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    • 1. 发明授权
    • METHOD FOR PRODUCING PHOSPHATE POLYMER
    • 生产磷酸酯聚合物的方法
    • EP1923409B1
    • 2010-11-24
    • EP06797751.2
    • 2006-09-04
    • Kao Corporation
    • SHIMODA, Masaaki, c/o Kao CorporationKONO, Yoshinao, c/o Kao CorporationTANISHO, Yoshiaki, c/o Kao CorporationHAMAI, Toshimasa, c/o Kao CorporationHAMADA, Daisuke, c/o Kao CorporationMORII, YoshikazuNAKA, Yoshihito, c/o Kao Corporation
    • C08F290/06C04B22/16C04B24/26C04B28/02C08F2/04
    • C04B24/246C04B28/02C04B2103/32C04B2103/408C08F220/28C08F230/02C08F275/00C08F290/06C08F290/061C08K5/5317
    • Disclosed is a method for producing a phosphate polymer wherein a monomer 1 represented by the general formula (1) below, a monomer 2 represented by the general formula (2) below and a monomer 3 represented by the general formula (3) below are copolymerized in a polymerization solvent having a dissolved oxygen concentration at 25°C of 0.01-4.0 mg/kg at a pH of 7 or less. Also disclosed is a method for producing a phosphate polymer wherein the monomers 1, 2 and 3 are copolymerized in the presence of a phosphonic acid chelating agent at a pH of 7 or less. Further disclosed is a method for producing a phosphate polymer using a mixed solution containing the monomers 1, 2 and 3, wherein the mixed solution is obtained by mixing the monomers 1-3 at a temperature of 10-50°C and polymerization is started within 72 hours after mixing of the monomers 1-3, while keeping the temperature of the mixed solution within the range of 10-50°C until the polymerization is started. (In the formula (1), R1 and R2 respectively represent a hydrogen atom or a methyl group; and R3 represents a hydrogen atom or -COO(AO)nX wherein AO represents an oxyalkylene group having 2-4 carbon atoms or an oxystyrene group, n represents a number of 3-200 which is an average mole number of added AO, and X represents a hydrogen atom or an alkyl group having 1-18 carbon atoms.). (In the formula (2), R4 represents a hydrogen atom or a methyl group; R5 represents an alkylene group having 2-12 carbon atoms; m1 represents a number of 1-30; and M represents a hydrogen atom, an alkali metal or an alkaline earth metal.). (In the formula (3), R6 and R8 respectively represent a hydrogen atom or a methyl group; R7 and R9 respectively represent an alkylene group having 2-12 carbon atoms; m2 and m3 respectively represent a number of 1-30; and M represents a hydrogen atom, an alkali metal or an alkaline earth metal.)
    • 本发明公开了一种磷酸酯类聚合物的制造方法,其中,将下述通式(1)表示的单体1,下述通式(2)表示的单体2和下述通式(3)表示的单体3共聚 在25℃下溶解氧浓度为0.01〜4.0mg / kg,pH7以下的聚合溶剂中进行。 还公开了一种生产磷酸酯聚合物的方法,其中单体1,2和3在膦酸螯合剂存在下在7或更低的pH下共聚合。 还公开了使用含有单体1,2和3的混合溶液制备磷酸酯聚合物的方法,其中混合溶液通过在10-50℃的温度下混合单体1-3而获得,并且聚合在 混合单体1-3后72小时,同时保持混合溶液的温度在10-50℃的范围内直到聚合开始。 (式(1)中,R 1和R 2分别表示氢原子或甲基; R 3表示氢原子或-COO(AO)nX,其中AO表示具有2-4个碳原子的氧化烯基或氧基苯乙烯基 n表示加成AO的平均摩尔数的3-200的数,X表示氢原子或具有1-18个碳原子的烷基)。 (式(2)中,R 4表示氢原子或甲基; R 5表示具有2-12个碳原子的亚烷基; m1表示1-30的数;并且M表示氢原子,碱金属或 一种碱土金属)。 (式(3)中,R6和R8分别表示氢原子或甲基; R7和R9分别表示具有2-12个碳原子的亚烷基; m2和m3分别表示1-30的数; M 代表氢原子,碱金属或碱土金属。)
    • 2. 发明公开
    • METHOD FOR PRODUCING PHOSPHATE POLYMER
    • VERFAHREN ZUR HERSTELLUNG VON PHOSPHATPOLYMER
    • EP1923409A1
    • 2008-05-21
    • EP06797751.2
    • 2006-09-04
    • Kao Corporation
    • SHIMODA, Masaaki, c/o Kao CorporationKONO, Yoshinao, c/o Kao CorporationTANISHO, Yoshiaki, c/o Kao CorporationHAMAI, Toshimasa, c/o Kao CorporationHAMADA, Daisuke, c/o Kao CorporationMORII, YoshikazuNAKA, Yoshihito, c/o Kao Corporation
    • C08F290/06C04B22/16C04B24/26C04B28/02C08F2/04
    • C04B24/246C04B28/02C04B2103/32C04B2103/408C08F220/28C08F230/02C08F275/00C08F290/06C08F290/061C08K5/5317
    • The present invention relates to a method for producing a phosphoric acid ester-based polymer, including copolymerizing a monomer 1 represented by the following formula (1), a monomer 2 represented by the following formula (2), and a monomer 3 represented by the following formula (3), at pH 7 or lower, in the present of a polymerization solvent having a dissolved oxygen concentration at 25°C of 0.01 to 4.0 mg/kg. The invention also relates to a method for producing a phosphoric acid ester-based polymer, including copolymerizing the monomers 1, 2 and 3 at pH 7 or lower, in the presence of a phosphonic acid-based chelating agent. The invention also relates to a method for producing a phosphoric acid ester-based polymer from a mixed solution containing the monomer 1, 2 and 3, including obtaining a mixed solution by mixing the monomers 1 to 3 at a temperature of 10 to 50°C, initiating a polymerization within 72 hours after the mixing of the monomers 1 to 3, and maintaining the temperature of the mixed solution in the range of 10 to 50°C until the polymerization is initiated:

