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1. 发明授权

US5536856A Production of carboxylic acid ester by esterification and apparatus thereof 失效
标题翻译：通过酯化制备羧酸酯及其装置
公开(公告)号：US5536856A
公开(公告)日：1996-07-16
申请号：US200314
申请日：1994-02-23
申请人： George E. Harrison , John Scarlett , Michael A. Wood , Donald H. McKinley
发明人： George E. Harrison , John Scarlett , Michael A. Wood , Donald H. McKinley
IPC分类号： B01D3/16 , B01D3/18 , B01D3/20 , B01J8/22 , C07C67/08 , C07C69/22 , C11C1/00
CPC分类号： C07C67/08 , B01D3/163 , B01D3/18 , B01D3/20 , B01J8/226
摘要： Esterification is carried out in a column reactor (14) in which there is a plurality of esterification trays (15) each having predetermined liquid hold-up and containing a charge of a solid esterification catalyst thereon. e.g. an ion exchange resin containing a --SO.sub.3 H and/or --COOH groups. A liquid phase containing the carboxylic acid component, e.g. a fatty acid mixture, flows down the column reactor from one esterification tray to the next downward one against an upflowing alcohol vapour stream, e.g. methanol vapour. Relatively dry alcohol vapour is injected (21) into the bottom of the column reactor. Water of esterification is removed from the top of the column reactor in the vapour stream (26), whilst ester product is recovered (23) from the sump of the reactor. As the liquid flows down the trays it encounters progressively drier alocohol and the esterification equilibrium reaction is driven further and further towards 100% ester formation. A polishing reactor (304) operated under liquid phase conditions may follow the column reactor, the ester-containing product from which is mixed with further alcohol before admission to the polishing reactor.
摘要翻译：酯化在柱反应器（14）中进行，其中存在多个具有预定液体滞留并在其上含有固体酯化催化剂的酯化塔板（15）。例如含有-SO 3 H和/或-COOH基团的离子交换树脂。含有羧酸组分的液相，例如脂肪酸混合物从塔式反应器中流出，从一个酯化塔板向下流动的醇蒸气流，甲醇蒸气。将相对干燥的醇蒸汽（21）注入塔式反应器的底部。在蒸馏物流（26）中从塔式反应器的顶部除去酯化水，同时从反应器的贮槽回收酯产物（23）。当液体向下流动时，它遇到逐渐干燥的醇，酯化平衡反应进一步向100％酯形成。在液相条件下操作的抛光反应器（304）可以在塔式反应器之后，含酯产物在进入抛光反应器之前与另外的醇混合。

2. 发明授权

US5157168A Process for the production of fatty alcohols 失效
标题翻译：生产脂肪醇的方法
公开(公告)号：US5157168A
公开(公告)日：1992-10-20
申请号：US721438
申请日：1991-08-12
申请人： Martyn Wilmott , George E. Harrison , John Scarlett , Michael A. Wood , Donald H. McKinley
发明人： Martyn Wilmott , George E. Harrison , John Scarlett , Michael A. Wood , Donald H. McKinley
IPC分类号： C07C29/149 , C07C29/80 , C07C31/02 , C07C31/125 , C07C67/03 , C07C67/08
CPC分类号： C07C29/177 , C07C29/149 , C07C67/03 , C07C67/08
摘要： An improved process for the production of fatty alcohols is provided. The fatty alcohols are produced by hydrogenation of lower alkyl esters, especially methyl esters, of fatty acids derived from natural triglycerides, under conditions which minimize formation of by-product alkanes and ethers. The hydrogenation is followed by refining of any resulting ester-containing hydrogenation product to produce a substantially ester free fatty alcohol.
摘要翻译： PCT No.PCT / GB90 / 00063 Sec。 371日期1991年8月12日 102（e）日期1991年8月12日PCT 1990年1月16日PCT PCT。出版物WO90 / 08121 日期为1990年7月26日。提供了用于生产脂肪醇的改进方法。在最小化副产物烷烃和醚的形成条件下，通过氢化衍生自天然甘油三酸酯的脂肪酸的低级烷基酯，特别是甲基酯来生产脂肪醇。氢化之后是任何所得含酯氢化产物的精制，以产生基本上无酯的脂肪醇。

