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    Purification of esters of tetrahydro-pyran-4-carboxylic acid
    4.
    发明授权
    Purification of esters of tetrahydro-pyran-4-carboxylic acid 失效
    四氢 - 吡喃-4-羧酸酯的纯化

    公开(公告)号：US5414097A

    公开(公告)日：1995-05-09

    申请号：US185179

    申请日：1994-01-24

    申请人： Rolf Fischer ,  Norbert Goetz ,  Thomas Kuekenhoehner ,  Harald Rust ,  Werner Schnurr

    发明人： Rolf Fischer ,  Norbert Goetz ,  Thomas Kuekenhoehner ,  Harald Rust ,  Werner Schnurr

    IPC分类号： C07D309/08

    CPC分类号： C07D309/08

    摘要： A process for purifying esters of tetrahydropyran-4-carboxylic acid of the formula I ##STR1## where R.sup.1 to R.sup.3 are each C.sub.1 -C.sub.4 -alkyl, and R.sup.2 and R.sup.3 are each additionally hydrogen, from mixtures produced in the reaction of butyrolactones of the formula II ##STR2## where R.sup.2 and R.sup.3 have the abovementioned meanings, and R.sup.4 is hydrogen, alkyl of 1-6 carbons or acyl of the formula --CO--R.sup.2, with alcohols of the formula R.sup.1 OH in the presence of oxide catalysts, by distillation, which entailsa) removing overhead, in a first column with 5-25 theoretical plates with a distillate pressure of 700-1100 mbar and a distillate temperature of 50.degree.-80.degree. C., an alcohol and up to 10% of the water,b) transferring the bottom product from the first column into a second column with 18-40 theoretical plates, into which a water entrainer is metered between plates 15 and 30, and is circulated, and which operates with a distillate pressure of 35-350 mbar and a distillate temperature of 18.degree.-70.degree. C., with the esters of tetrahydropyran-4-carboxylic acid being removed between plates 8 and 18 at 90.degree.-150.degree. C., and, where appropriate,c) feeding the bottom product from the second column into a third column with 5-25 theoretical plates, and returning the overhead products at a distillate pressure of 1-100 mbar and a distillate temperature of 90.degree.-140.degree. C. to the synthesis of the esters of tetrahydropyran-4-carboxylic acid.

    摘要翻译： 用于纯化式I的四氢吡喃-4-羧酸的酯的方法，其中R 1至R 3各自为C 1 -C 4 - 烷基，R 2和R 3各自为氢， 其中R 2和R 3具有上述含义，R 4是氢，1-6个碳的烷基或式-CO-R 2的酰基，其中式R 1 OH的醇在存在下 氧化物催化剂，通过蒸馏，其需要a）在具有5-25理论塔板的第一塔中，馏出物压力为700-1100毫巴，馏出物温度为50-80℃，醇和升高 至10％的水，b）将底部产物从第一塔转移到具有18-40理论塔板的第二塔中，其中在15和30之间计量水夹带剂，并循环，并且其以 馏出液压力为35-350毫巴，馏出物温度为18-70℃， 其中四氢吡喃-4-羧酸的酯在90℃-150℃下在板8和18之间除去，并且在适当的情况下，c）将底部产物从第二塔进料到具有5-25理论值的第三塔 将塔顶馏出物返回到馏出物压力为1-100毫巴，馏出液温度为90-140℃，以合成四氢吡喃-4-羧酸酯。

    Process for preparing 1,6 hexanediol with a level of purity over 99%
    5.
    发明授权
    Process for preparing 1,6 hexanediol with a level of purity over 99% 有权
    制备纯度超过99％的1,6己二​​醇的方法

    公开(公告)号：US6008418A

    公开(公告)日：1999-12-28

    申请号：US125976

    申请日：1998-08-28

    申请人： Karl Gerhard Baur ,  Rolf Fischer ,  Rolf Pinkos ,  Frank Stein ,  Harald Rust ,  Boris Breitscheidel

    发明人： Karl Gerhard Baur ,  Rolf Fischer ,  Rolf Pinkos ,  Frank Stein ,  Harald Rust ,  Boris Breitscheidel

    IPC分类号： B01J23/80 ,  B01J23/889 ,  C07B61/00 ,  C07C29/149 ,  C07C31/20

    CPC分类号： C07C29/149

    摘要： 1,6-Hexanediol is prepared from a carboxylic acid mixture comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols which is obtained as a by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol by water extraction of the reaction mixture, by esterification of the acids and hydrogenation whereina) the monocarboxylic and dicarboxylic acids present in the aqueous dicarboxylic acid mixture are reacted with a low molecular weight alcohol to give the corresponding carboxylic esters,b) the resulting esterification mixture is freed of excess alcohol and low boilers in a first distillation stage,c) the bottoms are fractionated in a second distillation stage to give an ester fraction essentially free of 1,4-cyclohexanediols and a fraction comprising at least the major part of the 1,4-cyclohexanediols,d) the ester fraction essentially free of 1,4-cyclohexanediols is catalytically hydrogenated ande) in a pure distillation stage, 1,6-hexanediol is isolated from the hydrogenation product in a manner known per se.

