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    • 3. 发明授权
    • Process for preparing essentially formic acid-free N-alkyl-N′-methylalkyleneureas
    • 基本上不含无甲酸的N-烷基-N'-甲基亚烷基脲的方法
    • US06554966B1
    • 2003-04-29
    • US09603195
    • 2000-06-26
    • Andreas KramerJohann-Peter MelderHeinz RütterGünter RieweWolfgang SiegelHans-Jürgen Weyer
    • Andreas KramerJohann-Peter MelderHeinz RütterGünter RieweWolfgang SiegelHans-Jürgen Weyer
    • B01D300
    • C07D239/10
    • The invention relates to a process for preparing essentially formic acid-free N-alkyl-N′-methylalkyleneureas of the formula with R1=H or CH3, R2=CnH2n+1 with n=1-4 and x=0 or 1, from the corresponding alkyleneureas by reaction with monomeric or polymerized formaldehyde in the presence of formic acid. This entails feeding the mixture, obtained in the reaction, of N-alkyl-N′-methylalkyleneurea and formic acid to the upper region of a distillation column, distilling without further additions and removing essentially formic acid-free N-alkyl-N′-methylalkyleneurea in the lower region of the column. The process parameters are set so that the pressure in the upper region of the column is at a higher level than in the lower region of the column, and the difference in pressure between the upper and lower regions of the column is from 10 to 100 mbar, and the temperature in the lower region of the column is higher than in the upper region of the column, with the difference in temperature between the upper and lower regions of the column being from 40° C. to 210° C.
    • 本发明涉及一种制备基本上无甲酸的N-烷基-N'-甲基亚烷基脲的方法,其中R1 = H或CH3,R2 = CnH2n + 1,其中n = 1-4和x = 0或1, 通过在甲酸存在下与单体或聚合的甲醛反应来制备相应的亚烷基脲。 这需要将N-烷基-N'-甲基亚烷基脲和甲酸的反应混合物加入到蒸馏塔的上部区域,无需进一步添加即可蒸馏除去基本上不含甲酸的N-烷基-N'- 甲基亚烷基脲在柱的下部区域。 设定工艺参数使得塔的上部区域中的压力处于比塔的下部区域更高的水平,并且塔的上部和下部区域之间的压力差为10至100mbar ,塔的下部区域的温度高于塔的上部区域,塔的上部和下部区域之间的温度差为40℃〜210℃。
    • 4. 发明授权
    • Processes for preparing ethylamines
    • 制备乙胺的方法
    • US07642382B2
    • 2010-01-05
    • US11908820
    • 2006-03-14
    • Till GerlachFrank HaeseAnton MeierJohann-Peter MelderHeinz Rütter
    • Till GerlachFrank HaeseAnton MeierJohann-Peter MelderHeinz Rütter
    • C07C209/16
    • C07C209/16C07C211/05
    • Processes comprising: (a) providing a first reactant comprising a bioethanol; and (b) reacting the first reactant with a second reactant comprising a component selected from the group consisting of ammonia, primary amines, secondary amines and mixtures thereof, in the presence of hydrogen and a catalytically effective amount of a heterogeneous hydrogenation/dehydrogenation catalyst to form an ethylamine; wherein the catalyst has been activated at a temperature of 100 to 500° C. for at least 25 minutes; wherein prior to activation the catalyst comprises: (i) 20 to 65% by weight of a support material comprising one or both of zirconium dioxide (ZrO2) and aluminum oxide (Al2O3), (ii) 1 to 30% by weight of oxygen-comprising compounds of copper, calculated as CuO, and (iii) 21 to 70% by weight of oxygen-comprising compounds of nickel, calculated as NiO; and wherein after activation the catalyst has a CO uptake capacity of >110 μmol of CO/g of the catalyst.
