公开(公告)号：US4886895A

公开(公告)日：1989-12-12

申请号：US306113

申请日：1989-02-06

申请人： Thomas A. Hardy ,  Edward N. Walsh

发明人： Thomas A. Hardy ,  Edward N. Walsh

IPC分类号： C07F9/09 ,  C07F9/40 ,  C08K5/521 ,  C08K5/5333 ,  D06M13/292

CPC分类号： D06M13/292 ,  C07F9/091 ,  C07F9/093 ,  C07F9/4006 ,  C08K5/521 ,  C08K5/5333 ,  C23F11/1673

摘要： There are disclosed multiphosphorus-containing compounds comprising phosphonate-containing or phosphate-containing phosphate esters. The compounds can be prepared by: (a) reacting a phosphonate-containing or phosphate-containing alcohol with phosphorus pentoxide following by reaction with an epoxide, (b) reacting a phosphonate-containing or phosphate-containing alcohol with a phosphorus oxyhalide, hydrolyzing any phosphorus halogen bonds and then reacting the resulting phosphoric acid derivative with an epoxide, (c) transesterifying a phosphonate-containing or phosphate-containing alcohol with a dialkyl phosphite, oxidizing the resulting compound to yield a phosphoric acid derivative and reacting the phosphoric acid derivative with an epoxide. The compounds are useful as flame retardant additives for polyurethanes and textiles.

摘要翻译： 公开了包含含膦酸酯或磷酸酯的磷酸酯的含有多磷的化合物。 化合物可以通过以下方法制备：（a）通过与环氧化物反应，使含膦酸酯或含磷酸酯的醇与五氧化二磷反应，（b）使含膦酸酯或含磷酸盐的醇与磷酰卤反应，将任何 磷卤素键，然后使所得磷酸衍生物与环氧化物反应，（c）将含膦酸酯或含磷酸酯的醇与亚磷酸二烷基酯酯交换，氧化所得化合物以产生磷酸衍生物，并使磷酸衍生物与 环氧化物。 该化合物可用作聚氨酯和纺织品的阻燃添加剂。

公开(公告)号：US4093651A

公开(公告)日：1978-06-06

申请号：US753119

申请日：1976-12-22

申请人： Milton L. Honig ,  Carl C. Greco ,  Edward N. Walsh

发明人： Milton L. Honig ,  Carl C. Greco ,  Edward N. Walsh

IPC分类号： C07C313/08 ,  C07C145/00

CPC分类号： C07C313/08

摘要： A method for improving the yield of perchloromethyl mercaptan by including in the reaction mixture phosphonates or phosphonites, in amounts effective to suppress the formation of undesirable byproducts, such as carbon tetrachloride and sulfur monochloride.

