WO2012099043A1 - Composition qui change de couleur en présence de chaleur humide et indicateur qui change de couleur en présence de chaleur humide - Google Patents

Composition qui change de couleur en présence de chaleur humide et indicateur qui change de couleur en présence de chaleur humide Download PDF

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WO2012099043A1
WO2012099043A1 PCT/JP2012/050688 JP2012050688W WO2012099043A1 WO 2012099043 A1 WO2012099043 A1 WO 2012099043A1 JP 2012050688 W JP2012050688 W JP 2012050688W WO 2012099043 A1 WO2012099043 A1 WO 2012099043A1
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bismuth
wet heat
compound
indicator
discoloration
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PCT/JP2012/050688
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English (en)
Japanese (ja)
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盛作 大城
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株式会社サクラクレパス
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00—Duplicating or marking methods; Sheet materials for use therein
    • B41M5/26—Thermography ; Marking by high energetic means, e.g. laser otherwise than by burning, and characterised by the material used
    • B41M5/28—Thermography ; Marking by high energetic means, e.g. laser otherwise than by burning, and characterised by the material used using thermochromic compounds or layers containing liquid crystals, microcapsules, bleachable dyes or heat- decomposable compounds, e.g. gas- liberating
    • B41M5/282—Thermography ; Marking by high energetic means, e.g. laser otherwise than by burning, and characterised by the material used using thermochromic compounds or layers containing liquid crystals, microcapsules, bleachable dyes or heat- decomposable compounds, e.g. gas- liberating using thermochromic compounds
    • B41M5/283—Inorganic thermochromic compounds
    • 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
    • C09D11/00—Inks
    • C09D11/50—Sympathetic, colour changing or similar inks
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K11/00—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00
    • G01K11/12—Measuring temperature based upon physical or chemical changes not covered by groups G01K3/00, G01K5/00, G01K7/00 or G01K9/00 using changes in colour, translucency or reflectance
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

Definitions

  • the present invention relates to a wet heat discoloration composition and a wet heat discoloration indicator useful for detecting the sterilization conditions and confirming completion of the sterilization treatment in the high pressure steam sterilization treatment used in the medical field and food field.
  • High-pressure steam sterilization is used in various fields such as the medical field and the food processing field.
  • the medical field for example, it is used for sterilization and sterilization of medical devices and medical instruments.
  • the field of food processing for example, it is used for sterilization in the production of retort food.
  • the methods for detecting the sterilization conditions and confirming the completion of the sterilization process in high-pressure steam sterilization are roughly divided into biological methods and chemical methods, but the latter method is superior in terms of simplicity and handling. ing.
  • a chemical method a method using an indicator in which a color-changing layer is formed with a color-changing ink composition (color-changing composition) is mainly used.
  • Patent Document 1 discloses that “a bismuth compound that is insoluble or hardly soluble in one or more kinds of water selected from bismuth sesquioxide, basic bismuth carbonate, bismuth hydroxide, basic bismuth nitrate, and basic bismuth acetate, and thiourea.
  • a composition comprising one or more thiourea compounds selected from methylthiourea, ethylthiourea, trimethylthiourea, tolylthiourea, diphenylthiourea, ditolylthiourea, phenylthiourea, and methylolthiourea, and a synthetic rubber-based resin.
  • the wet heat detection indicator characterized in that it is covered on a sheet base material by a substantially transparent synthetic resin.
  • (Claims) In the [Effects of the invention] column “This wet heat detection indicator is superior to conventional indicators in discoloration response at the completion of sterilization conditions and safety to the human body. It has a discoloration condition that is consistent with the conditions and retort sterilization conditions in the food field. "
  • the conventional wet heat detection indicator has the following problems.
  • the bismuth compound used in the conventional wet heat detection indicator does not dissolve in the organic solvent, so it is necessary to pulverize the bismuth compound when preparing the discolorable composition, and finely pulverize and disperse it.
  • An object of the present invention is to provide a wet heat discoloration composition and a wet heat discoloration indicator in which the bismuth compound is not pulverized when preparing the discoloration composition, and the problem of bismuth compound precipitation over time is improved.
