阅读说明：本技术 用发泡介质进行气-液两相高压反应的反应器 (Reactor for gas-liquid two-phase high-pressure reaction by foaming medium ) 是由 O·贝 P·策纳 M·艾克 R·帕切洛 M·施尔维斯 M·豪布纳 G·威格纳 G·特本 于 2019-09-03 设计创作，主要内容包括：一种用发泡介质进行气/液两相高压反应的反应器,其包含由圆柱形的垂直取向的细长壳体、底部和顶盖形成的内部,其中所述内部被内件划分成反混区和限制反混区,其中反混区和限制反混区可被反应混合物依次穿过,其中反混区包含用于引入气体和液体的装置和气体出口,还包含选自搅拌器、射流喷嘴和气体注入装置的至少一个混合装置,且限制反混区包含反应产物出口；第一圆柱形内部件,其在内部在反应器的纵向上延伸并将限制反混区与反混区分界；布置在限制反混区中的无规则填料、规整填料或液体可渗透托盘形式的防反混的第二内部件；和上升管,其下端布置在反混区内且其上端通入限制反混区以使来自反混区的液体可经由上升管上升到限制反混区,其中进入限制反混区的流从下方进入。配置所述反应器以使高压反应空间得到最优利用并基本避免后处理步骤或安排在高压反应下游的后续反应被泡沫污染。本发明进一步涉及在所述反应器中进行连续气/液两相高压反应的方法。(A reactor for gas/liquid two-phase high-pressure reactions with a foaming medium, comprising an interior formed by a cylindrical, vertically oriented, elongated shell, a bottom and a top, wherein the interior is divided by internals into a back-mixing zone and a restricted back-mixing zone, wherein the back-mixing zone and the restricted back-mixing zone are passable through in succession by the reaction mixture, wherein the back-mixing zone comprises means for introducing gas and liquid and a gas outlet, further comprising at least one mixing device selected from the group consisting of stirrers, jet nozzles and gas injection means, and the restricted back-mixing zone comprises a reaction product outlet; a first cylindrical inner member extending internally in the longitudinal direction of the reactor and delimiting a restricted back-mixing zone from the back-mixing zone; a second inner anti-back-mixing component in the form of random packing, structured packing or liquid permeable trays disposed in the restricted back-mixing zone; and a riser having a lower end disposed within the back-mixing zone and an upper end opening into the restricted back-mixing zone such that liquid from the back-mixing zone can rise through the riser to the restricted back-mixing zone, wherein the flow into the restricted back-mixing zone enters from below. The reactor is configured to allow optimum utilization of the high-pressure reaction space and to substantially avoid contamination of the post-treatment steps or subsequent reactions arranged downstream of the high-pressure reaction with foam. The invention further relates to a process for carrying out a continuous gas/liquid two-phase high-pressure reaction in said reactor.)

1. A reactor for gas/liquid two-phase high-pressure reactions with a foaming medium, comprising an interior formed by a cylindrical vertically oriented elongated shell, a bottom and a top,

wherein the interior is divided by internal pieces into a back-mixing zone and a restricted back-mixing zone, wherein the back-mixing zone and the restricted back-mixing zone are passable through in succession by the reaction mixture, wherein the back-mixing zone comprises means for introducing gas and liquid and a gas outlet, and further comprises at least one mixing means selected from a stirrer, a jet nozzle and a gas injection means, and the restricted back-mixing zone comprises a reaction product outlet,

a first cylindrical inner part which extends internally in the longitudinal direction of the reactor and delimits a restricted back-mixing zone from the back-mixing zone,

a second inner anti-back-mixing component in the form of random packings, structured packings or liquid-permeable trays arranged in the restricted back-mixing zone and

a riser having a lower end disposed within the back-mixing zone and an upper end opening into the restricted back-mixing zone such that liquid from the back-mixing zone can rise through the riser to the restricted back-mixing zone,

wherein the flow entering the restricted back-mixing zone enters from below.

2. The reactor of claim 1, wherein the volumetric ratio of the back-mixing zone to the limiting back-mixing zone is in the range of 0.25:1 to 4: 1.

3. Reactor according to claim 1 or 2, comprising at least one third inner member arranged in the upper half of the back-mixing zone and having a surface promoting the tendency of the foaming medium to coalesce.

4. Reactor according to any one of the preceding claims, comprising a fourth internals arranged at the lower end of the riser and substantially preventing gas from entering the riser.

5. The reactor of claim 4, wherein the fourth inner member is selected from the group consisting of a deflector weir and a U-shaped tube.

6. Reactor according to any one of the preceding claims, wherein the first inner member is arranged concentrically with the housing such that the restricted back mixing zone has a circular horizontal cross-section.

7. A process for carrying out a continuous gas/liquid two-phase high-pressure reaction, wherein gas and liquid are introduced into a back-mixing zone in a reactor according to any one of the preceding claims, the liquid is allowed to rise from the back-mixing zone to a restricted back-mixing zone via a riser, unconverted gas is at least partly withdrawn via a gas outlet, and reaction product is withdrawn at a reaction product outlet.

8. The process according to claim 7 for the preparation of a homogeneous rhodium hydrogenation catalyst comprising at least one CO ligand, wherein the liquid comprises dissolved CO-deficient rhodium hydrogenation catalyst and wherein the gas comprises hydrogen and carbon monoxide, wherein the reaction of the CO-deficient rhodium hydrogenation catalyst with the gas provides a rhodium hydrogenation catalyst that is hydrogenation active.

9. The process according to claim 8, wherein the CO-deficient rhodium hydrogenation catalyst comprises at least one chiral ligand, in particular chiralphos.

10. A method according to claim 8 or 9, wherein the liquid comprises a compound of formula (IV)

Wherein Z in formula (IV) represents CHR³R⁴And wherein the variable R¹、R²、R³、R⁴Independently of one another, in particular jointly, the following are:

R¹、R²are identical or different and represent phenyl which is unsubstituted or carries 1, 2 or 3 substituents selected from the group consisting of methyl and methoxy, where R¹And R²Each represents in particular unsubstituted phenyl;

R³represents C₁-to C₄-alkyl, especially methyl;

R⁴represents a group with P (═ O) R^4aR^4bC of a radical₁-to C₄Alkyl, especially CH₂-P(＝O)R^4aR^4bOr CH (CH)₃)-P(＝O)R^4aR^4bA group;

wherein

R^4a、R^4bAre identical or different and represent phenyl which is unsubstituted or carries 1, 2 or 3 substituents selected from the group consisting of methyl and methoxy, where R^4aAnd R^4bEach particularly preferably represents unsubstituted phenyl.

11. A process according to any one of claims 8 to 10 wherein the preformed reaction product is supplied to an asymmetric hydrogenation reaction with the substrate to be hydrogenated to provide a hydrogenation reaction mixture and the hydrogenation product is separated from the hydrogenation reaction mixture to provide a residue comprising the CO-deficient rhodium hydrogenation catalyst which is supplied to the preformed.

12. A process for producing optically active menthol, wherein optically active citronellal of formula (VI) is produced by the process according to claim 11

Wherein denotes an asymmetric center;

wherein the hydrogenation reaction comprises the asymmetric hydrogenation of geranial of formula (Va-1) or neral of formula (Vb-1) or a mixture comprising neral and geranial

Subjecting the optically active citronellal of formula (VI) to cyclization to provide optically active isopulegol, and hydrogenating the optically active isopulegol to provide optically active menthol.