Preparation of C10-C30-alkenes by partial hydrogenation of alkynes over fixed-bed supported palladium catalysts
    32.
    发明授权
    Preparation of C10-C30-alkenes by partial hydrogenation of alkynes over fixed-bed supported palladium catalysts 失效
    通过固定床负载的钯催化剂上的炔进行部分氢化制备C10-C30-烯烃

    公开(公告)号:US06365790B2

    公开(公告)日:2002-04-02

    申请号:US09734024

    申请日:2000-12-12

    IPC分类号: C07C2900

    摘要: Alkenes are prepared by partial hydrogenation of alkynes in the liquid phase at from 20 to 250° C. and hydrogen partial pressures of from 0.3 to 200 bar over fixed-bed supported palladium catalysts which are obtainable by heating the support material in the air, cooling, applying a palladium compound and, if required, additionally other metal ions for doping purposes, molding and processing to give monolithic catalyst elements, by a process in which A) alkynes of 10 to 30 carbon atoms are used as starting compounds, B) the palladium compound and, if required, the other metal ions are applied to the support material by impregnation of the heated and cooled support material with a solution containing palladium salts and, if required, other metal ions and subsequent drying, and C) from 10 to 2000 ppm of carbon monoxide (CO) are added to the hydrogenation gas or a corresponding amount of CO is allowed to form in the liquid phase by slight decomposition of a compound which is added to the reaction mixture and eliminates CO under the reaction conditions. The process is particularly advantageous if the partial hydrogenation is carried out in a tube reactor by the trickle-bed or liquid phase procedure with product recycling at cross-sectional loadings of from 20 to 500 m3/m2*h. The process is particularly suitable for the preparation of 3,7,11,15-tetramethyl-1-hexadecen-3-ol (isophytol), 3,7,11-trimethyl-l-dodecen-3-ol (tetrahydronerolidol), 3,7,11-trimethyl-1,4-dodecadien-3-ol, 3,7,11-trimethyl-1,6-dodecadien-3-ol (dihydronerolidol), 3,7-dimethyloct-1,6-dien-3-ol or 3,7-dimethyloct-1-en-3-ol from the corresponding alkynes.

    摘要翻译: 烯烃通过液相中炔烃在20至250℃的部分氢化和固定床负载的钯催化剂的0.3至200巴的氢分压来制备,其可通过加热空气中的载体材料,冷却 使用钯化合物,另外还需要另外的金属离子用于掺杂目的,通过使用10-30个碳原子的炔烃作为起始化合物的方法,模塑和加工以得到整体式催化剂元素,B)钯 如果需要,另外的金属离子通过用含有钯盐的溶液浸渍加热和冷却的载体材料以及如果需要的话其它金属离子并随后干燥而被施加到载体材料上,C)为10-2000ppm 的一氧化碳(CO)加入到氢化气体中,或者相应量的CO在液相中形成,通过轻微分解添加到真空中的化合物 并且在反应条件下消除CO。如果部分氢化在管式反应器中通过滴流床或液相方法进行,则该方法是特别有利的,其中产物回收的横截面负荷为20-500m 3 / m2 * h。 该方法特别适用于制备3,7,11,15-四甲基-1-十六碳烯-3-醇(异山梨糖醇),3,7,11-三甲基-1-十二碳烯-3-醇(四氢化吗啉醇),3 ,7,11-三甲基-1,4-十二碳二烯-3-醇,3,7,11-三甲基-1,6-十二碳二烯-3-醇(二氢吗啉醇),3,7-二甲基辛-1,6-二烯 - 3-醇或3,7-二甲基辛-1-烯-3-醇。

    Method for producing 1,4-butanediol
    33.
    发明授权
    Method for producing 1,4-butanediol 有权
    生产1,4-丁二醇的方法

    公开(公告)号:US06350924B1

    公开(公告)日:2002-02-26

    申请号:US09673134

    申请日:2000-10-11

    IPC分类号: C07C2700

    摘要: A process for preparing 1,4-butanediol and, if desired, &ggr;-butyrolactone and THF by oxidizing butane or benzene to form a product stream including maleic anhydride, absorbing maleic anhydride from the product stream with a high-boiling inert solvent in an absorption stage to give a liquid absorption product, esterifying the liquid absorption product with a C1-C5 esterifying alcohol in an esterification stage to form an esterification product comprising the corresponding diester and high-boiling inert solvent, then hydrogenating the esterification product to give a hydrogenation product which comprises the products of value, 1,4-butanediol and, if desired, &ggr;-butyrolactone and tetrahydrofuran and the esterifying alcohol and which is separated by distillation into the products of value and the esterifying alcohol, and recycling the esterifying alcohol to the esterification zone, which comprises separating the esterification product into the diester and the inert solvent by distillation under reduced pressure prior to the hydrogenation, recycling the inert solvent to the absorption stage, and hydrogenating the diester in the liquid phase over a fixed-bed catalyst.

