CN114902026B - Sheet set for pressure measurement and method for producing same, sheet for pressure measurement and method for producing same, dispersion liquid, and microcapsule - Google Patents
Sheet set for pressure measurement and method for producing same, sheet for pressure measurement and method for producing same, dispersion liquid, and microcapsule Download PDFInfo
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- CN114902026B CN114902026B CN202080085210.9A CN202080085210A CN114902026B CN 114902026 B CN114902026 B CN 114902026B CN 202080085210 A CN202080085210 A CN 202080085210A CN 114902026 B CN114902026 B CN 114902026B
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- 125000004450 alkenylene group Chemical group 0.000 description 1
- 125000000304 alkynyl group Chemical group 0.000 description 1
- 125000004419 alkynylene group Chemical group 0.000 description 1
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 1
- 150000001414 amino alcohols Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000010775 animal oil Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- VHNFAQLOVBWGGB-UHFFFAOYSA-N benzhydrylbenzene;3h-2-benzofuran-1-one Chemical class C1=CC=C2C(=O)OCC2=C1.C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 VHNFAQLOVBWGGB-UHFFFAOYSA-N 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000005018 casein Substances 0.000 description 1
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 description 1
- 235000021240 caseins Nutrition 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 238000005354 coacervation Methods 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 235000005687 corn oil Nutrition 0.000 description 1
- 239000002285 corn oil Substances 0.000 description 1
- 235000012343 cottonseed oil Nutrition 0.000 description 1
- 239000002385 cottonseed oil Substances 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 239000002781 deodorant agent Substances 0.000 description 1
- VILAVOFMIJHSJA-UHFFFAOYSA-N dicarbon monoxide Chemical compound [C]=C=O VILAVOFMIJHSJA-UHFFFAOYSA-N 0.000 description 1
- 125000001664 diethylamino group Chemical group [H]C([H])([H])C([H])([H])N(*)C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- CZZYITDELCSZES-UHFFFAOYSA-N diphenylmethane Chemical class C=1C=CC=CC=1CC1=CC=CC=C1 CZZYITDELCSZES-UHFFFAOYSA-N 0.000 description 1
- 239000013013 elastic material Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000000031 ethylamino group Chemical group [H]C([H])([H])C([H])([H])N([H])[*] 0.000 description 1
- 235000021323 fish oil Nutrition 0.000 description 1
- FWQHNLCNFPYBCA-UHFFFAOYSA-N fluoran Chemical compound C12=CC=CC=C2OC2=CC=CC=C2C11OC(=O)C2=CC=CC=C21 FWQHNLCNFPYBCA-UHFFFAOYSA-N 0.000 description 1
- 125000003983 fluorenyl group Chemical class C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 1
- 239000006081 fluorescent whitening agent Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 229940005740 hexametaphosphate Drugs 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- QDLAGTHXVHQKRE-UHFFFAOYSA-N lichenxanthone Natural products COC1=CC(O)=C2C(=O)C3=C(C)C=C(OC)C=C3OC2=C1 QDLAGTHXVHQKRE-UHFFFAOYSA-N 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 125000005647 linker group Chemical group 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- VUQUOGPMUUJORT-UHFFFAOYSA-N methyl 4-methylbenzenesulfonate Chemical group COS(=O)(=O)C1=CC=C(C)C=C1 VUQUOGPMUUJORT-UHFFFAOYSA-N 0.000 description 1
- CZXGXYBOQYQXQD-UHFFFAOYSA-N methyl benzenesulfonate Chemical group COS(=O)(=O)C1=CC=CC=C1 CZXGXYBOQYQXQD-UHFFFAOYSA-N 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 239000004006 olive oil Substances 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 125000001484 phenothiazinyl group Chemical class C1(=CC=CC=2SC3=CC=CC=C3NC12)* 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 229920005906 polyester polyol Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- FZYCEURIEDTWNS-UHFFFAOYSA-N prop-1-en-2-ylbenzene Chemical compound CC(=C)C1=CC=CC=C1.CC(=C)C1=CC=CC=C1 FZYCEURIEDTWNS-UHFFFAOYSA-N 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 230000004043 responsiveness Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 125000003003 spiro group Chemical group 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- 150000004654 triazenes Chemical class 0.000 description 1
- 150000004961 triphenylmethanes Chemical class 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 239000010938 white gold Substances 0.000 description 1
- 229910000832 white gold Inorganic materials 0.000 description 1
- XTUPUYCJWKHGSW-UHFFFAOYSA-L zinc;2-carboxy-4,6-bis(1-phenylethyl)phenolate Chemical compound [Zn+2].C=1C(C(C)C=2C=CC=CC=2)=C(O)C(C([O-])=O)=CC=1C(C)C1=CC=CC=C1.C=1C(C(C)C=2C=CC=CC=2)=C(O)C(C([O-])=O)=CC=1C(C)C1=CC=CC=C1 XTUPUYCJWKHGSW-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- 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
- B41M5/124—Duplicating or marking methods; Sheet materials for use therein using pressure to make a masked colour visible, e.g. to make a coloured support visible, to create an opaque or transparent pattern, or to form colour by uniting colour-forming components
- B41M5/165—Duplicating or marking methods; Sheet materials for use therein using pressure to make a masked colour visible, e.g. to make a coloured support visible, to create an opaque or transparent pattern, or to form colour by uniting colour-forming components characterised by the use of microcapsules; Special solvents for incorporating the ingredients
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L5/00—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Color Printing (AREA)
Abstract
The present invention provides a sheet set for pressure measurement and a method for producing the same, which are excellent in storage stability at low temperatures, and a sheet for pressure measurement and a method for producing the same. Another object of the present invention is to provide a dispersion and a microcapsule. The sheet set for pressure measurement of the present invention comprises: a1 st sheet having a1 st layer comprising microcapsules containing a solvent having a boiling point of 100 ℃ or higher and a color former; and a2 nd sheet having a2 nd layer containing a color developer, wherein the solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups, and the color developer contains 2 or more color developers containing aromatic groups.
Description
Technical Field
The present invention relates to a sheet set for pressure measurement and a method for producing the same, a sheet for pressure measurement and a method for producing the same, a dispersion liquid, and a microcapsule.
Background
In recent years, the necessity of measuring the distribution of pressure tends to increase due to the higher functionality and higher definition of products.
For example, patent document 1 proposes a sheet for pressure measurement using microcapsules in which a color former and a solvent for dissolving the color former are encapsulated.
Technical literature of the prior art
Patent literature
Patent document 1: japanese patent laid-open No. 55-137992
Disclosure of Invention
Technical problem to be solved by the invention
The present inventors have found that there is room for improvement in storage stability at low temperatures as a result of studies on the production of a sheet for pressure measurement described in patent document 1. Specifically, it is known that when the pressure measurement sheet is stored at a low temperature for a long period of time and then used, the color development concentration of the color development portion generated by the reaction of the color development agent and the color development agent in the pressure region may be significantly deteriorated with respect to the initial concentration (in other words, when the pressure measurement sheet immediately after production is used, the color development concentration of the color development portion generated by the reaction of the color development agent and the color development agent in the pressure region).
The present invention provides a sheet set for pressure measurement and a method for producing the same, which are excellent in storage stability at low temperatures, and a sheet for pressure measurement and a method for producing the same.
The present invention also provides a dispersion and a microcapsule.
Means for solving the technical problems
As a result of intensive studies to solve the above problems, the present inventors have found that the above problems can be solved by setting a specific composition of a color former encapsulated in a microcapsule and a solvent for dissolving the color former.
That is, it has been found that the above problems can be solved by the following configuration.
[ 1 ] A sheet set for pressure measurement, comprising:
A1 st sheet having a1 st layer comprising microcapsules containing a solvent having a boiling point of 100 ℃ or higher and a color former; and
A2 nd sheet having a2 nd layer containing a color developer,
The above solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups, and
The above-mentioned color former contains more than 2 kinds of color formers containing aromatic groups.
The sheet set for pressure measurement according to [2 ], wherein the aromatic group-containing solvent contains a solvent having 2 aromatic groups in the molecule.
The sheet set for pressure measurement according to [ 2], wherein the content of the solvent having 2 aromatic groups in the molecule is 50 mass% or more with respect to the total mass of the solvent having aromatic groups.
The sheet set for pressure measurement according to any one of [ 1] to [3 ], wherein the solvent having a boiling point of 100℃or higher contains 4 or more solvents containing an aromatic group.
The sheet set for pressure measurement according to any one of [1] to [ 4 ], wherein,
The solvent having a boiling point of 100 ℃ or higher further includes a solvent having an aliphatic structure,
The content of the aromatic group-containing solvent is 50 to 90 mass% relative to the total mass of the aromatic group-containing solvent and the aliphatic structure-containing solvent.
The pressure-measuring sheet set according to any one of [ 1 ] to [5 ], wherein an oil absorption amount of the aromatic group-containing solvent with respect to the 2 nd sheet is 2.0 to 20.0g/m 2.
The sheet set for pressure measurement according to any one of [ 1] to [ 6 ], wherein the arithmetic average roughness Ra of the 1 st sheet is 3.0 to 7.0. Mu.m.
The sheet set for pressure measurement according to any one of [ 1] to [7], wherein the arithmetic average roughness Ra of the 2 nd sheet is 1.2 μm or less.
The sheet set for pressure measurement according to any one of [1] to [ 8 ], wherein,
The 1 st sheet and the 2 nd sheet further have a support,
The support is a resin film.
[ 10 ] A sheet for pressure measurement, comprising:
layer 1 comprising microcapsules encapsulating a solvent having a boiling point of 100 ℃ or higher and a color former; and
A layer 2 which is disposed on the layer 1 and contains a color-developer,
The above solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups, and
The above-mentioned color former contains more than 2 kinds of color formers containing aromatic groups.
The sheet for pressure measurement according to [ 10 ], wherein the aromatic group-containing solvent contains a solvent having 2 aromatic groups in the molecule.
The sheet for pressure measurement according to [ 11 ], wherein the content of the solvent having 2 aromatic groups in the molecule is 50 mass% or more relative to the total mass of the solvent having aromatic groups.
The sheet for pressure measurement according to any one of [ 10 ] to [ 12 ], wherein the solvent having a boiling point of 100 ℃ or higher contains 4 or more solvents containing an aromatic group.
The sheet for pressure measurement according to any one of [ 10 ] to [ 13 ], wherein,
The solvent having a boiling point of 100 ℃ or higher further includes a solvent having an aliphatic structure,
The content of the aromatic group-containing solvent is 50 to 90 mass% relative to the total mass of the aromatic group-containing solvent and the aliphatic structure-containing solvent.
The sheet for pressure measurement according to any one of [ 10 ] to [ 14 ], wherein an oil absorption of the aromatic group-containing solvent of the layer 2 is 2.0 to 20.0g/m 2.
The sheet for pressure measurement according to any one of [ 10 ] to [ 15 ], further comprising a support,
The support is a resin film.
The method for producing a sheet set for pressure measurement according to any one of [1 ] to [ 9 ], comprising the steps of:
A layer 1 is formed by applying a layer 1-forming composition containing microcapsules containing a solvent having a boiling point of 100 ℃ or higher and a color former, and drying the obtained coating film.
[ 18 ] A method for producing the sheet for pressure measurement according to any one of [10 ] to [ 16 ], comprising the steps of:
A layer 1 is formed by applying a layer 1-forming composition containing microcapsules containing a solvent having a boiling point of 100 ℃ or higher and a color former, and drying the obtained coating film.
A dispersion for measuring pressure and forming a layer to be used in combination with a layer containing a color former, comprising microcapsules containing a solvent having a boiling point of 100 ℃ or higher and a color former,
The above solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups, and
The above-mentioned color former contains more than 2 kinds of color formers containing aromatic groups.
The dispersion of [ 20 ] the above-mentioned [ 19 ], wherein the solvent having a boiling point of 100℃or higher contains 4 or more solvents having an aromatic group.
A microcapsule comprising a solvent having a boiling point of 100 ℃ or higher and a color former,
The above solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups, and
The above-mentioned color former contains more than 2 kinds of color formers containing aromatic groups.
Effects of the invention
According to the present invention, a sheet set for pressure measurement having excellent storage stability at low temperature, a method for producing the same, and a sheet for pressure measurement having excellent storage stability at low temperature, and a method for producing the same can be provided. Further, according to the present invention, a dispersion liquid and a microcapsule can be provided.
Drawings
Fig. 1 is a cross-sectional view of an embodiment of a sheet set for pressure measurement.
