Production of N,N-Bis-(2-hydroxyalkyl)-aminomethane phosphonic acid
dialkyl esters
    2.
    发明授权
    Production of N,N-Bis-(2-hydroxyalkyl)-aminomethane phosphonic acid dialkyl esters 失效
    制备N,N-双 - (2-羟基烷基) - 氨基甲烷膦酸二烷基酯

    公开(公告)号:US4060571A

    公开(公告)日:1977-11-29

    申请号:US656034

    申请日:1976-02-06

    CPC分类号: C08K5/5353 C07F9/4006

    摘要: A process for the production of N,N-bis-(2-hydroxyalkyl)-aminomethane phosphonic acid dialkyl esters of the formula ##STR1## in which R is an optionally substituted alkyl radical with 2 to 10 carbon atoms, andR' is hydrogen or a lower alkyl radical with up to 6 carbon atoms,Comprising reacting an oxazolidine of the formula ##STR2## with a dialkyl phosphite in the presence of an acid ion exchanger. Preferably R is ethyl or isopropyl, R' is hydrogen or methyl, the ion exchanger is a sulfonated polystyrene resin and the reaction is effected at about 30.degree. to 120.degree. C, especially 60.degree. to 100.degree. C. The products are thereby obtained rapidly in higher purity than heretofore possible.

    摘要翻译: 制备式“IMAGE”的N,N-双 - (2-羟基烷基) - 氨基甲基膦酸二烷基酯的方法,其中R是任选取代的具有2至10个碳原子的烷基,R'是氢 或具有至多6个碳原子的低级烷基,在酸性离子交换剂的存在下,用亚磷酸二烷基酯包合反应式“OXAZOLIDINE”。 优选R是乙基或异丙基,R'是氢或甲基,离子交换剂是磺化聚苯乙烯树脂,反应在约30℃至120℃,特别是60℃至100℃下进行。从而快速获得产物 纯度比以前更高。

    1,1,1-Trifluoro-2-chloroethane as blowing agent for polyurethane foam
    3.
    发明授权
    1,1,1-Trifluoro-2-chloroethane as blowing agent for polyurethane foam 失效
    1,1,1-三氟-2-氯乙烷作为聚氨酯泡沫塑料的发泡剂

    公开(公告)号:US4177332A

    公开(公告)日:1979-12-04

    申请号:US932056

    申请日:1978-08-08

    IPC分类号: C08J9/12 C08J9/14 C08G18/14

    CPC分类号: C08J9/144

    摘要: In the production of a foamed synthetic material by the reaction of starting materials which undergo a polymerization, polycondensation or polyaddition reaction to produce a high molecular weight synthetic material in the presence of a blowing agent, e.g. a polyurethane, or by foaming an unfoamed thermoplastic synthetic material by means of a blowing agent, the improvement which comprises employing 1,1,1-trifluoro-2-chloroethane as the blowing agent, optionally in admixture with 1,1-difluoro-2-chloroethane.

    摘要翻译: 在通过在发泡剂的存在下进行聚合,缩聚或加聚反应以产生高分子量合成材料的起始材料的反应来生产发泡合成材料。 或通过发泡剂使未发泡的热塑性合成材料发泡的改进,其包括使用1,1,1-三氟-2-氯乙烷作为发泡剂,任选地与1,1-二氟-2 氯乙烷。

    Production of bromoaryl chlorophosphates
    4.
    发明授权
    Production of bromoaryl chlorophosphates 失效
    溴代溴代芳基酯的生产

