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    • 31. 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。
    • 33. 发明授权
    • Aluminum nitride powder and a process for the preparation thereof
    • 氮化铝粉末及其制备方法
    • US4923691A
    • 1990-05-08
    • US364013
    • 1989-06-09
    • Dieter PetersGero HeymerChristian May
    • Dieter PetersGero HeymerChristian May
    • C01B21/072
    • C01B21/072C01P2002/60C01P2004/62C01P2006/12C01P2006/60
    • An aluminum nitride powder has a crystallite size of 40 to 150 nm, measured by powder diffractometry and evaluated by the method of Scherrer, a primary particle size of 0.1 to 0.5 .mu.m, a specific surface according to BET of 5 to 50 m.sup.2 /g and a degree of whiteness of more than 91%, measured using light of a 400 to 700 nm wavelength against barium sulfate analytical reagent as standard of whitness.To prepare this aluminum nitride powder, metallic aluminum and monoamminealuminum chloride [AlCl.sub.3 (NH.sub.3)] are first molten together in an inert gas atmosphere at temperatures above 125.degree. C. and allowed to react with one another with evolution of hydrogen. 8 to 20 g of ammonia are then introduced per hour per mol of monoamminealuminum chloride into the aluminum-containing monoamminealuminum chloride melt at temperatures between 250.degree. and 400.degree. C., aluminum nitride being precipitated as a solid until the conversion of the aluminum is complete. The temperature of the melt is finally raised to more than 400.degree. C.
    • 氮化铝粉末的微晶尺寸为40〜150nm,用粉末衍射法测定,用Scherrer法评价,一次粒径为0.1〜0.5μm,BET比表面积为5〜50m 2 / g 白度为91%以上,采用400〜700nm波长的光作为白度标准测定硫酸钡分析试剂。 为了制备这种氮化铝粉末,首先在惰性气体气氛中,在高于125℃的温度下将金属铝和一氯化铝[AlCl 3(NH 3)]熔融在一起,并使其彼此发生氢气反应。 然后在250-400℃的温度下将8至20g的氨每小时每摩尔氯化单铝酸铵引入含铝单胺氯化铝熔体中,将氮化铝作为固体沉淀直到铝的转化完全 。 熔体的温度最终升至400℃以上。
    • 36. 发明授权
    • Process for the dearsenification of polyphosphoric acid
    • 多磷酸脱砷方法
    • US4399114A
    • 1983-08-16
    • US402941
    • 1982-07-29
    • Alexander MaurerGero HeymerMarkus Erpenbach
    • Alexander MaurerGero HeymerMarkus Erpenbach
    • C01B25/24C01B25/16
    • C01B25/24
    • The disclosure relates to a process for the continuous dearsenification of polyphosphoric acid with the aid of hydrogen sulfide in a gas admission zone. To this end, the disclosure provides for the acid to be dearsenified in a gas admission zone subdivided so as to comprise at least two separate liquid matter-receiving zones, each zone being separated from the other by means of a separate gas zone; for the liquid in each of the liquid matter-receiving zones to be maintained at a level 0.1 up to 10 cm high, without admission of gas; for hydrogen sulfide which remained unreacted in the individual liquid matter-receiving zones to be collected in the respective gas zone and for it to be finely redispersed in the liquid matter-receiving zone directly upstream of the respective gas zone by allowing the hydrogen sulfide to flow through a plurality of openings into the acid, the latter being delivered from the respective liquid-matter-receiving zone into the next downstream liquid-matter-receiving zone, and introduced thereinto directly below the liquid matter level therein; for precipitated arsenic sulfide to be separated from the acid coming from the lower end of the gas admission zone, and for the filtrate obtained to be freed from gaseous hydrogen sulfide in excess.
    • 本公开涉及在气体入口区借助硫化氢连续脱砷多磷酸的方法。 为此,本公开内容提供了在气体进入区域中进行脱砷的酸,其被细分为包括至少两个分离的液体物质接收区域,每个区域通过单独的气体区域与另一个区域分离; 使每个液体物质接收区域中的液体保持在0.1至10厘米高的水平,而不允许气体; 对于在各个液体物质接收区中保持未反应的硫化氢,其被收集在各个气体区中,并且通过允许硫化氢流动直接在各个气体区的上游被精细地再分散在液体物质接收区中 通过多个开口进入酸,后者从相应的液体接收区输送到下一个下游液体接收区,并直接在其中引入液体物质的下方; 使沉淀的硫化砷与气体入口区的下端的酸分离,得到的过滤得到的无水硫化氢的滤液。
    • 38. 发明授权
    • Process for making aqueous alkali metal phosphate solutions
    • 制备碱金属磷酸盐水溶液的方法
    • US4385041A
    • 1983-05-24
    • US326078
    • 1981-11-30
    • Klaus JoddenGero Heymer
    • Klaus JoddenGero Heymer
    • C01B25/30C01B15/16C01B25/26
    • C01B25/30
    • The invention relates to a process for making aqueous alkali metal phosphate solutions by subjecting aqueous alkali metal phosphite solutions to catalytic oxidation with oxygen or air. More particularly, oxygen or air in stoichiometric excess proportions is introduced into the aqueous alkali metal phosphite solution at about 30.degree. to 110.degree. C., at a pH-value of 0 to about 8, and in the presence of SiO.sub.2 or aluminum silicate containing at most 10 weight % Al.sub.2 O.sub.3, for as long as necessary to achieve conversion of the alkali metal phosphite to alkai metal phosphate. After completion of the oxidation, the aqueous solution is separated from the catalyst.
    • 本发明涉及通过使碱金属亚磷酸盐水溶液用氧气或空气进行催化氧化来制备碱金属磷酸盐水溶液的方法。 更具体地说,在约30℃至110℃,pH值为0至约8的条件下,在含碱金属亚磷酸盐水溶液中的化学计量过量的氧气或空气中,在含有 至多10重量%的Al 2 O 3,只要需要实现碱金属亚磷酸盐转化为磷酸金属。 氧化完成后,将水溶液与催化剂分离。
    • 40. 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。