  • the present inventor has found that the above object can be achieved when a specific bismuth compound is used, and the present invention has been completed.
  • a wet heat color-changing composition comprising a bismuth compound, a sulfur compound, a binder and an organic solvent, wherein the bismuth compound is an organic solvent-soluble organic bismuth compound.
  • the organic solvent-soluble organic bismuth compound includes bismuth salt of aliphatic carboxylic acid, bismuth salt of aromatic carboxylic acid, ⁇ -diketone complex of bismuth, alkoxide of bismuth, bismuth trifluoromethanesulfonate and triphenyl bismuth diacetate.
  • Item 4. The wet heat color-changing composition according to any one of Items 1 to 3, comprising a wet heat non-color-change dye and / or pigment. 5.
  • Item 7. The wet heat discoloration indicator according to Item 6, comprising a resin layer on the discoloration layer. 8).
  • Item 8. The wet heat color change indicator according to Item 6 or 7, further comprising a non-color change layer between the substrate and the color change layer.
  • the wet heat discoloration composition of the present invention is a wet heat discoloration composition containing a bismuth compound, a sulfur compound, a binder and an organic solvent, wherein the bismuth compound is an organic solvent-soluble organic bismuth. It is a compound.
  • the wet heat discoloration composition of the present invention having the above characteristics can be discolored by reacting a bismuth compound and a sulfur compound by heating to produce dark bismuth sulfide.
  • a step of pulverizing the bismuth compound is not necessary when preparing the wet heat discoloration composition, and the bismuth compound is precipitated over time.
  • Wet heat discoloration compositions with improved problems can be provided.
  • an organic solvent-soluble organic bismuth compound that reacts with a sulfur compound to produce black bismuth sulfide is used.
  • organic bismuth compounds soluble in organic solvents include, for example, bismuth salts of aliphatic carboxylic acids, bismuth salts of aromatic carboxylic acids, ⁇ -diketone complexes of bismuth, bismuth And at least one selected from the group consisting of bismuth trifluoromethanesulfonate and triphenyl bismuth diacetate.
  • bismuth salt of the aliphatic carboxylic acid examples include bismuth 2-ethylhexanoate, bismuth neodecanoate, bismuth citrate, and bismuth ammonium citrate.
  • bismuth salt of the aromatic carboxylic acid examples include basic bismuth gallate, bismuth subgallate, bismuth subsalicylate, bismuth naphthenate, and the like.
  • Examples of the ⁇ -diketone complex of bismuth include, for example, bismuth hexafluoro-2,4-pentandionate, tris (2,2,6,6-tetramethyl-3,5-heptanedionato) bismuth, bisasacetylacetonate Etc.
  • bismuth alkoxide examples include bismuth tert-pentaoxide.
  • bismuth compounds of the present invention at least one of bismuth neodecanoate, bismuth 2-ethylhexanoate and bismuth naphthenate is preferable.
  • the content of the bismuth compound of the present invention in the wet heat discoloration composition is not limited, but is preferably 5 to 50% by weight, more preferably 10 to 30% by weight.
  • the content of the bismuth compound of the present invention in the wet heat discoloration composition is not limited, but is preferably 5 to 50% by weight, more preferably 10 to 30% by weight.
  • the sulfur compound one that is white or light in color and reacts with the bismuth compound of the present invention to produce black bismuth sulfide is used.
  • the sulfur compound include at least one selected from the group consisting of a thiourea compound, a thiuram compound, a thiazole compound, a sulfur-containing amino acid compound, and a sulfur-containing organic acid compound.
  • thiourea compound examples include thiourea, 1,3-dimethyl-2-thiourea, 1,3-diethyl-2-thiourea, 1,3-ditolylthiourea, 2,2′-ditolylthiourea, , 3-Diphenyl-2-thiourea, 1-phenyl-2-thiourea, allylthiourea, 1-acetyl-2-thiourea, ethylenethiourea, trimethylthiourea, tolylthiourea, methylthiourea, ethylthiourea, 1-phenyl -3-thiosemicarbazide, 4-phenyl-3-thiosemicarbazide, thiocarbohydrazide, 1,3-bis (dimethylaminopropyl) -2-thiourea, tributylthiourea and the like.
