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    • 1. 发明授权
    • Production of an anticorrosive pigment on phosphate basis
    • 以磷酸盐为基础生产防腐颜料
    • US4294621A
    • 1981-10-13
    • US141135
    • 1980-04-16
    • Alexander MaurerRenate AdrianKlaus HestermannGero Heymer
    • Alexander MaurerRenate AdrianKlaus HestermannGero Heymer
    • C09D5/08C01B25/32C09C1/00C09C1/02C08K3/10
    • C01B25/322C01B25/325C09C1/02C01P2004/61C01P2006/12
    • 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.
    • 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。
    • 8. 发明授权
    • Production of organophosphines
    • 生产有机膦
    • US4073810A
    • 1978-02-14
    • US549172
    • 1975-02-12
    • Klaus HestermannBernd LippsmeierGero Heymer
    • Klaus HestermannBernd LippsmeierGero Heymer
    • B01J21/00C07B61/00C07F9/50C07F9/53C07F9/54
    • C07F9/5086C07F9/54
    • 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.
    • 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。
    • 10. 发明授权
    • Production of hydroxyalkylphosphine oxides
    • 生产羟烷基膦氧化物
    • US4076755A
    • 1978-02-28
    • US666699
    • 1976-03-15
    • Bernd LippsmeierKlaus Hestermann
    • Bernd LippsmeierKlaus Hestermann
    • C07F9/53C09K21/12
    • C09K21/12C07F9/5304
    • 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.
    • 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。