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1. 发明授权

US06632330B1 Process for purification of alkyl alkanoate 有权
标题翻译：纯化烷基链烷酸酯的方法
公开(公告)号：US06632330B1
公开(公告)日：2003-10-14
申请号：US09806112
申请日：2001-06-05
申请人： Stephen William Colley , Norman Harris , Colin Rathmell
发明人： Stephen William Colley , Norman Harris , Colin Rathmell
IPC分类号： B01D340
CPC分类号： C07C67/54 , C07C67/60 , C07C69/14
摘要： A process for the recovery of substantially pure alkyl alkanoate, such as ethyl acetate, from an impure feedstock. The impure feedstock is contacted with a selective hydrogenation catalyst in the presence of hydrogen in a selective hydrogenation zone maintained under selective hydrogenation conditions effective for selective hydrogenation of impurities containing reactive carbonyl groups thereby to hydrogenate the impurities to the corresponding alcohols. After recovery from the selective hydrogenation zone of a selectively hydrogenated reaction product mixture including the alkyl alkanoate and the corresponding alcohols, this is distilled in one or more distillation zones so as to produce substantially pure alkyl alkanoate therefrom which is recovered.
摘要翻译：从不纯的原料中回收基本上纯的烷基链烷酸酯如乙酸乙酯的方法。在选择性加氢区域中，在选择性加氢区域中，不纯的原料与选择性氢化催化剂接触，所述选择性加氢区域保持在有选择氢化含有反应性羰基的杂质的氢化条件下，从而将杂质氢化成相应的醇。从包括烷基链烷酸酯和相应的醇的选择性氢化反应产物混合物的选择性氢化区回收后，将其在一个或多个蒸馏区中蒸馏，从而从其中回收出基本上纯的烷基链烷酸酯。

2. 发明授权

US4795824A Process for the production of dialkyl maleates 失效
标题翻译：用于生产马来酸二烷基酯的方法
公开(公告)号：US4795824A
公开(公告)日：1989-01-03
申请号：US80060
申请日：1987-07-31
申请人： John W. Kippax , Colin Rathmell
发明人： John W. Kippax , Colin Rathmell
IPC分类号： C07C67/08 , C07C69/60 , C07C69/657 , C07C67/03
CPC分类号： C07C67/08 , C07C69/657 , Y10S203/02 , Y10S203/13
摘要： A process is described for the production of a dialkyl maleate by reaction of maleic anhydride with an alkyl alcohol in a monoesterification zone to form the corresponding monoalkyl maleate, followed by reaction of resulting monoalkyl maleate with further alkyl alcohol to form the corresponding dialkyl maleate, which includes the steps of supplying a first liquid feed comprising said monoalkyl maleate to a secondary esterification zone containing a charge of a solid esterification catalyst, supplying a second feed stream comprising said alkyl alcohol to said secondary esterification zone, maintaining said secondary esterification zone at an elevated temperature sufficient to form or to maintain therein a vaporous stream containing said alkyl alcohol, intimately contacting said first liquid feed in said secondary esterification zone in the presence of said catalyst with said vaporous feed stream, recovering from said secondary esterification zone a vaporous effluent stream containing, in addition to alkyl alcohol vapor, also water in vapor form, said water being produced in said secondary esterification zone by esterification of said monoalkyl maleate with said alkyl alcohol, and recovering from said secondary esterification zone a liquid product stream containing said dialkyl maleate.
摘要翻译：描述了通过在单酯化区域中马来酸酐与烷基醇反应生成马来酸二烷基酯以形成相应的马来酸单烷基酯，然后将马来酸单烷基酯与另外的烷基醇反应形成相应的马来酸二烷基酯，从而制备马来酸二烷基酯的方法，其中包括以下步骤：将含有所述马来酸单烷基酯的第一液体进料供给到含有固体酯化催化剂的二次酯化区，将包含所述烷基醇的第二进料流供应到所述仲酯化区，将所述仲酯化区保持在升高足以形成或保持含有所述烷基醇的蒸汽流的温度，在所述催化剂存在下与所述气态进料流紧密接触所述仲酯化区中的所述第一液体进料，从所述仲酯化区回收含有，一世除了烷基醇蒸气，还有蒸气形式的水，所述水通过所述马来酸单烷基酯与所述烷基醇的酯化在所述仲酯化区中产生，并从所述仲酯化区回收含有所述马来酸二烷基酯的液体产物流。

