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公开(公告)号：US20070282135A1
公开(公告)日：2007-12-06
申请号：US11447020
申请日：2006-06-06
申请人： Steffen Maas , Thorsten Johann , Michael Koch , Tilman Sirch , Stephan Schlitter , Stefan Rittinger , Michael Steiniger , Todd C. Spengeman
发明人： Steffen Maas , Thorsten Johann , Michael Koch , Tilman Sirch , Stephan Schlitter , Stefan Rittinger , Michael Steiniger , Todd C. Spengeman
IPC分类号： C07C45/62
CPC分类号： C07C29/141 , C07C31/20
摘要： Process for the catalytic hydrogenation of methylolalkanals of the general formula where R1 and R2 are each, independently of one another, a further methylol group or an alkyl group having from 1 to 22 carbon atoms or an aryl or aralkyl group having from 6 to 33 carbon atoms, in the liquid phase by means of hydrogen over a hydrogenation catalyst, wherein hydrogen is used in a molar ratio to methylolalkanal of greater than 1.
摘要翻译： 用于通式的羟甲基烷烃的催化氢化方法其中R 1和R 2各自彼此独立地是另外的羟甲基或具有1个 至22个碳原子或具有6至33个碳原子的芳基或芳烷基，在液相中通过氢气在氢化催化剂上氢化，其中氢以与羟甲基烷醛的摩尔比大于1。
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公开(公告)号：US20110272270A1
公开(公告)日：2011-11-10
申请号：US13144124
申请日：2010-01-07
IPC分类号： B01D3/36
CPC分类号： C07C29/80 , C07C29/141 , C07C45/75 , C07C45/82 , C07C31/22 , C07C31/245 , C07C47/19
摘要： The present invention relates to a process for recovering components from a low boiler mixture which is obtained in the distillation of hydrogenation effluents from the preparation of polymethylols, by multistage distillation of the low boiler mixture comprising a tertiary amine, water, methanol, polymethylol of the formula (I) methylolalkanal of the formula (II) alcohol of the formula (III) and an alkanal with a methylene group in the α position to the carbonyl group, and in which each R is independently a further methylol group or an alkyl group having 1 to 22 carbon atoms or an aryl or aralkyl group having 6 to 22 carbon atoms, a first distillation stage involving separating the low boiler mixture into a higher-boiling, predominantly water-rich fraction and into a lower-boiling aqueous organic fraction comprising the tertiary amine, and the second distillation stage involving separating the aqueous organic fraction from the first distillation stage into a predominantly amine-containing fraction and a further amine-depleted fraction, wherein the tertiary amine is trimethylamine or triethylamine, and the bottom temperature in the second distillation stage is 110° C. and more.
摘要翻译： 本发明涉及一种从低沸点混合物中回收组分的方法，该方法是从多羟甲基的制备中蒸馏氢化流出物获得的，通过多级蒸馏包含叔胺，水，甲醇，多羟甲基的低沸点混合物 式（I）式（II）醇的式（I）的羟甲基烷醛和式（III）的醇的亚烷基与在羰基的α位上具有亚甲基的链烷醛，其中每个R独立地是另外的羟甲基或具有 1至22个碳原子或具有6至22个碳原子的芳基或芳烷基，第一蒸馏阶段包括将低锅炉混合物分离成较高沸点，主要是富水部分和低沸点含水有机部分， 叔胺，第二蒸馏阶段将含水有机部分从第一蒸馏阶段分离成主要是胺 其中叔胺为三甲胺或三乙胺，第二蒸馏阶段的底部温度为110℃以上。
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公开(公告)号：US08884076B2
公开(公告)日：2014-11-11
申请号：US13133861
申请日：2009-12-07
CPC分类号： C07C29/141 , C07C29/80 , C08G18/56 , C08G63/16 , C08L67/00 , C08L75/04 , C07C31/245 , C07C31/20 , C07C31/22
摘要： The present invention relates to a process for distilling an aqueous polymethylol mixture which comprises a polymethylol of the formula (I) (HOCH2)2—C—R2 (I) in which each R is independently a further methylol group or an alkyl group having 1 to 22 carbon atoms or an aryl or aralkyl group having 6 to 22 carbon atoms, a tertiary amine, water and the adduct of tertiary amine and formic acid (amine formate), which comprises performing the distillation in a distillation column which is connected at the bottom to an evaporator, the bottom temperature being above the evaporation temperature of the monoester of formic acid and polymethylol (polymethylol formate) which forms during distillation. The present invention further relates to a composition comprising polymethylol and 1 to 10 000 ppm by weight of polymethylol formate, and to the use thereof.
