Method for preparing an amine hydrochloride suspension

Patent metadata

Field	Value
Publication number	US-12151997-B2
Application number	US-202318143981-A
Country	US
Kind code	B2
Filing date	May 5, 2023
Priority date	Jun 11, 2019
Publication date	Nov 26, 2024
Grant date	Nov 26, 2024

Abstract

The invention relates to a method for preparing a suspension of a hydrochloride of an organic amine, comprising the following steps of (i) initially charging at least one organic solvent in a reaction vessel to form a liquid level, (ii) adding hydrogen chloride, (iii) adding the organic amine, wherein the organic amine is added below the liquid level present in the reaction vessel and steps (ii) and (iii) are at least partly carried out simultaneously. Furthermore, the present invention also relates to a method wherein the suspension obtained after step (iii) is reacted in a step (iv) with phosgene to obtain the organic isocyanate corresponding to the organic amine used, to the corresponding organic isocyanate and to the use of the organic isocyanate for producing polyisocyanates.

First claim

The invention claimed is:

1. A method for preparing a suspension of a hydrochloride of an organic amine, comprising the following steps:
(i) initially charging at least one organic solvent in a reaction vessel to form a liquid level,
(ii) adding hydrogen chloride,
(iii) adding the organic amine,
wherein the organic amine is added below the liquid level present in the reaction vessel and steps (ii) and (iii) are at least partly carried out simultaneously,
where the organic amine is selected from the group consisting of 1,3-bis(aminomethyl)benzene (m-XDA),
wherein steps (ii) and (iii) are carried out while stirring with the aid of a stirring device comprising an aeration stirrer, paddle stirrer, or a dynamic mixer selected from the group consisting of disperser disks, rotor-stator systems and combinations thereof,
wherein hydrogen chloride is added as a gas either via an aeration stirrer or via a gas diffuser located below the stirring device.

2. The method according to claim 1 , wherein the temperature of the organic solvent in the reaction vessel prior to step (ii) is adjusted to −20 to 100° C.

3. The method according to claim 1 , wherein step (iii) is carried out using a dip tube.

4. The method according to claim 1 , wherein the at least one organic solvent is selected from the group consisting of aromatic hydrocarbons, halogenated aromatic hydrocarbons, esters, ethers, halogenated hydrocarbons and mixtures thereof.

5. The method according to claim 1 , wherein the organic amine is added as a solution in an inert solvent.

6. The method according to claim 5 , wherein the concentration of the organic amine in the solvent is 5 to 50% by weight, based on weight of the solution.

7. The method according to claim 1 , wherein the substance streams of hydrogen chloride and organic amine during steps (ii) and (iii) are in an equivalence ratio to each other of from 1:1 to 10:1.

8. The method according to claim 1 , wherein the end concentration of hydrochloride in the reaction mixture is 5 to 30% by weight.

9. The method according to claim 1 , wherein the suspension obtained after step (iii) is reacted in a step (iv) with phosgene to obtain an organic isocyanate corresponding to the organic amine used.

10. The method according to claim 1 , wherein the stirring device is selected from the group consisting of aeration stirrers and self-aspirating aeration stirrers.

Assignees

• Covestro Intellectual Property Gmbh & Co Kg

Inventors

• Merkel Michael
• Loddenkemper Tim
• Gerhartz Frank
• Hirschfeld Stefan

Classifications

• C08G18/758

  containing two or more cycloaliphatic rings · CPC title

• C07C209/74 Primary

  by halogenation, hydrohalogenation, dehalogenation, or dehydrohalogenation · CPC title

• C09D175/04

  Polyurethanes · CPC title

• C08G18/72

  Polyisocyanates or polyisothiocyanates · CPC title

• C07C265/14

  containing at least two isocyanate groups bound to the same carbon skeleton · CPC title