摘要翻译： 通过在反应混合物中包含膦酸盐或亚膦酸盐来提高全氯甲基硫醇的产率的方法，其用量有效地抑制不希望的副产物如四氯化碳和一氯化硫的形成。

公开(公告)号：US4044074A

公开(公告)日：1977-08-23

申请号：US669004

申请日：1976-03-22

申请人： Edward N. Walsh ,  Milton L. Honig

发明人： Edward N. Walsh ,  Milton L. Honig

IPC分类号： C07F9/40 ,  C08G63/692 ,  C08G79/04 ,  C08K5/51 ,  C08L101/00

CPC分类号： C08L101/00 ,  C07F9/4075 ,  C08G63/6924 ,  C08G79/04 ,  C08K5/51

摘要： Flame retardant polycarboxy alkyl and aryl phosphonates having the structural formula: ##STR1## ARE PREPARED, WHEREIN R is hydrocarbyl consisting of hydrogen and carbon and substituted hydrocarbyl including C.sub.2 -C.sub.10 alkylene, arylene, C.sub.7 -C.sub.20 alkylene substituted arylene, C.sub.3 -C.sub.20 cycloalkylene, C.sub.4 -C.sub.20 vinylene and derivatives of the foregoing containing non-labile pendant halogens, C.sub.1 -C.sub.6 alkyls, C.sub.1 -C.sub.6 haloalkyls, vinyls, ethers or C.sub.1 -C.sub.6 alkyl alcohol functions. R.sup.1 is hydrocarbyl consisting of hydrogen and carbon and substituted hydrocarbyl including C.sub.1 -C.sub.10 alkyl, aryl, C.sub.7 -C.sub.20 alkyl substituted aryl, C.sub.2 -C.sub.10 alkenyl, phenoxy, C.sub.1 -C.sub.10 alkoxy, aryloxy, or C.sub.3 -C.sub.20 cycloalkyl, and derivatives thereof containing non-liabile pendant halogens, C.sub.1 -C.sub.6 alkyls, C.sub.1 -C.sub.6 haloalkyls, vinyls, ethers, or C.sub.1 -C.sub.6 alkyl alcohol functions. R.sup.1 can also be: ##STR2## or OR.sup.4 H wherein R.sup.4 has the same definition as R, and R.sup.4 and R can be the same or different. R.sup.2, R.sup.3 and R.sup.5 are straight or branched C.sub.1 -C.sub.10 alkylene and can be the same or different. The integer represented by i is from about 2 to about 20 and the integers represented by m and n are different and are 0 or 1.The monomers are prepared by catalyzed transalkylation and the polymers are prepared by polycondensation of the monomers with diols or by polymeric transalkylation.

摘要翻译： 具有以下结构式的阻燃聚羧基烷基和芳基膦酸酯：（I）制备，其中R是由氢和碳组成的烃基和包括C 2 -C 10亚烷基，亚芳基，C 7 -C 20亚烷基取代的亚芳基，C 3 -C 20亚烷基取代的亚芳基的取代的烃基， C 20 -C 20亚环烷基，C 4 -C 20亚乙烯基和前述的衍生物包含非不稳定的侧挂卤素，C 1 -C 6烷基，C 1 -C 6卤代烷基，乙烯基，醚或C 1 -C 6烷基醇官能团。 R 1是由氢和碳组成的烃基和包括C 1 -C 10烷基，芳基，C 7 -C 20烷基取代的芳基，C 2 -C 10烯基，苯氧基，C 1 -C 10烷氧基，芳氧基或C 3 -C 20环烷基的取代的烃基，及其衍生物 C1-C6烷基，C1-C6卤代烷基，乙烯基，醚或C1-C6烷基醇官能团。 R1也可以是：其中R 4具有与R相同的定义，且R 4和R可以相同或不同。 R2，R3和R5是直链或支链C1-C10亚烷基，可以相同或不同。 由i表示的整数为约2至约20，由m和n表示的整数不同，为0或1。

公开(公告)号：US3965217A

公开(公告)日：1976-06-22

申请号：US494444

申请日：1974-08-05

申请人： Kyung S. Shim ,  Edward N. Walsh

发明人： Kyung S. Shim ,  Edward N. Walsh

IPC分类号： C07F9/09 ,  C08J9/00 ,  C07F9/40

CPC分类号： C08J9/0061 ,  C07F9/09 ,  C08J2375/04 ,  C08J2485/00

摘要： Stabilized products which are phosphorus containing oligomers having ##EQU1## linkages between phosphorus atoms and which are obtained by the self-condensation of .beta.-haloalkyl esters of pentavalent phosphorus acids or the condensation products of these esters with an alkyl ester of a pentavalent phosphorus acid are formed by terminating the condensation reaction when it is about 35-75% complete, said condensation being performed in the absence of a nucleophilic initiator, such as a sodium salt initiator. The lower degree of condensation in the product and the absence of the nucleophilic initiator during the condensation reaction, is responsible for the lesser degree of scorching in a polyurethane foam containing the product as compared to one which is formed by allowing the condensation reaction go to completion or by use of a nucleophilic initiator during the condensation. If desired, the final product can be post-treated with an alkylene oxide and/or water or alcohol or by extraction with an inert organic solvent.

