its properties.
- the aqueous phase solution was used as a continuous mobile phase of a membrane emulsifier, and the oil phase solution was used as a dispersed phase to obtain a microcapsule emulsion by a membrane emulsification method. Then, an aqueous solution of a curing agent was added to the obtained emulsion, and the temperature was raised to 50 ° C under stirring, and the reaction was continued for 4 hours, and then cooled to room temperature and water was added to adjust the solid content to 30%, thereby obtaining an electron-donating leuco dye precursor. Microcapsule dispersion.
- a 13 micron chromogenic layer was coated on a 75 micron PET substrate using a wire bar, and after drying, the chromogenic film material of the pressure test film of the present disclosure was obtained.
- the resulting chromonic film material was overlaid with the chromogenic film material in a manner opposite to the coating to test its properties.
- the aqueous phase solution was used as a continuous mobile phase of a membrane emulsifier, and the oil phase solution was used as a dispersed phase to obtain a microcapsule emulsion by a membrane emulsification method. Then, an aqueous solution of a curing agent was added to the obtained emulsion, and the temperature was raised to 50 ° C under stirring, and the reaction was continued for 4 hours, and then cooled to room temperature and water was added to adjust the solid content to 30%, thereby obtaining an electron-donating leuco dye precursor. Microcapsule dispersion.
- a 0.5 micron undercoat layer and a textured layer were sequentially coated with a wire bar, and a 12 micron chromonic layer was coated with a slope coater, dried, and wound to obtain the pressure of the present disclosure.
- a 13 micron chromogenic layer was coated on a 75 micron PET substrate using a wire bar, and after drying, the chromogenic film material of the pressure test film of the present disclosure was obtained.
- the resulting chromonic film material was overlaid with the chromogenic film material in a manner opposite to the coating to test its properties.
- the aqueous phase solution was used as a continuous mobile phase of a membrane emulsifier, and the oil phase solution was used as a dispersed phase to obtain a microcapsule emulsion by a membrane emulsification method. Then, an aqueous solution of a curing agent was added to the obtained emulsion, and the temperature was raised to 50 ° C under stirring, and the reaction was continued for 4 hours, and then cooled to room temperature and water was added to adjust the solid content to 30%, thereby obtaining an electron-donating leuco dye precursor. Microcapsule dispersion.
- a 0.5 micron undercoat layer and a textured layer were sequentially coated with a wire bar, and a 12 micron chromonic layer was coated with a slope coater, dried, and wound to obtain the pressure of the present disclosure.
- a 13 micron chromogenic layer was coated on a 75 micron PET substrate using a wire bar, and after drying, the chromogenic film material of the pressure test film of the present disclosure was obtained.
- the resulting chromonic film material was overlaid with the chromogenic film material in a manner opposite to the coating to test its properties.
- an aqueous phase solution was used as a continuous phase, and an oil phase solution was added under high-speed stirring at 750 rpm, and emulsified for 10 minutes to obtain a microcapsule emulsion. Then, an aqueous solution of a curing agent was added to the obtained emulsion, and the temperature was raised to 50 ° C under stirring, and the reaction was continued for 4 hours, and then cooled to room temperature and water was added to adjust the solid content to 30%, thereby obtaining an electron-donating leuco dye precursor. Microcapsule dispersion.
- a 0.5 micron undercoat layer was sequentially coated on a 75 micron PET substrate using a wire bar, and a 12 micron chromonic layer was coated with a slope coater, dried, and wound to obtain a chromonic film material of a pressure test film.
- a 13 micron chromogenic layer was coated on a 75 micron PET substrate using a wire bar, and after drying, the chromogenic film material of the pressure test film was obtained.
- the resulting chromonic film material was overlaid with the chromogenic film material in a manner opposite to the coating to test its properties.
- an aqueous phase solution was used as a continuous phase, and an oil phase solution was added under high-speed stirring at 950 rpm, and emulsified for 10 minutes to obtain a microcapsule emulsion. Then, an aqueous solution of a curing agent was added to the obtained emulsion, and the temperature was raised to 50 ° C under stirring, and the reaction was continued for 4 hours, and then cooled to room temperature and water was added to adjust the solid content to 30%, thereby obtaining an electron-donating leuco dye precursor. Microcapsule dispersion.
- a 0.5 micron undercoat layer and a textured layer were sequentially coated with a wire bar, and a 12 micron chromonic layer was coated with a slope coater, dried, and wound to obtain a pressure test film.
- Color film material On the 75 micron PET substrate, a 0.5 micron undercoat layer and a textured layer were sequentially coated with a wire bar, and a 12 micron chromonic layer was coated with a slope coater, dried, and wound to obtain a pressure test film. Color film material.
- a 13 micron chromogenic layer was coated on a 75 micron PET substrate using a wire bar, and after drying, the chromogenic film material of the pressure test film was obtained.
- the resulting chromonic film material was overlaid with the chromogenic film material in a manner opposite to the coating to test its properties.
- microcapsule dispersion was taken and tested by a BT-9300ST laser particle size distribution analyzer to obtain a particle size distribution D50 and a particle size distribution span of the microcapsule dispersion.
- the sheet coated with the undercoat layer and the uneven structure layer was taken, and the shortest distance between the five adjacent convex portions was measured under an electron microscope (SEM), and an average value was obtained to obtain an A value.
- SEM electron microscope
- the pressure test films obtained above were divided into two groups of I and II, and the following tests were carried out under conditions of 25 ° C and 10 ° C, respectively.
