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    Production of methylphosphine oxides
    2.
    发明授权
    Production of methylphosphine oxides 失效
    生产甲基膦氧化物

    公开(公告)号：US3980711A

    公开(公告)日：1976-09-14

    申请号：US549174

    申请日：1975-02-12

    申请人： Bernd Lippsmeier ,  Klaus Hestermann ,  Gero Heymer

    发明人： Bernd Lippsmeier ,  Klaus Hestermann ,  Gero Heymer

    IPC分类号： B01J31/00 ,  C07F9/53 ,  C07F9/02

    CPC分类号： C07F9/53

    摘要： Methylphosphine oxides of the general formula (I) ##EQU1## are produced from hydroxymethylphosphines of the general formula (II) ##EQU2## in which formulae R and R' each stand for identical or different alkyl-, cycloalkyl-, aralkyl- or aryl groups having from 1 to 18 carbon atoms, or carrying substituents being inert under the reaction conditions.The methylphosphine oxides are more particularly produced by subjecting the hydroxymethylphosphines to a rearrangement reaction with the aid of radical-yielding compounds.

    摘要翻译： 由通式（I）R HOCH2-P ANGLE（II）R'的羟甲基膦制备通式（I）的二甲基膦氧化物。其中式R和R'各自为 代表具有1至18个碳原子的相同或不同的烷基 - ，环烷基 - ，芳烷基 - 或芳基，或在反应条件下携带取代基是惰性的。

    Production of organophosphines
    3.
    发明授权
    Production of organophosphines 失效
    生产有机膦

    公开(公告)号：US4073810A

    公开(公告)日：1978-02-14

    申请号：US549172

    申请日：1975-02-12

    申请人： Klaus Hestermann ,  Bernd Lippsmeier ,  Gero Heymer

    发明人： Klaus Hestermann ,  Bernd Lippsmeier ,  Gero Heymer

    IPC分类号： B01J21/00 ,  C07B61/00 ,  C07F9/50 ,  C07F9/53 ,  C07F9/54

    CPC分类号： C07F9/5086 ,  C07F9/54

    摘要： Production of organophosphines of the general formula R.sub.n PH.sub.3-n, in which R stands for identical or different, substituted or unsubstituted alkyl, cycloalkyl or aralkyl groups having from 1 to 18 carbon atoms, preferably from 1 to 4 carbon atoms, more preferably from 1 to 2 carbon atoms, and n stands for a whole number within the range 1 and 3. The compounds are more particularly produced by continuously reacting hydrocarbon halides of the general formula RX, in which R has the meaning given hereinabove and X stands for halogen, especially for chlorine or bromine, with hydrogen phosphide, and primary or secondary organophosphines at temperatures within the range 100.degree. and 600.degree. C. and under pressures of up to 20 atmospheres in contact with a catalyst being placed in a reactor. Gaseous matter issuing from the reactor is cooled and the resulting organophosphonium halides (R.sub.n PH.sub.4-n)X are hydrolyzed in conventional manner to the corresponding organophosphines.

    摘要翻译： 制备通式RnPH3-n的有机膦，其中R代表相同或不同的取代或未取代的具有1至18个碳原子，优选1至4个碳原子的烷基，环烷基或芳烷基，更优选1至 2个碳原子，n表示1和3范围内的整数。化合物更特别地通过连续反应通式RX的卤代烃，其中R具有上文给出的含义，X代表卤素，特别是 对于氯或溴，与磷化氢以及初级或次级有机膦在100℃和600℃的温度范围内以及在与置于反应器中的催化剂接触的情况下在高达20个大气压的压力下进行。 将从反应器排出的气态物质冷却，并将所得的有机鏻卤化物（RnPH4-n）X以常规方式水解成相应的有机膦。

    Production of hydroxyalkylphosphine oxides
    5.
    发明授权
    Production of hydroxyalkylphosphine oxides 失效
    生产羟烷基膦氧化物

