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    • 3. 发明申请
    • VERFAHREN ZUR HERSTELLUNG VON ALPHA-HYDROXYCARBONSÄUREN
    • 用于生产α-羟基羧酸
    • WO2008009503A1
    • 2008-01-24
    • PCT/EP2007/055072
    • 2007-05-25
    • EVONIK RÖHM GMBHACKERMANN, JochenMAY, AlexanderGROPP, UdoSIEGERT, HermannVOGEL, BerndBRÖCKER, Sönke
    • ACKERMANN, JochenMAY, AlexanderGROPP, UdoSIEGERT, HermannVOGEL, BerndBRÖCKER, Sönke
    • C07C67/20C07C67/54C07C69/675
    • C07C67/20C07C67/54C07C69/675
    • Kontinuierliches Verfahren zur Herstellung von alpha-Hydroxycarbonsäureestern, bei welchem man als Edukte alpha-Hydroxycarbonsäureamid mit einem Alkohol in Gegenwart eines Katalysators unter Erhalt einer Produktmischung umsetzt, die alpha-Hydroxycarbonsäureester, Ammoniak, nicht umgesetztes alpha- Hydroxycarbonsäureamid sowie Alkohol und Katalysator, aufweist; wobei man a') Eduktströme umfassend als Edukte ein alpha- Hydroxycarbonsäureamid, einen Alkohol und einen Katalysator in einen Druckreaktor einspeist; b') die Eduktströme im Druckreaktor bei einem Druck im Bereich von 1 bar bis 100 bar miteinander umsetzt; c') die aus Schritt b) resultierende Produktmischung aufweisend alpha-Hydroxycarbonsäureester, nicht umgesetztes alpha-Hydroxycarbonsäureamid und Katalysator sowie Ammoniak und Alkohol aus dem Druckreaktor ausschleust; und d') die Produktmischung an Alkohol und Ammoniak abreichert, wobei Ammoniak bei einem Druck, der ständig größer als 1 bar gehalten wird, ohne Zuhilfenahme von zusätzlichen Strip-Mitteln abdestilliert wird. Das kontinuierliche Verfahren ist mit besonderem Vorteil großtechnisch anwendbar.
    • 用于制备α-羟基羧酸酯,的连续方法,其中所述起始材料的α-羟基羧酸酰胺在催化剂的存在下与醇,α-羟基酸,氨,未反应的α-羟基羧酰胺以及醇和催化剂,其包括反应,得到的产物混合物; 其中之一的“),其包括进料作为反应物,α-羟基羧酰胺,醇,并在压力反应器中的催化剂进料流; B“)在1巴的反应器压力为100巴的反应物流反应的范围内的压力; c“)中由步骤b得到的,包括α-羟基羧酸酯,未反应的α-羟基羧酸和催化剂,以及氨和醇从压力反应器产物混合物中)ausschleust; 和d“)的产物混合物在醇和氨,其中氨是在其被恒定地保持大于1巴无需其他汽提装置的帮助的压力蒸馏除去耗尽。 的连续方法在工业上是可应用特别有利。
    • 6. 发明申请
    • PROCESS FOR PREPARATION OF METHACRYLIC ACID AND METHACRYLIC ACID ESTERS
    • 制备甲基丙烯酸和甲基丙烯酸酯的方法
    • WO2013037136A1
    • 2013-03-21
    • PCT/CN2011/079776
    • 2011-09-16
    • EVONIK ROEHM GMBHSCHAEFER, HenningJONES, Jerald ASIEGERT, HermannBALDUF, Torsten
    • SCHAEFER, HenningJONES, Jerald ASIEGERT, HermannBALDUF, Torsten
    • C07C51/48C07C67/08C07C57/04C07C69/54B01D11/00
    • B01D11/043C07C29/10C07C51/48C07C31/04C07C57/04
    • The invention relates to a process for preparation of at least one of methacrylic acid and a methacrylic acid ester, and a process for treatment of an aqueous phase comprising at least one organic compound comprising process steps: a1) gas phase oxidation of at least one C 4 compound to obtain a reaction phase comprising methacrylic acid; a2) quenching of the reaction phase to obtain a crude aqueous phase comprising methacrylic acid; a3) extraction of at least a part of the methacrylic acid from the crude aqueous phase comprising methacrylic acid into an organic solvent to obtain a crude organic phase comprising methacrylic acid and a first aqueous phase, wherein the first aqueous phase comprises components i. at least 65 wt.%, preferably in the range of from 65 wt.% to 99.9 wt.