    公开(公告)号:US4144290A

    公开(公告)日:1979-03-13

    申请号:US848413

    申请日:1977-11-03

    IPC分类号: C07F9/14

    CPC分类号: C07F9/1406

    摘要: A process for the preparation of brominated aryl dichlorophosphates or diaryl chlorophosphates of the formula: ##STR1## WHEREIN R each independently is hydrogen, an alkoxy radical or alkyl radical containing 1 to 10 C-atoms, a perfluoroalkyl radical containing 1 to 10 C-atoms, halogen, the group --NO.sub.2, --SO.sub.3 H, Cl.sub.2 P(O)O-- or Cl.sub.2 P(O)OC.sub.6 H.sub.4 - CR'.sub.2 --,R.sup.1 each independently is hydrogen or an alkyl radical containing 1 to 4 C-atoms,X is an integer from 1 to 4,N is 1 or 2, andM is from 0.1 to 2,Comprising reacting the corresponding aryl dichlorophosphates or diaryl chlorophosphates, with a substantially equimolar mixture of bromine and chlorine at a temperature between about -10.degree. and 100.degree. C. Advantageously the bromine and chlorine are present as bromine chloride, the reaction is carried out at about 10.degree. to 60.degree. C. and the proportions, time and temperature of reaction are such that the degree of bromination is about 0.1 to 0.8 mol of bromine per phenyl nucleus.

    摘要翻译: 制备下式的溴代芳基二氯磷酸盐或二芳基氯代磷酸盐的方法:其中R独立地为氢,含有1至10个C原子的烷氧基或烷基,含有1至10个C原子的全氟烷基 ,卤素,-NO 2,-SO 3 H,Cl 2 P(O)O-或Cl 2 P(O)OC 6 H 4 -R CR 2 - ,R 1各自独立地为氢或含有1至4个C原子的烷基,X为整数 从1到4,N是1或2,M是从0。

    Use of perfluoroalkane sulphonamide salts as surface active agents
    5.
    发明授权
    Use of perfluoroalkane sulphonamide salts as surface active agents 失效
    使用全氟烷基磺酰胺盐作为表面活性剂

    公开(公告)号:US4370254A

    公开(公告)日:1983-01-25

    申请号:US148893

    申请日:1980-05-12

    摘要: Employing as surface active agents salts of perfluoroalkane sulphonamides, preferably of the formula ##STR1## in which R.sub.F is a perfluorinated aliphatic group having 4 to 20 C-atoms,R is a hydrogen atoms, an alkyl group having 1 to 4 C-atoms, a hydroxyalkyl group having 1 to 4 C-atoms or a cycloalkyl group having up to 6 C-atoms, andM is an alkali metal, an alkaline earth metal or an onium group of the formula[ZR.sub.2 R.sub.3 R.sub.4 R.sub.5 ].sup..sym., Z is phosphorus or nitrogen, andR.sub.2 to R.sub.5 each independently is a hydrogen atom, or an alkyl, hydroxyalkyl, or alkoxyalkyl group having 1 to 4 C-atoms per alkyl moiety.

    摘要翻译: 作为全氟烷基磺酰胺的表面活性剂,优选具有式“IMAGE”的RF是具有4至20个C原子的全氟化脂族基团,R是氢原子,具有1至4个C原子的烷基, 具有1至4个C原子的羟基烷基或具有至多6个C原子的环烷基,M是式[ZR2R3R4R5](+)的碱金属,碱土金属或鎓基,Z是磷 或氮,R2至R5各自独立地为氢原子,或每个烷基部分具有1至4个C原子的烷基,羟基烷基或烷氧基烷基。

    Preparation of triethyl phosphate
    6.
    发明授权
    Preparation of triethyl phosphate 失效
    磷酸三乙酯的制备

    公开(公告)号:US06673955B2

    公开(公告)日:2004-01-06

    申请号:US10302543

    申请日:2002-11-22

    IPC分类号: C07F902

    CPC分类号: C07F9/11

    摘要: The invention relates to a process for preparing triethyl phosphate by reacting phosphorus oxychloride with a greater than stoichiometric quantity of ethanol under reduced pressure at temperatures of from 0 to 50° C. in a reaction vessel, wherein a) the volatile components resulting from the reaction are predominantly condensed by means of a reflux condenser and the remaining volatile components are passed into a scrubber filled with water, b) after the end of the reaction, the reaction mixture is separated distillatively in an outgassing column into a top product and a bottom product which predominantly comprises triethyl phosphate, c) the top product of the outgassing column is combined with the contents of the scrubber and d) the contents of the scrubber are separated distillatively in an azeotropic distillation to obtain water and ethanol as top product and the ethanol, preferably after dewatering, is preferably returned to the reaction.