    公开(公告)号：US4076755A

    公开(公告)日：1978-02-28

    申请号：US666699

    申请日：1976-03-15

    申请人： Bernd Lippsmeier ,  Klaus Hestermann

    发明人： Bernd Lippsmeier ,  Klaus Hestermann

    IPC分类号： C07F9/53 ,  C09K21/12

    CPC分类号： C09K21/12 ,  C07F9/5304

    摘要： Production of tertiary hydroxyalkylphosphine oxides of general formula (I) ##STR1## in which R.sup.1 and R.sup.2 each stand for organic groups having from 1 to 18 carbon atoms, where R.sup.1 may be identical with R.sup.2 and R.sup.2 may be identical with R which stands for a radical of general formula (II) ##STR2## in which R.sup.3 and R.sup.4 equally stand for organic groups having from 1 to 18 carbon atoms and/or more preferably for hydrogen. The compounds are made from phosphines of general formula (III) ##STR3## in which R.sup.3 and R.sup.4 have the meanings given above, which are reacted in a single step operation with carbonyl compounds of general formula (IV) ##STR4## in which R.sup.3 and R.sup.4 equally have the meanings given above. The reaction is effected while adding at least one substance yielding hydroxyl ions and in the presence of water, and the resulting hydroxyalkylphosphine oxides are separated from the reaction product.

    摘要翻译： 其中R 1和R 2各自代表具有1至18个碳原子的有机基团，其中R 1可以与R 2和R 2相同，通式（Ⅰ）的叔羟烷基膦氧化物的制备可以与R相同， 代表通式（II）的基团（II），其中R 3和R 4均等于具有1至18个碳原子和/或更优选氢的有机基团。 化合物由通式（III）的膦制备，其中R 3和R 4具有上述含义，其在单步操作中与通式（IV）的羰基化合物（IMA）反应 IV），其中R3和R4同样具有上述含义。 在加入至少一种产生羟基离子的物质和水的存在下进行反应，并将所得羟烷基氧化膦与反应产物分离。

    Production of an anticorrosive pigment on phosphate basis
    6.
    发明授权
    Production of an anticorrosive pigment on phosphate basis 失效
    以磷酸盐为基础生产防腐颜料

    公开(公告)号：US4294621A

    公开(公告)日：1981-10-13

    申请号：US141135

    申请日：1980-04-16

    申请人： Alexander Maurer ,  Renate Adrian ,  Klaus Hestermann ,  Gero Heymer

    发明人： Alexander Maurer ,  Renate Adrian ,  Klaus Hestermann ,  Gero Heymer

    IPC分类号： C09D5/08 ,  C01B25/32 ,  C09C1/00 ,  C09C1/02 ,  C08K3/10

    CPC分类号： C01B25/322 ,  C01B25/325 ,  C09C1/02 ,  C01P2004/61 ,  C01P2006/12

    摘要： The invention relates to the production of phosphorus-containing anticorrosive pigments with a particle size of at most 20 microns by reacting one or more calcium or magnesium compounds with phosphoric acid or acid alkali metal or ammonium phosphates by intimately mixing an aqueous suspension or solution of the reactants inside a dispersing means rotating at a speed of 3000 to 10,000 rpm. More particularly, fine pulverulent calcium and magnesium compounds are converted, with agitation, together with water and, if desired, a water-soluble alkanol to a homogeneous suspension or solution. The suspension or solution is intimately mixed, inside the dispersing means at 0.degree. to 40.degree. C. and in an approximately stoichiometric ratio, with the phosphoric acid or acid phosphate solution. Resulting and precipitated pigment is separated and dried under mild conditions while maintaining its content of water of crystallization. The anticorrosive pigment is comprised of a homogeneous mixture and/or mixed crystals of which 10 to 95 mol % is calcium hydrogen phosphate dihydrate, the balance being magnesium hydrogen phosphate trihydrate. An at least 55 weight % proportion consists of particles with a size of up to 5 microns with a BET-surface of at least 1 m.sup.2 /g.