Fig. 2 is a view for explaining a use mode of the sheet set for pressure measurement.
Fig. 3 is a cross-sectional view of an embodiment of a sheet for pressure measurement.
Detailed Description
[ Sheet set for pressure measurement and method for producing same, sheet for pressure measurement and method for producing same, dispersion liquid, and microcapsule ]
The present invention will be described in detail below.
In the present specification, the numerical range indicated by the term "to" refers to a range including numerical values described before and after the term "to" as a lower limit value and an upper limit value.
In the numerical ranges described in stages in the present invention, the upper limit or the lower limit described in a certain numerical range may be replaced with the upper limit or the lower limit of the numerical range described in other stages. In the numerical ranges described in the present specification, the upper limit value or the lower limit value described in a certain numerical range may be replaced with the value shown in the examples.
As a feature of the sheet set for pressure measurement and the sheet for pressure measurement of the present invention, microcapsules (hereinafter also referred to as "specific microcapsules") which encapsulate a solvent and a color former having a boiling point of 100 ℃ or higher and satisfy the following conditions X and Y are used.
Condition X: the solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups.
Condition Y: the above-mentioned color former contains more than 2 kinds of color formers containing aromatic groups.
The sheet set for pressure measurement of the present invention having the above-described structure is excellent in storage stability at low temperatures. That is, the sheet set for pressure measurement and the sheet for pressure measurement of the present invention show a color development concentration that is not inferior to an initial concentration (color development concentration of a color development portion generated by a reaction between a color former and a color former in the case of using the sheet for pressure measurement immediately after production) in a color development portion generated by a reaction between a color former and a color former in a pressure-applied region even when the sheet set for pressure measurement and the sheet for pressure measurement are used after being stored for a long period of time at a low temperature.
The mechanism of action of the above structure and effect is not clear, but the present inventors speculate as follows. The present inventors have found that the color former encapsulated in the microcapsule is precipitated during long-term storage at low temperature, and this is one of the causes of deterioration in the color development concentration of the color former during use after long-term storage at low temperature.
In contrast, in the specific microcapsules, the composition of the color former and the solvent for dissolving the color former contained in the microcapsules is such that the above conditions X and Y are satisfied, thereby improving the solubility of the color former in the solvent at low temperatures. As a result, even when the pressure measurement sheet set and the pressure measurement sheet are stored at low temperatures for a long period of time and then used, the color former moves to the 2 nd layer containing the color former in a state of being dissolved in the solvent (in a state where precipitation can be suppressed) in the pressurized region, and easily penetrates into the inside of the 2 nd layer, and the color reaction between the color former and the color former is easily performed. That is, by the above mechanism, it can be presumed that deterioration of the color development concentration in the color development portion is suppressed.
When the boiling point of the solvent contained in the specific microcapsule is 100 ℃ or higher, the volatilization of the solvent is suppressed at the time of production and/or storage of the specific microcapsule and/or at the time of production and/or storage of the sheet set for pressure measurement and the sheet for pressure measurement, and is easily maintained in the specific microcapsule. This point is also presumed to be one of reasons why the color reaction between the color former and the color former in the pressurized region is more likely to occur when the pressure measurement sheet set and the pressure measurement sheet are used.
The structure of the sheet set for pressure measurement and the sheet for pressure measurement according to the present invention will be described in detail below. The production methods will be described in detail.
[ Embodiment 1]
Fig. 1 is a cross-sectional view of an embodiment of a sheet set for pressure measurement.
The sheet set 10 for pressure measurement includes a1 st sheet 16 and a2 nd sheet 22, the 1 st sheet 16 including a1 st support 12 and a1 st layer 14 including specific microcapsules 13 disposed on the 1 st support 12, and the 2 nd sheet 22 including a2 nd support 18 and a2 nd layer 20 including a developer disposed on the 2 nd support 18.
As shown in fig. 2, when the pressure measurement sheet set 10 is used, the 1 st sheet 16 and the 2 nd sheet 22 are stacked and used so that the 1 st layer 14 of the 1 st sheet 16 faces the 2 nd layer 20 of the 2 nd sheet 22. By pressurizing from at least one of the 1 st support 12 side of the 1 st sheet 16 and the 2 nd support 18 side of the 2 nd sheet 22 in the obtained laminate, the specific microcapsules 13 are ruptured in the pressurized region and the color former contained in the specific microcapsules 13 comes out of the specific microcapsules 13, thereby performing a color reaction with the color former in the 2 nd layer 20. As a result, color development proceeds in the pressurized region.
As will be described later, the 1 st sheet 16 may be provided with the 1 st layer 14, or may not be provided with the 1 st support 12. The 2 nd sheet 22 may have the 2 nd layer 20, or may not have the 2 nd support 18.
In fig. 1, the 1 st support 12 and the 1 st layer 14 are directly laminated, but the method is not limited thereto, and other layers (for example, an easy-to-adhere layer) may be disposed between the 1 st support 12 and the 1 st layer 14 as will be described later. In fig. 1, the 2 nd support 18 and the 2 nd layer 20 are directly laminated, but the method is not limited thereto, and other layers (for example, an easy-to-adhere layer) may be disposed between the 2 nd support 18 and the 2 nd layer 20 as will be described later.
The following describes the structure of the 1 st sheet 16 and the 2 nd sheet 22 constituting the sheet set 10 for pressure measurement in detail.
Sheet 1
The 1 st sheet 16 shown in fig. 1 has a1 st support 12 and a1 st layer 14 containing specific microcapsules 13.
The components are described in detail below.
< 1 St support >)
The 1 st support is a member for supporting the 1 st layer. In addition, in the case where the treatment can be performed by the 1 st layer itself, the 1 st sheet may not have the 1 st support.
The 1 st support may have any of a sheet shape, a film shape, and a plate shape.
The 1 st support may be a resin film or a synthetic paper.
Examples of the resin film include polyester films such as polyethylene terephthalate films, cellulose derivative films such as cellulose triacetate films, polyolefin films such as polypropylene and polyethylene, and polystyrene films.
Examples of the synthetic paper include synthetic paper (Yupo etc.) in which polypropylene, polyethylene terephthalate, etc. are biaxially stretched to form a plurality of micropores, synthetic paper made of synthetic fibers of polyethylene, polypropylene, polyethylene terephthalate, polyamide, etc., and synthetic paper in which these are laminated on one or both surfaces of a part of the paper.
Among them, from the viewpoint of further improving the color development density by pressurization and the viewpoint of excellent image quality after color development, a resin film or a synthetic paper is preferable, and a resin film is more preferable.
The thickness of the 1 st support is not particularly limited, and is preferably 10 to 200. Mu.m.
Layer 1
(Specific microcapsules)
Layer 1 contains specific microcapsules.
Hereinafter, first, the materials constituting the specific microcapsules will be described in detail.
Certain microcapsules typically have a core and a capsule wall for encasing a core material constituting the core (an encased component (also referred to as an encased component)).
The specific microcapsule is used as a core material (inner package component) and is internally packaged with a solvent with boiling point of more than 100 ℃ and a color former. The microcapsules contain the color former, so that the color former can be stably present until the microcapsules are broken by pressurization.
A particular microcapsule has a capsule wall with a core material enclosed therein.
As a material (wall material) of the capsule wall of the specific microcapsule, a known resin used as a wall material of a microcapsule in which a color former is encapsulated in the use of a pressure-sensitive copying paper or a thermal recording paper has been mentioned. Specific examples of the resin include polyurethane, polyurea, polyurethaneurea, melamine-formaldehyde resin and gelatin.
The capsule wall of a particular microcapsule is preferably substantially composed of a resin. The substantial resin composition means that the content of the resin is 90 mass% or more, preferably 100 mass% relative to the total mass of the capsule wall. That is, the capsule wall of a specific microcapsule is preferably composed of a resin.
The polyurethane is a polymer having a plurality of urethane bonds, and is preferably a reaction product formed from a raw material containing a polyol and a polyisocyanate.
The polyurea is a polymer having a plurality of urea bonds, and is preferably a reaction product formed from a raw material containing a polyamine and a polyisocyanate. In addition, the polyurea can be synthesized by reacting a part of the polyisocyanate with water to form a polyamine, and the polyisocyanate can be used instead of the polyamine.
The polyurethaneurea is a polymer having urethane bonds and urea bonds, and is preferably a reaction product formed from a raw material containing a polyol, a polyamine, and a polyisocyanate. In addition, when a polyol is reacted with a polyisocyanate, a part of the polyisocyanate reacts with water to form a polyamine, and as a result, polyurethaneurea can be obtained.
The melamine-formaldehyde resin is preferably a reaction product formed by polycondensation of melamine and formaldehyde.
The polyisocyanate is a compound having 2 or more isocyanate groups, and examples thereof include aromatic polyisocyanates and aliphatic polyisocyanates. The polyisocyanate may be, for example, an adduct (adduct) of a polyol such as trimethylolpropane and a 2-functional polyisocyanate.
The polyol is a compound having 2 or more hydroxyl groups, and examples thereof include low-molecular-weight polyols (for example, aliphatic polyols and aromatic polyols), "low-molecular-weight polyols" means polyols having a molecular weight of 400 or less, polyvinyl alcohols, polyether polyols, polyester polyols, polylactone polyols, castor oil polyols, polyolefin polyols, and hydroxyl group-containing amine compounds (for example, amino alcohols, for example, propylene oxide or ethylene oxide adducts of amino compounds such as ethylenediamine, that is, N, N, N ', N' -tetrakis [ 2-hydroxypropyl ] ethylenediamine, and the like).
The polyamine is a compound having 2 or more amino groups (primary amino groups or secondary amino groups), and examples thereof include aliphatic polyamines such as diethylenetriamine, triethylenetetramine, 1, 3-propanediamine and hexamethylenediamine; epoxy compound adducts of aliphatic polyamines; alicyclic polyamines such as piperazine; heterocyclic diamines such as 3, 9-bis-aminopropyl-2, 4,8, 10-tetraoxaspiro- (5, 5) undecane.
The average particle diameter of the specific microcapsules is not particularly limited, but is preferably 1 to 100. Mu.m, more preferably 3 to 50. Mu.m, and still more preferably 5 to 30. Mu.m.
The average particle diameter of the specific microcapsules can be controlled by adjusting the production conditions of the specific microcapsules, and the like.
The average particle diameter of the specific microcapsules is determined by the following method.
The image taken from the surface of layer 1 was analyzed by an optical microscope (OLYMPUS BX60, size of field of view: 320 μm×450 μm), the long diameters (particle diameters) of 30 microcapsules were measured from the largest microcapsules in order, and these were arithmetically averaged to obtain an average value. This operation was performed at 5 arbitrary sites (5 fields of view) of layer 1, and the average value obtained at each site was determined, and the obtained value was set as the average particle diameter of the microcapsules. The long diameter is the longest diameter when the microcapsules are observed.
The average particle diameter of the microcapsules contained in the dispersion liquid can be measured by a laser diffraction/scattering particle diameter distribution measuring apparatus (manufactured by LA-960/HORIBA corporation).
The number average wall thickness of the capsule wall of the specific microcapsule is not particularly limited, but is preferably 0.01 to 2.0 μm, more preferably 0.02 to 1.0 μm, from the viewpoint of excellent pressure responsiveness.
The wall thickness of the specific microcapsules is the thickness (μm) of the capsule wall of the capsule particles forming the specific microcapsules, and the number average wall thickness is the average value obtained by measuring the thickness (μm) of each of the 20 specific microcapsules by a Scanning Electron Microscope (SEM). More specifically, a cross-sectional slice of the 1 st sheet having the 1 st layer containing the specific microcapsules was prepared, the cross-section was observed at 15000 times by SEM, and any 20 specific microcapsules having particle diameters ranging from (value of average particle diameter of specific microcapsules) ×0.9 to (value of average particle diameter of specific microcapsules) ×1.1 were selected, and then the cross-section of each selected specific microcapsule was observed to obtain the thickness of the capsule wall and calculate the average value.
The ratio (δ/Dm) of the number average wall thickness δ of the specific microcapsules to the average particle diameter of the specific microcapsules is not particularly limited, and is usually 0.001 or more. Among them, from the viewpoint of excellent color development density according to pressure, it is preferable that the relationship of formula (1) is satisfied.
Formula (1) delta/Dm > 0.001
That is, the above ratio (δ/Dm) is preferably more than 0.001. The ratio (δ/Dm) is preferably 0.002 or more. The upper limit is not particularly limited, but is preferably 0.2 or less.
Color former
The specific microcapsules encapsulate the chromonic agent.
