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12 条记录 (耗时 0.03 秒)

    Production of bromoaryl chlorophosphates
    2.
    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

    申请人： Karl-Heinz Mitschke

    发明人： Karl-Heinz Mitschke

    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
    3.
    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

    申请人： Karl-Heinz Mitschke ,  Hans Niederprum

    发明人： Karl-Heinz Mitschke ,  Hans Niederprum

    IPC分类号： C11D1/12 ,  B01F17/00 ,  B01F17/26 ,  C11D1/00 ,  C11D1/88 ,  G03C1/38 ,  G03C5/305

    CPC分类号： G03C1/385 ,  B01F17/0057 ,  C11D1/004 ,  G03C5/3053

    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。

    Production of N,N-Bis-(2-hydroxyalkyl)-aminomethane phosphonic acid dialkyl esters
    4.
    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

    申请人： Manfred Kapps ,  Karl-Heinz Mitschke ,  Reinhard Schliebs

    发明人： Manfred Kapps ,  Karl-Heinz Mitschke ,  Reinhard Schliebs

    IPC分类号： C07F9/38 ,  B01J31/00 ,  C07B61/00 ,  C07F9/40 ,  C08K5/5353

    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。

    Preparation of triethyl phosphate
    5.
    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

    申请人： Karl-Heinz Mitschke ,  Kaspar Hallenberger ,  Ottfried Schlak ,  Johannes Kaulen

    发明人： Karl-Heinz Mitschke ,  Kaspar Hallenberger ,  Ottfried Schlak ,  Johannes Kaulen

    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
    7.
    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

    申请人： Karl-Heinz Mitschke ,  Klaus Geisler ,  Hans Niederprum

    发明人： Karl-Heinz Mitschke ,  Klaus Geisler ,  Hans Niederprum

    IPC分类号： C07C311/09 ,  C07C67/00 ,  C07C301/00 ,  C07C303/40 ,  C07C311/02 ,  C07C143/74

    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

    申请人： Karl-Heinz Mitschke ,  Hans Niederprum ,  Johann-Nikolaus Meussdoerffer

    发明人： Karl-Heinz Mitschke ,  Hans Niederprum ,  Johann-Nikolaus Meussdoerffer

    IPC分类号： C07C309/06 ,  C07C67/00 ,  C07C301/00 ,  C07C303/32 ,  C07F7/12 ,  C07C87/30

    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。

    Production of high viscosity phosphoric and phosphonic acid aryl esters
    10.
    发明授权
    Production of high viscosity phosphoric and phosphonic acid aryl esters 失效
    生产高粘度磷酸和膦酸芳基酯

    公开(公告)号：US4212832A

    公开(公告)日：1980-07-15

    申请号：US936987

    申请日：1978-08-25

    申请人： Karl-Heinz Mitschke ,  Reinhard Schliebs

    发明人： Karl-Heinz Mitschke ,  Reinhard Schliebs

    IPC分类号： C08K5/00 ,  C07F9/12 ,  C08G16/02 ,  C08G79/00 ,  C08G79/02 ,  C08K5/51 ,  C08L1/00 ,  C08L27/00 ,  C08L67/00 ,  C07F9/09

    CPC分类号： C08G16/0243

    摘要： A process for the production of a relatively high molecular weight phosphoric or phosphonic acid aryl ester, comprising reacting a phosphoric or phosphonic acid aryl ester with formaldehyde in the presence of sulphuric acid at a temperature from about 10.degree. to 120.degree. C. Advantageously, the aryl ester is of the formula ##STR1## in which R is a hydrogen atom, an alkyl group having from 1 to 6 carbon atoms, a halogen atom, an aryloxy group, or an aryl group;R.sub.1 is a group OC.sub.6 H.sub.m R.sub.n in which m+n=5, an alkyl group, a haloalkyl group or an optionally substituted aryl group;R.sub.2 is a group OC.sub.6 H.sub.m R.sub.n, in which m+n=5; andn is from 1 to 3,about 0.5 mole of formaldehyde in the form of paraformaldehyde or trioxane is employed per mole of aryl ester, about 1.5 to 2 moles of sulphuric acid are used per mole of aryl ester, the sulphuric acid is employed as a solution of at least about 95% concentration, and the reaction is effected at a temperature of about 40.degree. to 80.degree. C. in the presence of an inert solvent. The products are new and useful as flame-proofing agents in the production of laminated papers and polyesters, as fire-retarding plasticizers in plastics such as PVC, as additives to plastics such as polyphenylene oxides and also as low-flammability hydraulic oils.

    摘要翻译： 一种生产相对高分子量磷酸或膦酸芳酯的方法，包括在硫酸存在下，在约10-120℃的温度下使磷酸或膦酸芳基酯与甲醛反应。有利的是， 芳基酯为其中R为氢原子，具有1至6个碳原子的烷基，卤原子，芳氧基或芳基的式“IMAGE”+ TR“IMA” R1是其中m + n = 5，烷基，卤代烷基或任选取代的芳基的基团OC6HmRn; R2是OC6HmRn基团，其中m + n = 5; 并且n为1至3，每摩尔芳基酯使用约0.5摩尔以多聚甲醛或三恶烷形式的甲醛，每摩尔芳基酯使用约1.5至2摩尔硫酸，硫酸用作 至少约95％浓度的溶液，并且在约40℃至80℃的温度下在惰性溶剂的存在下进行反应。 该产品在生产层压纸和聚酯中作为阻燃剂是新型的并且是有用的，作为塑料如PVC的阻燃增塑剂，作为塑料如聚苯醚的添加剂以及低可燃性液压油。