Thermal recording medium
A thermal recording medium and recording layer technology, applied in temperature recording method, copying/marking method, printing, etc., can solve the problems of being unsuitable for practical application and expensive resin
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[0052] Containing R represented by formula (I) now f The method for the preparation of diols is described more specifically.
[0053] First, in an equivalent ratio, in a solvent-free manner or in an organic solvent, with or without the presence of a common polymerization catalyst for polyurethane (for example, organometallic compounds, tertiary amines, etc.), at 0-150 ° C, preferably 20 At -90°C, react a fluorine-containing compound with an active hydrogen-containing group and a diisocyanate, so that the resulting reaction product contains one free isocyanate group (NCO / OH≈2) in its molecule.
[0054] At 50°C or lower than 50°C, preferably at 40°C or lower than 40°C, more preferably at 30°C or lower than 30°C, the above-mentioned fluorine-containing compound with one free isocyanate group is added dropwise to Among the dialkanolamines mentioned above.
[0055] Under these conditions, the isocyanate group reacts selectively with the amino group [Ann.Chem., 562, 205 (1949)] be...
reference example 1
[0112] Reference Example 1 [Synthesis of Fluorinated Diol (1-A)]
[0113] In a reaction vessel equipped with a stirrer, a thermometer, a nitrogen inlet tube and a reflux condenser, flush with nitrogen, dissolve toluene-2,4-diisocyanate (17.4 parts) in ethyl acetate (50 parts), and dissolve the resulting solution It was heated to 60°C, at which temperature 2-(perfluorooctyl)ethanol (46.4 parts) powder was gradually added with sufficient stirring. After the addition, isophorone diisocyanate and 2-(perfluorooctyl)ethanol were reacted at 80° C. for 3 hours to form a perfluoroalkyl-containing one-terminal isocyanate (A).
[0114] Next, under stirring, diethanolamine (10.5 parts) was mixed into ethyl acetate (10 parts) at a temperature lower than 10° C., and the reaction mixture containing compound (A) was added dropwise to the resulting solution, and each addition was observed. Exothermic reaction that occurs when the reaction mixture contains compound (A). Therefore, the dropwis...
reference example 2
[0117] Reference Example 2 [Synthesis of Fluorinated Diol (I-B)]
[0118] In addition to replacing toluene-2,4-diisocyanate and 2-(perfluorooctyl)ethanol with isophorone diisocyanate and 2-(perfluoro-7-methyloctyl)ethanol respectively in the same equivalent, Others In the same manner as in Reference Example 1, a fluorine-containing diol white powder having the following structural formula (I-B) was obtained. (Yield: 95%, melting point: 132°C, hydroxyl number: 138).
[0119]
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