3. 发明授权

US5138106A Fatty alcohols 失效
标题翻译：脂肪醇
公开(公告)号：US5138106A
公开(公告)日：1992-08-11
申请号：US721437
申请日：1991-08-12
申请人： Martyn Wilmott , George E. Harrison , John Scarlett , Michael A. Wood , Donald H. McKinley
发明人： Martyn Wilmott , George E. Harrison , John Scarlett , Michael A. Wood , Donald H. McKinley
IPC分类号： C07C29/149 , C07C29/80 , C07C31/02 , C07C31/125 , C07C67/03
CPC分类号： C07C29/149 , C07C67/03
摘要： An improved process for refining alcohols produced by hydrogenation of esters wherein the crude hydrogenation product still contains a minor amount of unconverted ester starting material. In one embodiment, the process includes a method for recovering fatty alcohol or alcohols from a fatty alcohol fraction containing a major molar amount of at least one fatty alcohol and a minor molar amount of at least one lower alkyl fatty acid ester. In another embodiment, there is provided a process for the production of fatty alcohols which comprises, in addition to other steps, hydrogenating a lower alkyl fatty acid ester to yield a mixture of a lower alkanol, a fatty alcohol fraction and a minor amount of unreacted lower alkyl fatty acid ester.
摘要翻译： PCT No.PCT / GB90 / 00065 Sec。 371日期1991年8月12日 102（e）日期1991年8月12日PCT 1990年1月16日PCT PCT。公开号WO90 / 08123 日本1990年7月26日。一种用于精制醇的氢化制备的醇的改进方法，其中粗制氢化产物仍含有少量未转化的酯起始原料。在一个实施方案中，该方法包括从含有主要摩尔量的至少一种脂肪醇和少量摩尔量的至少一种低级烷基脂肪酸酯的脂肪醇级分中回收脂肪醇或醇的方法。在另一个实施方案中，提供了一种生产脂肪醇的方法，除了其它步骤之外，还包括将低级烷基脂肪酸酯氢化以产生低级烷醇，脂肪醇级分和少量未反应的混合物低级烷基脂肪酸酯。

4. 发明授权

US4919765A Process for the purification of tetrahydrofuran 失效
标题翻译：四氢呋喃纯化方法
公开(公告)号：US4919765A
公开(公告)日：1990-04-24
申请号：US222727
申请日：1988-07-22
申请人： Peter R. Wilkes , John Scarlett , George E. Harrison
发明人： Peter R. Wilkes , John Scarlett , George E. Harrison
IPC分类号： C07D307/08
CPC分类号： C07D307/08 , Y10S203/09 , Y10S203/14
摘要： Tetrahydrofuran is recovered by a two stage distillation procedure from a crude hydrogenation product resulting from vapor phase hydrogenation of diethyl maleate and containing water, ethanol and a minor amount of n-butanol, and possibly also dissolved hydrogen, in addition to butane-1,4-diol, gamma-butyrolactone and "heavies" such as diethyl ethoxysuccinate. In the first distillation stage, conveniently operated substantially at atmospheric pressure, ethanol, water, and tetrahydrofuran are recovered as overhead product, are condensed to separate the condensible components from a hydrogen stream which can be vented, and then redistilled in the presence of a molar excess of a hydroxylic solvent containing at least two hydroxyl groups, such as butane-1,4-diol, in a second distillation zone. Pure tetrahydrofuran is recovered as overhead product from the second distillation zone, while the bottom product therefrom is stripped in a third distillation zone of tetrahydrofuran, ethanol and water which are recycled to the first distillation zone and the stripped bottom product is recycled to the second distillation zone.
摘要翻译：四氢呋喃通过两步蒸馏方法从粗制氢化产物回收，粗制氢化产物由马来酸二乙酯的气相氢化产生，并含有水，乙醇和少量正丁醇，以及可能还含有溶解的氢，除了丁烷-1,4 - 二醇，γ-丁内酯和“重质”如乙氧基琥珀酸二乙酯。在第一蒸馏阶段，基本上在大气压下操作，回收乙醇，水和四氢呋喃作为塔顶产物，冷凝，将可冷凝组分与可排出的氢气流分离，然后在摩尔浓度存在下重新蒸馏在第二蒸馏区中过量含有至少两个羟基的羟基溶剂如丁烷-1,4-二醇。从第二蒸馏区回收作为塔顶产物的纯四氢呋喃，同时将其底部产物从四氢呋喃，乙醇和水的第三蒸馏区中汽提，再循环至第一蒸馏区，将汽提的底部产物再循环至第二蒸馏区。

