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    Process for preparing liquid triaryl thiophosphate mixtures
    2.
    发明授权
    Process for preparing liquid triaryl thiophosphate mixtures 失效
    制备液体三芳基硫代磷酸盐混合物的方法

    公开(公告)号：US4724265A

    公开(公告)日：1988-02-09

    申请号：US863656

    申请日：1986-05-15

    Applicant: Fred Jaffe ,  Alan M. Aaronson

    Inventor： Fred Jaffe ,  Alan M. Aaronson

    IPC: C07F9/145 ,  C07F9/18 ,  C08K5/51 ,  C07F9/165

    CPC classification number: C07F9/145 ,  C07F9/18

    Abstract: Liquid mixed triaryl thiophosphate mixtures can be prepared by forming a mixture of phenol and substituted phenols, forming a phosphite from that mixture and sulfurizing the phosphite, washing the thiophosphate with aqueous base, and drying the so washed thiophosphate under mild conditions. The products are liquid while containing at least 25 percent symmetrical triaryl thiophosphate. Colorless and odorless products are prepared.

    Abstract translation: 液体混合的三芳基硫代磷酸盐混合物可以通过形成苯酚和取代的酚的混合物，从该混合物形成亚磷酸盐并硫化亚磷酸盐，用碱水溶液洗涤硫代磷酸盐，并在温和条件下干燥洗涤过的硫代磷酸盐。 该产品是液体的，同时含有至少25％的对称三芳基硫代磷酸酯。 无色无味的产品已经准备好了。

    Process for producing diethyl phosphite
    3.
    发明授权
    Process for producing diethyl phosphite 失效
    生产亚磷酸二乙酯的方法

    公开(公告)号：US4342709A

    公开(公告)日：1982-08-03

    申请号：US214072

    申请日：1980-12-08

    Applicant: Fred Jaffe

    Inventor： Fred Jaffe

    IPC: C07F9/142 ,  C07F9/141

    CPC classification number: C07F9/142

    Abstract: A process of producing diethyl phosphite by reacting an excess of triethyl phosphite with phosphorous acid. The improved process results in a high quality diethyl phosphite product having low acidity that is suitable as an intermediate for most uses requiring a low acidity diethyl phosphite.

    Abstract translation: 通过使过量的亚磷酸三乙酯与亚磷酸反应来生产亚磷酸二乙酯的方法。 改进的方法产生具有低酸度的高质量亚磷酸二乙酯产物，其适合作为需要低酸性亚磷酸二乙酯的大多数用途的中间体。

    Process for the synthesis of diethyl ethylphosphonate
    4.
    发明授权
    Process for the synthesis of diethyl ethylphosphonate 失效
    合成乙基膦酸二乙酯的方法

    公开(公告)号：US5473093A

    公开(公告)日：1995-12-05

    申请号：US370940

    申请日：1995-01-10

    Applicant: Fred Jaffe

    Inventor： Fred Jaffe

    IPC: C07F9/40

    CPC classification number: C07F9/4075

    Abstract: 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.

    Abstract translation: 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 。

    Polyurethane foam having a flame retardant oligomeric phosphate ester
    6.
    发明授权
    Polyurethane foam having a flame retardant oligomeric phosphate ester 失效
    具有阻燃低聚磷酸酯的聚氨酯泡沫

    公开(公告)号：US4458035A

    公开(公告)日：1984-07-03

    申请号：US440788

    申请日：1982-11-12

    Applicant: Thomas A. Hardy ,  Fred Jaffe

    Inventor： Thomas A. Hardy ,  Fred Jaffe

    IPC: C07F9/09 ,  C08G79/04 ,  C08J9/00 ,  C08G18/14

    CPC classification number: C08J9/0038 ,  C07F9/093 ,  C08G79/04 ,  C08J2375/04

    Abstract: 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.

    Abstract translation: 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。

    Method of preparing stable condensation products using a Lewis acid catalyst and products thereof
    8.
    发明授权
    Method of preparing stable condensation products using a Lewis acid catalyst and products thereof 失效
    使用路易斯酸催化剂及其产物制备稳定的缩合产物的方法

    公开(公告)号：US4012463A

    公开(公告)日：1977-03-15

    申请号：US665840

    申请日：1976-03-11

    Applicant: Edward N. Walsh ,  Fred Jaffe ,  Milton L. Honig ,  Kyung S. Shim ,  Mervin E. Brokke

    Inventor： Edward N. Walsh ,  Fred Jaffe ,  Milton L. Honig ,  Kyung S. Shim ,  Mervin E. Brokke

    IPC: C08G65/26 ,  C08G79/04 ,  C07F9/08

    CPC classification number: C08G65/269 ,  C08G65/2639 ,  C08G65/2642 ,  C08G65/2645 ,  C08G65/2675 ,  C08G79/04

    Abstract: The neutralization of products which are phosphorus containing oligomers having ##STR1## linkages between phosphorus atoms and which are obtained by the self-condensation of .beta.-halo-alkyl esters of pentavalent phosphorus acids or by the condensation of these esters with an alkyl ester of a pentavalent phosphorus acid is accomplished by reaction with an alkylene oxide, either alone or in combination with water or an alcohol having the formula ROH where R is a C.sub.1 -C.sub.20 alkyl group, and is enhanced by heating the products with a Lewis acid to promote alcoholysis reactions between labile groups contained therein and structures formed by alkylene oxide neutralization of free acid groups. The stabilized product formed by this process gives a better cure when incorporated in a polyurethane foam.

    Abstract translation: 在磷原子之间具有键的含磷低聚物的产物的中和，其通过五价磷酸的β-卤代 - 烷基酯的自缩合或通过这些酯与烷基酯的缩合获得 五价磷酸通过与环氧烷单独或与水或具有式ROH的醇（其中R是C 1 -C 20烷基）组合进行反应来实现，并且通过用路易斯酸加热产物以促进醇解 其中所含的不稳定基团与游离酸基团的氧化烯中和形成的结构之间的反应。 当通过该方法形成的稳定化产物在掺入聚氨酯泡沫中时会得到更好的固化。

    Synthesis of a hydrocarbylvinylphosphonic acid hydrocarbyl ester
    9.
    发明授权
    Synthesis of a hydrocarbylvinylphosphonic acid hydrocarbyl ester 失效
    烃基乙烯基膦酸烃基酯的合成

    公开(公告)号：US06429329B1

    公开(公告)日：2002-08-06

    申请号：US08711135

    申请日：1996-09-09

    Applicant: Alan M. Aaronson ,  John Tomko ,  Jeffrey E. Telschow ,  Johannes Hermanus Boelee ,  Fred Jaffe

    Inventor： Alan M. Aaronson ,  John Tomko ,  Jeffrey E. Telschow ,  Johannes Hermanus Boelee ,  Fred Jaffe

    IPC: C07F940

    CPC classification number: C07F9/4015 ,  C07F9/4006

    Abstract: 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.

    Abstract translation: 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。

    Method of preparing oligomeric phosphate esters
    10.
    发明授权
    Method of preparing oligomeric phosphate esters 失效
    制备低聚磷酸酯的方法

    公开(公告)号：US4382042A

    公开(公告)日：1983-05-03

    申请号：US318288

    申请日：1981-11-04

    Applicant: Thomas A. Hardy ,  Fred Jaffe

    Inventor： Thomas A. Hardy ,  Fred Jaffe

    IPC: C07F9/09 ,  C08G79/04 ,  C08J9/00

    CPC classification number: C08J9/0038 ,  C07F9/093 ,  C08G79/04 ,  C08J2375/04

    Abstract: 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.

    Abstract translation: 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。

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