The term "color former" refers to a compound that develops color from a colorless state by contact with a color former described later. The color former is preferably an electron donating pigment precursor (a precursor of a color developing pigment). That is, as the color former, an electron donating leuco dye is preferable.
More than 2 of the color-forming agents encapsulated in the specific microcapsules are color-forming agents containing an aromatic group (hereinafter also referred to as "specific color-forming agents"). In other words, the specific microcapsule contains, as the color former, 2 or more kinds of color formers containing aromatic groups.
Wherein "comprising an aromatic group" means an aromatic ring group comprising a single ring and/or a condensed polycyclic aromatic ring group within a molecule.
Examples of the aromatic ring include an aromatic hydrocarbon ring and an aromatic heterocyclic ring.
The aromatic hydrocarbon ring may be any of a monocyclic ring and a condensed polycyclic ring as described above. The aromatic hydrocarbon ring may have a substituent. In the case where the aromatic hydrocarbon ring has a plurality of substituents, the substituents may be bonded to each other to form an alicyclic ring. In other words, the aromatic hydrocarbon ring may be an aromatic hydrocarbon ring having an alicyclic structure (e.g., a benzolactone ring).
The number of carbon atoms of the aromatic hydrocarbon ring is not particularly limited, but is preferably 6 to 30, more preferably 6 to 18, and still more preferably 6 to 10.
Examples of the monocyclic aromatic hydrocarbon ring include benzene rings.
Examples of the aromatic hydrocarbon ring having a condensed polycyclic ring include naphthalene rings.
The upper aromatic heterocycle may be any of monocyclic and condensed polycyclic as described above. The aromatic heterocycle may have a substituent. In the case where the aromatic heterocyclic ring has a plurality of substituents, the substituents may be bonded to each other to form an alicyclic ring. In other words, the aromatic heterocycle may be an aromatic heterocycle having an alicyclic structure.
Examples of the hetero atom contained in the aromatic heterocyclic ring include a nitrogen atom, an oxygen atom and a sulfur atom. The number of ring members of the aromatic heterocycle is not particularly limited, and is preferably 5 to 18.
Examples of the aromatic heterocyclic ring include a pyridine ring, a pyridazine ring, a pyrimidine ring, a pyrazine ring, a triazine ring, a thiophene ring, a thiazole ring, an imidazole ring, a xanthene ring, and a benzoxanthene ring.
The number of aromatic groups in the specific color former is not particularly limited, and may be 1 or 2 or more. In the case where the specific color former contains 2 or more aromatic groups, the 2 aromatic groups may be bonded to each other via substituents that may be present on each aromatic group to form a polycyclic structure (excluding condensed polycyclic structures).
As the specific color former, a color former known in the use of pressure-sensitive copying paper or thermal recording paper can be used as long as it contains an aromatic group.
Specific examples of the color former include triphenylmethane phthalide compounds, fluoran parent compounds, phenothiazine compounds, indolyl phthalide compounds, azaindolyl phthalide compounds, white gold amine compounds, rhodamine lactams, triphenylmethane compounds, diphenylmethane compounds, triazene compounds, spiropyran compounds, and fluorene compounds.
For details of the above-mentioned compounds, refer to the descriptions of Japanese patent application laid-open No. 5-257272 and WO 2009/8238 [0029] to [0034 ].
The specific coloring agent is preferably a coloring agent containing a xanthene ring in a molecule from the viewpoint of more excellent storage stability at low temperature and more excellent color density.
The molecular weight of the specific color former is not particularly limited, but is preferably 300 or more. The upper limit is not particularly limited, but is preferably 1000 or less.
Specific examples of the color former include 3- (4-diethylamino-2-ethoxyphenyl) -3- (1-ethyl-2-methylindol-3-yl) -4-azaphthalide, 3- (4-diethylamino-2-ethoxyphenyl) -3- (1-n-octyl-2-methylindol-3-yl) phthalide, 3- [2, 2-bis (1-ethyl-2-methylindol-3-yl) vinyl ] -3- (4-diethylaminophenyl) -phthalide, 2-anilino-6-dibutylamino-3-methylfluoran precursor, 6-diethylamino-3-methyl-2- (2, 6-stubble amino) -fluoran precursor, 2- (2-chloroanilino) -6-dibutylamino fluoran precursor, 3-bis (4-dimethylaminophenyl) -6-dimethylaminophthalide, 2-anilino-6-diethylamino-3-methylfluoran precursor, and, 9- [ ethyl (3-methylbutyl) amino ] spiro [ 12H-benzo [ a ] xanthene-12, 1 '(3' H) isobenzofuran ] -3 '-one and 2' -methyl-6 '- (N-p-tolyl-N ethylamino) spiro [ isobenzofuran-1 (3H), 9' - [9H ] xanthene ] -3-one, 3',6' -bis (diethylamino) -2- (4-nitrophenyl) spiro [ isoindole-1, 9 '-xanthene ] -3-one, 6' - (diethylamino) -1',3' -dimethylfluoran parent, and the like. Further, as specific color-forming agents, pink-DCF and Orange-DCF (both Hodogaya Chemical Co., ltd.) can also be used.
The content of the specific color former is preferably 50 to 100% by mass, more preferably 80 to 100% by mass, and even more preferably 90 to 100% by mass, based on the total amount of the color former.
Solvent with boiling point above 100deg.C
The specific microcapsule is internally coated with a solvent with boiling point of above 100deg.C. The term "boiling point" refers to a boiling point at atmospheric pressure.
The boiling point of the solvent contained in the specific microcapsule is preferably 120℃or higher, more preferably 150℃or higher, and further preferably 200℃or higher. The upper limit of the boiling point is not particularly limited, and is, for example, 400℃or lower.
The solvent having a boiling point of 100 ℃ or higher, which is encapsulated in the specific microcapsule, contains 2 or more solvents containing aromatic groups. In other words, the specific microcapsules have a boiling point of 100 ℃ or higher and contain 2 or more solvents containing aromatic groups (hereinafter also referred to as "specific solvents").
Wherein "comprising an aromatic group" means an aromatic ring group comprising a single ring and/or a condensed polycyclic aromatic ring group within a molecule.
Examples of the aromatic ring contained in the aromatic ring group include an aromatic hydrocarbon ring and an aromatic heterocyclic ring.
The aromatic hydrocarbon ring may be any of a monocyclic ring and a condensed polycyclic ring as described above. The aromatic hydrocarbon ring may have a substituent. In the case where the aromatic hydrocarbon ring has a plurality of substituents, the substituents may be bonded to each other to form an alicyclic ring. In other words, the aromatic hydrocarbon ring may be an aromatic hydrocarbon ring having an alicyclic structure.
The number of carbon atoms of the aromatic hydrocarbon ring is not particularly limited, but is preferably 6 to 30, more preferably 6 to 18, and still more preferably 6 to 10.
Examples of the monocyclic aromatic hydrocarbon ring include benzene rings.
Examples of the aromatic hydrocarbon ring having a condensed polycyclic ring include naphthalene rings.
The upper aromatic heterocycle may be any of monocyclic and condensed polycyclic as described above. The aromatic heterocycle may have a substituent. In the case where the aromatic heterocyclic ring has a plurality of substituents, the substituents may be bonded to each other to form an alicyclic ring. In other words, the aromatic heterocycle may be an aromatic heterocycle having an alicyclic structure.
Examples of the hetero atom contained in the aromatic heterocyclic ring include a nitrogen atom, an oxygen atom and a sulfur atom. The number of ring members of the aromatic heterocycle is not particularly limited, and is preferably 5 to 18.
Examples of the aromatic heterocyclic ring include a pyridine ring, a pyridazine ring, a pyrimidine ring, a pyrazine ring, a triazine ring, a thiophene ring, a thiazole ring, an imidazole ring, and a xanthene ring.
The number of aromatic groups in the specific solvent is not particularly limited, and may be 1 or 2 or more. In the case where the specific solvent contains 2 or more aromatic groups, the 2 aromatic groups may be bonded to each other via substituents which may be present on each aromatic group to form a polycyclic structure (excluding condensed polycyclic structures).
Among the specific solvents, a solvent containing 2 aromatic groups is preferable from the viewpoint of more excellent storage stability at low temperature and more excellent color development concentration.
The lower limit of the content of the specific solvent having 2 aromatic groups in the molecule is, for example, 5 mass% or more, and is preferably 50 mass% or more, more preferably 70 mass% or more, from the viewpoint of further excellent storage stability at low temperatures and further excellent color development concentration, relative to the total mass of the specific solvent. The upper limit of the content of the specific solvent having 2 aromatic groups in the molecule is, for example, 100 mass% or less.
The molecular weight of the specific solvent is not particularly limited, and is usually 100 or more. Of these, 150 or more is preferable. The upper limit is not particularly limited, but is preferably 1000 or less, more preferably 500 or less, and further preferably 300 or less.
The specific solvent is, for example, a compound represented by the following general formula (1), preferably a compound represented by the following general formulae (1A) to (1C), and more preferably a compound represented by the following general formula (1A) from the viewpoint of more excellent storage stability at low temperatures and more excellent color development concentration.
[ Chemical formula 1]
In the general formula (1), m 1 represents 0 or 1. M 1 is preferably 1 from the viewpoint of further excellent storage stability at low temperature and further excellent color development concentration.
M 1 represents the case of 0:
In the case where m 1 represents 0, ar 1 represents an aromatic ring having a substituent represented by-L A-RA (hereinafter, also referred to as "substituent W").
Examples of the aromatic ring represented by Ar 1 include an aromatic hydrocarbon ring and an aromatic heterocyclic ring. As the aromatic hydrocarbon ring and the aromatic heterocyclic ring, there are mentioned.
In substituent W, L A represents a single bond, an oxysulfonyl group (× 1-SO2-O-*2) or a sulfonyloxy group (× 1-O-SO2-*2). In addition, × 1 denotes a bonding position to Ar 1, and× 2 denotes a bonding position to R A.
In the substituent W, R A represents a 1-valent aliphatic hydrocarbon group.
The aliphatic hydrocarbon group having a valence of 1 represented by R A may be any of a saturated aliphatic hydrocarbon group having a valence of 1 and an unsaturated aliphatic hydrocarbon group having a valence of 1. Further, the compound may be any of a linear, branched, and cyclic compound. The number of carbon atoms of the 1-valent aliphatic hydrocarbon group is not particularly limited, and is, for example, 1 to 15, preferably 1 to 10, more preferably 1 to 6, and still more preferably 1 to 4. Examples of the above-mentioned aliphatic hydrocarbon group having a valence of 1 include an alkyl group, an alkenyl group and an alkynyl group, and an alkyl group is preferable.
The aliphatic hydrocarbon group having a valence of 1 may have a substituent.
The aromatic ring represented by Ar 1 may have 1 substituent represented by-L A-RA or may have 2 or more substituents.
M 1 represents the case of 1:
In the case where m 1 represents 1, ar 1 and Ar 2 each independently represent a 1-valent aromatic group which may have a substituent.
Examples of the 1-valent aromatic group represented by Ar 1 and Ar 2 include a 1-valent aromatic hydrocarbon group and a 1-valent aromatic heterocyclic group. As the aromatic hydrocarbon ring contained in the 1-valent aromatic hydrocarbon group and the aromatic heterocycle contained in the 1-valent aromatic heterocycle group, it is described. The 1-valent aromatic hydrocarbon group and the 1-valent aromatic heterocyclic group can be formed by removing 1 hydrogen atom from the aromatic hydrocarbon ring and the aromatic heterocyclic ring.
Among them, a 1-valent aromatic hydrocarbon group is preferable, and a phenyl group is more preferable as a 1-valent aromatic group represented by Ar 1 and Ar 2.
The 1-valent aromatic groups represented by Ar 1 and Ar 2 may have a substituent. The substituent is not particularly limited, but a non-aromatic substituent is preferable, and examples thereof include the substituent W described above.
L 1 represents a single bond, a 2-valent aliphatic hydrocarbon group, or a 2-valent linking group represented by the following general formula (L A).
[ Chemical formula 2]
In the above general formula (L A), R 1 represents a 1-valent aromatic group which may have a substituent.
In the general formula (1), R 1 has the same meaning as Ar 1 and Ar 2 (i.e., an aromatic group of 1 valence which may have a substituent) when m 1 represents 1, and the preferable mode is the same.
