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    • 1. 发明申请
    • PROCESS FOR PREPARATION OF METHACRYLIC ACID AND METHACRYLIC ACID ESTER
    • 制备甲基丙烯酸和甲基丙烯酸酯的方法
    • WO2013037131A1
    • 2013-03-21
    • PCT/CN2011/079764
    • 2011-09-16
    • EVONIK ROEHM GMBHJONES, Jerald ABALDUF, TorstenSCHAEFER, Henning
    • JONES, Jerald ABALDUF, TorstenSCHAEFER, Henning
    • C07C51/42C07C51/43C07C51/44C07C51/48C07C67/08C07C69/54C07C57/04C07C57/07B01D9/00B01D11/00
    • B01D9/0013B01D9/0045C07C51/48C07C67/08C07C67/52C07C67/58C07C57/04C07C69/54
    • 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, based on the total weight of the first aqueous phase, wherein the sum of the weight amounts of i. and ii. is 100 wt.%; 200700659 4 a4) separation and optionally purification of at least a part of the methacrylic acid from the crude organic phase comprising methacrylic acid; a5) optionally, esterification of at least a part of the methacrylic acid obtained in step a4); b) crystallisation of at least a part of the water from at least a part of the first aqueous phase obtained in process step a3) to form a crystallised aqueous phase as second aqueous phase and a mother liquor, wherein the mother liquor comprises at least one component ii.; c) at least partial separation of the crystallised aqueous phase from the mother liquor.
    • 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)至少一个C的气相氧化 4化合物,得到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% 基于第一水相的总重量,除了用作萃取剂的有机溶剂之外的化合物,其中i。 和ii。 为100重量%; a)从包含甲基丙烯酸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)从方法步骤a3)中获得的至少一部分第一水相结晶至少一部分水,形成作为第二水相和母液的结晶水相,其中母液包含至少一种 组分ii; c)将结晶的水相与母液至少部分分离。
    • 2. 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。
    • 3. 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
    • WO2013037134A1
    • 2013-03-21
    • PCT/CN2011/079774
    • 2011-09-16
    • EVONIK ROEHM GMBHSCHAEFER, HenningBALDUF, Torsten
    • SCHAEFER, HenningBALDUF, Torsten
    • C07C51/42C07C51/43C07C51/44C07C51/48C07C67/08C07C69/54C07C57/04C07C57/07B01D9/00B01D11/00
    • B01D9/0045B01D9/0013B01D9/0036C07C29/10C07C51/42C07C51/43C07C51/44C07C51/48C07C31/04C07C57/04
    • The invention relates to a process for preparation of at least one of methacrylic acid and a methacrylic acid ester, 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. 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 wt.% to 20 wt.% of at least one organic compound, 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 comprising methacrylic acid; 200700658 55 a5) optionally, esterification of at least a part of the methacrylic acid obtained in step a4); b) separation of at least a part of the water comprised in the first aqueous phase obtained in step a3) from at least a part of at least one component ii. to obtain a second aqueous phase and an organic phase, wherein the organic phase comprises at least one component ii., and wherein the second aqueous phase is depleted in at least one component ii. compared to the first aqueous phase; c) optionally, separation of at least a part of at least one organic compound from the second aqueous phase obtained in process step b) to obtain a third aqueous phase; d) optionally, separation of at least a part of at least one component ii from the organic phase obtained in process step b), to a process for treatment of an aqueous phase comprising at least one organic compound, and a device for production of at least one of methacrylic acid and a methacrylic ester.
    • 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,包括步骤:a1)至少一种C 4化合物的气相氧化,得到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萃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%的范围内,基于 第一水相的总重量,和ii。 不大于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.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比至重量百分比至重量百分比至二十二重量百分比,甚至更优选约5重量%至21重量%,还更优选至重量百分比至20重量% 化合物,基于第一水相的总重量,其中i。 和ii。 为100重量%; a4)从包含甲基丙烯酸的粗有机相中分离并任选地纯化至少一部分甲基丙烯酸; a)任选地,在步骤a4)中获得的至少一部分甲基丙烯酸酯化; b)将步骤a3)中获得的第一水相中包含的水的至少一部分与至少一种组分ii的至少一部分分离。 以获得第二水相和有机相,其中所述有机相包含至少一种组分ii。,并且其中所述第二水相在至少一种组分ii中耗尽。 与第一水相相比; c)任选地,将方法步骤b)中获得的至少一种有机化合物的至少一部分与第二水相分离以获得第三水相; d)任选地,将至少一种组分ii的至少一部分与方法步骤b)中获得的有机相分离为包含至少一种有机化合物的水相的处理方法和用于生产 甲基丙烯酸和甲基丙烯酸酯中的至少一种。