摘要翻译： 具有磷原子之间具有|| -OCCO- |键的含磷低聚物的稳定化产物，其通过五价磷酸的β-卤代烷基酯的自缩合或这些酯与烷基酯的缩合产物 当其完全约35-75％时终止缩合反应形成五价磷酸，所述缩合在不存在亲核引发剂如钠盐引发剂的情况下进行。 与缩合反应中的亲核性引发剂相比，缩合反应中的缩合度低，不含亲核性引发剂，与通过使缩合反应完成而形成的聚氨酯泡沫体相比，含有该产品的聚氨酯泡沫体的焦烧程度较小 或在冷凝期间使用亲核引发剂。 如果需要，最终产物可用环氧烷和/或水或醇进行后处理，或用惰性有机溶剂萃取。

公开(公告)号：US4604330A

公开(公告)日：1986-08-05

申请号：US562319

申请日：1983-12-16

申请人： Edward N. Walsh

发明人： Edward N. Walsh

IPC分类号： H01M8/08

CPC分类号： H01M8/08

摘要： This invention relates to a novel intermediate temperature fuel cell electrolyte, fuel cells containing this electrolyte and a process for operating these fuel cells.The fuel cell electrolyte composition comprises one or more phosphonic acids. Typical phosphonic acids are compounds of the formula ##STR1## wherein R is a moiety derived from hydroxyalkyl, alkyl, phenyl, alkylphenyl, vinyl, haloalkyl, halophenyl, halomethylphenyl, vinyl, amine, ammonia and ##STR2## and m represents an integer from 1 to 3 and n represents 0 (zero) or the integer 1. This electrolyte composition can further comprise phosphoric acid.The fuel cell electrolyte composition can include a gelling agent and can be effectively used in fuel cells wherein the fuel is hydrogen, the oxidizer is oxygen and the operating temperature is between about 100.degree. C. and 250.degree. C.

公开(公告)号：US3991142A

公开(公告)日：1976-11-09

申请号：US548312

申请日：1975-02-10

申请人： Edward N. Walsh ,  Milton L. Honig

发明人： Edward N. Walsh ,  Milton L. Honig

IPC分类号： C07F9/141 ,  C08K5/51 ,  C08J9/00

CPC分类号： C08K5/51 ,  C07F9/1411 ,  Y10S521/906

摘要： There are disclosed novel fire retardant compositions comprising blends of ordinarily flammable synthetic resins and foams together with bis(2,3-dibromopropyl) phosphite. Such blends are found to display excellent flame retardant properties. Also disclosed is an improved method for the preparation of the bis(2,3-dibromopropyl) phosphite.

摘要翻译： 公开了包含通常可燃合成树脂和泡沫与双（2,3-二溴丙基）亚磷酸酯的共混物的新型阻燃组合物。 发现这种共混物显示出优异的阻燃性能。 还公开了制备双（2,3-二溴丙基）亚磷酸酯的改进方法。

公开(公告)号：US3970729A

公开(公告)日：1976-07-20

申请号：US494685

申请日：1974-08-05

申请人： Edward N. Walsh ,  Kyung Sup Shim

发明人： Edward N. Walsh ,  Kyung Sup Shim

IPC分类号： C07F9/38 ,  C07F9/40 ,  C08G65/00 ,  C08G65/26 ,  C08F2/44

CPC分类号： C07F9/4006 ,  C07F9/4075 ,  C10M2223/065 ,  C10N2240/08

摘要： Di-polyoxyalkylene hydroxymethylphosphonate is prepared by contacting phosphorous acid and formaldehyde, or a formaldehyde polymer such as trioxane or paraformaldehyde, preferably in an aqueous medium, to yield a hydroxymethylphosphonic acid intermediate. The intermediate is then contacted wiyth an alkylene oxide selected from ethylene oxide, propylene oxide or butylene oxide to yield di-polyoxyalkylene hydroxymethylphosphonate having the structureal formula: ##EQU1## wherein R is CH.sub.2, ##EQU2## n + m = 2-10. Di-polyoxyalkylene hydroxymethylphosphonate is utilized as a flame retardant, a stabilizer for polyester film and as a plasticizer for cellulose acetate and polyvinyl acetate, among others.

