公开(公告)号：US3890399A

公开(公告)日：1975-06-17

申请号：US28629272

申请日：1972-09-05

Applicant: HOECHST AG

Inventor： GEHRMANN KLAUS ,  OHORODNIK ALEXANDER ,  DETTMEIER ODO ,  BERNS HEINZ-JOSEF

IPC: E04B1/00 ,  B01J8/22 ,  B01J27/00 ,  C07B61/00 ,  C07C17/00 ,  C07C17/358 ,  C07C21/09 ,  C07C67/00 ,  C07C21/04

CPC classification number: C07C21/09 ,  B01J8/228 ,  C07C17/358 ,  Y02P20/584

Abstract: Heterogeneous catalytic reactions are carried out continuously in liquid phase. To this end, a suspension of liquid starting material and particulate catalyst together with resulting reaction product is continuously conveyed upwardly in a reaction zone by the introduction, in accordance with the principle of an air-lift pump, of a gas near the bottom of the reaction zone, and recycled downwardly through a reflux line to the bottom of the reaction zone, the path of liquid material through the reflux line being interrupted by an injector system situated in a closed catalyst-separating zone containing recycle liquid; following establishment of the reaction equilibrium, starting material is continuously supplied to the reaction zone and crude, catalystfree recycle liquid is continuously removed near the head of the catalyst-separating zone, and recycle liquid which is to be removed is caused to travel through the catalyst-separating zone with the injector system therein towards the recycle liquid outlet at a velocity smaller than the sedimentation velocity of the catalyst under the operational conditions prevailing. More particularly, 1,4-dichlorobutene-2 is isomerized to 3,4dichlorobutene-1. To achieve this the reaction zone is supplied continuously with 1,4-dichlorobutene-2 or with a commercial mixture of 3,4-dichlorobutene-1 and 1,4-dichlorobutene-2; an inert gas is introduced into the bottom portion of said reaction zone; liquid material is heated to boiling therein; 3,4dichlorobutene-1 is distilled off near the head of said reaction zone; 3,4-dichlorobutene-1 is conveyed to a distilling zone and fractionated therein until pure; pure 3,4-dichlorobutene-1 is condensed in a cooling zone; and 1,4-dichlorobutene-2 having high-boiling fractions enriched therein is isolated near the head of the separating zone.

Abstract translation: 非均相催化反应在液相中连续进行。 为此，将液体原料和颗粒催化剂与所得反应产物一起悬浮在反应区中，通过根据空气提升泵的原理引入靠近底部的气体而连续输送 反应区，并通过回流管线向下循环到反应区的底部，液体材料通过回流管线的路径被位于包含再循环液体的封闭催化剂分离区域中的喷射器系统中断; 在反应平衡建立之后，将原料连续地供应到反应区，并在催化剂分离区的头部附近连续除去粗的无催化剂的再循环液体，并将要除去的再循环液体通过 其中注射器系统的催化剂分离区以其在主要操作条件下的催化剂的沉降速度小于再循环液体出口。

公开(公告)号：US3923917A

公开(公告)日：1975-12-02

申请号：US53121374

申请日：1974-12-10

Applicant: HOECHST AG

Inventor： OHORODNIK ALEXANDER ,  GEHRMANN KLAUS ,  LEGUTKE GUNTER ,  VIERLING HERMANN

IPC: B01J27/00 ,  B01J31/04 ,  B01J31/30 ,  B01J37/24 ,  C07B61/00 ,  C07C1/00 ,  C07C2/38 ,  C07C7/148 ,  C07C11/30 ,  C07C67/00 ,  C07C11/22 ,  C07C21/20

CPC classification number: B01J31/30 ,  B01J31/0225 ,  B01J31/0237 ,  B01J31/0271 ,  B01J31/04 ,  B01J37/24 ,  C07C2/38 ,  C07C2527/122 ,  C07C11/30