    • 方法包括:(a)提供包含生物乙醇的第一反应物; 和(b)使第一反应物与包含选自氨,伯胺,仲胺及其混合物的组分的第二反应物在氢气和催化有效量的非均相氢化/脱氢催化剂存在下反应至 形成乙胺; 其中所述催化剂已经在100至500℃的温度下活化至少25分钟; 其中在活化之前,催化剂包括:(i)20至65重量%的包含二氧化锆(ZrO 2)和氧化铝(Al 2 O 3)中的一种或两种的载体材料,(ii)1至30重量% 包括以CuO计算的铜化合物,和(iii)以NiO计算的含有21重量%的含氧化合物的镍; 并且其中在活化后,催化剂的CO吸收能力为> 110molol的CO / g催化剂。
    • 8. 发明申请
    • Method for producing an ethylamine
    • 乙胺的制造方法
    • US20090234163A1
    • 2009-09-17
    • US11908820
    • 2006-03-14
    • Till GerlachFrank HaeseAnton MeierJohann-Peter MelderHeinz Rütter
    • Till GerlachFrank HaeseAnton MeierJohann-Peter MelderHeinz Rütter
    • C07C209/16
    • C07C209/16C07C211/05
    • Processes comprising: (a) providing a first reactant comprising a bioethanol; and (b) reacting the first reactant with a second reactant comprising a component selected from the group consisting of ammonia, primary amines, secondary amines and mixtures thereof, in the presence of hydrogen and a catalytically effective amount of a heterogeneous hydrogenation/dehydrogenation catalyst to form an ethylamine; wherein the catalyst has been activated at a temperature of 100 to 500° C. for at least 25 minutes; wherein prior to activation the catalyst comprises: (i) 20 to 65% by weight of a support material comprising one or both of zirconium dioxide (ZrO2) and aluminum oxide (Al2O3), (ii) 1 to 30% by weight of oxygen-comprising compounds of copper, calculated as CuO, and (iii) 21 to 70% by weight of oxygen-comprising compounds of nickel, calculated as NiO; and wherein after activation the catalyst has a CO uptake capacity of >110 μmol of CO/g of the catalyst.
    • 方法包括:(a)提供包含生物乙醇的第一反应物; 和(b)使第一反应物与包含选自氨,伯胺,仲胺及其混合物的组分的第二反应物在氢气和催化有效量的非均相氢化/脱氢催化剂存在下反应至 形成乙胺; 其中所述催化剂已经在100至500℃的温度下活化至少25分钟; 其中在活化之前,催化剂包括:(i)20至65重量%的包含二氧化锆(ZrO 2)和氧化铝(Al 2 O 3)中的一种或两种的载体材料,(ii)1至30重量% 包括以CuO计算的铜化合物,和(iii)以NiO计算的含有21重量%的含氧化合物的镍; 并且其中在活化后,催化剂的CO吸收能力为> 110molol的CO / g催化剂。
    • 9. 发明授权
    • Process for fractionating water-containing crude amine mixtures from amine synthesis
    • 从胺合成分馏含水粗胺混合物的方法
    • US06986833B2
    • 2006-01-17
    • US10272011
    • 2002-10-17
    • Andreas WölfertHeinz RütterStefan RittingerMark WehingerAurelie AlemanyWilli Schmidt
    • Andreas WölfertHeinz RütterStefan RittingerMark WehingerAurelie AlemanyWilli Schmidt
    • B01D3/14C07C209/84
    • C07D295/03C07C209/86C07D207/04C07D211/04Y10S203/20C07C211/04C07C211/08
    • An amine-containing mixture containing one or more amines, water, low-boilers and optionally high-boilers is fractionated by a process having the steps (iii) and (iv) and optionally the steps (i), (ii) and (v): (i) a (first) low-boiler fraction is separated off from the amine-containing mixture by distillation, (ii) a (first) high-boiler fraction is separated off from the amine-containing mixture by distillation, (iii) the amine-containing mixture is extracted with sodium hydroxide solution, producing an aqueous, sodium-hydroxide-containing first phase and an aqueous-organic, amine-, (further) low-boiler- and possibly (further) high-boiler-containing second phase, (iv) the aqueous-organic second phase, is distilled, producing essentially anhydrous amine as bottom-phase take off or sidestream takeoff in the stripping part of the distillation column, an amine/water azeotrop as sidestream takeoff in the enrichment part of the column and a (further) low-boiler fraction as overhead takeoff, and recycling the amine/water azeotrop to the extraction step (iii), (v) the essentially anhydrous amine is further purified of fractionated.
    • 含有一种或多种胺,水,低锅炉和任选的高锅炉的含胺混合物通过具有步骤(iii)和(iv)和任选的步骤(i),(ii)和(v ):(i)(第一)低沸点馏分通过蒸馏从含胺混合物中分离出来,(ii)通过蒸馏将(第一)高沸点级分馏分与含胺混合物分离,(iii) )将含胺混合物用氢氧化钠溶液萃取,产生含氢氧化钠的含水氢氧化物的第一相和含水有机胺,(进一步)低沸点和可能(进一步)含高沸点的 第二相,(iv)蒸馏有机相第二相,在蒸馏塔的汽提部分中产生基本上无水的胺作为底部脱气或侧流起飞,在富集部分中作为侧流起飞的胺/水共沸物 的柱和另外的低沸点馏分作为架空起飞, 并将胺/水共沸物再循环至提取步骤(iii),(v)将基本上无水的胺进一步纯化分离。