  • thiuram compound examples include tetramethylthiuram disulfide, tetraethylthiuram disulfide, tetrabutylthiuram disulfide, tetrakis (2-ethylhexyl) thiuram disulfide, tetramethylthiuram monosulfide, and dipentamethylenethiuram tetrasulfide.
  • thiazole compound examples include 2-mercaptobenzothiazole, dibenzothiazolyl disulfide, 2-mercaptobenzothiazole zinc salt, cyclohexylamine salt of 2-mercaptobenzothiazole, 2- (N, N′-diethylthiocarbamoylthio). ) Benzothiazole, 2- (morpholinodithio) benzothiazole, 2-aminobenzothiazole.
  • sulfur-containing amino acid compound examples include methionine, cysteine, thiamine nitrate, and the like.
  • sulfur-containing organic acid compound examples include thiosalicylic acid, thioglycolic acid, and saccharin.
  • At least one of 1,3-ditolylthiourea, 1,3-diphenyl-2-thiourea and 1-phenyl-2-thiourea is preferable.
  • the particle size of the sulfur compound is not limited, but is preferably 20 ⁇ m or less, and more preferably 5 ⁇ m or less.
  • a sulfur compound that is soluble in an organic solvent is more preferable.
  • the content of the sulfur compound in the wet heat discoloration composition is not limited, but is preferably 1 to 50% by weight, more preferably 5 to 25% by weight.
  • the content of the sulfur compound in the wet heat discoloration composition is not limited, but is preferably 1 to 50% by weight, more preferably 5 to 25% by weight.
  • the binder is not limited as long as it is a resin capable of forming a coating film.
  • Such resins include styrene-acrylic acid copolymer resins, styrene-butadiene copolymer resins, styrene-maleic acid copolymer resins, styrene-maleic acid ester copolymer resins, and vinyl acetate-acrylic acid.
  • Copolymer resin polyvinyl alcohol resin, polyvinyl butyral resin, polyvinyl pyrrolidone resin, silicon resin, rosin resin, terpene resin, phenol resin, alkyd resin, polyester resin, polyether resin, acrylic resin, polyurethane resin, natural rubber, synthetic rubber Petroleum resin, epoxy resin, ketone resin, maleic acid resin, coumarin resin, polyamide resin, alkylphenol resin, rosin-modified resin, cellulose resin and the like. These resins can be used alone or in admixture of two or more, and at least one of styrene-acrylic acid copolymer resin, polyvinyl butyral resin, phenol resin, rosin modified resin and synthetic rubber is particularly preferable.
  • the content of the binder in the wet heat discoloration composition is not limited, but is preferably 5 to 30% by weight, more preferably 10 to 20% by weight. By setting the content of the binder within the above range, the durability of the coating film can be favorably maintained while maintaining the effects of the invention.
  • the organic solvent is not particularly limited as long as it can dissolve the bismuth compound of the present invention and a binder, and examples thereof include alcohols, polyhydric alcohols, glycol ethers, esters, ketones, aliphatic hydrocarbons, and alicyclic rings. Organic solvents such as aromatic hydrocarbons and aromatic hydrocarbons. Of these organic solvents, glycol ether solvents are preferred.
  • the content of the organic solvent in the wet heat color-changing composition is not limited, but is preferably 20 to 80% by weight, more preferably 30 to 60% by weight. From the content of such organic solvent, the content may be adjusted according to the type of binder and the viscosity required for the wet heat discoloration composition.
  • the viscosity of the wet heat color-changing composition can be adjusted by adjusting the content of the binder and / or organic solvent in the wet heat color change composition. By adjusting the viscosity, it is possible to provide a wet heat discoloration composition (ink) having a viscosity suitable for various printing techniques.
  • the wet heat discoloration composition preferably has a viscosity of less than 5000 mPa ⁇ s.
  • the viscosity suitable for silk screen printing is about 500 to 5000 mPa ⁇ s
  • the viscosity suitable for gravure printing is 10 About 500 mPa ⁇ s.
  • an extender a wet heat non-discoloring dye, an ink additive, and the like may be blended as necessary.
  • Examples of the bulking agent include bentonite, activated clay, alumina, talc, calcium carbonate, silica and the like.