摘要翻译： 本发明涉及一种蒸馏水性多羟甲基混合物的方法，该方法包括式（I）的多羟甲基（HOCH 2）2 -C-R 2（I），其中每个R独立地是另外的羟甲基或具有1 至22个碳原子或具有6至22个碳原子的芳基或芳烷基，叔胺，水和叔胺和甲酸（甲酸胺）的加合物，其包括在蒸馏塔中进行蒸馏，所述蒸馏塔在 底部到蒸发器，底部温度高于在蒸馏期间形成的甲酸和多羟甲基（多羟甲基甲酸酯）的单酯的蒸发温度。 本发明还涉及一种包含多羟甲基和1-10万重量ppm的多羟甲基甲酸酯的组合物及其用途。
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公开(公告)号：US20100113836A1
公开(公告)日：2010-05-06
申请号：US12529197
申请日：2008-02-25
CPC分类号： C07C45/75 , C07C29/141 , C07C45/82 , C07C47/19 , C07C31/20
摘要： The preparation of hydroxypivalaldehyde is effected by aldolizing isobutyraldehyde with formaldehyde and subsequently working up the resulting reaction effluent by distillation, wherein the reaction effluent is fed to a distillation column which is operated at a top pressure in the range from 0.5 to 1.5 bar and in which a two-stage condensation is provided in the top region, in which the vapors are first conducted into a partial condenser operated at a temperature in the range from 50 to 80° C., whose condensate is recycled at least partly into the distillation column, and in which the vapors uncondensed in the partial condenser are fed to a downstream condenser operated at a temperature in the range from −40 to +30° C., whose condensate is at least partly discharged.
摘要翻译： 羟基新戊醛的制备通过用甲醛醛化异丁醛和随后通过蒸馏处理所得反应流出物来实现，其中将反应流出物进料到蒸馏塔中，该蒸馏塔在0.5-1.5巴的最高压力下操作，其中 在顶部区域中提供两级冷凝，其中蒸气首先被导入到在50-80℃的温度下操作的部分冷凝器，其冷凝物至少部分地再循环到蒸馏塔中， 并且其中在部分冷凝器中未冷凝的蒸气被供给到在-40至+ 30℃的温度范围内操作的下游冷凝器，其冷凝物至少部分地排出。
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公开(公告)号：US08933277B2
公开(公告)日：2015-01-13
申请号：US13144124
申请日：2010-01-07
CPC分类号： C07C29/80 , C07C29/141 , C07C45/75 , C07C45/82 , C07C31/22 , C07C31/245 , C07C47/19
摘要： A process is provided for recovering components from a low boiler mixture which is obtained in the distillation of hydrogenation effluents from the preparation of polymethylols, by multistage distillation of the low boiler mixture having a tertiary amine, water, methanol, a polymethylol, a methylolalkanal, an alcohol and an alkanal with a methylene group in the alpha position to the carbonyl group. A first distillation stage involves separating the low boiler mixture into a higher-boiling, predominantly water-rich fraction and into a lower-boiling aqueous organic fraction having the tertiary amine. A second distillation stage involves separating the aqueous organic fraction from the first distillation stage into a predominantly amine-containing fraction and a further amine-depleted fraction. The tertiary amine is trimethylamine or triethylamine and the bottom temperature in the second distillation stage is at least 110° C.
摘要翻译： 提供了一种从低沸点混合物中回收组分的方法，该组合物是从制备聚羟甲基的蒸馏氢化流出液中获得的，通过多级蒸馏具有叔胺，水，甲醇，多羟甲基，羟甲基烷醛， 醇和与在羰基的α位置具有亚甲基的链烷烃。 第一蒸馏阶段包括将低沸点混合物分离成较高沸点，主要是富水级分并进入具有叔胺的低沸点含水有机部分。 第二蒸馏阶段包括从第一蒸馏阶段将含水有机部分分离成主要是含胺的馏分和另外的胺消耗部分。 叔胺是三甲胺或三乙胺，第二蒸馏阶段的底部温度至少为110℃
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公开(公告)号：US20120004472A1
公开(公告)日：2012-01-05
申请号：US13133861
申请日：2009-12-07
CPC分类号： C07C29/141 , C07C29/80 , C08G18/56 , C08G63/16 , C08L67/00 , C08L75/04 , C07C31/245 , C07C31/20 , C07C31/22
摘要： The present invention relates to a process for distilling an aqueous polymethylol mixture which comprises a polymethylol of the formula (I) (HOCH2)2—C—R2 (I) in which each R is independently a further methylol group or an alkyl group having 1 to 22 carbon atoms or an aryl or aralkyl group having 6 to 22 carbon atoms, a tertiary amine, water and the adduct of tertiary amine and formic acid (amine formate), which comprises performing the distillation in a distillation column which is connected at the bottom to an evaporator, the bottom temperature being above the evaporation temperature of the monoester of formic acid and polymethylol (polymethylol formate) which forms during distillation. The present invention further relates to a composition comprising polymethylol and 1 to 10 000 ppm by weight of polymethylol formate, and to the use thereof.