The aliphatic hydrocarbon group having a valence of 2 represented by L 1 may be any of a saturated aliphatic hydrocarbon group having a valence of 2 and an unsaturated aliphatic hydrocarbon group having a valence of 2. Further, the compound may be any of a linear, branched, and cyclic compound. The number of carbon atoms of the 2-valent aliphatic hydrocarbon group is not particularly limited, and is, for example, 1 to 10, preferably 1 to 6, more preferably 1 to 4, and still more preferably 1 or 2. Examples of the aliphatic hydrocarbon group having a valence of 2 include an alkylene group, an alkenylene group, and an alkynylene group, and alkylene groups are preferable. In the aliphatic hydrocarbon group having a valence of 2, the carbon atom may be substituted with a valence of 2 represented by > c=ch 2.
Among these, preferred is L 1, which is a single bond or a 2-valent aliphatic hydrocarbon group.
[ Chemical formula 3]
In the general formula (1A), L 11 represents a single bond or a 2-valent aliphatic hydrocarbon group.
The aliphatic hydrocarbon group having a valence of 2 represented by L 11 has the same meaning as the aliphatic hydrocarbon group having a valence of 2 represented by L 1 in the general formula (1), and the preferable mode is the same.
R 11 and R 12 each independently represent a non-aromatic substituent.
The non-aromatic substituent represented by R 11 and R 12 is not particularly limited, but is preferably an aliphatic hydrocarbon group having a valence of 1, and specifically, the same non-aromatic substituent as the aliphatic hydrocarbon group having a valence of 1 represented by R A in the above substituent W may be mentioned. Among them, an alkyl group having 1 to 4 carbon atoms is preferable, and an alkyl group having 1 to 3 carbon atoms is more preferable.
N 11 and n 12 each independently represent an integer of 0 to 5. n 11 and n 12 are preferably integers of 0 to 2. Of these, it is preferable that either one of n 11 and n 12 represents 1 or 2 and the other represents 0 or 1.
When n 11 and n 12 represent integers of 2 or more, a plurality of R 11 and a plurality of R 12 may be the same or different from each other.
Specific examples of the solvent represented by the general formula (1A) include 1, 2-dimethyl-4- (1-phenylethyl) benzene, 1, 3-dimethyl-4- (1-phenylethyl) benzene, 1, 4-dimethyl-2- (1-phenylethyl) benzene, 1- (ethylphenyl) -1-phenylethane, isopropylbiphenyl (e.g., 4-isopropylbiphenyl), diisopropylbiphenyl (e.g., 4' -isopropylbiphenyl), and α -methylstyrene dimer.
[ Chemical formula 4]
In the general formula (1B), L 21 represents a single bond, an oxysulfonyl group (× 1-SO2-O-*2) or a sulfonyloxy group (× 1-O-SO2-*2). Further, 1 represents a bonding position to the phenyl group represented by the general formula (1B), and 2 represents a bonding position to R 22.
R 21 represents a non-aromatic substituent. The meaning of the non-aromatic substituent represented by R 21 is the same as that of the non-aromatic substituent represented by R 11 in the general formula (1A), and the preferable mode is also the same.
N 21 represents an integer of 0 to 5. n 21 is preferably an integer representing 0 to 2.
When n 21 represents an integer of 2 or more, a plurality of R 21 may be the same or different from each other.
R 22 represents a 1-valent aliphatic hydrocarbon group. Examples of the 1-valent aliphatic hydrocarbon group represented by R 22 include the same aliphatic hydrocarbon groups as the 1-valent aliphatic hydrocarbon group represented by R A in the substituent W.
Specific examples of the solvent represented by the general formula (1B) include a benzenesulfonic acid methyl group, a p-toluenesulfonic acid methyl group, and a linear alkylbenzene having 1 to 15 carbon atoms.
[ Chemical formula 5]
In the general formula (1C), R 31、R32 and R 33 each independently represent a non-aromatic substituent.
The non-aromatic substituents represented by R 31、R32 and R 33 have the same meaning as the non-aromatic substituent represented by R 11 in the general formula (1A), and the preferable mode is also the same.
N 31、n32 and n 33 each independently represent an integer of 0 to 5. n 31、n32 and n 33 are preferably integers each independently representing 0 to 2.
When n 31、n32 and n 33 represent integers of 2 or more, a plurality of R 31, a plurality of R 32 and a plurality of R 33 may be the same or different from each other.
Specific examples of the solvent represented by the general formula (1C) include tricresyl phosphate and tricresyl phosphate.
From the viewpoint of further excellent storage stability at low temperatures and further excellent color development concentration, it is preferable that any one of the specific solvents contained in the solvent containing an aromatic group is selected from the solvents represented by the above general formula (1A).
The specific solvents contained in the specific microcapsules are 2 or more, preferably 3 or more, and more preferably 4 or more. Examples of the combination of 4 or more specific solvents included in the specific microcapsules include a combination of 1, 2-dimethyl-4- (1-phenylethyl) benzene, 1, 3-dimethyl-4- (1-phenylethyl) benzene, 1, 4-dimethyl-2- (1-phenylethyl) benzene and 1- (ethylphenyl) -1-phenylethane.
The specific microcapsules preferably contain a solvent having an aliphatic structure as a solvent having a boiling point of 100 ℃ or higher. The solvent containing an aliphatic structure can contribute to the formation of the capsule wall as will be described later.
The term "containing an aliphatic structure" means that a non-aromatic hydrocarbon group is contained in a molecule. In the above-mentioned non-aromatic hydrocarbon group, the carbon atom in the hydrocarbon group may be substituted with a hetero atom, a carbonyl carbon or the like. The hydrocarbon group may have a substituent.
In addition, the solvent containing an aliphatic structure does not contain an aromatic group. In other words, the solvent having an aliphatic structure does not contain an aromatic ring in the molecule. Therefore, solvents containing an aromatic group and an aliphatic structure are classified as solvents containing an aromatic group.
The solvent containing an aliphatic structure is not particularly limited, and examples thereof include aliphatic hydrocarbons such as diethyl succinate, methyl laurate, and isoalkanes (for example, isoalkanes having 10 or more carbon atoms); natural animal and vegetable oils such as soybean oil, corn oil, cottonseed oil, rapeseed oil, olive oil, coconut oil, castor oil and fish oil, and natural high boiling fractions such as mineral oil.
The aliphatic structure-containing solvent may be used alone or in combination of 1 or more than 2.
When the specific microcapsule contains a solvent having an aliphatic structure as a solvent having a boiling point of 100 ℃ or higher, the content of the specific solvent is preferably 50.0 to 90.0 mass% relative to the total mass of the solvent having an aliphatic structure and the specific solvent, from the viewpoint of further excellent storage stability at low temperature and further excellent color development concentration, and more preferably 75.0 to 90.0 mass% from the viewpoint of further excellent color development concentration.
In the specific microcapsules, the mass ratio of the solvent having a boiling point of 100 ℃ or higher to the color former (mass of the solvent having a boiling point of 100 ℃ or higher/mass of the color former) is preferably in the range of 98/2 to 30/70, more preferably in the range of 97/3 to 40/60, from the viewpoint of further excellent color forming concentration.
The specific microcapsule may contain, in addition to the above-described components, 1 or more additives such as a light stabilizer, an antioxidant, paraffin wax, and a deodorant, if necessary.
The specific microcapsules may contain a color former which does not contain a solvent having a boiling point of less than 100 ℃ (for example, ketones such as methyl ethyl ketone, esters such as ethyl acetate, alcohols such as isopropyl alcohol, and the like) and aromatic groups, within a range which does not inhibit the effect of the present invention.
(Method for producing specific microcapsules)
The method for producing the specific microcapsule is not particularly limited, and examples thereof include known methods such as interfacial polymerization, internal polymerization, phase separation, external polymerization, and coacervation. Among them, the interfacial polymerization method is preferable.
Hereinafter, an interfacial polymerization method will be described, taking as an example a method for producing a specific microcapsule in which the capsule wall is polyurea or polyurethaneurea.
The interfacial polymerization method is preferably one comprising a step of dispersing an oil phase containing a color former, a solvent having a boiling point of 100 ℃ or higher, and a capsule wall material (for example, a raw material containing at least 1 selected from the group consisting of a polyisocyanate, a polyol, and a polyamine in a reaction system to produce a polyamine by reacting the polyisocyanate with water, or a step of preparing an emulsion by dispersing an oil phase containing an emulsifier in an aqueous phase (emulsification step) and a step of polymerizing a capsule wall material at an interface between the oil phase and the aqueous phase to form a capsule wall and form a microcapsule containing the color former (encapsulation step).
The mass ratio of the total amount of the polyol and the polyamine to the amount of the polyisocyanate (total amount of the polyol and the polyamine/amount of the polyisocyanate) in the raw materials is not particularly limited, but is preferably 0.1/99.9 to 30/70, more preferably 1/99 to 25/75.
In the emulsification step, the solvent having a boiling point of 100 ℃ or higher preferably contains at least a specific solvent and a solvent containing an aliphatic structure. In addition, the solvent containing an aliphatic structure is likely to precipitate as a polyisocyanate as a raw material of the capsule wall, and can contribute to the formation of the capsule wall.
The type of the emulsifier used in the emulsification step is not particularly limited, and examples thereof include a dispersant and a surfactant.
Examples of the dispersant include polyvinyl alcohol.
Layer 1 comprises the specific microcapsules described above.
The content of the specific microcapsules in the layer 1 is not particularly limited, but is preferably 60 to 98 mass%, more preferably 75 to 95 mass%, relative to the total mass of the layer 1.
The content of the color former in the layer 1 is not particularly limited, but is preferably 0.1 to 2.0g/m 2, more preferably 0.2 to 1.0g/m 2.
Layer 1 may contain other ingredients in addition to the specific microcapsules described above.
Examples of the other components include a polymer binder, an inorganic filler (for example, colloidal silica), a fluorescent whitening agent, an antifoaming agent, a penetrating agent, an ultraviolet absorber, a surfactant, and a preservative.
The mass per unit area (solid content coating amount) (g/m 2) of the 1 st layer is not particularly limited, and is, for example, 0.5 to 20.0g/m 2, more preferably 0.5 to 10.0g/m 2.
< Method of Forming layer 1 >)
The method for forming the 1 st layer is not particularly limited, and a known method can be used.
For example, there is a method in which a layer 1 composition comprising a solvent having a boiling point of 100 ℃ or higher is applied to a layer 1 support, and the coating film is dried as necessary.
The layer 1 composition contains at least a specific microcapsule and a solvent having a boiling point of preferably 100 ℃ or higher. The microcapsule dispersion obtained by the interfacial polymerization method described above may be used as the composition for forming layer 1.
The layer 1 composition may contain other components that may be contained in the layer 1.
The method of applying the layer 1 forming composition is not particularly limited, and examples of the coating machine used in the application include a gas knife coater, a bar coater, a curtain coater, a gravure coater, a squeeze coater, a die coater, a slide bead coater, and a blade coater.
After the layer 1 forming composition is applied to the layer 1 support, the coating film may be dried as necessary. The drying treatment may be a heating treatment.
Although the method of forming the 1 st layer on the 1 st support is described above, the method is not limited to the above, and for example, the 1 st sheet formed of the 1 st layer may be formed by peeling the temporary support after forming the 1 st layer on the temporary support.
The temporary support is not particularly limited as long as it is a releasable support.
< Other parts >)
The 1 st sheet may have other members than the 1 st support and the 1 st layer described above.
For example, the 1 st sheet may have an easy-to-adhere layer between the 1 st support and the 1 st layer for improving adhesion between the two.
The thickness of the adhesive layer is not particularly limited, but is preferably 0.005 to 0.2. Mu.m, more preferably 0.01 to 0.1. Mu.m.
From the viewpoint of further excellent color development density and further excellent image quality (resolution), the arithmetic average roughness Ra of the 1 st sheet is preferably 3.0 to 7.0 μm. The arithmetic average roughness Ra of the 1 st sheet means the arithmetic average roughness Ra of the surface of the 1 st sheet on the side (the side in contact with the 2 nd sheet) opposite to the 1 st sheet when the sheet set for pressure measurement is used. In the case where the 1 st layer is located on the outermost surface on the side opposite to the 2 nd sheet in the 1 st sheet, the arithmetic average roughness Ra corresponds to the arithmetic average roughness Ra of the surface on the side opposite to the 1 st support side of the 1 st layer.
In addition, the arithmetic average roughness Ra of the 1 st sheet in the present specification means JIS B0681-6: 2014, and an arithmetic average roughness Ra specified in 2014. Further, as the measurement device, a scanning white light interferometer using an optical interference system (specifically, newView5020: stich mode, objective lens×50 times, intermediate lens×0.5 times manufactured by Zygo corporation) was used.