      wherein R 1 and R 2 each represent a hydrogen atom or a methyl group; and R 3 represents a hydrogen atom or -COO(AO) n X [wherein AO represents an oxyalkylene group or oxystyrene group having 2 to 4 carbon atoms; n represents an average number of added moles of AO, and is a number from 3 to 200; and X represents a hydrogen atom or an alkyl group having 1 to 18 carbon atoms],

      wherein R 4 represents a hydrogen atom or a methyl group; R 5 represents an alkylene group having 2 to 12 carbon atoms; m1 represents a number from 1 to 30; and M represents a hydrogen atom, an alkali metal or an alkaline earth metal, and

      wherein R 6 and R 8 each represent a hydrogen atom or a methyl group; R 7 and R 9 each represent an alkylene group having 2 to 12 carbon atoms; m2 and m3 each represent a number from 1 to 30; and M represents a hydrogen atom, an alkali metal or an alkaline earth metal.
    • 本发明涉及一种磷酸酯系聚合物的制造方法,其包括使下述式(1)表示的单体1,下述式(2)所示的单体2和由下式(2)表示的单体3 在25℃下的溶解氧浓度为0.01〜4.0mg / kg的聚合溶剂中,在pH7以下的下述式(3)表示。 本发明还涉及磷酸酯系聚合物的制造方法,其包括在pH7以下的单体1,2和3在膦酸系螯合剂的存在下共聚。 本发明还涉及从含有单体1,2和3的混合溶液中制备磷酸酯系聚合物的方法,包括通过在10〜50℃的温度下混合单体1〜3得到混合溶液 在混合单体1至3之后的72小时内开始聚合,并将混合溶液的温度保持在10至50℃的范围内,直至开始聚合:其中R 1和R 2各自表示氢 原子或甲基; 和R 3表示氢原子或-COO(AO)n X [其中AO表示氧化烯基或具有2〜4个碳原子的氧苯乙烯基; n表示AO的平均加成摩尔数,为3〜200的数; X表示氢原子或碳原子数1〜18的烷基],其中,R 4表示氢原子或甲基。 R 5表示碳原子数2〜12的亚烷基。 m1表示1〜30的数; M表示氢原子,碱金属或碱土金属,R 6和R 8各自表示氢原子或甲基, R 7和R 9各自表示碳原子数2〜12的亚烷基。 m2和m3每个代表从1到30的数字; M表示氢原子,碱金属或碱土金属。