    摘要翻译： 本发明涉及通过使一种或多种钙或镁化合物与磷酸或酸性碱金属或铵磷酸盐反应，通过将下列物质的水性悬浮液或溶液紧密混合，从而生产粒径至多为20微米的含磷防腐颜料 分散装置内的反应物以3000至10,000rpm的速度旋转。 更具体地，精细的粉末状钙和镁化合物在搅拌下与水一起转化，如果需要，将水溶性链烷醇转化成均匀的悬浮液或溶液。 悬浮液或溶液在分散装置内在0℃至40℃下以大约化学计量比与磷酸或酸式磷酸盐溶液紧密混合。 将所得沉淀的颜料分离并在温和条件下干燥，同时保持其结晶水含量。 防腐颜料由均匀的混合物和/或其中10〜95摩尔％为磷酸氢钙二水合物的混合晶体组成，余量为磷酸氢二氢钙三水合物。 至少55重量％的比例由尺寸高达5微米，BET表面至少为1m 2 / g的颗粒组成。

    Production of alkylphosphines
    7.
    发明授权
    Production of alkylphosphines 失效
    生产烷基膦

    公开(公告)号：US4156697A

    公开(公告)日：1979-05-29

    申请号：US823140

    申请日：1977-08-09

    申请人： Klaus Hestermann ,  Hartfrid Vollmer ,  Gero Heymer ,  Ernst-Gunther Schlosser

    发明人： Klaus Hestermann ,  Hartfrid Vollmer ,  Gero Heymer ,  Ernst-Gunther Schlosser

    IPC分类号： C07F9/50

    CPC分类号： C07F9/5004 ,  Y02P20/582

    摘要： Alkyl phosphines of the general formula:R.sub.n PH.sub.3-n (I)are made. To this end hydrogen phosphide, a primary or a secondary phosphine is reacted with an alkylamine of the general formula:R.sub.n NH.sub.3-n (II)in a molar ratio of 0.1 to 10 mols of the alkylamine of formula II per mol of hydrogen phosphide or primary or secondary phosphine. The reaction is effected at a 150.degree. to 400.degree. C., at atmospheric pressure or a superatmospheric pressure up to 1 atmosphere gauge, and in contact with a catalyst comprising active carbon, copper (II) chromite, or one or more metals of Group Ib or VIII of the Periodic System of the elements. The starting materials are passed through a reaction zone at a rate which permits a contact time between them and the catalyst of 0.1 to 400 seconds.

    摘要翻译： 具有以下通式的烷基膦：

    Production of alkyl phosphines
    8.
    发明授权
    Production of alkyl phosphines 失效
    烷基膦的生产

    公开(公告)号：US4150058A

    公开(公告)日：1979-04-17

    申请号：US904027

    申请日：1978-05-08

    申请人： Klaus Hestermann ,  Gero Heymer

    发明人： Klaus Hestermann ,  Gero Heymer

    IPC分类号： C07F9/50

    CPC分类号： C07F9/5004 ,  Y02P20/582

    摘要： Alkyl phosphines are made. To this end, phosphorus in vapor form is reacted with steam and an alkyl amine at elevated temperature in contact with a carbon catalyst placed in a reactor, the reactants being used individually or in admixture with one another.

