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    • 1. 发明授权
    • Process for the synthesis of diethyl ethylphosphonate
    • 合成乙基膦酸二乙酯的方法
    • US5473093A
    • 1995-12-05
    • US370940
    • 1995-01-10
    • Fred Jaffe
    • Fred Jaffe
    • C07F9/40
    • C07F9/4075
    • Diethyl ethylphosphonate is formed by the catalytic rearrangement of triethyl phosphite in a reaction medium at elevated temperature, preferably using an ethyl iodide as the rearrangement catalyst, employing a heel of diethyl ethylphosphonate in the reaction medium when the reaction is begun with maintaining of the reaction medium at a temperature above the boiling point of the triethyl phosphite (for example, a temperature of from about 175.degree. C. to about 185.degree. C.) and addition of the triethyl phosphite to the reaction medium at a rate slow enough to maintain that temperature.
    • 乙基膦酸二乙酯是通过在升高的温度下在反应介质中催化重排亚磷酸三乙酯形成的,优选使用乙基碘作为重排催化剂,当反应开始时,保持反应介质,在反应介质中使用二乙基膦酸二乙酯的脚跟 在高于亚磷酸三乙酯的沸点(例如约175℃至约185℃的温度)的温度下加入亚磷酸三乙酯至足以保持该温度的速率的反应介质中 。
    • 3. 发明授权
    • Polyurethane foam having a flame retardant oligomeric phosphate ester
    • 具有阻燃低聚磷酸酯的聚氨酯泡沫
    • US4458035A
    • 1984-07-03
    • US440788
    • 1982-11-12
    • Thomas A. HardyFred Jaffe
    • Thomas A. HardyFred Jaffe
    • C07F9/09C08G79/04C08J9/00C08G18/14
    • C08J9/0038C07F9/093C08G79/04C08J2375/04
    • Flame retardant oligomeric phosphate ester compositions having the structural formula: ##STR1## are prepared, wherein R is C.sub.1 -C.sub.10 alkyl or haloalkyl, R.sup.1 and R.sup.2 can be the same or different and are hydrogen, C.sub.1 -C.sub.10 alkyl or haloalkyl and n is an integer from zero to about 10.The method of preparing the compositions comprises reacting P.sub.2 O.sub.5 with a trialkyl or tris(haloalkyl)phosphate in the presence of about 0.01% to about 5% of a phosphite at a temperature from about 0.degree.-200.degree. C. A polyphosphate ester having P--O--P bonds is formed which is then reacted with an epoxide to yield the oligomeric phosphate ester flame retardant compositions.Alternatively, a method of preparing similar compositions comprises reacting P.sub.2 O.sub.5 with a trialkyl or tris (haloalkyl)phosphite at a temperature from about 0.degree. C. to about 200.degree. C. A mixed polyphosphate-polyphosphite ester having P--O--P bonds is formed which is then oxidized to yield a polyphosphate having P--O--P bonds; which is then reacted with an epoxide to yield the oligomeric phosphate ester flame retardant compositions.
    • 制备具有以下结构式的阻燃低聚磷酸酯组合物:其中R为C1-C10烷基或卤代烷基,R1和R2可以相同或不同,为氢,C1-C10烷基或卤代烷基,n为 制备组合物的方法包括在大约0.01%至大约5%的亚磷酸盐的存在下,在约0℃-200℃的温度下使P 2 O 5与三烷基或三(卤代烷基)磷酸酯反应 形成具有POP键的聚磷酸酯,然后与环氧化物反应,得到低聚磷酸酯阻燃剂组合物。 或者,制备相似组合物的方法包括在约0℃至约200℃的温度下使P2O5与三烷基或三(卤代烷基)亚磷酸酯反应。形成具有POP键的混合多磷酸酯 - 多亚磷酸酯,然后氧化 产生具有POP键的多磷酸盐; 然后将其与环氧化物反应以产生低聚磷酸酯阻燃剂组合物。
    • 9. 发明授权
    • Synthesis of a hydrocarbylvinylphosphonic acid hydrocarbyl ester
    • 烃基乙烯基膦酸烃基酯的合成
    • US06429329B1
    • 2002-08-06
    • US08711135
    • 1996-09-09
    • Alan M. AaronsonJohn TomkoJeffrey E. TelschowJohannes Hermanus BoeleeFred Jaffe
    • Alan M. AaronsonJohn TomkoJeffrey E. TelschowJohannes Hermanus BoeleeFred Jaffe
    • C07F940
    • C07F9/4015C07F9/4006
    • A process for the synthesis of a hydrocarbylvinyl-1-phosphonic acid hydrocarbyl ester, such as a 1-phenylvinylphosphonic acid dialkyl ester, which utilizes: (a) the base catalyzed addition (preferably using a nonnucleophilic strong organic base) of a hydrocarbyl phosphite, such as a dialkyl phosphite containing no more than about eight carbon atoms in either of its alkyl groups, to an aldehyde or methyl ketone, such as a phenyl ketone, as exemplified by acetophenone, to form a hydrocarbyl 1-hydroxy-1-hydrocarbylphosphonate, such as a dialkyl 1-hydroxy-1-phenylalkylphosphonate compound; (b) the acid-catalyzed esterification (preferably acetylation) of the compound from (a) with an acid anhydride to form an acylated intermediate; and (c) the removal of carboxylic acid (preferably at a temperature of from about 50° C. to about 215° C. under reduced or atmospheric pressure) from the intermediate from (b) to form the desired hydrocarbylvinylphosphonic acid hydrocarbyl ester, such as a 1-phenylvinylphosphonic acid dialkyl ester.