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

US5406004A Hydrogenation process for the preparation of alcohols and diols utilizing gas and liquid phases 失效
标题翻译：使用气相和液相制备醇和二醇的氢化方法
公开(公告)号：US5406004A
公开(公告)日：1995-04-11
申请号：US175546
申请日：1993-12-30
申请人： Philip H. D. Eastland , John Scarlett , Michael W. M. Tuck , Michael A. Wood
发明人： Philip H. D. Eastland , John Scarlett , Michael W. M. Tuck , Michael A. Wood
IPC分类号： B01J23/42 , B01J23/60 , B01J23/72 , B01J23/889 , B01J23/89 , C07B53/00 , C07B61/00 , C07C29/141 , C07C29/145 , C07C29/149 , C07C31/125 , C07C31/20 , C07C31/27 , C07C31/13
CPC分类号： C07C31/276 , C07C29/149 , C07B2200/09 , C07C2101/14
摘要： A process is described for the production of a hydroxylic compound selected from alcohols and diols by hydrogenation of a corresponding hydrogenatable material selected from monoesters of carboxylic acids, monoesters of dicarboxylic acids, diesters of dicarboxylic acids, lactones, and mixtures of two or more thereof which comprises:(a) providing a hydrogenation zone containing a charge of a granular heterogeneous ester hydrogenation catalyst;(b) supplying to the hydrogenation zone a vaporous feed stream containing hydrogen and a hydrogenatable material selected from monoesters of carboxylic acids, monoesters of dicarboxylic acids, diesters of dicarboxylic acids, lactones, and mixtures of two or more thereof, at an inlet temperature which is above the dew point of the mixture;(c) maintaining the hydrogenation zone under temperature and pressure conditions which are conducive to effecting hydrogenation of esters;(d) recovering from the hydrogenation zone a two phase product stream containing a hydroxylic compound selected from alcohols and diols at an exit temperature which is below its dew point.In a preferred process the hydrogenatable material comprises dimethyl cyclohexanedicarboxylate.
摘要翻译：描述了通过氢化可选择的可羧化材料的羧酸，二羧酸的单酯，二羧酸的二酯，内酯以及它们的两种或更多种的混合物来制备选自醇和二醇的羟基化合物的方法。包括：（a）提供含有粒状非均相酯加氢催化剂装料的氢化区; （b）向加氢区供应含有氢气和可氢化材料的气态进料流，所述氢气和可氢化材料选自羧酸的单酯，二羧酸的单酯，二羧酸的二酯，内酯，以及它们的两种或多种的混合物，高于混合物的露点; （c）在有利于酯化氢化的温度和压力条件下保持氢化区; （d）从氢化区回收含有选自醇和二醇的羟基化合物的出口温度低于其露点的两相产物流。在优选的方法中，可氢化材料包括环己烷二羧酸二甲酯。