- the above microcapsules are cut into a size of 3 cm ⁇ 3 cm, and then the chromonic sheet containing the electron-donating leuco dye precursor and the color developing sheet containing the electron-accepting compound are overlapped in a coating manner, and It is placed between two smooth planes, and the entire sheet is subjected to full coverage to make it saturated with color. Then, the two sheets that are overlapped are peeled off, and the color developing portion of the color developing sheet is measured by an X. rite color difference meter.
- the initial concentration value OD0 of the non-color-developing portion of the color-developing sheet was measured by the same method using the concentration value OD1, and the actual color development density OD was obtained by using OD1-OD0.
- ODI-ODII the difference ⁇ OD between the two groups of sheets at the same pressure at different temperatures can be obtained.
- A (1.5 ⁇ OD, ⁇ OD ⁇ 0.2): no dye is precipitated at 10 ° C, and can be used normally;
- the pressure test film obtained above was cut into a size of 20 cm ⁇ 20 cm, and then the color-developing sheet containing the electron-donating leuco dye precursor and the color-developing sheet containing the electron-accepting compound were overlapped in a coating manner. And placed between the two smooth planes, the entire sheet is fully covered and pressed to make it color, after which the overlapping two sheets are peeled off and randomly measured on the color developing sheet by X.rite color difference meter.
- the color concentration value ODi of the different regions of the group is obtained, and the average value OD is obtained, and the maximum error value ⁇ OD is obtained, and the ⁇ OD is divided by the OD to obtain the percentage value X.
- the pressure test film obtained above was cut into a size of 10 cm ⁇ 10 cm, and 5 regions were randomly taken, and the appearance of the microcapsules was observed by an electron microscope.
- A The size particles spread evenly, without agglomeration
- the pressure test film prepared by the technical solution of the present disclosure can meet the use requirements of the low temperature environment, and can Achieve high sensitivity, high resolution pressure distribution testing.
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Abstract
Description
Claims (8)
- 一种发色膜,其包括:基材、依序层叠在基材上的底涂层、凹凸结构层和发色层,该发色层包含微胶囊,该微胶囊内包含有给电子性无色染料前体。
- 根据权利要求1所述的发色膜,其中所述微胶囊的粒度分布D50为5μm-15μm,并且粒度分布跨度span为0.5~1.2,该span=(D90-D10)/D50,其中D90表示微胶囊的累计粒度分布数达到90%时所对应的粒径,D50表示微胶囊的累计粒度分布数达到50%时所对应的粒径;而D10表示微胶囊的累计粒度分布数达到10%时所对应的粒径。
- 根据权利要求1所述的发色膜,其中所述微胶囊内包有给电子性无色染料前体和溶剂组成的染料溶液,其中每100份的染料溶液含有3份~12份的给电子性无色染料前体。
- 根据权利要求1-3任一项所述的发色膜,其中所述给电子性无色染料前体选自荧烷类化合物、吲哚基肽酮类化合物、罗丹明内酰胺类化合物、螺吡喃类化合物或吩噻嗪类化合物;所述溶剂选自二芳基烷烃类、二芳基烯烃类、烷基萘类、脂肪族烃类、天然动植物油类或矿物油。
- 根据权利要求4所述的发色膜,其中所述给电子性无色染料前体选自结晶紫内酯或无色亚甲基蓝;所述溶剂选自1-苯基-1-二甲基苯基乙烷、二异丙基萘、异烷烃、玉米油、蓖麻油或菜籽油。
- 一种压力测试膜,其包含:发色膜层,该发色膜层包含根据权利要求1-5中任一项所述的发色膜;以及显色膜层,该显色膜层含有受电子性化合物的显色材料。
- 一种制备权利要求1-5中任一项所述的发色膜的方法,其包括:通过将水性树脂溶于水中,加入助剂并搅拌均匀,制成底涂层浆料;通过将活性稀释剂加入UV树脂并搅拌均匀,加入光引发剂或助剂并搅拌均匀制成凹凸结构层浆料;通过配置含有给电子性无色染料前体的油相和水相,采用膜乳化法将油相加入水相形成乳液,再加入固化剂搅拌均匀,并升温至50℃反应4小时后制成微胶囊分散液,再加入粘合剂和水并搅拌均匀制成发色层浆料;并且在基材上涂布底涂层浆料,再在底涂层上依次涂布凹凸结构层浆料、发色层浆料以得到可用于压力测试膜的发色膜。
- 一种制备权利要求6所述的压力测试膜的方法,其包括:通过将水性树脂溶于水中,加入助剂并搅拌均匀,制成底涂层浆料;通过将活性稀释剂加入UV树脂并搅拌均匀,加入光引发剂或助剂并搅拌均匀制成凹凸结构层浆料;通过配置含有给电子性无色染料前体的油相和水相,采用膜乳化法将油相加入水相形成乳液,再加入固化剂搅拌均匀,并升温至50℃反应4小时后制成微胶囊分散液,再加入粘合剂和水并搅拌均匀制成发色层浆料;通过将活性白土加入水中并搅拌进行预分散,然后用砂磨机砂磨制成活性白土水分散液,加入粘合剂搅拌均匀制成显色层浆料;在基材上涂布底涂层浆料,再在底涂层上依次涂布凹凸结构层浆料、发色层浆料以得到可用于压力测试膜的发色膜,并且在基材上涂布显色层浆料以得到可用于压力测试膜的显色膜;并且将所述发色膜与所述显色膜结合成所述压力测试膜。
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