摘要翻译： 通过使亚磷酸和甲醛或甲醛聚合物如三恶烷或多聚甲醛，优选在水性介质中接触，制备羟基甲基膦酸二聚氧化烯，得到羟甲基膦酸中间体。 然后将中间体与选自环氧乙烷，环氧丙烷或环氧丁烷的环氧烷接触，得到具有以下结构式的二聚氧化亚烷基羟甲基膦酸酯：O＆amp; L-H-CH 2RO-P-ORCH 2 -OH | CH 2 OH; 其中R是CH 2，-CH-或-CH- | CH 3 CH 2 | CH 3 n + m = 2-10。 二聚氧化烯羟甲基膦酸酯用作阻燃剂，聚酯膜的稳定剂和醋酸纤维素和聚乙酸乙烯酯的增塑剂等。

公开(公告)号：US3962374A

公开(公告)日：1976-06-08

申请号：US494427

申请日：1974-08-05

申请人： Kyung S. Shim ,  Edward N. Walsh

发明人： Kyung S. Shim ,  Edward N. Walsh

IPC分类号： C07F9/09 ,  C07F9/40

摘要： Products which are phosphorus containing oligomers having ##EQU1## linkages between phosphorus atoms and which are obtained by the self-condensation of .beta.-haloalkyl esters of pentavalent phosphorus acids or by the condensation of these esters with an alkyl ester of a pentavalent phosphorus acid are extracted with an inert organic solvent. The soluble portion of said products after recovery from the solvent can be incorporated in a polyurethane foam formulation to give a foam which will have less scorching than a foam containing the original condensation product that has not been extracted.

摘要翻译： 磷类低聚物的产物，其中磷原子之间具有| -O-CCO- |键，它们是通过五价磷酸的β-卤代烷基酯的自缩合或通过这些酯与烷基酯的缩合得到的 用惰性有机溶剂萃取五价磷酸。 所述产物在从溶剂中回收后的可溶部分可以加入到聚氨酯泡沫制剂中，以产生比含有未提取的原始缩合产物的泡沫更少的焦烧泡沫。

公开(公告)号：US3943200A

公开(公告)日：1976-03-09

申请号：US488632

申请日：1974-07-15

申请人： Milton L. Honig ,  Edward N. Walsh

发明人： Milton L. Honig ,  Edward N. Walsh

IPC分类号： C07F9/40 ,  C09K21/12

CPC分类号： C09K21/12 ,  C07F9/4006

摘要： Bis alkyl phosphorus esters of dicarboxylic acids having the formula ##EQU1## where R' is a C.sub.1 -C.sub.8 alkyl or haloalkyl group, preferably a C.sub.1 -C.sub.4 alkyl or haloalkyl group, and R is a C.sub.1 -C.sub.8 divalent hydrocarbon group are disclosed. The compounds are formed by the reaction of a tertiary phosphite having the formula P(OR').sub.3 with a haloalkyl ester of a dicarboxylic acid having the formula XCH.sub.2 C(O)ORO(O)CCH.sub.2 X, where X is chlorine, bromine or iodine. The compounds have utility as flame retardants and as sequesterants for metallic cation.

摘要翻译： 具有式OOOO的二元羧酸的双烷基磷酯平行平行的并行对偶平行（R'O）2PCH2COROCCH2P（OR'）2其中R'是C1-C8烷基或卤代烷基，优选C1-C4烷基或卤代烷基，以及 R是C1-C8二价烃基。 通过具有式P（OR'）3的叔亚磷酸酯与具有式XCH2C（O）ORO（O）CCH2X的二羧酸的卤代烷基酯反应形成化合物，其中X是氯，溴或碘。 这些化合物具有作为阻燃剂和金属阳离子螯合剂的作用。

公开(公告)号：US3931361A

公开(公告)日：1976-01-06

申请号：US535883

申请日：1974-12-23

申请人： Fred Jaffe ,  Silvio L. Giolito ,  Edward N. Walsh

发明人： Fred Jaffe ,  Silvio L. Giolito ,  Edward N. Walsh

IPC分类号： C07F9/02 ,  C07F9/12 ,  C08K5/523

CPC分类号： C08K5/523 ,  C07F9/025 ,  C07F9/12

摘要： A method for decolorizing and stabilizing alkylphenyl esters of phosphoric acid which comprises contacting the esters with an effective amount of a sodium salt selected from the group consisting of sodium dithionite and sodium formaldehyde sulfoxylate for a sufficient length of time to decolorize and stabilize the esters against subsequent color formation.

摘要翻译： 一种使磷酸烷基苯基酯脱色和稳定的方法，其包括使酯与有效量的选自连二亚硫酸钠和甲醛次硫酸钠的钠盐接触足够长的时间以使酯脱色并稳定 颜色形成。