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    • 4. 发明专利
    • Process for preparing glycidyl acrylate or glycidyl methacrylate
    • DE3126943A1
    • 1982-03-25
    • DE3126943
    • 1981-07-08
    • MITSUBISHI GAS CHEMICAL CO
    • TAKASHINA NAOMITSUSHINKAWA SHIGERUIWASAKI NAOKIFUJITA ROKUROTAKAOKA TAKEAKI
    • C07D301/30C07D303/16
    • An improved process for preparing glycidyl acrylate or glycidyl methacrylate is indicated, in which process acrylic acid or methacrylic acid is neutralised with an alkali metal carbonate and/or an alkali metal bicarbonate, which is suspended in an excess of an epihalohydrin, with the formation of an alkali metal acrylate or alkali metal methacrylate, the water which is formed in the neutralisation reaction is subsequently virtually removed from the reaction system as an azeotrope with the epihalohydrin, and subsequently a catalyst is added to the reaction system and the alkali metal acrylate or alkali metal methacrylate is esterified with the epihalohydrin, with 1) the neutralisation reaction being carried out at a temperature not exceeding 108 DEG C and with the gradual addition of acrylic acid or methacrylic acid to the suspension of the alkali metal carbonate and/or alkali metal bicarbonate in the epihalohydrin, and the quantity of the alkali metal carbonate and/or the alkali metal bicarbonate being at least about 1.1 equivalents per equivalent of the acrylic acid or methacrylic acid, 2) the neutralisation reaction and the esterification reaction being carried out while air is being blown into the reaction system, and 3) the reaction mixture being mixed with water after the esterification, the organic layer being separated off from the aqueous layer and the organic layer then being subjected to distillation.
    • 6. 发明专利
    • METHACRYLIC RESIN HAVING RESISTANCE TO THERMAL DECOMPOSITION AND ITS PRODUCTION
    • JPH07206906A
    • 1995-08-08
    • JP59094
    • 1994-01-07
    • MITSUBISHI GAS CHEMICAL CO
    • KUWABARA SHOJIROFUJITA ROKUROKUROKAWA MASAHIRO
    • C08F2/00C08F2/06C08F6/00C08F6/06C08F20/14
    • PURPOSE:To obtain the subject resin having a thermal decomposition resistance, by continuous polymerization of a methyl methacrylate solution in specific concentrations of a radical polymerization initiator and a chain transfer agent under a specific condition in complete mixing vessels of two steps connected in a series and in a plug flow type reactor. CONSTITUTION:By using complete mixing vessels of two-step connected in a series and a plug flow type reactor, methyl methacrylate alone or a composition containing 71-95wt.% of a monomer mixture composed of 75wt.% or more of methyl methacrylate and 25wt.% or less of 1-3C alkyl acrylates, with 29-5wt.% of a solvent is adjusted to have a polymerization initiator concentration of 1.0X10 -1.6 mole % and a chain transfer agent concentration of 1X10 -1.0 mole %, and continuously polymerized at a polymerization temperature of 100-170 deg.C in every vessel of the process, with an average retention time in complete mixing vessels set at 5-7000 fold of a half life of the polymerization initiator and with a flow through time in the reactors set at 5-50 fold as above to obtain the objective resin having 5% or less of a thermal decomposition rate DW, expressed by the formula before its history of a post treatment [gammaWi is a content (wt.%) of a polymer having a double bond in its chain end in i-th vessel; RAi is a concentration of acrylate in i-th vessel (mole %); DELTAMi is a consumed monomer concentration in i-th vessel].
    • 7. 发明专利
    • METHACRYLIC RESIN HAVING RESISTANCE TO THERMAL DECOMPOSITION AND ITS PRODUCTION
    • JPH07206905A
    • 1995-08-08
    • JP58994
    • 1994-01-07
    • MITSUBISHI GAS CHEMICAL CO
    • KUWABARA SHOJIROFUJITA ROKUROKUROKAWA MASAHIRO
    • C08F2/00C08F2/06C08F6/00C08F6/06C08F20/14C08F220/10
    • PURPOSE:To obtain the subject resin having properties of less foaming, coloring and generating odor, by continuously polymerizing methyl methacrylate in a solution in the presence of a specific radical polymerization initiator and a specific chain transfer agent under specific conditions in respect to their concentrations in complete mixing vessels of two-step connected in a series. CONSTITUTION:By using complete mixing vessels of two-step connected in a series, methyl methacrylate alone or a composition containing 71-95wt.% of a monomer mixture consisting of 75wt.% or more of methyl methacrylate and 25wt.% or less of a 1-4C, alkylacrylate, and 29-5wt.% of a solvent, is adjusted to have a polymerization initiator concentration of 5.0X10 -1.2 mole % and a chain transfer agent concentration of 1.0X10 -1.0 mole %, and continuously polymerized at a polymerization temperature in first vessel of 100-170 deg.C, and in second vessel of 130-170 deg.C, with an average retention time set at 5-7000 fold of a half life of the polymerization initiator, by keeping a polymerization efficiency of 70-90%, to obtain a resin having 5% or less of a DW value before a history of after treatment, expressed by the formula [DW is decreasing weight ratio (wt.%); gammaWi is a content of a polymer having a double bond in its chain end in the i-th vessel (wt.%); RAi is a concentration of acrylate (mole %); and DELTAMi is a concentration of consumed monomer in the i-th vessel].