Abstract: Monovinylacetylene is produced by an improved process, wherein acetylene is introduced at temperatures within the range 40* and 100*C and under acetylene gas pressures within the range 0.01 and 10 atmospheres (gauge) into a Nieuwland catalyst type solution being an aqueous copper(I) chloride solution in hydrochloric acid, which is used in admixture with between 0.1 and 10 weight% of an alkali metal salt of an aminocarboxylic acid or of an aminosulfonic acid and in further admixture with an organic monovinylacetylene solvent boiling at temperatures higher than about 150*C, immiscible with the solution and containing at least 40 weight% of indan together with further mononuclear aromates; wherein the catalyst solution and the solvent are mechanically dispersed by introducing acetylene thereinto with the resultant formation of a homogeneous catalyst liquid having between 25 and 85% by volume of the solvent therein; wherein monovinylacetylene is continually stripped off from the dispersed solvent, which is saturated with monovinylacetylene, by introducing an excess of acetylene gas thereinto; and wherein pure monovinylacetylene is recovered from the issuing gas mixture. The improved process comprises more particularly concentrating the catalyst solution by evaporating water therefrom and dissolving additional copper(I) chloride in the catalyst solution so concentrated.

Abstract translation: 通过改进的方法制备单乙炔基乙炔，其中乙炔在40℃和100℃的温度和在0.01和10个大气压（表压）范围内的乙炔气体压力下引入Nieuwland催化剂型溶液中，其为铜（I ）氯化物溶液，其与0.1至10重量％的氨基羧酸或氨基磺酸的碱金属盐的混合物与进一步与高于约150℃的沸点沸点的有机单乙烯基乙炔溶剂混合使用 C，与溶液不混溶，并含有至少40重量％的茚满和另外的单核芳香; 其中催化剂溶液和溶剂通过向其中引入乙炔而机械分散，从而形成其中溶剂的体积的体积的体积的体积的体积的25至85％ 其中通过向其中引入过量的乙炔气体而从单乙炔基乙炔饱和的分散溶剂中连续剥离单乙烯基乙炔; 并且其中从所述发出气体混合物中回收纯单乙烯基乙炔。 改进的方法包括通过从其中蒸发水而更加特别地浓缩催化剂溶液，并将另外的氯化亚铜（I）溶解在如此浓缩的催化剂溶液中。

公开(公告)号：US3864281A

公开(公告)日：1975-02-04

申请号：US38775573

申请日：1973-08-13

Applicant: HOECHST AG

Inventor： OHORODNIK ALEXANDER ,  GEHRMANN KLAUS ,  HUNDECK JOACHIM ,  VIERLING HERMANN

IPC: C07C53/16 ,  B01J23/44 ,  B01J35/10 ,  B01J37/02 ,  C07C51/00 ,  C07C51/377 ,  C07C67/00 ,  B01J11/08

CPC classification number: C07C51/377 ,  B01J21/08 ,  B01J23/44 ,  B01J35/0053 ,  B01J35/1019 ,  B01J35/1047 ,  B01J35/108 ,  C07C53/16

Abstract: Production of a catalyst comprised of a fine-particulate carrier and palladium metal for the partial dehalogenation of di- and/or trichloracetic acids in the presence of hydrogen to produce monochloracetic acid, wherein the dry porous carrier is impregnated with a palladium salt solution and the palladium absorbed by the carrier is reduced to palladium metal with the use of a suitable reducing agent. More particularly the palladium metal is concentrated exclusively on the surface of the carrier by impregnating and partially saturating the dry, fineparticulate carrier with the pure palladium salt solvent; by continuing impregnation until complete saturation of the carrier so pretreated with the necessary quantity of palladium salt solution; and by reducing the palladium salt applied to the carrier to palladium in known manner.

Abstract translation: 生产由细颗粒载体和钯金属组成的催化剂，用于在氢气存在下二 - 和/或三氯乙酸的部分脱卤反应产生一氯乙酸，其中干燥多孔载体用钯盐溶液浸渍， 使用合适的还原剂将载体吸收的钯还原成钯金属。 更具体地，钯金属仅通过用纯钯盐溶剂浸渍并部分饱和干燥的细颗粒载体而集中在载体的表面上; 通过持续浸渍直到载体完全饱和，由此用必要量的钯盐溶液预处理; 并以已知的方式将作用于载体的钯盐还原成钯。

公开(公告)号：US3901660A

公开(公告)日：1975-08-26

申请号：US41139073

申请日：1973-10-31

Applicant: HOECHST AG

Inventor： OHORODNIK ALEXANDER ,  SENNEWALD KURT ,  HUNDECK JOACHIM ,  STUTZKE PAUL

IPC: B01J8/00 ,  B01J8/18 ,  B01J8/22 ,  C07C51/377 ,  C07C53/16

CPC classification number: B01J8/228 ,  B01J8/006 ,  B01J8/1836 ,  B01J2208/00176 ,  C07C51/377 ,  C07C53/16