    • 用于合成烃基乙烯基-1-膦酸烃基酯的方法,例如1-苯基乙烯基膦酸二烷基酯,其利用:(a)碱式催化加成(优选使用非亲核强有机碱)的亚磷酸烃基酯, 例如其烷基中含有不超过约8个碳原子的亚磷酸二烷基酯,如苯乙酮等醛或甲基酮,如苯乙酮所示,形成1-羟基-1-烃基膦酸烃基, 例如1-羟基-1-苯基烷基膦酸二烷基酯化合物; (b)来自(a)的化合物与酸酐进行酸催化酯化(优选乙酰化)以形成酰化中间体; 和(c)从(b)的中间体除去羧酸(优选在减压或大气压下在约50℃至约215℃的温度下)以形成所需的烃基乙烯基膦酸烃基酯, 作为1-苯基乙烯基膦酸二烷基酯。
    • 10. 发明授权
    • Method of preparing oligomeric phosphate esters
    • 制备低聚磷酸酯的方法
    • US4382042A
    • 1983-05-03
    • US318288
    • 1981-11-04
    • Thomas A. HardyFred Jaffe
    • Thomas A. HardyFred Jaffe
    • C07F9/09C08G79/04C08J9/00
    • C08J9/0038C07F9/093C08G79/04C08J2375/04
    • Flame retardant oligomeric phosphate ester compositions having the structural formula: ##STR1## are prepared, wherein R is C.sub.1 -C.sub.10 alkyl or haloalkyl, R.sup.1 and R.sup.2 can be the same or different and are hydrogen, C.sub.1 -C.sub.10 alkyl or haloalkyl and n is an integer from zero to about 10.The method of preparing the compositions comprises reacting P.sub.2 O.sub.5 with a trialkyl or tris(haloalkyl)phosphate in the presence of about 0.01% to about 5% of a phosphite at a temperature from about 0.degree.-200.degree. C. A polyphosphate ester having P--O--P bonds is formed which is then reacted with an epoxide to yield the oligomeric phosphate ester flame retardant compositions.Alternatively, a method of preparing similar compositions comprises reacting P.sub.2 O.sub.5 with a trialkyl or tris(haloalkyl)phosphite at a temperature from about 0.degree. C. to about 200.degree. C. A mixed polyphosphate-polyphosphite ester having P--O--P bonds is formed which is then oxidized to yield a polyphosphate having P--O--P bonds; which is then reacted with an epoxide to yield the oligomeric phosphate ester flame retardant compositions.
    • 制备具有以下结构式的阻燃低聚磷酸酯组合物:其中R为C1-C10烷基或卤代烷基,R1和R2可以相同或不同,为氢,C1-C10烷基或卤代烷基,n为 制备组合物的方法包括在大约0.01%至大约5%的亚磷酸盐的存在下,在约0℃-200℃的温度下使P 2 O 5与三烷基或三(卤代烷基)磷酸酯反应 形成具有POP键的聚磷酸酯,然后与环氧化物反应,得到低聚磷酸酯阻燃剂组合物。 或者,制备相似组合物的方法包括在约0℃至约200℃的温度下使P2O5与三烷基或三(卤代烷基)亚磷酸酯反应。形成具有POP键的混合多磷酸酯 - 多亚磷酸酯,然后氧化 产生具有POP键的多磷酸盐; 然后将其与环氧化物反应以产生低聚磷酸酯阻燃剂组合物。