摘要翻译： 本发明涉及一种蒸馏水性多羟甲基混合物的方法，该方法包括式（I）的多羟甲基（HOCH 2）2 -C-R 2（I），其中每个R独立地是另外的羟甲基或具有1 至22个碳原子或具有6至22个碳原子的芳基或芳烷基，叔胺，水和叔胺和甲酸（甲酸胺）的加合物，其包括在蒸馏塔中进行蒸馏，所述蒸馏塔在 底部到蒸发器，底部温度高于在蒸馏期间形成的甲酸和多羟甲基（多羟甲基甲酸酯）的单酯的蒸发温度。 本发明还涉及一种包含多羟甲基和1-10万重量ppm的多羟甲基甲酸酯的组合物及其用途。
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公开(公告)号：US07767865B2
公开(公告)日：2010-08-03
申请号：US12529197
申请日：2008-02-25
CPC分类号： C07C45/75 , C07C29/141 , C07C45/82 , C07C47/19 , C07C31/20
摘要： The preparation of hydroxypivalaldehyde is effected by aldolizing isobutyraldehyde with formaldehyde and subsequently working up the resulting reaction effluent by distillation, wherein the reaction effluent is fed to a distillation column which is operated at a top pressure in the range from 0.5 to 1.5 bar and in which a two-stage condensation is provided in the top region, in which the vapors are first conducted into a partial condenser operated at a temperature in the range from 50 to 80° C., whose condensate is recycled at least partly into the distillation column, and in which the vapors uncondensed in the partial condenser are fed to a downstream condenser operated at a temperature in the range from −40 to +30° C., whose condensate is at least partly discharged.
摘要翻译： 羟基新戊醛的制备通过用甲醛醛化异丁醛和随后通过蒸馏处理所得反应流出物来实现，其中将反应流出物进料到蒸馏塔中，该蒸馏塔在0.5-1.5巴的最高压力下操作，其中 在顶部区域中提供两级冷凝，其中蒸气首先被导入到在50-80℃的温度下操作的部分冷凝器，其冷凝物至少部分地再循环到蒸馏塔中， 并且其中在部分冷凝器中未冷凝的蒸气被供给到在-40至+ 30℃的温度范围内操作的下游冷凝器，其冷凝物至少部分地排出。
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公开(公告)号：US20090069604A1
公开(公告)日：2009-03-12
申请号：US12279792
申请日：2007-02-23
申请人： Steffen Maas , Thorsten Johann , Michael Koch , Tilman Sirch , Stephan Schlitter , Stefan Rittinger , Michael Steiniger
发明人： Steffen Maas , Thorsten Johann , Michael Koch , Tilman Sirch , Stephan Schlitter , Stefan Rittinger , Michael Steiniger
IPC分类号： C07C45/62
CPC分类号： C07C29/141 , C07C31/20 , C07C31/22 , C07C31/245
摘要： A process for catalytically hydrogenating methylolalkanals of the general formula in which R1 and R2 are each independently a further methylol group or an alkyl group having from 1 to 22 carbon atoms or an aryl or aralkyl group having from 6 to 33 carbon atoms, in the liquid phase over a hydrogenation catalyst, which comprises setting a pH of from 7.0 to 9.0 in the hydrogenation effluent by adding at least one tertiary amine, an inorganic base or an inorganic or organic acid to the hydrogenation feed.