    摘要翻译: 通过氧化丁烷或苯来制备1,4-丁二醇和(如果需要的话)γ-丁内酯和THF以形成包含马来酸酐的产物流的方法,在吸收中用高沸点惰性溶剂从产物流中吸收马来酸酐 阶段以得到液体吸收产物,在酯化阶段用C1-C5酯化醇酯化液体吸收产物以形成包含相应的二酯和高沸点惰性溶剂的酯化产物,然后氢化酯化产物得到氢化产物 其包括价值的产物,1,4-丁二醇,如果需要的话,γ-丁内酯和四氢呋喃和酯化醇,并通过蒸馏分离成产物和酯化醇,并将酯化醇再循环到酯化反应 其包括通过蒸馏分离酯化产物成二酯和惰性溶剂 在氢化之前在减压下进行反应,将惰性溶剂循环到吸收阶段,并在固定床催化剂中使液相中的二酯氢化。

    Preparation of citral
    34.
    发明授权
    Preparation of citral 有权
    柠檬醛的制备

    公开(公告)号:US06175044B1

    公开(公告)日:2001-01-16

    申请号:US09404548

    申请日:1999-09-24

    IPC分类号: C07C4551

    摘要: 3,7-Dimethyl-2,6-octadien-1-al of formula I is prepared continuously by: thermally cleaving, in the presence or absence of an acid catalyst, 3-methyl-2-buten-1-al diprenyl acetal of formula II: thereby eliminating 3-methyl-2-buten-1-ol of formula III and yielding cis/trans-prenyl 3-methylbutadienyl ether of formula IV: thermally rearranging the resultant butadienyl ether of formula IV thereby yielding 2,4,4-trimethyl-3-formyl-1,5-hexadiene of formula V: subsequently rearranging intermediate (V) thereby yielding citral product of formula I, which comprises: as the reaction proceeds, continuously distilling the reaction mixture thereby continuously removing prenol, which is formed by degradation of acetal II, and the intermediates of formula IV and V and any citral product which is formed during the reaction; and thermally rearranging said intermediates of formula IV and V at a temperature of 100-200° C. in the absence or presence of said prenol to form citral product.

    摘要翻译: 通过以下方式连续制备式I的3,7-二甲基-2,6-辛二烯-1-醇:在存在或不存在酸催化剂的情况下,热裂解3-甲基-2-丁烯-1-al阮内烯 式II:由此除去式III的3-甲基-2-丁烯-1-醇,得到式IV的顺/反 - 异戊烯基3-甲基丁二烯基醚:热重新排列所得的式IV的丁二烯基醚,由此得到2,4,4 式V的 - 三甲基-3-甲酰基-1,5-己二烯:随后重新排列中间体(V),从而产生式I的柠檬醛产物,其包括:随着反应的进行,连续蒸馏反应混合物,从而连续除去前醇, 由缩醛II的降解形成,以及式IV和V的中间体以及在反应期间形成的任何柠檬醛产物; 在不存在或存在所述prenol的情况下,在100-200℃的温度下热处理所述式IV和V的中间体,以形成柠檬醛产物。

    Production of anhydrous or substantially anhydrous formic acid
    36.
    发明授权
    Production of anhydrous or substantially anhydrous formic acid 失效
    生产无水或基本无水的甲酸

    公开(公告)号:US4326073A

    公开(公告)日:1982-04-20

    申请号:US131501

    申请日:1980-03-18

    CPC分类号: C07C51/09 C07C51/48

    摘要: Anhydrous or substantially anhydrous formic acid is obtained by hydrolysis of methyl formate, in a process wherein(a) methyl formate is hydrolyzed,(b) the methanol and excess methyl formate are distilled from the hydrolysis mixture obtained,(c) the bottom product of distillation (b), consisting of formic acid and water, is extracted, in a liquid-liquid extraction, with an extractant which in the main takes up the formic acid,(d) the resulting extract phase, consisting of formic acid, the extractant and a part of the water, is subjected to distillation,(e) the top product obtained from this distillation and consisting of all or part of the water introduced into the distillation, and part of the formic acid, is recycled, as vapor, into the lower part of the distillation column of stage (b),(f) the bottom product of distillation stage (d), consisting of the extractant, with or without part of the water, and the greater part of the formic acid, is separated by distillation into anhydrous or substantially anhydrous formic acid and the extractant, and(g) the extractant leaving stage (f) is recycled to the process.