Abstract: Heterogeneous catalytic reactions are carried out continuously in liquid phase. A substantially uniform suspension of liquid starting material and fine particulate catalyst together with resulting reaction product is continuously conveyed upwardly in a reaction zone by the introduction, in accordance with the principle of an airlift pump, of a gas or vaporous material near the bottom of the reaction zone, and recycled downwardly through a reflux line to the bottom of the reaction zone. The path of liquid material through the reflux line is interrupted by an injector system situated in a closed catalyst-separating zone containing reaction product. Following establishment of the reaction equilibrium, starting material is continuously supplied near the bottom of the reaction zone and crude but catalyst-free reaction product continuously removed near the head of the catalyst-separating zone. Reaction product which is to be removed is caused to travel through the catalyst-separating zone with the injector system therein towards the reaction product outlet at a velocity smaller than the sedimentation velocity of the catalyst under the prevailing operational conditions.

公开(公告)号：US3882167A

公开(公告)日：1975-05-06

申请号：US36386373

申请日：1973-05-25

Applicant: HOECHST AG

Inventor： LOHMAR ELMAR ,  OHORODNIK ALEXANDER ,  GEHRMANN KLAUS ,  STUTZKE PAUL

IPC: C07C69/54 ,  B01J8/22 ,  B01J19/18 ,  C07C67/08

CPC classification number: B01J19/1862 ,  B01J8/228 ,  B01J2219/00094 ,  B01J2219/00101 ,  C07C67/08 ,  Y10S203/06 ,  C07C69/54

Abstract: Improved process permitting heterogeneous catalytic reactions to be carried out continuously in liquid phase, wherein a suspension of liquid starting material and fine particulate catalyst together with resulting reaction product is continuously conveyed upwardly in a reaction zone, in accordance with the principle underlying an airlift pump, by the introduction of a gas into, near the bottom of, the reaction zone, and recycled downwardly through a by-pass reflux line to the bottom of the reaction zone, the recycled liquid material passing through an injector system interrupting its flow, the said system being situated in the bypass reflux line in a closed catalyst-separating zone containing reaction product; wherein, following establishment of the reaction equilibrium, starting material is continuously supplied to the reaction zone and crude, catalyst-free reaction product is removed near the head of the catalyst-separating zone; wherein reaction product, which is to be removed from the catalystseparating zone, is caused to flow upwardly through the catalystseparating zone with the injector system therein towards the reaction product outlet at velocity smaller than the sedimentation velocity of the catalyst in the catalyst-separating zone under the operational conditions prevailing. The improved process is more particularly used for esterifying arcylic acid in contact with an acid ion exchanger as a catalyst, at elevated temperature and under pressures substantially between 0.01 and 1 atmosphere absolute. To this end, the reaction zone is continuously supplied with a starting mixture of acrylic acid and an alkanol having between 4 and 6 carbon atoms; an inert gas is introduced into, near the bottom of, the reaction zone; the resulting suspension is heated to boiling; an azeotropic mixture of water originating from the esterification, alkanol and/or ester, is distilled off in a distillation zone placed directly above the head of the reaction zone; the azeotropic mixture is condensed and separated into a specifically lighter, predominantly organic phase and into a specifically heavier, predominantly aqueous phase, the organic phase being recycled to the head of the distillation zone and/or to the reaction zone; and resulting crude alkyl acrylate is removed near the head of the catalyst-separating zone.

Abstract translation: 改进的方法允许在液相中连续进行非均相催化反应，其中根据空气提升泵的原理，液体原料和细颗粒催化剂的悬浮液与所得反应产物一起在反应区中向上连续输送， 通过将气体引入到反应区的底部附近，并通过旁路回流管向下循环到反应区的底部，再循环的液体材料通过一个中断其流动的喷射器系统，所述的 系统位于包含反应产物的封闭催化剂分离区中的旁路回流管线中; 其中，在建立反应平衡之后，将原料连续地供应到反应区，在催化剂分离区的头部附近除去粗的无催化剂的反应产物; 其中将从催化剂分离区除去的反应产物通过其中的注射器系统向上流过催化剂分离区，其速度小于催化剂中催化剂的沉降速度朝向反应产物出口 分区在现行的运行条件下。