7. 发明授权

US5395991A Process for the production of alcohols and diols 失效
标题翻译：制备醇和二醇的方法
公开(公告)号：US5395991A
公开(公告)日：1995-03-07
申请号：US175545
申请日：1993-12-30
申请人： John Scarlett , Michael W. M. Tuck , Michael A. Wood
发明人： John Scarlett , Michael W. M. Tuck , Michael A. Wood
IPC分类号： C07C29/136 , C07B61/00 , C07C29/149 , C07C31/02 , C07C31/20 , C07C31/27 , C07C29/147 , C07C27/04 , C07C29/143
CPC分类号： C07C29/149 , C07C31/276 , C07C2101/14 , Y02P20/584
摘要： A hydrogenation process is described for the production of a hydroxylic compound selected from alcohols and diols by hydrogenation of a corresponding unsaturated organic compound selected from esters, diesters and lactones which involves use of two hydrogenation zones (11, 36), each containing a charge of a hydrogenation catalyst (12, 37). In a first phase of operation one of the hydrogenation zones (36 or 11) is in standby condition and a stream of hot hydrogen-containing gas is passed therethrough. Meanwhile a vaporous feed stream comprising a hydrogen-containing gas and the unsaturated organic compound to be hydrogenated, e.g. dimethyl 1,4-cyclohexanedicarboxylate, is fed to the active zone (11 or 36). This feed stream can include the gas stream from the first mentioned hydrogenation zone (36 or 11). In a second phase of operation the roles of the reactors (11, 36) are switched so that the zone (36 or 11) previously in reactivation condition becomes the active zone whilst the zone that was formerly active (11 or 36) goes into reactivation condition and its partially deactivated catalyst charge is reactivated by the hot hydrogen-containing gas stream.
摘要翻译：描述了氢化方法，用于通过氢化选自酯，二酯和内酯的相应的不饱和有机化合物来制备选自醇和二醇的羟基化合物，其包括使用两个氢化区（11,36），每个含有氢化催化剂（12,37）。在第一阶段的操作中，一个氢化区（36或11）处于待机状态，热的含氢气体流通过。同时，包含含氢气体和待氢化的不饱和有机化合物的气态进料流，例如。 1,4-环己烷二羧酸二甲酯进料到活性区（11或36）。该进料流可以包括来自第一个所述氢化区（36或11）的气流。在第二阶段操作中，反应器（11,36）的作用被切换，使得先前处于再活化状态的区域（36或11）变为活性区域，而先前有活性的区域（11或36）进入再活化条件和其部分失活的催化剂装料通过含氢气的气流再活化。

8. 发明授权

US5395986A 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：US5395986A
公开(公告)日：1995-03-07
申请号：US174314
申请日：1993-12-30
申请人： John Scarlett , Michael A. Wood
发明人： John Scarlett , Michael A. Wood
IPC分类号： B01J23/42 , B01J23/44 , B01J23/60 , B01J23/72 , B01J23/86 , B01J23/889 , C07B53/00 , C07B61/00 , C07C29/149 , C07C31/27
CPC分类号： C07C29/149 , C07C31/276 , C07C2101/14
摘要： A process is described for the production of cyclohexanedimethanol having a trans-:cis-isomer ratio greater than about 1:1 by hydrogenation of a dialkyl (e.g. dimethyl) cyclohexanedicarboxylate having a trans-:cis-isomer ratio less than about 1:1 which comprises:(a) providing a hydrogenation zone containing a charge of a granular heterogeneous ester hydrogenation catalyst;(b) supplying to the hydrogenation zone a vaporous feed stream containing hydrogen and a hydrogenarable material comprising a dialkyl cyclohexanedicarboxylate at an inlet temperature which is above its dew point of the mixture;(c) maintaining the hydrogenation zone under temperature and pressure conditions which are conducive to effecting hydrogenation of esters;(d) passing the vaporous feed stream through the hydrogenation zone; and(e) recovering from the hydrogenation zone a product stream containing cyclohexanedimethanol having a trans-:cis-isomer ratio greater than 1:1.In this process it is preferred to use dimethyl 1,4-cyclohexanedicarboxylate to produce 1,4-cyclohexanedimethanol.
摘要翻译：描述了通过氢化具有反式 - 顺式异构体比例小于约1:1的二烷基（例如二甲基）环己烷二羧酸酯制备具有大于约1:1的反式 - 顺式 - 异构体比例的环己烷二甲醇的方法，其中包括：（a）提供含有粒状非均相酯加氢催化剂装料的氢化区; （b）在高于其混合物露点的入口温度下向氢化区供应含有氢的气态进料流和包含环己烷二羧酸二烷基酯的可氢化材料; （c）在有利于酯化氢化的温度和压力条件下保持氢化区; （d）使蒸汽进料流通过氢化区; 和（e）从氢化区回收含有反式 - 顺式异构体比大于1:1的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。

