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    • 1. 发明授权
    • Process for the production of cyclohexanedimethanol
    • 环己烷二甲醇生产方法
    • US5387752A
    • 1995-02-07
    • US174321
    • 1993-12-30
    • John ScarlettMichael A. WoodColin Rathmell
    • John ScarlettMichael A. WoodColin Rathmell
    • B01J23/86C07B61/00C07C29/136C07C29/149C07C31/27
    • C07C31/276C07C29/149C07C2101/14
    • 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.
    • 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。
    • 3. 发明授权
    • Production of carboxylic acid ester by esterification and apparatus
thereof
    • 通过酯化制备羧酸酯及其装置
    • US5536856A
    • 1996-07-16
    • US200314
    • 1994-02-23
    • George E. HarrisonJohn ScarlettMichael A. WoodDonald H. McKinley
    • George E. HarrisonJohn ScarlettMichael A. WoodDonald H. McKinley
    • B01D3/16B01D3/18B01D3/20B01J8/22C07C67/08C07C69/22C11C1/00
    • C07C67/08B01D3/163B01D3/18B01D3/20B01J8/226
    • 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.
    • 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。
    • 4. 发明授权
    • Process for the production of alcohols and diols
    • 制备醇和二醇的方法
    • US5395991A
    • 1995-03-07
    • US175545
    • 1993-12-30
    • John ScarlettMichael W. M. TuckMichael A. Wood
    • John ScarlettMichael W. M. TuckMichael A. Wood
    • C07C29/136C07B61/00C07C29/149C07C31/02C07C31/20C07C31/27C07C29/147C07C27/04C07C29/143
    • C07C29/149C07C31/276C07C2101/14Y02P20/584
    • 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.
    • 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。
    • 5. 发明授权
    • Process for the production of cyclohexanedimethanol
    • 环己烷二甲醇生产方法
    • US5395986A
    • 1995-03-07
    • US174314
    • 1993-12-30
    • John ScarlettMichael A. Wood
    • John ScarlettMichael A. Wood
    • B01J23/42B01J23/44B01J23/60B01J23/72B01J23/86B01J23/889C07B53/00C07B61/00C07C29/149C07C31/27
    • C07C29/149C07C31/276C07C2101/14
    • 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.
    • 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。
    • 10. 发明授权
    • Process for the production of a dialkyl maleate
    • 马来酸二烷基酯的制备方法
    • US4765869A
    • 1988-08-23
    • US80058
    • 1987-07-31
    • Norman HarrisColin RathmellKeith TurnerJohn Scarlett
    • Norman HarrisColin RathmellKeith TurnerJohn Scarlett
    • C07C67/60C07C67/08C07C67/54C07C69/60B01D3/14
    • C07C67/08C07C67/54Y10S203/20
    • 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.
    • 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。