  • Non-wet heat non-discoloring pigments for example, CI Direct Yellow 12, 27, 98, CI Direct Red 1, 4, 28, CI Direct Orange 8, 26, 29, CI Direct Brown 2 , 44,58,106,209, CI Acid Orange 74, CI Acid Red 111, CI Acid Blue 113,117,120, CI Acid Green 9,19,44, CI Acid Brown 13, CI Moldant Brown 19, CI Disperse Red 9, CI Solvent Yellow 16, 21,29,56,61, CI Solvent Orange 1,2,14,37,40, CI Solvent Red 1,8,23,30,49,81,82,83,84,100,109,121, CI Solvent Violet 8,21,27 CI solvent brown 20 and the like.
  • the ink additive examples include a known ink additive such as a leveling agent, an antifoaming agent, an ultraviolet absorber, and a surface conditioner.
  • the wet heat discoloration composition of the present invention can be prepared by uniformly mixing these components.
  • the binder and the organic solvent are first stirred with a dissolver or the like. At that time, if the binder is difficult to dissolve, it may be stirred while heating.
  • the heating temperature is not limited, but it may usually be about 40 to 80 ° C.
  • the sulfur compound is dissolved or dispersed.
  • a known mixer such as a ball mill, bead mill, three rolls, rotary homogenizer, high-pressure homogenizer, etc. Add and mix evenly.
  • the bismuth compound of the present invention is added and dissolved.
  • an extender, a wet heat non-color-changing dye, and an ink additive are added and further stirred.
  • the wet heat discoloration indicator of the present invention is obtained by forming a discoloration layer formed from a wet heat discoloration composition on a substrate.
  • the type of substrate is not particularly limited, and known materials can be applied.
  • metal / alloy materials aluminum foil, stainless steel foil, tin foil, tin foil, etc.
  • plastics polyyester, cellophane, acetylcellulose, ethylcellulose, polyethylene, polypropylene, polyvinyl chloride, hydrochloric acid rubber, polystyrene, polycarbonate, polyvinyl alcohol) , Polyvinyl fluoride, polyamide, polyfluorinated ethylene film, etc.
  • fibers paper, wood material, non-woven fabric, woven fabric, other fiber sheets
  • inorganic materials ceramics, glass, concrete, plaster
  • synthetic resin fiber paper synthetic paper
  • synthetic paper such as polypropylene synthetic paper and polyethylene synthetic paper can also be suitably used.
  • a discoloration layer composed of a wet heat discoloration composition (ink) may be formed on the substrate by printing or the like.
  • the thickness of the discoloration layer can be appropriately set according to the type of substrate, but is usually about 0.1 to 100 ⁇ m (preferably 0.5 to 50 ⁇ m).
  • the discoloration layer can be performed according to a known printing method such as silk screen printing, gravure printing, offset printing, letterpress printing, flexographic printing, and the like.
  • a known printing method such as silk screen printing, gravure printing, offset printing, letterpress printing, flexographic printing, and the like.
  • it can be formed by a roller, brushing, spraying, or the like.
  • each layer can also be formed by immersing a base material in ink. It is particularly suitable for materials into which ink penetrates, such as paper and nonwoven fabric. In the present invention, a printing method is particularly suitable.
  • a non-discoloring layer can be provided between the base material and the discoloring layer.
  • the non-discoloring layer can be formed of an ink that does not change color in a high-pressure steam atmosphere.
  • any ink can be used as long as it does not change color in a high-pressure steam atmosphere.
  • a commercially available normal color ink can also be used as such an ink.
  • water-based ink, oil-based ink, solventless ink, and the like can be used.
  • well-known letterpress ink, gravure ink, screen ink, offset ink, etc. can be used properly according to the printing method.
  • the ink in the non-discoloring layer may contain components (for example, a resin-based binder, a filler, a solvent, etc.) blended in a known ink.
  • components for example, a resin-based binder, a filler, a solvent, etc.