    摘要翻译： PCT No.PCT / EP97 / 00980 Sec。 371日期1998年8月28日 102（e）1998年8月28日PCT PCT 1997年2月28日PCT公布。 公开号WO97 / 31882 日期1991年9月4日6,6-己二醇由包含己二酸，6-羟基己酸和少量1,4-环己二醇的羧酸混合物制备，其作为副产物在环己烷氧化成环己酮/ 环己醇通过水提取反应混合物，通过酸的酯化和氢化，其中存在于二羧酸水溶液混合物中的单羧酸和二羧酸与低分子量醇反应得到相应的羧酸酯，b）得到的 酯化混合物在第一蒸馏阶段中不含过量的醇和低沸点，c）在第二蒸馏阶段对塔底物进行分馏，得到基本上不含1,4-环己烷二醇的酯馏分和至少包含至少大部分 1,4-环己烷二醇，d）基本上不含1,4-环己烷二醇的酯馏分是催化氢化的，e）在纯蒸馏阶段， 以本身已知的方式从加氢产物中分离出1,6-己二醇。

    Separation of 1,4-butanediol from hydrogenation mixtures
    6.
    发明授权
    Separation of 1,4-butanediol from hydrogenation mixtures 失效
    从氢化混合物中分离出1,4-丁二醇

    公开(公告)号：US5342488A

    公开(公告)日：1994-08-30

    申请号：US18496

    申请日：1993-02-17

    申请人： Hans-Juergen Gosch ,  Harald Rust ,  Rolf Fischer ,  Claus Hechler ,  Rolf Pinkos

    发明人： Hans-Juergen Gosch ,  Harald Rust ,  Rolf Fischer ,  Claus Hechler ,  Rolf Pinkos

    IPC分类号： C07C29/80 ,  C07C29/82 ,  C07C31/20 ,  B01D3/00 ,  C07C27/00

    CPC分类号： C07C29/80 ,  Y10S203/20

    摘要： A process for the separation of 1,4-butanediol from mixtures obtained by the catalytic hydrogenation of maleates, fumarates, and/or succinates, which also contain tetrahydrofuran, water, C.sub.1 -C.sub.4 alcohols, succinic diesters, hydroxybutyrates, alkylhydroxyalkyl succinates, gamma-butyrolactone and butyrates, in addition to 1,4-butanediol, comprising the following steps:a) separating, in a first column having an actual number of plates of from 20 to 70 and operated at a top pressure of from 50 to 1100 mbar and preferably from 50 to 500 mbar and a top temperature of from 40.degree. to 120.degree. C., alcohol, water and tetrahydrofuran, as overhead product,b) feeding the bottom product of the first column into a second column having an actual number of plates of from 30 to 90 and withdrawing the overhead product consisting of alcohol and butyrate and obtained at a top pressure of from 45 to 250 mbar and a top temperature of from 45.degree. to 120.degree. C., and withdrawing gamma-butyrolactone and butyrates through a side outlet, and feeding the bottom product to a phase separator,c) feeding the 1,4-butanediol-enriched bottom phase of the liquid two-phase mixture coming from the phase separator to a third column having an actual number of plates of from 30 to 90, alcohol being distilled off as overhead product at a top pressure of from 45 to 250 mbar and a top temperature of from 45.degree. to 120.degree. C., and the azeotrope comprising 1,4 -butanediol and succinic diester is withdrawn as a sidestream and recycled to the phase separator, whilst 1,4-butanediol is removed together with alkyl-hydroxyalkyl succinate, butyl hydroxybutyrate, and high-boiling fractions as bottoms, andd) separating the succinate-enriched top phase in the phase separator.

    摘要翻译： 还含有四氢呋喃，水，C 1 -C 4醇，琥珀酸二酯，羟基丁酸酯，琥珀酸烷基羟基烷基酯，γ-丁内酯和/或琥珀酸酯的马来酸盐，富马酸盐和/或琥珀酸盐的催化氢化得到的混合物的分离方法， 丁内酯和丁酸酯除了1,4-丁二醇外还包括以下步骤：a）在具有20至70的实际板数的第一塔中分离并在50至1100毫巴的最高压力下操作，以及 优选为50至500毫巴，顶部温度为40至120℃，醇，水和四氢呋喃作为塔顶产物，b）将第一塔的底部产物进料到具有实际数量的板的第二塔 30至90份，并取出由醇和丁酸盐组成的塔顶产物，并在顶部压力为45至250毫巴，顶部温度为45至120℃下获得，并将γ-丁内酯和丁酸酯 通过侧出口将底部产物供给到相分离器中，c）将来自相分离器的液体两相混合物的富含1,4-丁二醇的底相进料到具有实际数量的板的第三塔 为30至90，在顶部压力为45至250毫巴，顶部温度为45至120℃的条件下，蒸馏出作为塔顶产物的醇，由1,4-丁二醇和琥珀酸二酯组成的共沸物为 作为侧流回收并循环到相分离器中，而1,4-丁二醇与琥珀酸烷基 - 羟基烷基酯，羟基丁酸丁酯和作为塔底产物的高沸点馏分一起除去，以及d）在相中分离富含琥珀酸酯的顶相 分隔器。