3. 发明授权

US06809217B1 Process for the preparation of ethyl acetate 有权
标题翻译：乙酸乙酯的制备方法
公开(公告)号：US06809217B1
公开(公告)日：2004-10-26
申请号：US09806184
申请日：2001-06-05
申请人： Stephen William Colley , Christopher Richard Fawcett , Colin Rathmell , Michael William Marshall Tuck
发明人： Stephen William Colley , Christopher Richard Fawcett , Colin Rathmell , Michael William Marshall Tuck
IPC分类号： C07C6902
CPC分类号： C07C67/54 , C07C67/40 , C07C67/60 , C07C69/14
摘要： Ethanol is dehydrogenated in the presence of hydrogen over a dehydrogenation catalyst, for example, a copper on silica catalyst. The liquefiable products present in the resulting intermediate reaction product mixture are selectively hydrogenated over a suitable catalyst, such as 5% ruthenium on carbon, so as selectively to hydrogenate reactive carbonyl-containing by-products to the corresponding alcohols. Butan-2-one and n-butyraldehyde are thereby hydrogenated to 2-butanol and n-butanol respectively. A two stage distillation procedure is then used to purify the selectively hydrogenated product. A first distillate of ethyl acetate, ethanol and water produced in the first distillation zone is redistilled in the second distillation zone, thereby producing a bottom product comprising, typically, from about 99.8 mol % to about 99.95 mol % ethyl acetate and an overhead second distillate, which has a different composition from that produced in the first distillation zone and which is returned to the first distillation zone.
摘要翻译：乙醇在氢气存在下脱氢脱氢催化剂，例如二氧化硅催化剂上的铜。存在于所得中间反应产物混合物中的可液化产物在合适的催化剂如5％钌碳上选择氢化，以便选择性地将反应性羰基副产物氢化成相应的醇。因此，丁-2-酮和正丁醛分别氢化成2-丁醇和正丁醇。然后使用两阶段蒸馏程序来纯化选择性氢化产物。在第二蒸馏区中重新蒸馏在第一蒸馏区中产生的乙酸乙酯，乙醇和水的第一馏出物，从而产生通常为约99.8mol％至约99.95mol％乙酸乙酯和塔顶第二馏出物的底部产物，其具有与在第一蒸馏区中产生的组分不同的组成并且返回到第一蒸馏区。

4. 发明授权

US4751334A Process for the production of butane-1,4-diol 失效
标题翻译：丁烷-1,4-二醇的制备方法
公开(公告)号：US4751334A
公开(公告)日：1988-06-14
申请号：US901450
申请日：1986-07-21
申请人： Keith Turner , Mohammad Sharif , Colin Rathmell , John W. Kippax , Anthony B. Carter , John Scarlett , Arthur J. Reason , Norman Harris
发明人： Keith Turner , Mohammad Sharif , Colin Rathmell , John W. Kippax , Anthony B. Carter , John Scarlett , Arthur J. Reason , Norman Harris
IPC分类号： C07C29/149 , C07C29/17 , C07D307/08 , C07C29/136 , C07C31/20
CPC分类号： C07C29/149 , C07C29/177 , C07D307/08
摘要： Butane-1,4-diol is produced by vapor phase hydrogenolysis of an alkyl ester of a C.sub.4 dicarboxylic acid, e.g. diethyl maleate, over a reduced Cu-Cr or Cu-Zn mixed oxide catalyst. Two adiabatic hydrogenolysis zones are used. The mixture exiting the first of these zones is cooled (by, for example, 5.degree. C.) and the resulting cooled mixture is fed to the second zone in which is reequilibriates at a lower temperature to increase the butane-1,4-diol yield at the expense of gamma-butyrolactone. Typical reaction conditions include use of temperatures of 150.degree. C. to 200.degree. C., pressures of 25 to 70 bar, and a H.sub.2 :ester molar ratio of 100:1 to 800:1. When using a maleate ester it is often advantageous to hydrogenate this to the corresponding succinate ester in an upstream hydrogenation zone prior to entry to the first hyrogenolysis zone.
摘要翻译： PCT No.PCT / GB85 / 00524 Sec。一九八六年七月二十一日 102（e）日期1986年7月21日PCT提交1985年11月18日PCT公布。出版物WO86 / 03189 日期：1986年6月5日。丁烷-1,4-二醇是通过C4二羧酸烷基酯的气相氢解制备的。马来酸二乙酯，还原的Cu-Cr或Cu-Zn混合氧化物催化剂。使用两个绝热的氢解区。将离开这些区域中的第一个区域的混合物冷却（例如5℃），将得到的冷却的混合物进料至第二区域，在较低温度下将其重新配位，以增加丁烷-1,4-二醇产量以γ-丁内酯为代价。典型的反应条件包括使用150℃至200℃的温度，25至70巴的压力和100:1至800:1的H 2：酯摩尔比。当使用马来酸酯时，通常有利的是在进入第一个氢解区之前将其氢化为上游氢化区中的相应的琥珀酸酯。