    摘要翻译： 制备烷基膦。 为此，蒸气形式的磷与蒸汽和烷基胺在升高的温度下与放置在反应器中的碳催化剂接触，反应物单独使用或彼此混合使用。

    Production of phosphine
    9.
    发明授权
    Production of phosphine 失效
    生产磷化氢

    公开(公告)号：US4091078A

    公开(公告)日：1978-05-23

    申请号：US736556

    申请日：1976-10-28

    申请人： Klaus Hestermann ,  Jurgen Stengel ,  Gero Heymer ,  Christian May

    发明人： Klaus Hestermann ,  Jurgen Stengel ,  Gero Heymer ,  Christian May

    IPC分类号： C01B25/06 ,  C01B25/00

    CPC分类号： C01B25/06

    摘要： Phosphine is produced from elementary yellow phosphorus and an aqueous alkali metal hydroxide solution in the presence of an alcohol. The phosphine is more particularly made by using an alcohol having from 5 to 10 carbon atoms and a dissolving power for yellow phosphorus of more than 5 g/l; suspending the phosphorus with agitation in the said alcohol in a reaction zone; reacting the resulting suspension with the alkali metal hydroxide solution at temperatures lower than the boiling point of the alcohol; and collecting the resulting issuing gaseous phosphine.

    摘要翻译： 在醇的存在下，由元素黄磷和碱金属氢氧化物水溶液生产磷化氢。 膦更特别地通过使用具有5至10个碳原子的醇和大于5g / l的黄磷的溶解力来制备; 在反应区内搅拌将磷悬浮在所述醇中; 在低于醇的沸点的温度下使得到的悬浮液与碱金属氢氧化物溶液反应; 并收集产生的发出的气态膦。

    Production of tertiary phosphine oxides
    10.
    发明授权
    Production of tertiary phosphine oxides 失效
    生产叔膦氧化物

    公开(公告)号：US4091012A

    公开(公告)日：1978-05-23

    申请号：US780989

    申请日：1977-03-24

    申请人： Hartfrid Vollmer ,  Georg Elsner ,  Bernd Lippsmeier ,  Klaus Hestermann

    发明人： Hartfrid Vollmer ,  Georg Elsner ,  Bernd Lippsmeier ,  Klaus Hestermann

    IPC分类号： B01J27/00 ,  B01J31/00 ,  C07B61/00 ,  C07F9/53 ,  C07C120/00

    CPC分类号： C07F9/5304

    摘要： Production of tertiary phosphine oxides which contain nitrile groups and correspond to the following general formula I: ##STR1## in which R.sup.1 and R.sub.2 each stand for a straight or branched, identical or different alkyl, cycloalkyl, aryl, alkylaryl or aralkyl group having 1 to 18 carbon atoms, and in which R.sup.1 or R.sub.2 may be identical with R, which stands for a radical of the following general formula II: ##STR2## in which R.sup.3 and R.sup.4 each stand for a straight or branched, identical or different alkyl, cycloalkyl, aryl, alkylaryl or aralkyl group having 1 to 18 carbon atoms, and/or hydrogen atoms. The tertiary phosphine oxides are made by reacting a phosphine of the following general formula III: ##STR3## in which R.sup.5 has the same meaning as R.sup.3 and R.sup.6 has the same meaning as R.sup.4 but is no hydrogen, with an .alpha.,.beta.-unsaturated nitrile of the following general formula IV: ##STR4## in which R.sup.3 and R.sup.4 have the meanings given above. The reaction is effected in a single stage in the presence of water or a water-solvent mixture and the above formula I compounds are separated from the reaction product.

    摘要翻译： 制备含有腈基并且对应于以下通式I的叔膦氧化物：其中R 1和R 2各自表示直链或支链，相同或不同的具有1个碳原子的烷基，环烷基，芳基，烷基芳基或芳烷基 至18个碳原子，其中R 1或R 2可以与R相同，其代表下列通式II的基团：其中R 3和R 4各自代表直链或支链，相同或不同的烷基 ，具有1至18个碳原子的环烷基，芳基，烷基芳基或芳烷基，和/或氢原子。 叔膦氧化物通过使下列通式III的膦：其中R 5具有与R 3相同的含义，R 6具有与R 4相同的含义，但不具有氢，具有α，β-不饱和的 腈，其中R 3和R 4具有上述含义。 反应在水或水 - 溶剂混合物存在下在单一阶段进行，并且上述式I化合物与反应产物分离。