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    PROCESS FOR THE PRODUCTION OF NEOPENTYLGLYCOL USING FORMALDEHYDE WITH A LOW METHANOL CONTENT
    4.
    发明申请
    PROCESS FOR THE PRODUCTION OF NEOPENTYLGLYCOL USING FORMALDEHYDE WITH A LOW METHANOL CONTENT 审中-公开

    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.

    Process for preparing polyalcohols from formaldehyde having a low formic acid content
    5.
    发明授权
    Process for preparing polyalcohols from formaldehyde having a low formic acid content 有权
    从具有低甲酸含量的甲醛制备多元醇的方法

    公开(公告)号：US07462747B2

    公开(公告)日：2008-12-09

    申请号：US11797007

    申请日：2007-04-30

    申请人： Timan Sirch ,  Michael Steiniger ,  Steffen Maas ,  Stefan Rittinger ,  Stephan Schlitter ,  Maria Guixa ,  Todd C. Spengeman ,  Jeffrey T. Andress

    发明人： Timan Sirch ,  Michael Steiniger ,  Steffen Maas ,  Stefan Rittinger ,  Stephan Schlitter ,  Maria Guixa ,  Todd C. Spengeman ,  Jeffrey T. Andress

    IPC分类号： C07C37/20 ,  C07C27/04 ,  C07C29/14

    CPC分类号： C07C29/141 ,  C07C45/75 ,  C07C47/19 ,  C07C31/20 ,  C07C33/26

    摘要： The invention relates to a process for preparing polymethylol compounds of the formula (I) where the radicals R 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 22 carbon atoms, by condensation of aldehydes having from 2 to 24 carbon atoms with formaldehyde in an aldol reaction using tertiary amines as catalyst to form alkanals of the formula (II) where the radicals R each independently have one of the abovementioned meanings, and subsequent hydrogenation of the latter. The particular inventive feature of this process is that the aldol reaction is carried out using an aqueous formaldehyde solution having a formic acid content of

    摘要翻译： 本发明涉及一种制备式（I）的多羟甲基化合物的方法，其中基团R各自独立地为另外的羟甲基或具有1至22个碳原子的烷基或具有1至22个碳原子的芳基或芳烷基， 6至22个碳原子，通过使用叔胺作为催化剂在醛醇反应中将具有2至24个碳原子的醛与甲醛缩合形成式（II）的链烷基，其中基团R各自独立地具有上述含义之一 ，随后后者的氢化。 该方法的具体发明特征是醛醇反应使用甲酸含量<150ppm，优选<100ppm的甲醛水溶液进行。 以这种方式进行，有利地可以以目标方式防止副产物的形成，从而可以提高所需的多羟甲基化合物的产率。

    PROCESS FOR PREPARING POLYALCOHOLS FROM FORMALDEHYDE HAVING A LOW FORMIC ACID CONTENT
    6.
    发明申请
    PROCESS FOR PREPARING POLYALCOHOLS FROM FORMALDEHYDE HAVING A LOW FORMIC ACID CONTENT 有权
    由具有低酸性含量的甲醛制备多元醇的方法

    公开(公告)号：US20080167506A1

    公开(公告)日：2008-07-10

    申请号：US11797007

    申请日：2007-04-30

    申请人： Timan Sirch ,  Michael Steiniger ,  Steffen Maas ,  Stefan Rittinger ,  Stephan Schlitter ,  Maria Guixa ,  Todd C. Spengeman ,  Jeffrey T. Andress

    发明人： Timan Sirch ,  Michael Steiniger ,  Steffen Maas ,  Stefan Rittinger ,  Stephan Schlitter ,  Maria Guixa ,  Todd C. Spengeman ,  Jeffrey T. Andress

    IPC分类号： C07C29/00

    CPC分类号： C07C29/141 ,  C07C45/75 ,  C07C47/19 ,  C07C31/20 ,  C07C33/26

    摘要： The invention relates to a process for preparing polymethylol compounds of the formula (I) (HOCH2)2—C—R2   (I) where the radicals R 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 22 carbon atoms, by condensation of aldehydes having from 2 to 24 carbon atoms with formaldehyde in an aldol reaction using tertiary amines as catalyst to form alkanals of the formula (II) where the radicals R each independently have one of the abovementioned meanings, and subsequent hydrogenation of the latter. The particular inventive feature of this process is that the aldol reaction is carried out using an aqueous formaldehyde solution having a formic acid content of

