Shell-and-tube heat exchange reactor for carrying out a catalytic gas-phase partial oxidation reaction and process for carrying out a catalytic gas-phase partial oxidation

Patent metadata

Field	Value
Publication number	US-2025352975-A1
Application number	US-202318874169-A
Country	US
Kind code	A1
Filing date	Jun 2, 2023
Priority date	Jun 14, 2022
Publication date	Nov 20, 2025
Grant date	—

Abstract

A shell-and-tube heat exchange reactor for carrying out a catalytic gas-phase partial oxidation reaction comprises a shell-side heat exchange passage for circulating a heat transfer medium and a reaction passage comprising a plurality of reaction tubes; an inlet for introducing the reactant stream to the reaction passage; and an outlet from the reaction passage for recovering an effluent stream from the reaction tubes. The reaction tubes comprise a reactant pre-heating zone adjacent to the inlet, and a reaction zone downstream of the reactant pre-heating zone, the reaction zone having a catalytically active wire matrix insert having at least on a part of its surface a catalytically active precious metal. The reactor requires less frequent maintenance in the form of regeneration and/or replacement of the catalyst. The catalyst can be easily placed into the reaction tubes, and be removed therefrom. Only the portion of the entire reactant stream that travels near the hot reaction tube wall is heated up. Consequently, the portion of the reactant stream flowing in the center of the reaction tube is not heated to the reaction temperature and blind reactions of the unstable starting materials are thus reduced or even avoided.

First claim

1 .- 20 . (canceled)

21 . A shell-and-tube heat exchange reactor for carrying out a catalytic gas-phase partial oxidation reaction comprising
a shell-side heat exchange passage for circulating a heat transfer medium and a reaction passage comprising a plurality of reaction tubes; an inlet for introducing the reactant stream to the reaction passage; and an outlet from the reaction passage for recovering an effluent stream from the reaction tubes;
wherein the reaction tubes comprise
a reactant pre-heating zone adjacent to the inlet, and
a reaction zone downstream of the reactant pre-heating zone, the reaction zone having a catalytically active wire matrix insert having at least on a part of its surface a catalytically active precious metal.

22 . The shell-and-tube heat exchange reactor of claim 21 , wherein the reactant pre-heating zone has an essentially free cross section or has a wire matrix insert having zero or limited catalytic activity.

23 . The shell-and-tube heat exchange reactor of claim 21 , wherein the ratio of the length of the reaction zone to the length of the reactant pre-heating zone is in the range of from 0.01 to 100.

24 . The shell-and-tube heat exchange reactor of claim 21 , wherein the reaction zone comprises an alternating series of regions having catalytically active wire matrix inserts and regions having an essentially free cross section or having wire matrix inserts having zero or limited catalytic activity.

25 . The shell-and-tube heat exchange reactor of claim 21 , wherein the reaction tubes comprise an effluent cooling zone downstream of the reaction zone, wherein the effluent cooling zone has an essentially free cross section or has a wire matrix insert having zero or limited catalytic activity.

26 . The shell-and-tube heat exchange reactor of claim 21 , wherein the catalytically active precious metal is selected from copper, silver, palladium, platinum, ruthenium, and rhodium.

27 . The shell-and-tube heat exchange reactor of claim 22 , wherein the wire matrix insert having zero or limited catalytic activity is made of an inert material.

28 . The shell-and-tube heat exchange reactor of claim 21 , wherein the catalytically active wire matrix inserts comprise an elongated core having a plurality of wire loops extending from the elongated core, wherein the wire loops are longitudinally arranged and helically shifted, and wherein the wire loops comprise a massive precious metal wire, or a wire coated with a precious metal.

29 . The shell-and-tube heat exchange reactor of claim 28 , wherein the elongated core comprises at least two longitudinal core wire members, which are twisted around each other to form core wire windings, and the wire loops are accommodated in the core wire windings.

30 . The shell-and-tube heat exchange reactor of claim 28 , wherein the ratio of the inner diameter of the reaction tube to the diameter of the massive precious metal wire or the wire coated with a precious metal is in the range of about 10 to 100.

31 . The shell-and-tube heat exchange reactor of claim 21 , wherein the reaction zone has a void fraction of 0.60 to 0.99.

32 . The shell-and-tube heat exchange reactor of claim 21 , wherein the catalytically active wire matrix insert is adapted to enable radial mixing of the laminar boundary layer of the reactant stream into the bulk reactant stream through the reaction tubes.

33 . A process for carrying out a catalytic gas-phase partial oxidation reaction, the process comprising: introducing a reactant stream into the inlet of the shell-and-tube heat exchange reactor of claim 21 , wherein the reactant stream comprises a partially oxidizable organic substrate and molecular oxygen.

34 . The process according to claim 33 , wherein the flow of the reactant stream inside the pre-heating zone is essentially laminar.

35 . The process according to claim 33 , wherein the flow of the reactant stream inside the reaction zone containing the catalytically active wire matrix insert is characterized by a Reynolds number of 12000 or less.

36 . The process according to claim 33 for the manufacture of an aldehyde, wherein the precious metal is silver and the partially oxidizable organic substrate is an alcohol.

37 . The process according to claim 36 , wherein the alcohol is isoprenol, and wherein the isoprenol is obtained by reacting at least one formaldehyde source and isobutylene in a reactor to obtain isoprenol.

38 . The process according to claim 36 , wherein the partially oxidizable organic substrate is isoprenol, wherein the process additionally comprises at least one of αα, ββ and γγ:
αα) purifying of isoprenol by subjecting a stream of crude isoprenol containing isoprenol, water and formaldehyde, or an isoprenol containing fraction thereof, to distillation in a low-boiler separation tower operated at a pressure of 2 bara or higher, to obtain a distillate stream containing aqueous formaldehyde and a bottoms stream containing isoprenol essentially free of formaldehyde;
ββ) maintaining in the reactant stream a weight ratio of formaldehyde to isoprenol of less than 0.04;
γγ) treating the (iso)prenol to remove organically bound nitrogen from the (iso)prenol by contacting the isoprenol with a weakly acidic solid adsorbent prior to contacting with the catalytically active wire matrix insert.

39 . A process for the preparation of 3,7-dimethyl-octa-2,6-dienal (citral), the process comprising: obtaining prenal by the process according to claim 36 , further comprising the steps of condensing the prenal with prenol to obtain diprenyl acetal of prenal; and subjecting the diprenyl acetal of prenal to cleaving conditions to obtain citral via prenyl (3-methyl-butadienyl) ether and 2,4,4-trimethyl-3-formyl-1,5-hexadiene.

40 . A process for the preparation of a citral-derived chemical, comprising preparing citral by the process according to claim 39 , and at least one of ααα, βββ or (βββ plus γγγ):
ααα) converting the citral to obtain menthol;
βββ) converting the citral to geraniol and/or nerol;
γγγ) converting the geraniol and/or nerol to obtain linalool.

Assignees

• Basf Se

Inventors

• Reining Sven
• Olbert Gerhard
• Boehling Ralf
• Gauer Jochen
• Ehrhardt Kai Rainer

Classifications

• C07C47/21

  with only carbon-to-carbon double bonds as unsaturation · CPC title

• C07C45/38

  being a primary hydroxyl group · CPC title

• B01J2219/19

  Details relating to the geometry of the reactor · CPC title

• B01J2219/00159

  controlling multiple zones along the direction of flow, e.g. pre-heating and after-cooling · CPC title

• B01J2219/00081

  Tubes · CPC title