  • the wet heat discoloration indicator of the present invention is discolored under wet heat conditions, whether or not the high-pressure steam sterilizer with the wet heat discoloration indicator is in a wet heat environment by indexing the degree of discoloration under wet heat conditions in advance. Can be accurately determined. Therefore, according to the wet heat discoloration indicator of the present invention, when performing high-pressure steam sterilization, it is accurately determined whether the wet heat conditions suitable for the sterilization process are obtained, or whether the sterilization process is reliably completed under the wet heat conditions. Judgment can be made. In general, the temperature for autoclaving is 121 ° C. or 134 ° C.
  • the wet heat discoloration indicator of the present invention can be used as an indicator card as it is (Usage form 1).
  • a wet heat discoloration indicator is housed in a water vapor permeable holder and can be used as a process test tool for a high-pressure steam sterilizer (hereinafter referred to as “test tool”) (Usage form 2).
  • test tool a high-pressure steam sterilizer
  • a laminated body in which a wet heat discoloration indicator and at least one gas permeation regulator selected from a porous sheet, a foam sheet, and crepe paper are overlapped and sandwiched between both sides by a gas permeable body is provided with small holes.
  • indicator pack for pre-vacuum test of a high-pressure steam sterilizer (hereinafter referred to as “indicator pack”) (Usage form 3).
  • indicator pack for pre-vacuum test of a high-pressure steam sterilizer
  • these three types of usage patterns are examples, and other usage patterns can be adopted as necessary.
  • test tool of usage pattern 2 includes a case 2 (bundling means), a sheet member group 6, a biological or data logger indicator 10, and a wet heat discoloration indicator 11.
  • Case 2 is composed of a main body 2a and a lid 2b.
  • the main body 2a is provided with a clasp 3 so that the clasp 3 can be fixed to the main body 2a when the lid 2b is closed.
  • the lid 2b and the main body 2a are provided with a plurality of (16 in total) lid holes 5 and main body holes 4 through which steam passes.
  • These body 2a and lid 2b are made of, for example, stainless steel (SUS304, etc.), aluminum, copper, titanium, various alloys, polyester, nylon, Teflon (registered trademark), polycarbonate, polyethylene, polypropylene, glass, borosilicate glass, Pyrex (registered) (Trademark), alumina, zirconia, glass lining, enamel, and the like.
  • the sheet member group 6 includes an upper sheet 7, an intermediate sheet 8, and a lower sheet 9.
  • one upper sheet 7, six intermediate sheets 8, and one lower sheet 9 are provided.
  • the upper sheet 7 and the lower sheet 9 may be two or more.
  • the intermediate sheet 8 disposed in the intermediate portion has an accommodation hole 8a.
  • Each sheet is not necessarily a single material, but is a vapor-permeable material such as paper and pulp that can be obtained at low cost and can withstand multiple exposures to high-pressure steam.
  • a material is preferable. For example, if the material is composed of 100% pulp, it can withstand about 20 to 30 tests.
  • the depth of the accommodation hole 8a is increased as the number of intermediate sheets 8 is increased.
  • a biological or data logger indicator 10 is accommodated in the accommodation hole 8a. Therefore, the depth of the accommodation hole 8a is set to be a depth that can accommodate the biological type or data logger type indicator 10 and a dimension equal to or smaller than the depth (H) of the case 2.
  • the sheet member group 6 can be accurately stacked by aligning the positions of the notch portions 12 of each sheet.
  • a test tool is obtained by housing 6 in the case 2. Then, by placing the test device in the high-pressure steam sterilizer and confirming the discoloration of the wet heat discoloration indicator, whether or not the wet heat conditions suitable for the sterilization process are obtained, or the sterilization process has been completed reliably under the wet heat conditions. Whether it can be accurately determined.
  • FIG. 2 is a cross-sectional perspective view of the indicator pack.
  • the indicator pack shown in FIG. 2 includes a wet heat discoloration indicator 13 and at least one gas permeation regulator 14 selected from a porous sheet, a foam sheet and crepe paper, and gas permeable bodies 15a ( 151, 152, and 153) and 15b (154, 155, and 156) are laminated by an outer skin 17 provided with small holes 16.
  • the gas permeation adjuster 14 is a porous sheet for facilitating the inflow and outflow of air and steam to the center of the indicator pack, and is disposed between the wet heat discoloration indicator 13 and the gas permeable body 15b. .