When the arithmetic average roughness Ra of the 1 st sheet is 3.0 μm or more, the color former is often in a sufficient amount, and thus a higher color formation concentration tends to occur. On the other hand, when the arithmetic average roughness Ra of the 1 st sheet is 7.0 μm or less, the 2 nd layer of the 2 nd sheet can properly absorb the solvent flowing out together with the color former by the disintegration of the specific microcapsules in the pressurized region, and therefore good image quality with less penetration can be obtained.
In addition, the arithmetic average roughness Ra of the 1 st sheet can be controlled by adjusting the solid content coating amount of the 1 st layer forming composition and adjusting the amount of the specific microcapsules in the 1 st layer of the 1 st sheet.
Sheet 2
The 2 nd sheet 22 shown in fig. 1 includes a 2 nd support 18 and a 2 nd layer 20 including a developer, which is disposed on the 2 nd support 18.
The components are described in detail below.
< 2 Nd support >)
The 2 nd support is a member for supporting the 2 nd layer. In addition, in the case where the processing can be performed by the layer 2 itself, the layer 2 sheet may not have the layer 2 support.
The mode of the 2 nd support is the same as that of the 1 st support described above, and therefore, the description thereof is omitted.
< Layer 2 >
Layer 2 is the layer containing the developer.
The color former is a compound which has no color-developing function but has a property of developing a color of the color former by contact with the color former. The color former is preferably an electron accepting compound.
Examples of the color-developing agent include inorganic compounds and organic compounds, and those described in WO2009/8248[0055] to [0056] are preferable. The metal salt of the acidic clay, the activated clay or the aromatic carboxylic acid is preferable from the viewpoint of further excellent color development concentration and image quality after color development.
The content of the color former in the layer 2 is not particularly limited, but is preferably 50 to 95% by mass, more preferably 70 to 90% by mass, based on the total mass of the layer 2.
The color developer may be used alone or in combination of at least 2 kinds.
The content of the color former in the layer 2 is not particularly limited, but is preferably 1.0 to 40g/m 2. When the color former is an inorganic compound, the content of the color former is preferably 2.0 to 30g/m 2, more preferably 3.0 to 20g/m 2.
The layer 2 may contain other components than the above-described developer.
Examples of the other components include a polymer binder, a pigment, an optical brightening agent, an antifoaming agent, a penetrating agent, an ultraviolet absorber, a surfactant, and a preservative.
Examples of the polymer binder include synthetic and natural polymers such as styrene-butadiene copolymer, polyvinyl acetate, polyacrylate, polyvinyl alcohol, polyacrylic acid, maleic anhydride-styrene copolymer, olefin resin, modified acrylate copolymer, starch, casein, gum arabic, gelatin, carboxymethyl cellulose or salts thereof, and methyl cellulose.
Examples of the pigment include heavy calcium carbonate, light calcium carbonate, talc, and titanium dioxide.
The thickness of the 2 nd layer is not particularly limited, but is preferably 0.5 to 30. Mu.m, more preferably 3.5 to 30. Mu.m.
The mass per unit area (solid content coating amount) (g/m 2) of the layer 2 is not particularly limited, and is, for example, 0.5 to 30.0g/m 2, more preferably 3.5 to 30.0g/m 2.
< Method of Forming layer 2 >)
The method for forming the layer 2 is not particularly limited, and a known method can be used.
For example, a method of applying a layer 2 forming composition containing a color developer to a layer 2 support and optionally drying the composition is mentioned.
The layer 2-forming composition may be a dispersion in which a color-developer is dispersed in water or the like. When the developer is an inorganic compound, the dispersion liquid in which the developer is dispersed can be prepared by mechanically dispersing the inorganic compound in water. In addition, when the color former is an organic compound, the color former can be prepared by mechanically dispersing the organic compound in water or dissolving the organic compound in an organic solvent.
The composition for forming a layer 2 may contain other components that may be contained in the layer 2.
The method of applying the layer 2 forming composition is not particularly limited, and examples thereof include a method using a coater used when applying the layer 1 forming composition.
After the layer 2 forming composition is applied to the layer 2 support, the coating film may be dried as necessary. The drying treatment may be a heating treatment.
Although the method of forming the 2 nd layer on the 2 nd support is described above, the method is not limited to the above, and for example, the 2 nd sheet formed of the 2 nd layer may be formed by peeling the temporary support after forming the 2 nd layer on the temporary support.
The temporary support is not particularly limited as long as it is a releasable support.
< Other parts >)
The 2 nd sheet may have other members than the 2 nd support and the 2 nd layer.
For example, the 2 nd sheet may have an easy-to-adhere layer between the 2 nd support and the 2 nd layer for improving adhesion between the two.
Examples of the method of the easy-to-adhere layer include the method of the easy-to-adhere layer that the 1 st sheet may have.
As described above, the 1 st sheet and the 2 nd sheet are stacked so that the 1 st layer of the 1 st sheet and the 2 nd layer of the 2 nd sheet face each other, and the stack is pressed and used.
From the viewpoint of further excellent color development concentration, the oil absorption of the specific solvent with respect to the 2 nd sheet is preferably 2.0 to 20.0g/m 2. When the oil absorption of the specific solvent with respect to the 2 nd sheet is 2.0g/m 2 or more, the solution containing the color former and the specific solvent which flows out due to the disintegration of the specific microcapsule is easily absorbed by the 2 nd layer of the 2 nd sheet in the pressurized region, and a higher color development concentration is easily generated. On the other hand, when the oil absorption of the specific solvent with respect to the 2 nd sheet is 20.0g/m 2 or less, the solution containing the color former and the specific solvent, which flows out due to the disintegration of the specific microcapsule, cannot reach the deep part of the 2 nd layer of the 2 nd sheet in the pressurized region, and as a result, the amount of the color former existing in the surface layer region of the 2 nd layer is large, and a higher color former concentration is likely to occur.
The oil absorption amount of the specific solvent with respect to the 2 nd sheet was obtained by obtaining the difference between the weight of the 2 nd sheet before the specific solvent was absorbed and the weight of the 2 nd sheet after the specific solvent was absorbed, and converting the difference into a unit area.
From the viewpoint of further excellent color development density and further excellent image quality (resolution), the arithmetic average roughness Ra of the 2 nd sheet is preferably 1.2 μm or less. The arithmetic average roughness Ra of the 2 nd sheet means the arithmetic average roughness Ra of the surface of the 2 nd sheet on the side (the side in contact with the 1 st sheet) opposite to the 1 st sheet when the sheet set for pressure measurement is used. In the case where the 2 nd layer is the outermost surface on the side opposite to the 1 st sheet in the 2 nd sheet, the arithmetic average roughness Ra corresponds to the arithmetic average roughness Ra of the surface on the side opposite to the 2 nd support side of the 2 nd layer.
In addition, the arithmetic average roughness Ra of the 2 nd sheet in the present specification means JIS B0681-6: 2014, and an arithmetic average roughness Ra specified in 2014. Further, as the measurement device, a scanning white light interferometer using an optical interference system (specifically, newView5020 manufactured by Zygo corporation: micro mode, objective lens×50 times, and intermediate lens×0.5 times) was used.
Method for manufacturing sheet set for pressure measurement
The method for producing the 1 st sheet and the 2 nd sheet included in the sheet set for pressure measurement is as described above. The method for producing the sheet set for pressure measurement preferably includes a step of applying a layer 1 composition containing microcapsules each containing a solvent having a boiling point of 100 ℃ or higher and a color former, and drying the obtained coating film to form a layer 1.
The method of forming the 1 st layer using the 1 st layer forming composition is as described in embodiment 1.
[ Embodiment 2]
Fig. 3 is a cross-sectional view of an embodiment of a sheet for pressure measurement.
The pressure measurement sheet 30 includes, in order, a support 32, a layer 220 containing a color developer, and a layer 114 containing specific microcapsules 13.
When the pressure measurement sheet 30 is used, pressurization is performed from at least one of the support 32 side and the 1 st layer 14 side, and the specific microcapsules 13 are ruptured in the pressurized region, so that the color former contained in the specific microcapsules 13 comes out of the specific microcapsules 13, and the color former in the 2 nd layer 20 undergoes a color reaction. As a result, color development proceeds in the pressurized region.
As will be described later, the pressure measurement sheet 30 may be provided with the 1 st layer 14 and the 2 nd layer 20, or may be provided without the support 32.
In fig. 3, the support 32 and the 2 nd layer 20 are directly laminated, but the method is not limited to this, and other layers (for example, an easy-to-adhere layer) may be disposed between the support 32 and the 2 nd layer 20 as will be described later.
Although the pressure measurement sheet 30 having the support 32, the 2 nd layer 20, and the 1 st layer 14 in this order is disclosed in fig. 3, the pressure measurement sheet is not limited to this embodiment, and may be a pressure measurement sheet having the support 32, the 1 st layer 14, and the 2 nd layer 20 in this order.
The 1 st layer 14 and the 2 nd layer 20 in the pressure measurement sheet 30 are the same members as the 1 st layer 14 and the 2 nd layer 20 described in embodiment 1 above, and therefore, the description thereof is omitted.
Hereinafter, the support 32 will be mainly described in detail.
Support body
The support is a member for supporting the 1 st layer and the 2 nd layer. In the case where the laminate of the 1 st layer and the 2 nd layer can be handled by itself, the pressure measurement sheet may not have a support.
The preferred embodiment of the support is the same as that of the 1 st support described above, and therefore, the description thereof will be omitted.
Method for producing sheet for measuring pressure
The method for producing the sheet for pressure measurement is not particularly limited, and a known method can be used.
The method for producing the sheet for pressure measurement preferably includes a step of applying a layer 1 composition containing microcapsules containing a solvent having a boiling point of 100 ℃ or higher and a color former, and optionally drying the obtained coating film to form a layer 1.
As a specific example of a method for producing a sheet for pressure measurement, the following method can be given: the layer 1 is formed by applying a layer 2-forming composition containing a color developer to a support, optionally drying the composition, forming a layer 2 on the support, further applying a layer 1-forming composition containing a specific microcapsule and a solvent having a boiling point of 100 ℃ or higher to the layer 2, and optionally drying the coating film.
The method of forming the 1 st layer using the 1 st layer forming composition is as described in embodiment 1. The method for forming the 2 nd layer using the composition for forming the 2 nd layer is also as described in embodiment 1.
Other parts
The pressure measurement sheet may include other members than the support, the 2 nd layer, and the 1 st layer.
For example, the pressure measurement sheet may have an easy-to-adhere layer between the support and the 2 nd layer for improving adhesion between the support and the 2 nd layer.
Examples of the method of the easy-to-adhere layer include the method of the easy-to-adhere layer that the 1 st sheet may have.
As described above, the pressure measurement sheet is used by pressurizing the surface thereof.
From the viewpoint of further excellent color development concentration, the oil absorption of the specific solvent with respect to the layer 2 is preferably 2.0 to 20.0g/m 2. When the oil absorption of the specific solvent with respect to the layer 2 is 2.0g/m 2 or more, the solution containing the color former and the specific solvent which flows out due to the disintegration of the specific microcapsule is easily absorbed by the layer 2 in the pressurized region, and a higher color development concentration is easily generated. On the other hand, when the oil absorption of the specific solvent with respect to the layer 2 is 20.0g/m 2 or less, the solution containing the color former and the specific solvent which flows out due to the disintegration of the specific microcapsule in the pressurized region does not reach the deep part of the layer 2, and as a result, the amount of the color former existing in the surface layer region of the layer 2 is large, and a higher color former concentration is likely to occur.
The sheet set for pressure measurement and the use of the sheet for pressure measurement according to the present invention are not particularly limited, and examples thereof include pressure measurement at the time of manufacturing an electronic component (pressure measurement in a bonding process of a liquid crystal panel, confirmation of pressure distribution in a solder printing process of a printed board, confirmation of pressure distribution in a crimping process of an integrated circuit or wiring, etc.), pressure measurement at the time of manufacturing a vehicle (cylinder gasket surface pressure measurement of an engine, pressure measurement of flange surfaces of various sealing portions, and ground contact pressure confirmation of a tire).
[ Embodiment 3]
In embodiment 3, a dispersion (hereinafter, also simply referred to as "dispersion 1") for forming a layer to be used in combination with a layer containing a color former for pressure measurement, and microcapsules containing a solvent having a boiling point of 100 ℃ or higher and a color former are given.
In the dispersion 1, the solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups, and the color former contains 2 or more color formers containing aromatic groups.
The details of the components contained in the 1 st dispersion are as described above.