%, more preferably in the range of from 70 wt.% to 99.8 wt.% water, yet more preferably in the range of from 75 wt.% to 99 wt.%, more preferably in the range of from 76 wt.% to 98.5 wt.%, more preferably in the range of from 77 wt.% to 98 wt.%, even more preferably in the range of from 78 wt.% to 97.5 wt.%, even more preferably in the range of from 79 wt.% to 95 wt.%, yet more preferably in the range of from 80 wt.% to 90 wt.% water, based on the total weight of the first aqueous phase, and ii. not more than 35 wt.%, preferably in the range of from 0.1 wt.% to 35 wt.%, preferably in the range of from 0.2 wt.% to 30 wt.%, more preferably in the range of from 1 wt.% to 25 wt.%, yet more preferably in the range of from 1.5 wt.% to 24 wt.%, more preferably in the range of from 2 wt.% to 23 wt.%, even more preferably in the range of from 2.5 wt.% to 22 wt.%, even more preferably in the range of from 5 wt.% to 21 wt.%, yet more preferably in the range of from 10 wt.% to 20 wt.% of at least one organic compound other than the organic solvent used as extraction agent in process step a3), based on the total weight of the first aqueous phase, wherein the sum of the weight amounts of i. and ii. is 100 wt.%; a4) separation and optionally purification of at least a part of the methacrylic acid from the crude organic phase obtained in process step a3); a5) optionally, esterification of at least a part of the methacrylic acid obtained in step a4); b) extraction of at least a part of, preferably all of the first aqueous phase obtained in step a3) with an extraction agent to form an extraction phase comprising component ii. and a second aqueous phase, the second aqueous phase being depleted in component ii. compared to the first aqueous phase; c) at least partial separation of the second aqueous phase obtained in step b) from the extraction phase obtained in step b); d) optionally, at least partial separation of at least one organic compound from the second aqueous phase obtained in step c), to obtain a third aqueous phase which is depleted in at least one organic compound compared to the second aqueous phase. e) optionally, separation of at least a part of the extraction agent from the extraction phase to obtain an extract comprising at least one component ii..
    • 本发明涉及一种制备甲基丙烯酸和甲基丙烯酸酯中的至少一种的方法,以及一种包含至少一种有机化合物的水相处理方法,包括以下步骤:a1)至少一种C4的气相氧化 化合物以获得包含甲基丙烯酸的反应相; a2)淬灭反应相以获得包含甲基丙烯酸的粗水相; a3)将甲基丙烯酸的至少一部分从包含甲基丙烯酸的粗制水相中提取到有机溶剂中以获得包含甲基丙烯酸和第一水相的粗有机相,其中所述第一水相包含组分i。 至少65重量%,优选在65重量%至99.9重量%的范围内,更优选在70重量%至99.8重量%的水范围内,还更优选在75重量% 重量百分比至99重量%,更优选在76重量%至98.5重量%的范围内,更优选在77重量%至98重量%的范围内,甚至更优选在 从78重量%至97.5重量%,甚至更优选在79重量%至95重量%的范围内,还更优选在80重量%至90重量%的水范围内,基于 第一水相的总重量,和ii。 不超过35重量%,优选在0.1重量%至35重量%的范围内,优选在0.2重量%至30重量%的范围内,更优选在1重量%至30重量%的范围内。 %至25重量%,还更优选在1.5重量%至24重量%的范围内,更优选在2重量%至23重量%的范围内,甚至更优选在 至少一种有机物的重量百分数为2.5%至22%,甚至更优选为5%至21%,还有更优选为10%至20% 在工艺步骤a3)中用作提取剂的有机溶剂以外的化合物,基于第一水相的总重量,其中i。 和ii。 为100重量%; a4)从方法步骤a3)中获得的粗有机相中分离和任选地纯化至少一部分甲基丙烯酸; a5)任选地,在步骤a4)中获得的至少一部分甲基丙烯酸的酯化; b)用提取剂萃取步骤a3)中获得的至少一部分,优选全部第一水相,以形成包含组分ii的萃取相。 和第二水相,第二水相在组分ii中耗尽。 与第一水相相比; c)将步骤b)中获得的第二水相与步骤b)中获得的萃取相至少部分分离; d)任选地,至少部分分离步骤c)中获得的第二水相中的至少一种有机化合物,以获得与第二水相相比耗尽至少一种有机化合物的第三水相。 e)任选地,将至少一部分萃取剂与提取相分离以获得包含至少一种组分的提取物。