5. 发明授权

US5387752A Process for the production of cyclohexanedimethanol 失效
标题翻译：环己烷二甲醇生产方法
公开(公告)号：US5387752A
公开(公告)日：1995-02-07
申请号：US174321
申请日：1993-12-30
申请人： John Scarlett , Michael A. Wood , Colin Rathmell
发明人： John Scarlett , Michael A. Wood , Colin Rathmell
IPC分类号： B01J23/86 , C07B61/00 , C07C29/136 , C07C29/149 , C07C31/27
CPC分类号： C07C31/276 , C07C29/149 , C07C2101/14
摘要： A process is described for the production of cyclohexanedimethanol by hydrogenation of a dialkyl cyclohexanedicarboxylate which comprises:(a) providing a hydrogenation zone containing a charge of a granular heterogeneous ester hydrogenation catalyst;(b) forming a vaporous feed stream of a hydrogen-containing gas,and a hydrogenatable material comprising a dialkyl cyclohexanedicarboxylate at a feed temperature which is in the range of from about 150.degree. C. to about 350.degree. C. and which is above the dew point of the feed stream and at a feed pressure in the range of from about 150 psia (about 10.34 bar) to about 2000 psia (about 137.90 bar), said vaporous feed stream having a known hydrogen-containing gas:dialkyl cyclohexanedicarboxylate ratio;(c) supplying the vaporous feed stream to the hydrogenation zone;(d) maintaining hydrogenation conditions in the hydrogenation zone which are effective to maintain the reaction mixture in contact with the hydrogenation catalyst above its dew point;(e) passing the vaporous feed stream through the hydrogenation zone; and(f) recovering from the hydrogenation zone a product stream containing cyclohexanedimethanol.In this process it is preferred to use dimethyl 1,4-cyclohexanedicarboxylate to produce 1,4-cyclohexanedimethanol.
摘要翻译：描述了通过氢化环己烷二羧酸二烷基酯制备环己烷二甲醇的方法，其包括：（a）提供含有粒状异质酯加氢催化剂装料的氢化区; （b）在约150℃至约350℃的进料温度下形成含氢气体的蒸气进料流和包含环己烷二羧酸二烷基酯的可加氢材料，其高于进料流的露点和进料压力在约150psia（约10.34巴）至约2000psia（约137.90巴）的范围内，所述气态进料流具有已知的含氢气体：环己烷二羧酸二烷基酯比; （c）将蒸气进料流供应到氢化区; （d）保持加氢区中的氢化条件，其有效地使反应混合物与氢化催化剂接触高于其露点; （e）使蒸汽进料流通过氢化区; 和（f）从氢化区回收含有环己烷二甲醇的产物流。在该方法中，优选使用1,4-环己烷二羧酸二甲酯来制备1,4-环己烷二甲醇。

6. 发明授权

US4765869A Process for the production of a dialkyl maleate 失效
标题翻译：马来酸二烷基酯的制备方法
公开(公告)号：US4765869A
公开(公告)日：1988-08-23
申请号：US80058
申请日：1987-07-31
申请人： Norman Harris , Colin Rathmell , Keith Turner , John Scarlett
发明人： Norman Harris , Colin Rathmell , Keith Turner , John Scarlett
IPC分类号： C07C67/60 , C07C67/08 , C07C67/54 , C07C69/60 , B01D3/14
CPC分类号： C07C67/08 , C07C67/54 , Y10S203/20
摘要： A continuous process is described for the production of a substantially acid free dialkyl maleate, for example diethyl maleate, from a feed stream containing a major amount of dialkyl maleate and a minor amount of the corresponding monoalkyl maleate. This comprises continuously distilling the feed stream in a primary distillation zone, which can comprise a single distillation column or a series of distillation columns connected in series, so as to give (i) a bottom fraction containing monoalkyl maleate and dialkyl maleate in admixture, (ii) a vaporous fraction comprising alkanol, and (iii) an intermediate fraction that is substantially free from alkanol and comprises a major proportion of diethyl maleate and a minor proportion of maleic anhydride. The intermediate fraction (iii) is redistilled in a secondary distillation zone to yield (i) an overhead fraction containing maleic anhydride and (ii) a bottom fraction containing substantially acid free dialkyl maleate. The vaporous stream can be condensed to recover alkanol for recycle to a dialkyl maleate production facility.
摘要翻译：描述了从含有主要量的马来酸二烷基酯和少量相应的马来酸单烷基酯的进料流中生产基本上无酸的马来酸二烷基酯，例如马来酸二乙酯的连续方法。这包括在主蒸馏区中连续蒸馏进料流，该蒸馏区可以包括单个蒸馏塔或串联连接的一系列蒸馏塔，从而得到（i）含有马来酸单烷基酯和马来酸二烷基酯的底部馏分的混合物（ ii）包含链烷醇的蒸气馏分，和（iii）基本上不含链烷醇并包含主要比例的马来酸二乙酯和少量马来酸酐的中间馏分。中间馏分（iii）在二次蒸馏区中重蒸馏，得到（i）含有马来酸酐的塔塔馏分和（ii）含有基本上无酸的马来酸二烷基酯的塔底馏分。可以将气态物流冷凝以回收链烷醇以再循环至马来酸二烷基酯生产设备。