    摘要翻译: 在(a)甲酸甲酯水解的过程中,(甲)甲醇和过量的甲酸甲酯从得到的水解混合物中蒸馏得到,(c)甲酸叔丁酯的底部产物 蒸馏(b)由甲酸和水组成,在液 - 液萃取中用主要萃取甲酸的萃取剂萃取,(d)所得提取相由甲酸,萃取剂 和一部分水进行蒸馏,(e)由该蒸馏获得的顶部产物,并且由引入蒸馏的全部或部分水和部分甲酸作为蒸气循环进入 阶段(b)的蒸馏塔的下部,(f)蒸馏阶段(d)的底部产物,由萃取剂组成,有或没有部分水和大部分甲酸分离 通过蒸馏成无水 粗粉或基本上无水的甲酸和萃取剂,和(g)离开阶段(f)的萃取剂再循环到该方法中。

    Process for preparing mercaptoalkyl carboxylates
    37.
    发明授权
    Process for preparing mercaptoalkyl carboxylates 有权
    巯基烷基羧酸盐的制备方法

    公开(公告)号:US08907119B2

    公开(公告)日:2014-12-09

    申请号:US13591398

    申请日:2012-08-22

    IPC分类号: C07C319/12 C07C319/22

    摘要: In the acid-catalyzed esterification of mercaptoalkyl alcohols by means of carboxylic acids to form mercaptoalkly carboxylates, formation of undesirable, usually sparingly soluble by-products usually occurs. The process of the invention in the absence of acid catalysts avoids the formation of such by-products. Particularly when the esterification of the invention is carried out as reactive distillation using reactive column and residence vessel, good degrees of conversion can also be obtained without acid catalyst and at the same time the formation of the by-products can be largely avoided.

    摘要翻译: 在巯基烷基醇通过羧酸进行酸催化酯化形成巯基羧酸酯时,通常会发生不期望的,通常微溶的副产物。 在没有酸催化剂的情况下,本发明的方法避免了这种副产物的形成。 特别是当本发明的酯化作为使用反应性柱和驻留容器的反应蒸馏进行时,也可以在没有酸催化剂的情况下获得良好的转化率,同时可以大大地避免副产物的形成。

    Process for continuous hydrogenation or hydrogenating amination
    39.
    发明授权
    Process for continuous hydrogenation or hydrogenating amination 有权
    连续氢化或氢化胺化的方法

    公开(公告)号:US08163963B2

    公开(公告)日:2012-04-24

    申请号:US12090377

    申请日:2006-10-16

    IPC分类号: C07C45/00

    摘要: A process is described for continuously hydrogenating unsaturated compounds, in which particles of a first hydrogenation catalyst are suspended in a liquid phase in which an unsaturated compound is dissolved, the liquid phase, in the presence of a hydrogenous gas at a first partial hydrogen pressure and at a first temperature, is conducted through a packed bubble column reactor in cocurrent counter to the direction of gravity, the effluent from the bubble column reactor is sent to a gas-liquid separation, the liquid phase is sent to a crossfiltration to obtain a retentate and a filtrate, the retentate is recycled into the bubble column reactor and the filtrate, in the presence of a hydrogenous gas at a second partial hydrogen pressure and at a second temperature, is passed over a bed of a second hydrogenation catalyst, wherein the second partial hydrogen pressure is at least 10 bar higher than the first partial hydrogen pressure.

    摘要翻译: 描述了在第一部分氢气压力下在氢气存在下将不饱和化合物连续氢化的方法,其中第一氢化催化剂的颗粒悬浮在其中溶解不饱和化合物的液相中,液相,以及 在第一个温度下,通过气泡塔反应器与重力方向并流,将来自泡罩塔反应器的流出物送入气液分离,将液相送至交叉过滤,得到滞留物 和滤液,将滞留物再循环到泡罩塔反应器中,并且在第二部分氢气压力和第二温度下在氢气存在下将滤液通过第二氢化催化剂床,其中第二 部分氢气压力比第一部分氢气压力高至少10巴。

    Process for the Preparation of Formic Acid
    40.
    发明申请
    Process for the Preparation of Formic Acid 有权
    制备甲酸的方法

    公开(公告)号:US20110319657A1

    公开(公告)日:2011-12-29

    申请号:US13171598

    申请日:2011-06-29

    IPC分类号: C07C53/02

    CPC分类号: C07C51/09 C07C51/44 C07C53/02

    摘要: Process for obtaining formic acid by thermal separation of a stream comprising formic acid and a tertiary amine (I), in which a liquid stream comprising formic acid and a tertiary amine (I) in a molar ratio of from 0.5 to 5 is produced by combining tertiary amine (I) and a formic acid source, from 10 to 100% by weight of the secondary components present therein are separated off and formic acid is removed by distillation in a distillation apparatus at a bottom temperature of from 100 to 300° C. and a pressure of from 30 to 3000 hPa abs from the liquid stream obtained, the bottom discharge from the distillation apparatus being separated into two liquid phases and the upper liquid phase being recycled to the formic acid source and the lower liquid phase being recycled for separating off the secondary components and/or to the distillation apparatus.

    摘要翻译: 通过热分离包含甲酸和叔胺(I)的流来获得甲酸的方法,其中包含摩尔比为0.5至5的甲酸和叔胺(I)的液体流通过组合 分离叔胺(I)和甲酸源,10至100重量%存在于其中的次要组分,并在蒸馏装置中在100-300℃的底部温度下蒸馏除去甲酸。 从得到的液体流中的压力为30〜3000hPa abs,将来自蒸馏装置的底部排出物分离成两液相,将上液相再循环至甲酸源,将下液相回收分离 脱离第二组分和/或蒸馏装置。