    摘要翻译: 本发明涉及通过在反应容器中在0至50℃的温度下在减压下使磷酰氯与大于化学计量的乙醇反应来制备磷酸三乙酯的方法,其中a)由反应产生的挥发性组分为 主要通过回流冷凝器冷凝,剩余的挥发性成分进入填充有水的洗涤器,b)在反应结束后,将反应混合物在脱气塔中蒸馏分离成顶部产物和底部产物, 主要包括磷酸三乙酯,c)除气塔的顶部产物与洗涤器的内容物组合,d)洗涤器的内容物在共沸蒸馏中蒸馏分离,得到水和乙醇作为顶级产物和乙醇,优选在 脱水,优选返回到反应中。

    Process for the preparation of hydroxyalkylperfluoroalkane sulphonamides
    8.
    发明授权
    Process for the preparation of hydroxyalkylperfluoroalkane sulphonamides 失效
    羟烷基全氟烷烃磺酰胺的制备方法

    公开(公告)号:US4265831A

    公开(公告)日:1981-05-05

    申请号:US54338

    申请日:1979-07-02

    CPC分类号: C07C311/02

    摘要: A process for the preparation of a hydroxyalkylperfluoroalkane sulphonamide of the formula ##STR1## wherein R.sub.F is a perfluoroalkyl group having from 1 to 20 carbon atoms;R and R' each independently is hydrogen or an alkyl, hydroxyalkyl, haloalkyl, cycloalkyl, aralkyl, alkenyl or aryl radical; andm and n each independently is an integer from 1 to about 30,comprising reacting a perfluoroalkylsulphonamide of the formula ##STR2## with an epoxide of the formula ##STR3## in the presence of a basic catalyst.

    摘要翻译: 一种制备式IMAGE的羟烷基全氟烷烃磺酰胺的方法,其中RF是具有1至20个碳原子的全氟烷基; R和R'各自独立地是氢或烷基,羟基烷基,卤代烷基,环烷基,芳烷基,烯基或芳基; 并且m和n各自独立地为1至约30的整数,包括在碱性催化剂存在下使式“IMAGE”的全氟烷基磺酰胺与式“IMAGE”的环氧化物反应。

    Production of tetraethyl ammonium perfluoroalkyl sulphonate
    9.
    发明授权
    Production of tetraethyl ammonium perfluoroalkyl sulphonate 失效
    生产全氟烷基磺酸四乙基铵

    公开(公告)号:US4168277A

    公开(公告)日:1979-09-18

    申请号:US858499

    申请日:1977-12-07

    CPC分类号: C07C309/00 C07F7/123

    摘要: Production of tetraethyl ammonium perfluoroalkyl sulphonates (C.sub.2 H.sub.5).sub.4 N.sym.R.sub.F SO.sub.3 .crclbar., wherein R.sub.F represents a perfluorinated alkyl radical with about 4 to 10 carbon atoms, by reacting crude perfluoroalkyl sulphonic acid fluoride, i.e. perfluoroalkyl sulphonic acid fluoride which has not been especially purified, with triethylamine and an ethoxy silane, preferably dimethyl diethoxy silane, methyl triethoxy silane or tetraethoxy silane in an inert solvent at temperatures of about 10.degree. to 60.degree. C., preferably about 20.degree. to 40.degree. C. The process according to the invention is particularly suitable for the production of tetraethyl ammonium perfluorooctane sulphonate.

    摘要翻译: 制备全氟烷基磺酸四乙基铵(C 2 H 5)4 N(+)RFSO 3( - ),其中RF表示具有约4至10个碳原子的全氟烷基,通过使全氟烷基磺酸氟化物即即未全氟烷基磺酸氟化物 特别是用三乙胺和乙氧基硅烷,优选二甲基二乙氧基硅烷,甲基三乙氧基硅烷或四乙氧基硅烷在惰性溶剂中,在约10℃至60℃,优选约20℃至40℃的温度下纯化。根据 本发明特别适用于生产全氟辛烷磺酸四乙基铵。