The 1 st dispersion may be the 1 st layer-forming composition.
The 1 st dispersion usually contains a solvent for dispersing the microcapsules (a solvent not encapsulated in the microcapsules). The type of the solvent contained in the 1 st dispersion is not particularly limited, and examples thereof include water and an organic solvent. The organic solvent may be, for example, a solvent having a boiling point of 100℃or higher, which is used for preparing the 1 st dispersion.
The 1 st dispersion was used for forming a layer (corresponding to the 1 st layer) for pressure measurement, similarly to the 1 st layer-forming composition.
The 1 st dispersion may be used in combination with a dispersion used for forming a layer containing a color-developer (hereinafter, also referred to simply as "2 nd dispersion"). That is, the 1 st dispersion and the 2 nd dispersion may be used as a set (dispersion set).
The 2 nd dispersion is a dispersion containing a color developer.
The 2 nd dispersion may be the composition for forming a 2 nd layer.
Examples of the color developer contained in the 2 nd dispersion include those contained in the 2 nd layer-forming composition.
The 2 nd dispersion usually contains a solvent. The type of the solvent contained in the 2 nd dispersion is not particularly limited, and examples thereof include water and an organic solvent.
The 1 st dispersion preferably contains no coarse particles, for the reason that the dispersion can be applied to a curved surface without irregularities and is not clogged in a coating system such as spraying.
For the same reason as described above, the average particle diameter of the microcapsules is preferably 1 to 50. Mu.m.
For the same reason as described above, the 2 nd dispersion preferably contains no coarse particles.
For the same reason as described above, the color-developer contained in the 2 nd dispersion is preferably an organic compound. The organic compound is preferably a metal salt of an aromatic carboxylic acid, more preferably a metal salt of salicylic acid, and still more preferably a zinc salt of salicylic acid.
The above-mentioned dispersion 1 can be applied to an object whose pressure measurement is difficult to be performed in a sheet such as a sheet set for pressure measurement and a sheet for pressure measurement. More specifically, the pressure measurement can be performed by applying the 1 st dispersion in a desired amount to a region of the pressure measurement target where the pressure measurement is required, and forming a layer containing the microcapsules in the region of the region, without being affected by the surface shape of the pressure measurement target. In particular, the present invention can be preferably applied to a case where the pressure in the curved surface is measured. More specifically, the 1 st dispersion was applied to the curved surface portion to form a layer containing microcapsules, and pressure measurement was possible.
In addition, as described above, the layer formed from the 1 st dispersion was used in combination with a layer containing a color developer for pressure measurement. Therefore, similarly to the case of using the 1 st dispersion, the pressure measurement can be performed by applying the required amount of the 2 nd dispersion to the region of the pressure measurement target where the pressure measurement is required, and disposing the layer containing the color-developer and the layer containing the microcapsules adjacently.
In general, the layer containing microcapsules and the layer containing the color-developer are laminated and arranged in a region of the pressure measurement target where pressure measurement is required, but any layer may be arranged on the pressure measurement target side. In other words, the 1 st dispersion and the 2 nd dispersion may be applied first to the region of the pressure measurement target where the pressure measurement is required.
As described above, by pressurizing the surfaces coated with the 1 st dispersion and the 2 nd dispersion from the other side, the microcapsules are ruptured in the pressurized region, and the color former enclosed in the microcapsules comes out of the microcapsules, comes into contact with the color former, and performs a color reaction with the color former. As a result, color development proceeds in the pressurized region.
The method of applying the 1 st dispersion and the 2 nd dispersion is not particularly limited, and examples thereof include roll coating, spray coating, brush coating and dip coating.
The 1 st dispersion and the 2 nd dispersion may be applied directly to the measurement surface of the object to be measured, or may be applied via a film, paper, or the like.
The coating amounts of the 1 st dispersion and the 2 nd dispersion can be set according to the measurement application, but are preferably 2 to 40g/m 2 in terms of solid matter conversion from the viewpoint of obtaining good color development and color development distribution.
[ Embodiment 4]
In embodiment 4, a dispersion liquid (hereinafter, also simply referred to as "dispersion liquid for forming a pressure measurement layer") containing microcapsules and a color former, each of which contains a solvent having a boiling point of 100 ℃ or higher, and a color former is used to form a layer for pressure measurement.
In the 3 rd dispersion, the solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups, and the color former contains 2 or more color formers containing aromatic groups.
The microcapsules contained in the 3 rd dispersion may be those contained in the 1 st layer-forming composition.
Examples of the color developer contained in the 3 rd dispersion include a color developer contained in the 2 nd layer forming composition.
The 3 rd dispersion usually contains a solvent for dispersing the microcapsules (a solvent not encapsulated in the microcapsules). The type of the solvent contained in the 3 rd dispersion is not particularly limited, and examples thereof include water and an organic solvent.
The 3 rd dispersion may be a composition in which the color-developer is mixed with the 1 st layer-forming composition, or a composition in which the 2 nd layer-forming composition is mixed with the 1 st layer-forming composition.
Further, the 3 rd dispersion preferably contains no coarse particles, for the reason that the coating can be applied to a curved surface without irregularities and that the coating does not clog in a coating system such as spraying.
For the same reason as described above, the average particle diameter of the microcapsules is preferably 1 to 50. Mu.m.
For the same reason as described above, the color-developer contained in the 3 rd dispersion is preferably an organic compound. The organic compound is preferably a metal salt of an aromatic carboxylic acid, more preferably a metal salt of salicylic acid, and still more preferably a zinc salt of salicylic acid.
Since the 3 rd dispersion liquid contains the microcapsules containing the color former and the color former, the pressure measurement can be performed only by the layer formed by coating the 3 rd dispersion liquid.
That is, the 3 rd dispersion liquid can be applied to an object in which pressure measurement is difficult to be performed in a sheet such as a sheet set for pressure measurement and a sheet for pressure measurement, as in the 1 st dispersion liquid and the 2 nd dispersion liquid. More specifically, the pressure measurement can be performed by applying the 3 rd dispersion in a desired amount to a region of the pressure measurement target where the pressure measurement is required, and forming a layer in the region, without being affected by the surface shape of the pressure measurement target.
Examples of the method and conditions for applying the 3 rd dispersion include the method and conditions for applying the 1 st dispersion and the 2 nd dispersion described above.
The 1 st dispersion, the 2 nd dispersion and the 3 rd dispersion described above can be used for various purposes.
Examples thereof include confirmation of pressure distribution in molding processing of various components, bodies, and the like in manufacturing of automobiles and aircrafts, confirmation of pressure distribution in assembling processing of building materials, confirmation of pressure distribution in processes such as curved surface processing of electronic products, confirmation of impact force given to goods accompanying transportation, confirmation of each mold in manufacturing of metal products, confirmation of each mold in molding processing of resin products, confirmation of pressure distribution in the ingot of tablets in medical products, confirmation of pressure distribution in furniture surfaces such as sofa seating surfaces, confirmation of pressure distribution of stationery such as grip force given to writing tools, confirmation of impact force given to sports goods such as balls made of elastic materials, and confirmation of gaps (clearances) between upper and lower teeth in the dental goods.
Examples
The present invention will be described in further detail with reference to examples. The materials, amounts used, ratios, processing contents, processing sequences, and the like shown in the following examples can be appropriately changed without departing from the gist of the present invention. Accordingly, the scope of the present invention should not be construed in a limiting manner by the examples shown below. Unless otherwise specified, the following "parts" and "%" are based on mass.
[ Production of sheet set for pressure measurement ]
[ Example 1]
Preparation of microcapsules containing color-former
3',6' -Bis (diethylamino) -2- (4-nitrophenyl) spiro [ isoindol-1, 9 '-xanthene ] -3-one (Hodogaya Chemical co., ltd. Manufactured, pink-DCF) 3 parts, 6' - (diethylamino) -1',3' -dimethylbutane parent (Hodogaya Chemical co., ltd. Manufactured, orange-DCF) 4 parts were dissolved as a colorant in 50 parts of a mixture of 1, 2-dimethyl-4- (1-phenylethyl) benzene, 1, 3-dimethyl-4- (1-phenylethyl) benzene, 1, 4-dimethyl-2- (1-phenylethyl) benzene, 1- (ethylphenyl) -1-phenylethane (manufactured by plummet-fine chemical company, SRS-101) to obtain a solution a. Next, 0.3 part of N, N' -tetrakis (2-hydroxypropyl) ethylenediamine (ADEKA CORPORATION, ADEKA POLYETHER EDP-300) dissolved in 13 parts of synthetic isoalkane (Idemitsu Kosan co., ltd., IP Solvent 1620) and 2.5 parts of methyl ethyl ketone was added to the stirred solution a, thereby obtaining a solution B. Further, 2.5 parts of trimethylolpropane adduct (DIC CORPORATION, BURNOCK D-750) of toluene diisocyanate dissolved in 6 parts of ethyl acetate was added to the stirred solution B to obtain a solution C. Then, the above solution C was added to a solution in which 7 parts of polyvinyl alcohol (PVA-217E, kuraray co., ltd.) was dissolved in 140 parts of water, and emulsified and dispersed. 200 parts of water was added to the emulsified and dispersed solution, and the solution was heated to 70℃with stirring, stirred for 1 hour, and then cooled. Further, water was added to adjust the concentration, and a microcapsule liquid containing a color former having a solid content of 20% by mass was obtained.
The average particle diameter of the obtained microcapsules encapsulating the color former was 20. Mu.m. The average particle diameter was measured by an optical microscope and by the method described above.
Production of sheet set for pressure measurement
(Production of sheet 1)
18 Parts of the obtained microcapsule liquid in which a color former was encapsulated, 10 parts of water, 1.8 parts of colloidal silica (NISSAN CHEMICAL Industries, ltd.), SNOWTEX 30, solid content 30%), 2 parts of a 1% aqueous solution of sodium carboxymethyl cellulose (DKS co.ltd., SEROGEN a), 4.5 parts of a 1% aqueous solution of sodium carboxymethyl cellulose (DKS co.ltd., SEROGEN EP), 1 part of a 15% aqueous solution of a side chain alkylbenzene sulfonic acid amine salt (DKS co.ltd., NEOGEN t.), 0.2 parts of a 1% aqueous solution of polyoxyethylene polyoxypropylene lauryl ether (DKS co.ltd., nogen LP-70), and 0.2 parts of a 1% aqueous solution of sodium-bis (3, 4,5, 6-nonafluorohexyl) -2-sulfonyloxy octanoic acid (FUJIFILM Corporation, W-AHE) were mixed to obtain a composition for forming a layer 1.
The obtained composition for forming layer 1 was coated on a polyethylene terephthalate (PET) sheet having a thickness of 75 μm by a bar coater so that the mass after drying became 6.0g/m 2. Subsequently, the obtained coating film was dried at 80 ℃ to form a1 st layer, thereby producing a1 st sheet.
(Production of sheet No. 2)
To the obtained dispersion were added 100 parts of activated clay (Mizusawa Industrial Chemicals, ltd., shilton F-242), 0.5 part of Na hexametaphosphate (Nippon Chemical Industry co., ltd., sodium hexametaphosphate), 15 parts of 10% aqueous sodium hydroxide, and 240 parts of water as a developer, 30 parts of an olefin resin (ARAKAWA CHEMICAL INDUSTRIES, LTD., polymaron482, 25% by mass solid content concentration), 35 parts of a modified acrylate copolymer (Zeon Corporation, nippon LX814, 46% by mass solid content concentration), 80 parts of a 1% aqueous solution of sodium carboxymethyl cellulose (DKS co.ltd., SEROGEN EP), 18 parts of a 15% aqueous solution of Na alkyl benzene sulfonate (DKS co.ltd., NEOGEN t.), 20 parts of a 1% aqueous solution of polyoxyethylene polyoxypropylene lauryl ether (DKS co.ltd., nogen LP-70), 20 parts of sodium-bis (3, 4,5, 6-nonafluorohexyl) -2-sulfonyl oxy (498) (498% by mass solid content), and 20 parts of a solution of an aqueous solution of water-in which a color-developer was coated, and a color-developer was prepared.
The coating liquid containing the color developer was applied to a polyethylene terephthalate (PET) sheet having a thickness of 75. Mu.m, so that the solid content coating amount was 7.0g/m 2. Next, the obtained coating film was dried to form a2 nd layer, whereby a2 nd sheet was obtained.