9. 发明授权

US5387753A Process for the preparation of alcohols and diols 失效
标题翻译：醇和二醇的制备方法
公开(公告)号：US5387753A
公开(公告)日：1995-02-07
申请号：US174319
申请日：1993-12-30
申请人： John Scarlett , Michael W. M. Tuck , Michael A. Wood
发明人： John Scarlett , Michael W. M. Tuck , Michael A. Wood
IPC分类号： B01J23/72 , B01J23/889 , B01J23/90 , B01J38/10 , C07B61/00 , C07C27/02 , C07C29/10 , C07C29/149 , C07C31/00 , C07C31/20 , C07C31/27 , C07C35/14 , C07C27/04 , C07C31/135 , C07C31/18 , C07C33/14
CPC分类号： B01J23/8892 , C07C29/149 , C07C35/14 , Y02P20/584
摘要： A process is described for reactivating an at least partially deactivated copper-containing ester hydrogenation catalyst which has undergone deactivation through use in hydrogenation of an unsaturated organic compound selected from esters of C.sub.8 to C.sub.22 monocarboxylic acids, diesters of dicarboxylic acids, and lactones, to yield a corresponding hydroxylic compound selected from alcohols and diols which comprises contacting the at least partially deactivated copper-containing catalyst at an effective reactivation temperature and for an effective period of time with a stream of hydrogen-containing gas which is substantially free from the unsaturated organic compound thereby to reactivate the at least partially deactivated copper-containing catalyst.
摘要翻译：描述了一种方法，用于重新激活至少部分失活的含铜酯氢化催化剂，其通过用于氢化选自C8至C22单羧酸的酯，二羧酸和内酯的二酯的不饱和有机化合物而失活，以产生选自醇和二醇的相应的羟基化合物，其包括使所述至少部分失活的含铜催化剂在有效的再活化温度下和有效的一段时间内与基本上不含不饱和有机化合物的含氢气体流接触从而使至少部分失活的含铜催化剂再活化。

10. 发明授权

US5030609A Process for producing a hydrogenation catalyst of copper chromite 失效
标题翻译：亚铬酸铜加氢催化剂的制备方法
公开(公告)号：US5030609A
公开(公告)日：1991-07-09
申请号：US224686
申请日：1988-07-27
申请人： Keith Turner , Mohammad Sharif , John Scarlett , Anthony B. Carter , Geoffrey Webb
发明人： Keith Turner , Mohammad Sharif , John Scarlett , Anthony B. Carter , Geoffrey Webb
IPC分类号： C07D295/02 , B01J23/86 , B01J35/10 , B01J37/08 , B01J37/18 , C07B31/00 , C07B35/02 , C07B61/00 , C07C27/00 , C07C29/136 , C07C29/14 , C07C29/141 , C07C29/145 , C07C29/149 , C07C31/20 , C07C33/22 , C07C67/00 , C07D307/08 , C07D307/33
CPC分类号： B01J37/08 , B01J23/868 , B01J35/0053 , B01J35/006 , B01J37/18
摘要： A copper chromite hydrogenation catalyst of enhanced activity is obtained by an ante-pre-reduction treatment in which a copper chromite catalyst precursor is soaked in a reducing atmosphere at temperatures below a pre-reduction temperature (typically about 140.degree. C.) at which appreciable pre-reduction of the catalyst can be detected. This catalyst is characterized by particles of reduced copper substantially all of which have an average particle size of less than about 300.times.10.sup.-10 m (300.ANG.), which have an average particle size of less than about 100.times.10.sup.-10 m (100.ANG.), and which are substantially uniformly distributed on a chromium-containing support. Typically such catalysts exhibit a copper surface area of about 18.5 m.sup.2 /g as determined by N.sub.2 O decomposition at 20.degree. C., compared to a corresponding copper surface area of 4.5 m.sup.2 /g for a catalyst which has been produced by conventional pre-reduction of the same catalyst precursor.

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