  • the size is preferably about the same as the wet heat discoloration indicator 13.
  • the gas permeation adjuster 14 is a material that has a property of ensuring a vapor flow path without being clogged and clogged even when the wet heat discoloration indicator 13 or the gas permeable body 15b is pressed by depressurization or pressurization. Is used.
  • a porous sheet such as a fluororesin porous sheet and a silicone resin porous sheet
  • a foam sheet such as a urethane resin foam sheet and a vinyl chloride resin foam sheet
  • crepe paper can be used.
  • a thickness of about 5 mm is sufficient in order to suitably adjust the inflow amount of steam.
  • the gas permeable bodies 15a and 15b may be any material that contains air and can transmit heated steam.
  • integrally compressed cotton or glass fiber, heat resistant nonwoven fabric, paper, cork, pulp can be used.
  • a vapor impermeable film is used for the outer skin 17.
  • vapor impermeable films include metal foils such as aluminum, copper, stainless steel, and tin; polyester, nylon, Teflon (registered trademark), polycarbonate, polyacetal, polyimide, polyvinylidene chloride, ethylene-vinyl acetate copolymer, Synthetic resin films such as polypropylene; laminated films of these films can be used.
  • a heat-fusible resin layer or an adhesive layer may be provided on the surface of the outer skin 17 in order to facilitate sealing of the package.
  • the heat-fusible resin layer for example, biaxially stretched polypropylene, unstretched polypropylene, ethylene-vinyl alcohol copolymer, or ionomer resin can be used.
  • the adhesive layer include ethylene-vinyl acetate copolymer, polyurethane rubber, copolymer polyamide, vinyl chloride-vinyl acetate-maleic acid copolymer, ethylene-acrylic copolymer, styrene-butadiene rubber (SBR), An ionomer resin or the like can be used.
  • the usage method of the indicator pack is as follows. First, the indicator pack is placed in a high-pressure steam sterilizer and sterilization is started in a normal sterilization cycle. When the inside of the high-pressure steam sterilizer is exhausted with a vacuum pump, the air in the indicator pack is exhausted through the small holes 16 on the upper surface and the lower surface of the outer skin 17. Next, pressurized steam is introduced into the autoclave. The pressurized steam penetrates into the gas permeable bodies 15a and 15b from the small holes 16 of the outer skin 17, and penetrates and is guided toward the center of the indicator pack.
  • the vacuum pump When the vacuum pump operates normally and the air in the high-pressure steam sterilizer is suitably discharged, the steam is subjected to wet heat discoloration directly from the gas permeable body 15a or from the gas permeable body 15b through the gas permeation control body 14. It reaches the indicator 13 and the wet heat discoloration indicator 13 is colored. After completion of the sterilization cycle, the indicator pack is taken out from the high-pressure steam sterilizer, the outer skin 17 is broken, and the color development state of the wet heat discoloration indicator 13 is confirmed.
  • the wet heat discolorable composition of the present invention can be discolored by reacting a bismuth compound and a sulfur compound by heating to produce dark bismuth sulfide.
  • a step of pulverizing the bismuth compound is not necessary when preparing the wet heat discoloration composition, and the bismuth compound is precipitated over time.
  • Wet heat discoloration compositions with improved problems can be provided.
  • Examples 1-8 and Comparative Examples 1-2 (Production of wet heat discoloration composition and wet heat discoloration indicator) Of the components shown in Table 1, the organic solvent and the binder were first stirred with a dissolver. When the binder was difficult to dissolve, it was dissolved by heating. Next, the bismuth compound was added and stirred thoroughly. Thus, ten kinds of wet heat color-changing compositions (inks) of Examples 1 to 8 and Comparative Examples 1 to 2 were prepared.
  • the above inks were printed on high-quality paper using a bar coater to form a discoloration layer.
  • Test example 1 (discoloration test) Each wet heat discoloration indicator was subjected to wet heat treatment at 134 ° C. for 8 minutes using an autoclave (high pressure steam sterilizer: “FLC-H06SEZ” manufactured by Sakura Seiki Co., Ltd.).