    摘要翻译： 本发明涉及一种制备式（I）的多羟甲基化合物的方法，其中式（I）<？in-line-formula description =“In-line Formulas”end =“lead”→（HOCH 2 （I）<？in-line-formula description =“In-line Formulas”end =“tail”？>其中基团R各自独立地 另一个羟甲基或具有1至22个碳原子的烷基或具有6至22个碳原子的芳基或芳烷基，通过醛醛反应中具有2至24个碳原子的醛与甲醛缩合 使用叔胺作为催化剂形成式（II）的链烷基，其中基团R各自独立地具有上述含义之一，随后氢化后者。 该方法的具体发明特征是醛醇反应使用甲酸含量<150ppm，优选<100ppm的甲醛水溶液进行。 以这种方式进行，有利地可以以目标方式防止副产物的形成，从而可以提高所需的多羟甲基化合物的产率。

    Process for Preparing Polymethylols
    7.
    发明申请
    Process for Preparing Polymethylols 有权
    制备多羟基睾酮的方法

    公开(公告)号：US20110272270A1

    公开(公告)日：2011-11-10

    申请号：US13144124

    申请日：2010-01-07

    申请人： Stephan Schlitter ,  Michael Steiniger ,  Stefan Rittinger ,  Tilman Sirch ,  Steffen Maas

    发明人： Stephan Schlitter ,  Michael Steiniger ,  Stefan Rittinger ,  Tilman Sirch ,  Steffen Maas

    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。

    Method for preparing polymethylols
    8.
    发明授权
    Method for preparing polymethylols 有权
    多羟甲基纤维素的制备方法

    公开(公告)号：US08884076B2

    公开(公告)日：2014-11-11

    申请号：US13133861

    申请日：2009-12-07

    申请人： Tilman Sirch ,  Michael Steiniger ,  Steffen Maas ,  Stefan Rittinger ,  Stephan Schlitter

    发明人： Tilman Sirch ,  Michael Steiniger ,  Steffen Maas ,  Stefan Rittinger ,  Stephan Schlitter

    IPC分类号： C07C27/04 ,  C08G63/16 ,  C08G18/56 ,  C07C29/80 ,  C07C29/141 ,  C08L67/00 ,  C08L75/04

    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。

    METHOD FOR PRODUCING HYDROXY PIVALIN ALDEHYDE AND NEOPENTYL GLYCOL
    9.
    发明申请
    METHOD FOR PRODUCING HYDROXY PIVALIN ALDEHYDE AND NEOPENTYL GLYCOL 有权
    用于生产羟脯氨酸醛酸和甘氨酸的方法

    公开(公告)号：US20100113836A1

    公开(公告)日：2010-05-06

    申请号：US12529197

    申请日：2008-02-25

    申请人： Tilman Sirch ,  Michael Steiniger ,  Steffen Maas ,  Stefan Rittinger ,  Stephan Schlitter

    发明人： Tilman Sirch ,  Michael Steiniger ,  Steffen Maas ,  Stefan Rittinger ,  Stephan Schlitter

    IPC分类号： C07C45/45 ,  C07C31/20

    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。

    Process for preparing polymethylols
    10.
    发明授权
    Process for preparing polymethylols 有权
    制备多羟基甲基纤维素的方法

    公开(公告)号：US08933277B2

    公开(公告)日：2015-01-13

    申请号：US13144124

    申请日：2010-01-07

    申请人： Stephan Schlitter ,  Michael Steiniger ,  Stefan Rittinger ,  Tilman Sirch ,  Steffen Maas

    发明人： Stephan Schlitter ,  Michael Steiniger ,  Stefan Rittinger ,  Tilman Sirch ,  Steffen Maas

    IPC分类号： C07C27/28 ,  C07C29/80 ,  C07C31/24 ,  B01D3/34 ,  C07C29/141 ,  C07C45/75 ,  C07C45/82

    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℃