[ Example 2]
Preparation of microcapsules containing color-former
A microcapsule containing a color former was prepared in the same manner as in example 1 except that 50 parts of SRS-101 (manufactured by tabacco Jinzheng fine chemical company limited) was changed to 50 parts of a mixture of 1,2, 4-trimethylbenzene, 1,3, 5-trimethylbenzene, 1,2, 3-trimethylbenzene, cumene and xylene (manufactured by ENEOS Corporation, hysol 100).
Production of sheet set for pressure measurement
A sheet set for pressure measurement of example 2 was produced in the same manner as in example 1, except that the obtained microcapsules containing a color former were used.
[ Example 3]
Preparation of microcapsules containing color-former
Microcapsules containing a color former were prepared in the same manner as in example 1 except that 3 parts of Pink-DCF (Hodogaya Chemical Co., ltd.) and 4 parts of Orange-DCF (Hodogaya Chemical Co., ltd.) were changed to 4 parts of the compound represented by the following structure (A) (YAMADA CHEMICAL CO., LTD., manufactured, red 500) and 4 parts of the compound represented by the following structure (B) (YAMADA CHEMICAL CO., LTD., manufactured, red 520).
Compounds represented by Structure (A)
[ Chemical formula 6]
Compounds represented by Structure (B)
[ Chemical formula 7]
Production of sheet set for pressure measurement
A sheet set for pressure measurement of example 3 was produced in the same manner as in example 1, except that the obtained microcapsules containing a color former were used.
Examples 4 to 7
Preparation of microcapsules containing color-former
A microcapsule containing a color former was prepared in the same manner as in example 1 except that 50 parts of SRS-101 (manufactured by tabacco positive fine chemical company limited) was changed to 50 parts of the solvent described in the column "solvent containing an aromatic group" in table 1 (in the column "type" of the column "solvent containing an aromatic group" in table 1, the numerical values in brackets described in the same manner as in the solvent type indicate the mixing ratio (mass basis)).
Production of sheet set for pressure measurement
A sheet set for pressure measurement of examples 4 to 7 was produced in the same manner as in example 1, except that the obtained microcapsules containing the color former were used.
Example 8
Production of sheet set for pressure measurement
In the production of the 1 st sheet, a pressure measurement sheet set of example 8 was produced in the same manner as in example 1, except that the obtained 1 st layer forming composition was applied to a polyethylene terephthalate (PET) sheet having a thickness of 75 μm by a bar coater so that the mass after drying became 12.0g/m 2, and the obtained coating film was dried at 80 ℃.
[ Example 9]
Production of sheet set for pressure measurement
In the production of the 2 nd sheet, a sheet set for pressure measurement of example 9 was produced in the same manner as in example 1, except that a coating liquid containing a color developer was applied to a polyethylene terephthalate (PET) sheet having a thickness of 75 μm so that the solid content application amount became 3.5g/m 2, and the obtained coating film was dried to form the 2 nd layer.
[ Example 10]
Production of sheet set for pressure measurement
In the production of the 2 nd sheet, a sheet set for pressure measurement of example 10 was produced in the same manner as in example 1, except that a coating liquid containing a color developer was applied to a polyethylene terephthalate (PET) sheet having a thickness of 75 μm so that the solid content application amount became 1.8g/m 2, and the obtained coating film was dried to form the 2 nd layer.
[ Example 11]
Preparation of microcapsules containing color-former
A microcapsule containing a color former was prepared in the same manner as in example 1 except that 50 parts of SRS-101 (manufactured by tabacco positive fine chemical company limited) was changed to 47 parts, and 13 parts of IP Solvent 1620 (manufactured by Idemitsu Kosan co., ltd.) was changed to 16 parts.
Production of sheet set for pressure measurement
A sheet set for pressure measurement of example 11 was produced in the same manner as in example 1, except that the obtained microcapsules containing a color former were used.
Comparative example 1
Preparation of microcapsules containing color-former
A microcapsule containing a color former was prepared in the same manner as in example 1 except that 50 parts of SRS-101 (manufactured by tabacco positive fine chemical company limited) was changed to 47 parts of 4-isopropyl biphenyl, and 13 parts of IP Solvent 1620 (manufactured by Idemitsu Kosan co., ltd.) was changed to 16 parts.
Production of sheet set for pressure measurement
A sheet set for pressure measurement of comparative example 1 was produced in the same manner as in example 1, except that the obtained microcapsules containing a color former were used.
Comparative example 2
Preparation of microcapsules containing color-former
Microcapsules containing a color former were prepared in the same manner as in example 4 except that 3 parts of Pink-DCF (Hodogaya Chemical Co., ltd.) and 4 parts of Orange-DCF (Hodogaya Chemical Co., ltd.) were changed to 7 parts of Pink-DCF (Hodogaya Chemical Co., ltd.).
Production of sheet set for pressure measurement
A sheet set for pressure measurement of comparative example 1 was produced in the same manner as in example 4, except that the obtained microcapsules containing a color former were used.
[ Measurement and evaluation ]
[ Measurement of oil absorption (g/m 2) of aromatic group-containing solvent with respect to sheet 2 ]
After the aromatic group-containing solvent (for example, "SRS-101" in example 1) was permeated through the entire 2 nd sheet, the aromatic group-containing solvent overflowed without being absorbed into the sheet was wiped off. Next, a value obtained by subtracting the weight of the 2 nd sheet before the permeation of the solvent containing an aromatic group from the weight of the 2 nd sheet after the permeation of the solvent containing an aromatic group was obtained, and the oil absorption per 1m 2 of the 2 nd sheet was calculated.
[ Measurement of the arithmetic average roughness Ra of the 1 st sheet and the 2 nd sheet ]
The method for measuring the arithmetic average roughness Ra of the 1 st sheet (the arithmetic average roughness Ra corresponding to the surface on the opposite side of the PET sheet side of the 1 st layer) and the arithmetic average roughness Ra of the 2 nd sheet (the arithmetic average roughness Ra corresponding to the surface on the opposite side of the PET sheet side of the 2 nd layer) is as described above.
[ Evaluation of color development concentration ]
< Measurement of concentration (DA) of color Forming portion formed in sheet 2 >
The 1 st sheet and the 2 nd sheet produced in each of examples and comparative examples were used to evaluate the sheet set for pressure measurement. Specifically, the 1 st sheet and the 2 nd sheet cut to a size of 5cm×5cm are overlapped so that the surface of the 1 st layer of the 1 st sheet and the surface of the 2 nd layer of the 2 nd sheet are in contact, thereby obtaining a laminate. Next, the laminate was pressed under a pressure of 1.0MPa by a press (manufactured by DSF-C1-A, AIDA ENGINEERING, LTD.) to develop a color. After that, the 1 st sheet and the 2 nd sheet constituting the laminate were peeled off, and the Density (DA) of the color development part formed on the 2 nd sheet was measured from the support (PET sheet) surface side via the support by using a density meter RD-19 (manufactured by X-Rite Inc).
< Calculation of color development concentration ΔD1 >
In addition, an initial concentration (DB) of the unused 2 nd sheet was measured from the side of the support (PET sheet) surface with the support interposed therebetween by using a concentration meter RD-19 (manufactured by X-Rite Inc). Then, the initial density DB is subtracted from the density DA to obtain the color formation density Δd1, and the evaluation is performed according to the following evaluation standard. "B" is a range that can be allowed in practical use.
The results are shown in table 1.
< Evaluation criterion >
"A": Δd1 is 0.7 or more (color development is clearly observed).
"B": Δd1 is 0.2 or more and less than 0.7 (color development is slightly observed).
"C": Δd1 is less than 0.2 (little color development is observed).
[ Evaluation of storage Property ]
After the 1 st sheet was stored for 1 week at-30 ℃, the temperature was returned to the normal temperature, and the concentration (DA') of the color forming portion formed in the 2 nd sheet was measured by the same method as the above-described < measurement of the concentration (DA) of the color forming portion formed in the 2 nd sheet >.
In addition, an initial concentration (DB) of the unused 2 nd sheet was measured from the side of the support (PET sheet) surface with the support interposed therebetween by using a concentration meter RD-19 (manufactured by X-Rite Inc). Then, the initial density DB is subtracted from the density DA ', and the color development density Δd1' is obtained.
Next, the color development density Δd1' is subtracted from the color development density Δd1, and the color development density difference Δd2 before and after storage is obtained. Based on the obtained Δd2 value, evaluation was performed according to the following evaluation criteria. "B" is a range that can be allowed in practical use.
The results are shown in table 1.
< Evaluation criterion >
"A": Δd2 is 0.1 or less (no change is observed).
"B": Δd2 exceeds 0.1 and is 0.3 or less (slightly observed change).
"C": Δd2 exceeds 0.3 (a large change is observed).
[ Evaluation of image quality (resolution) ]
The surface of the 1 st layer of the unused 1 st sheet was observed by an optical microscope, and the average particle diameter of the microcapsules (microcapsule diameter D (μm)) was determined. The method for measuring the average particle diameter of the microcapsules is as described above.
Then, the surface of the 2 nd layer of the 2 nd sheet after color development was observed by an optical microscope, and the average dot diameter (color development dot diameter D' (μm)) of the color development dot was obtained. From the obtained values, a color point diameter D' (μm) with respect to the microcapsule diameter D (μm) was obtained, and evaluated according to the following evaluation criteria.
The specific measurement method of the color point diameter D' (μm) is as follows.
Color point diameter D' (μm): the image of the surface of the 2 nd layer of the 2 nd sheet after the color development was taken from the surface of the 2 nd layer was analyzed by an optical microscope (OLYMPUS BX60, size of field of view: 320 μm×450 μm), the long diameters of 30 color development points were measured in order from the largest color development point, and these were arithmetically averaged to obtain an average value. This operation was performed at 5 arbitrary sites (5 fields of view) in layer 2, the average of the averages obtained at the respective sites was obtained, and the obtained value was set as the average dot diameter (color dot diameter D' (μm)) of the color dots. The long diameter is the longest diameter when the color point is observed.
The results are shown in table 1.
< Evaluation criterion >
"A": D'/D is less than 50 (high image quality).
"B": D'/D is 50 or more and less than 300 (medium image quality).
"C": D'/D is 300 or more (low image quality).
Table 1 is shown below.
In table 1, in the column "type" of the "solvent containing an aromatic group", the numerical values in brackets simultaneously described in the solvent type indicate the mixing ratio (mass basis). For example, in the case of example 4, it is shown that 4-isopropylbiphenyl and 4,4' -diisopropylbiphenyl are contained in a mass ratio of 50/50 as the solvent containing an aromatic group.
In Table 1, "SRS-101" in the column "solvent containing aromatic group" is a mixture of 1, 2-dimethyl-4- (1-phenylethyl) benzene, 1, 3-dimethyl-4- (1-phenylethyl) benzene, 1, 4-dimethyl-2- (1-phenylethyl) benzene and 1- (ethylphenyl) -1-phenylethane (manufactured by Kagaku Jinzheng fine chemical Co., ltd.). Namely, 4 solvents containing 2 aromatic groups are contained in the molecule.
In Table 1, "Hysol 100" in the column of "solvent containing aromatic group" is a mixture of 1,2, 4-trimethylbenzene, 1,3, 5-trimethylbenzene, 1,2, 3-trimethylbenzene, cumene and xylene (manufactured by ENEOS Corporation). That is, 3 solvents containing 1 aromatic group are contained in the molecule.
In table 1, "sink-DCF" and "Orange-DCF" in the column of "developer" (manufactured by Hodogaya Chemical co., ltd.) and "Red500" and "Red520" (manufactured by YAMADA CHEMICAL co., ltd.) correspond to the developer containing an aromatic group.
In table 1, "content (%) of the solvent containing an aromatic group" means content (%) of the solvent containing an aromatic group with respect to the total mass of the solvent containing an aromatic group and the solvent containing an aliphatic structure.
In table 1, "presence or absence of a solvent having 2 aromatic groups in a molecule" column, "a" means that the solvent having an aromatic group contains a solvent having 2 aromatic groups in a molecule, and "B" means that the solvent having an aromatic group does not contain a solvent having 2 aromatic groups in a molecule.
In table 1, "content (%) of a solvent containing 2 aromatic groups in a molecule" refers to content (%) of a solvent containing 2 aromatic groups in a molecule with respect to the total mass of the solvent containing aromatic groups.
From the results shown in table 1, the sheet set for pressure measurement of examples is excellent in storage stability at low temperatures. Further, the color development density of the sheet set for pressure measurement of the example was found to be high.
Further, it was confirmed from a comparison of example 1 and example 2 that when the solvent containing an aromatic group contains a solvent containing 2 aromatic groups in the molecule, the storage stability at low temperature was more excellent and the color development concentration was also more excellent.