  • Test example 2 (sedimentation test) About the wet heat color-change composition immediately after preparation, the presence or absence of the sediment component was confirmed visually. The results are shown in Table 1. ⁇ Discussion ⁇ In Examples 1 to 8 using an organic solvent-soluble bismuth compound, discoloration in a wet heat state was confirmed by a discoloration test, and the presence of precipitated components was not recognized. On the other hand, in Comparative Examples 1 and 2 using a bismuth compound insoluble in an organic solvent (bismuth oxide FP), discoloration in a wet heat state was confirmed by a discoloration test, but the presence of a sedimentary component was confirmed, and It can be seen that the discoloration composition is inferior to Examples 1 to 8 in terms of preparation and storage.
  • bismuth oxide FP bismuth oxide FP

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Abstract

La présente invention vise à procurer une composition qui change de couleur en présence de chaleur humide et sur un indicateur qui change de couleur en présence de chaleur humide, à l'aide desquels une pulvérisation d'un composé de bismuth lors de la préparation d'une composition changeant de couleur n'est pas nécessaire, et le problème de précipitation du composé de bismuth au cours du temps est résolu. A cet effet, la présente invention porte sur une composition qui change de couleur en présence de chaleur humide et qui comprend un composé de bismuth, un composé de soufre, un liant et un solvant organique, dans laquelle composition le composé de bismuth est un composé de bismuth organique soluble dans un solvant organique. La composition qui change de couleur en présence de chaleur humide selon la présente invention change de couleur quand, lorsqu'elle est chauffée, le composé de bismuth et le composé de soufre réagissent de façon à générer un sulfure de bismuth profondément coloré.
PCT/JP2012/050688 2011-01-20 2012-01-16 Composition qui change de couleur en présence de chaleur humide et indicateur qui change de couleur en présence de chaleur humide WO2012099043A1 (fr)

Applications Claiming Priority (2)

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JP2011-009979 2011-01-20
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WO2014007194A1 (fr) * 2012-07-02 2014-01-09 株式会社サクラクレパス Composition et indicateur qui changent de couleur par sensibilité à l'humidité/température
JP2014051596A (ja) * 2012-09-07 2014-03-20 Sakura Color Products Corp 湿熱変色性組成物及び湿熱変色インジケータ
CN116004057A (zh) * 2022-12-12 2023-04-25 山东高创医疗器械国家研究院有限公司 一种防水型压力蒸汽灭菌指示物及其制备方法

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JP2004168387A (ja) * 2002-11-21 2004-06-17 Toppan Printing Co Ltd インジケータ付き蓋材及び蓋材仮止めシール
WO2010078422A2 (fr) * 2008-12-31 2010-07-08 3M Innovative Properties Company Composition d'indicateur chimique, indicateurs et procédés

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JPH0462746B2 (fr) * 1989-02-10 1992-10-07 Nippon Yushi Kk
US5916816A (en) * 1996-09-27 1999-06-29 Minnesota Mining And Manufacturing Company Steam sterilization indicator compositions
JPH1180703A (ja) * 1997-09-04 1999-03-26 Nichiyu Giken Kogyo Kk 加熱変色性組成物と熱履歴検知用インジケータ
JP2004168387A (ja) * 2002-11-21 2004-06-17 Toppan Printing Co Ltd インジケータ付き蓋材及び蓋材仮止めシール
WO2010078422A2 (fr) * 2008-12-31 2010-07-08 3M Innovative Properties Company Composition d'indicateur chimique, indicateurs et procédés

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Publication number Priority date Publication date Assignee Title
WO2014007194A1 (fr) * 2012-07-02 2014-01-09 株式会社サクラクレパス Composition et indicateur qui changent de couleur par sensibilité à l'humidité/température
JP2014051596A (ja) * 2012-09-07 2014-03-20 Sakura Color Products Corp 湿熱変色性組成物及び湿熱変色インジケータ
CN116004057A (zh) * 2022-12-12 2023-04-25 山东高创医疗器械国家研究院有限公司 一种防水型压力蒸汽灭菌指示物及其制备方法
CN116004057B (zh) * 2022-12-12 2024-08-23 山东威高集团医用高分子制品股份有限公司 一种防水型压力蒸汽灭菌指示物及其制备方法

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