7. 发明授权

US5395987A Preparation of cyclohexanedimethanol with a particular ratio 失效
标题翻译：以特定比例制备环己烷二甲醇
公开(公告)号：US5395987A
公开(公告)日：1995-03-07
申请号：US175502
申请日：1993-12-30
申请人： Colin Rathmell , Richard C. Spratt , Michael W. M. Tuck
发明人： Colin Rathmell , Richard C. Spratt , Michael W. M. Tuck
IPC分类号： B01J23/889 , C07B61/00 , C07C27/02 , C07C29/149 , C07C31/27 , C07C31/13 , C07C27/04
CPC分类号： C07C31/276 , C07C29/149 , C07C2101/14
摘要： A continuous process is described for the production of 1,4-cyclohexanedimethanol (CHDM) having a desired or predetermined trans-:cis- isomer ratio by catalytic hydrogenation of a dialkyl 1,4-cyclohexanedicarboxylate in the presence of an ester hydrogenation catalyst. The process is capable of being operated for an extended period of time during which the hydrogenation catalyst declines in catalytic activity and comprises feeding a vaporous mixture of the dialkyl 1,4-cyclohexanedicarboxylate and hydrogen to a hydrogenation zone containing the hydrogenation catalyst and recovering CHDM product. The degree of conversion of the dialkyl 1,4-cyclohexanedicarboxylate at a particular combination of temperature and pressure is related to the trans-:cis- isomer ratio of the CHDM product and may be varied by adjusting at least one feed condition selected from (i) the dialkyl 1,4-cyclohexanedicarboxylate feed rate and (ii) the hydrogen-containing gas:dialkyl 1,4-cyclohexanedicarboxylate molar ratio. As catalyst activity declines during operation of the process over an extended period of time at a particular combination of temperature and pressure, the degree of conversion of the dialkyl 1,4-cyclohexanedicarboxylate and/or the trans-:cis- isomer ratio of the CHDM product may be maintained at a constant value by adjusting at least one of the feed conditions referred to above. The determination of the Actual Activity and Reference Activity of the catalyst and the Actual and Effective Residence Times are included in the hydrogenation process.
摘要翻译：描述了在酯加氢催化剂存在下通过催化氢化1,4-环己烷二羧酸二烷基酯生产具有所需或预定的反式 - 顺式 - 异构体比例的1,4-环己烷二甲醇（CHDM）的连续方法。该方法能够长时间运行，在此期间氢化催化剂催化活性下降，并且包括将1,4-环己烷二羧酸二烷基酯和氢气的蒸气混合物进料到含氢化催化剂的氢化区和回收CHDM产物。在特定的温度和压力组合下，1,4-环己烷二羧酸二烷基酯的转化度与CHDM产物的反式 - 顺式 - 异构体比例有关，并且可以通过调节至少一种进料条件来改变，所述进料条件选自（i ）1,4-环己烷二羧酸二烷基酯进料速率和（ii）含氢气体：1,4-环己烷二羧酸二烷基酯摩尔比。随着催化剂活性在特定的温度和压力组合下长时间运行过程中催化剂活性下降，1,4-环己烷二羧酸二烷基酯的转化率和/或CHDM的反式 - 顺式异构体比例可以通过调节至少一种上述进料条件将产物保持在恒定值。催化剂的实际活性和参考活性的确定以及实际和有效的停留时间包括在加氢过程中。

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