    Starter for the devulcanisation of scrap rubber
    7.
    发明授权
    Starter for the devulcanisation of scrap rubber 有权

    公开(公告)号：US10131760B2

    公开(公告)日：2018-11-20

    申请号：US15623599

    申请日：2017-06-15

    申请人： Harald Rust

    发明人： Harald Rust

    IPC分类号： B29B17/00 ,  C08J11/12 ,  B29B17/04 ,  B29C47/00 ,  B29C47/60 ,  C08J11/04 ,  B29K21/00 ,  B29C47/10 ,  B29C47/42 ,  B29K105/26 ,  B29K105/24

    摘要： A method of devulcanizing crosslinked rubber uses a planetary roller extruder with a central spindle, planetary spindles, a housing, and a feed part. The method includes feeding vulcanized rubber through the feed part into the housing, rotating the central spindle about its rotational axis and thereby causing the planetary spindles to rotate about their rotational axes and revolve about the central spindle. This generates mechanical and thermal stress on the vulcanized rubber by kneading and/or crushing of the vulcanized rubber, breaking or destroying the molecular chains or bonds of the vulcanized rubber. The method further includes at least one of (A) adding particles of the vulcanized rubber eccentrically to the center of the planetary roller extruder module between the planetary spindles and (B) mechanically pressing particles of the vulcanized rubber between the planetary spindles with a crammer feeder.

    Method for producing hexanediol
    10.
    发明授权
    Method for producing hexanediol 失效
    己二醇的制备方法

    公开(公告)号：US06727395B1

    公开(公告)日：2004-04-27

    申请号：US10018338

    申请日：2001-12-19

    申请人： Frank Stein ,  Thomas Krug ,  Thomas Nöbel ,  Harald Rust

    发明人： Frank Stein ,  Thomas Krug ,  Thomas Nöbel ,  Harald Rust

    IPC分类号： C07C2700

    CPC分类号： C07C29/149 ,  C07C31/20

    摘要： A process for preparing 1,6-hexanediol from a carboxylic acid mixture comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols which is obtained as by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol after water extraction of the reaction mixture followed by extraction with aqueous sodium hydroxide solution, by esterification of the acids and hydrogenation comprises a) liberating the carboxylic acids from the alkaline extract by addition of a mineral acid, b) fractionating the organic phase comprising carboxylic acids to give a distillate comprising the low molecular weight monocarboxylic acids and a residue comprising adipic acid and 6-hydroxycaproic acid, c) reacting the monocarboxylic an dicarboxylic acids present in the aqueous dicarboxylic acid mixture with a low molecular weight alcohol to give the corresponding carboxylic esters, d) freeing the esterification mixture obtained of excess alcohol and low boilers in a first distillation step, e) fractionating the bottom product in a second distillation step to give an ester fraction essentially free of 1,4-cyclohexanediols and a fraction comprising at least the major part of the 1,4-cyclohexanediols, f) catalytically hydrogenating the ester fraction which is essentially free of 1,4-cyclohexanediols and g) isolating 1,6-hexanediol from the hydrogenation product in a manner known per se in a final distillation step.

    摘要翻译： 从包含己二酸，6-羟基己酸和少量1,4-环己二醇的羧酸混合物制备1,6-己二醇的方法，其在水提取后在环己烷氧化成环己酮/环己醇时作为副产物获得 的反应混合物，然后用氢氧化钠水溶液萃取，通过酸的酯化和氢化反应，包括a）通过加入无机酸从碱性提取物中释放出羧酸，b）将包含羧酸的有机相分馏得到馏出物 包括低分子量单羧酸和包含己二酸和6-羟基己酸的残基，c）使一元羧酸与二羧酸混合物中存在的二羧酸与低分子量醇反应，得到相应的羧酸酯，d）释放 在第一馏出物中获得过量酒精和低锅炉的酯化混合物 e步骤，e）在第二蒸馏步骤中分馏底部产物，得到基本上不含1,4-环己烷二醇的酯馏分和至少包含大部分1,4-环己烷二醇的馏分，f）催化氢化酯 基本上不含1,4-环己烷二醇的馏分，和g）在最终蒸馏步骤中以本身已知的方式从氢化产物中分离出1,6-己二醇。