From the comparison of examples 1,5, 6 and 7, it was confirmed that when the content of the solvent containing 2 aromatic groups in the molecule was 50 mass% or more relative to the total mass of the solvent containing aromatic groups, the storage stability at low temperature was more excellent and the color development concentration was also more excellent.
From a comparison between example 1 and example 8, it was confirmed that when the mass per unit area (g/m 2) of the 1 st layer of the 1 st sheet (see column "solid content coating amount g/m 2" in table 1) was adjusted to 10.0g/m 2 or less, the image quality (resolution) of the color-formed portion formed in the 2 nd sheet was further excellent when the arithmetic average roughness Ra of the 1 st sheet was set to 3.0 to 7.0 μm.
From the comparison of examples 1, 9 and 10, it was confirmed that the quality (g/m 2) per unit area of the 2 nd layer of the 2 nd sheet (see column "solid content application amount g/m 2" in table 1) was adjusted to 3.5g/m 2 or more, and that the quality (resolution) of the image formed in the color-developed portion of the 2 nd sheet was further excellent when the oil absorption (g/m 2) of the aromatic group-containing solvent relative to the 2 nd sheet was set to 2.0 to 20.0g/m 2 or more.
Further, from the comparison between example 1 and example 11, it was confirmed that the color development concentration was more excellent when the content of the solvent containing 2 aromatic groups in the molecule was 75.0 mass% or more relative to the total mass of the solvent containing aromatic groups.
From the results of table 1, the sheet set for pressure measurement of the comparative example did not satisfy the desired requirements.
In addition, although the above-described embodiment using the pressure measurement sheet set including the 1 st sheet and the 2 nd sheet was shown, the pressure measurement sheets were produced by sequentially stacking the 2 nd layer and the 1 st layer on the support, and the same test as described above was performed, and the same results as those in each example were obtained. For example, the same results as in example 1 were obtained by preparing a pressure measurement sheet having a support, the 2 nd layer, and the 1 st layer in this order by disposing the 2 nd layer and the 1 st layer prepared in example 1 on a polyethylene terephthalate sheet, and performing the above-mentioned evaluation (color development density evaluation, storage property evaluation, and image quality (resolution) evaluation).
[ Example 12 ]
The dispersion set was spray-applied to a curved surface member, and the evaluation of storage stability and color development concentration was performed.
Specifically, the microcapsule liquid containing the color former prepared in example 1 was prepared as the 1 st dispersion liquid, and the dispersion liquid containing the color former prepared in example 1 was prepared as the 2 nd dispersion liquid.
< Evaluation of storage stability and evaluation of color formation concentration)
The 1 st dispersion was applied to a metal plate (concave mirror/convex mirror (r=100 mm) made of stainless steel (SUS 304)) as an object to be coated by a coater, and dried for 24 hours to form a1 st layer, and then the 2 nd dispersion was applied to the 1 st layer by a coater to form a 2 nd layer. The same metal plate was placed from above the coated face so as to cover the coating area, and pressurization based on a pressure of 10Mpa was performed by a press (product name: H1F35-1, manufactured by Komatsu ltd.) for 120 seconds. After the completion of the pressurization, the metal plate placed on the upper portion was removed, and the color development distribution in the application region were visually confirmed, and it was confirmed that the color development was performed at a sufficient density for visual observation and the color development distribution was visually confirmed as a sufficient color development density difference.
Then, after the 1 st dispersion was stored for 1 week at-30 ℃, the temperature was returned to the normal temperature, and the color of the coated area was developed by the pressure treatment using the metal plate in the same procedure as described above, and the color development and color development distribution of the coated area were visually confirmed. As a result, almost no change in color development was observed as compared with the case of not storing at low temperature.
[ Example 13 ]
Storage stability and color development concentration were evaluated in the same manner as in example 12 except that the dispersion containing the color developer prepared in example 1 was changed to a zinc 3, 5-bis (α -methylbenzyl) salicylate dispersion (SANKO co., ltd. Manufactured, LR-220, solid content concentration 41 mass%) so that the solid content concentration was 20 mass%, and the brush coater was changed to spray coating. As a result, it was confirmed that color development was sufficiently observed in a visually identifiable density, that color development distribution was visually identifiable in a sufficiently identifiable density difference, and that no color development change was substantially observed as compared with the case of not storing at a low temperature, in the same manner as in example 12.
[ Example 14 ]
The results of the evaluation of the color development density were confirmed in the same manner as in example 13 except that the order of application of the 1 st dispersion and the 2 nd dispersion was changed, and the color development was confirmed to be sufficiently intense for visual observation and the color development distribution was visually recognized with a sufficiently different color development density in the same manner as in example 13.
[ Example 15 ]
The results of the evaluation of the color development density were confirmed in the same manner as in example 13 except that the 1 st dispersion and the 2 nd dispersion were mixed in advance to prepare the 3 rd dispersion, and the 3 rd dispersion was used to apply the coating at the specific position, and the color development distribution was visually recognized at a sufficient density and with a sufficient color development density difference in the same manner as in example 13.
[ Comparative example 3]
Storage stability and color development concentration were evaluated in the same manner as in example 12 except that the 1 st dispersion was used as the microcapsule liquid containing the color former prepared in comparative example 1. As a result, it was confirmed that the color was developed at a sufficient density for visual observation and the color development distribution was visually recognized at a sufficient color development density difference, but the color development was insufficient as compared with the case where the film was not stored at a low temperature.
Symbol description
10-Sheet set for pressure measurement, 12-1 st support, 13-specific microcapsules, 14-1 st layer, 16-1 st sheet, 18-2 nd support, 20-2 nd layer, 22-2 nd sheet, 30-sheet for pressure measurement, 32-support.
Claims (17)
1. A sheet set for pressure measurement, comprising:
A1 st sheet having a1 st layer comprising microcapsules containing a solvent having a boiling point of 100 ℃ or higher and a color former; and
A2 nd sheet having a2 nd layer containing a color developer,
The solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups, the solvent containing aromatic groups contains a solvent containing 2 aromatic groups in the molecule, the content of the solvent containing 2 aromatic groups in the molecule is 50 mass% or more relative to the total mass of the solvent containing aromatic groups, and
The color former contains more than 2 kinds of color formers containing aromatic groups.
2. The sheet set for pressure measurement according to claim 1, wherein,
The solvent having a boiling point of 100 ℃ or higher contains 4 or more kinds of the aromatic group-containing solvents.
3. The sheet set for pressure measurement according to claim 1 or 2, wherein,
The solvent having a boiling point of 100 ℃ or higher further comprises a solvent having an aliphatic structure,
The content of the aromatic group-containing solvent is 50 to 90 mass% relative to the total mass of the aromatic group-containing solvent and the aliphatic structure-containing solvent.
4. The sheet set for pressure measurement according to claim 1 or 2, wherein,
The oil absorption of the aromatic group-containing solvent with respect to the 2 nd sheet was 2.0g/m 2～20.0g/m2.
5. The sheet set for pressure measurement according to claim 1 or 2, wherein,
The 1 st sheet has an arithmetic average roughness Ra of 3.0-7.0 μm.
6. The sheet set for pressure measurement according to claim 1 or 2, wherein,
The 2 nd sheet has an arithmetic average roughness Ra of 1.2 μm or less.
7. The sheet set for pressure measurement according to claim 1 or 2, wherein,
The 1 st sheet and the 2 nd sheet also have a support,
The support is a resin film.
8. A sheet for pressure measurement, comprising:
layer 1 comprising microcapsules encapsulating a solvent having a boiling point of 100 ℃ or higher and a color former; and
A layer 2 disposed on the layer 1 and containing a color-developer,
The solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups, the solvent containing aromatic groups contains a solvent containing 2 aromatic groups in the molecule, the content of the solvent containing 2 aromatic groups in the molecule is 50 mass% or more relative to the total mass of the solvent containing aromatic groups, and
The color former contains more than 2 kinds of color formers containing aromatic groups.
9. The sheet for pressure measurement according to claim 8, wherein,
The solvent having a boiling point of 100 ℃ or higher contains 4 or more kinds of the aromatic group-containing solvents.
10. The sheet for pressure measurement according to claim 8 or 9, wherein,
The solvent having a boiling point of 100 ℃ or higher further comprises a solvent having an aliphatic structure,
The content of the aromatic group-containing solvent is 50 to 90 mass% relative to the total mass of the aromatic group-containing solvent and the aliphatic structure-containing solvent.
11. The sheet for pressure measurement according to claim 8 or 9, wherein,
The oil absorption of the aromatic group-containing solvent with respect to the layer 2 was 2.0g/m 2～20.0g/m2.
12. The sheet for pressure measurement according to claim 8 or 9, further comprising a support,
The support is a resin film.
13. A method for producing the sheet set for pressure measurement according to any one of claims 1 to 7, comprising the steps of:
A layer 1 is formed by applying a layer 1-forming composition containing microcapsules containing a solvent having a boiling point of 100 ℃ or higher and a color former, and drying the obtained coating film.
14. A method for producing the sheet for pressure measurement according to any one of claims 8 to 12, comprising the steps of:
A layer 1 is formed by applying a layer 1-forming composition containing microcapsules containing a solvent having a boiling point of 100 ℃ or higher and a color former, and drying the obtained coating film.
15. A dispersion for measuring pressure and forming a layer to be used in combination with a layer containing a color former, comprising microcapsules containing a solvent having a boiling point of 100 ℃ or higher and a color former,
The solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups, the solvent containing aromatic groups contains a solvent containing 2 aromatic groups in the molecule, the content of the solvent containing 2 aromatic groups in the molecule is 50 mass% or more relative to the total mass of the solvent containing aromatic groups, and
The color former contains more than 2 kinds of color formers containing aromatic groups.
16. The dispersion according to claim 15, wherein,
The solvent having a boiling point of 100 ℃ or higher contains 4 or more kinds of the aromatic group-containing solvents.
17. A microcapsule comprises solvent with boiling point of 100deg.C or above and color former,
The solvent having a boiling point of 100 ℃ or higher contains 2 or more solvents containing aromatic groups, the solvent containing aromatic groups contains a solvent containing 2 aromatic groups in the molecule, the content of the solvent containing 2 aromatic groups in the molecule is 50 mass% or more relative to the total mass of the solvent containing aromatic groups, and
The color former contains more than 2 kinds of color formers containing aromatic groups.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2019-225447 | 2019-12-13 | ||
| JP2019225447 | 2019-12-13 | ||
| PCT/JP2020/043972 WO2021117494A1 (en) | 2019-12-13 | 2020-11-26 | Pressure measurement sheet set and production method therefor, pressure measurement sheet and production method therefor, dispersion liquid, and microcapsules |
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| Publication Number | Publication Date |
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| CN114902026A CN114902026A (en) | 2022-08-12 |
| CN114902026B true CN114902026B (en) | 2024-05-07 |
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| CN202080085210.9A Active CN114902026B (en) | 2019-12-13 | 2020-11-26 | Sheet set for pressure measurement and method for producing same, sheet for pressure measurement and method for producing same, dispersion liquid, and microcapsule |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP7163514B2 (en) |
| CN (1) | CN114902026B (en) |
| TW (1) | TW202124137A (en) |
| WO (1) | WO2021117494A1 (en) |
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| JP2607924B2 (en) | 1988-08-09 | 1997-05-07 | 日本石油化学株式会社 | Pressure-sensitive copying material |
| JP4986750B2 (en) | 2007-07-11 | 2012-07-25 | 富士フイルム株式会社 | Material for pressure measurement |
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2020
- 2020-11-26 WO PCT/JP2020/043972 patent/WO2021117494A1/en active Application Filing
- 2020-11-26 JP JP2021563843A patent/JP7163514B2/en active Active
- 2020-11-26 CN CN202080085210.9A patent/CN114902026B/en active Active
- 2020-12-10 TW TW109143551A patent/TW202124137A/en unknown
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| JPH0247085A (en) * | 1988-08-09 | 1990-02-16 | Nippon Petrochem Co Ltd | Pressure sensitive copy material |
| EP0596510A1 (en) * | 1992-11-05 | 1994-05-11 | Fuji Photo Film Co., Ltd. | Process for producing microcapsules |
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Also Published As
| Publication number | Publication date |
|---|---|
| TW202124137A (en) | 2021-07-01 |
| JP7163514B2 (en) | 2022-10-31 |
| CN114902026A (en) | 2022-08-12 |
| WO2021117494A1 (en) | 2021-06-17 |
| JPWO2021117494A1 (en) | 2021-06-17 |
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