摘要翻译： 一种催化氢化通式的羟甲基烷烃的方法，其中R 1和R 2各自独立地为在另外的羟甲基或具有1至22个碳原子的烷基或具有6至33个碳原子的芳基或芳烷基，在液体 其包括通过向氢化进料中加入至少一种叔胺，无机碱或无机或有机酸将氢化流出物中的pH设定为7.0至9.0来进行。
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公开(公告)号：US07388116B2
公开(公告)日：2008-06-17
申请号：US11447020
申请日：2006-06-06
申请人： Steffen Maas , Thorsten Johann , Michael Koch , Tilman Sirch , Stephan Schlitter , Stefan Rittinger , Michael Steiniger , Todd C Spengeman
发明人： Steffen Maas , Thorsten Johann , Michael Koch , Tilman Sirch , Stephan Schlitter , Stefan Rittinger , Michael Steiniger , Todd C Spengeman
IPC分类号： C07C27/04
CPC分类号： C07C29/141 , C07C31/20
摘要： Process for the catalytic hydrogenation of methylolalkanals of the general formula where R1 and R2 are each, independently of one another, a further methylol group or an alkyl group having from 1 to 22 carbon atoms or an aryl or aralkyl group having from 6 to 33 carbon atoms, in the liquid phase by means of hydrogen over a hydrogenation catalyst, wherein hydrogen is used in a molar ratio to methylolalkanal of greater than 1.
摘要翻译： 用于通式的羟甲基烷烃的催化氢化方法其中R 1和R 2各自彼此独立地是另外的羟甲基或具有1个 至22个碳原子或具有6至33个碳原子的芳基或芳烷基，在液相中通过氢气在氢化催化剂上氢化，其中氢以与羟甲基烷醛的摩尔比大于1。
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10.发明申请公开(公告)号：US20080004475A1
公开(公告)日：2008-01-03
申请号：US11476161
申请日：2006-06-28
申请人： Tilman Sirch , Michael Steiniger , Steffen Mass , Stefan Rittinger , Stephan Schlitter , Ludwig E. Heck , Todd C. Spengeman , Jeffrey T. Andress
发明人： Tilman Sirch , Michael Steiniger , Steffen Mass , Stefan Rittinger , Stephan Schlitter , Ludwig E. Heck , Todd C. Spengeman , Jeffrey T. Andress
IPC分类号： C07C29/74
CPC分类号： C07C29/141 , C07C45/75 , C07C45/82 , C07C47/19 , C07C47/04 , C07C31/20 , C07C31/22 , C07C31/245
摘要： A process is provided for the preparation of polymethylol compounds of formula (I): (HOCH2)2—C—(R)2 , (I) in which the radicals R independently of one another are each a further methylol group, an alkyl group having from 1 to 22 C atoms or an aryl or aralkyl group having from 6 to 22 C atoms, by (a) condensing aldehydes having from 2 to 24 C atoms with formaldehyde in an aldol reaction using tertiary amines as a catalyst to give alkanals of formula (II): in which the radicals R independently of one another are each as defined above, (b) then separating, by distillation, the reaction mixture obtained into a bottom product comprising predominantly the compounds of formula II and a low-boiling stream consisting of unconverted or partially converted starting materials, and (c) hydrogenating the distillation bottom, wherein the aldol reaction is carried out with an aqueous formaldehyde solution having a methanol content of 0.35 to 0.5% by weight of methanol, the low-boiling stream is separated off at a pressure of 1 to 3 bar and temperatures of 100 to 135° C. and completely or partially recycled into the aldol reaction. This procedure advantageously makes it possible specifically to prevent the formation of by-products and hence to increase the yield of the desired polymethylol compound.We have found that this object is achieved by a process for the preparation of polymethylol compounds of formula (I): (HOCH2)2—C—(R)2 , (I) in which the radicals R independently of one another are each a further methylol group, an alkyl group having from 1 to 22 C atoms or an aryl or aralkyl group having from 6 to 22 C atoms, by (a) condensing aldehydes having from 2 to 24 C atoms with formaldehyde in an aldol reaction using tertiary amines as a catalyst to give alkanals of formula (II): in which the radicals R independently of one another are each as defined above, (b) then separating, by distillation, the reaction mixture obtained (aldolization product) into a bottom product comprising predominantly the compounds of formula II and a low-boiling stream consisting of unconverted or partially converted starting materials, and (c) hydrogenating the distillation bottom, wherein the aldol reaction is carried out with an aqueous formaldehyde solution having a methanol content of 0.35 to 0.5% by weight, the separation of the low-boiling stream is effected at a pressure of 1.1 to 3 bar, preferably 1.5 bar, and a temperature of 100 to 135° C., preferably of 102 to 125° C., and the low-boiling stream is completely or partially recycled into the aldol reaction, preferably the entire low-boiling stream being recycled. In the aldol reaction, a partially converted starting compound of formula (III): can also be formed in which the radicals R independently of one another are each hydrogen or are as defined above. According to the invention, this partially converted starting compound of formula (III), together with the desired alkanal of formula (II), is separated from the other by-products and the unreacted starting compounds and reacted again in an aldol reaction with formaldehyde having a methanol content of 0.35% by weight to 0.5% by weight, using tertiary amines as a catalyst.
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