METHOD FOR PREPARING AN AMINE HYDROCHLORIDE SUSPENSION
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.
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.
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, particularly chlorinated 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 steps (ii) and (iii) are carried out while stirring with the aid of an aeration stirrer, paddle stirrer or a dynamic mixer selected from the group consisting of disperser disks, rotor-stator systems and combinations thereof.
10 . The method according to claim 1 , wherein the organic amine is selected from the group consisting of aromatic amines.
11 . The method according to claim 1 , 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.
12 . The organic isocyanate, obtainable by the method according to claim 11 , selected from the group consisting of 1,5-diisocyanatopentane (PDI), 1,6-diisocyanatohexane (HDI), 1-isocyanato-3,5,5-trimethyl-5-isocyanatomethylcyclohexane (IPDI), 1,3-bis(isocyanatomethyl)benzene (m-XDI), isomers of bis(isocyanatomethyl)cyclohexane (H6-XDI), isomers of bis(isocyanatomethyl)norbornane (NBDI), 2,4,4-trimethylhexamethylenediamine, 2,2,4-trimethylhexamethylenediamine and mixtures thereof.
13 . In a process for producing polyisocyanates comprising one of isocyanurate groups, polyisocyanates comprising uretdione groups, polyisocyanates comprising biuret groups, polyisocyanates comprising urethane or allophanate groups, polyisocyanates comprising oxadiazinetrione groups or iminooxadiazinedione groups and/or uretonimine-modified polyisocyanates, the improvement comprising including the organic isocyanate according to claim 12 .
14 . One of polyisocyanates comprising isocyanurate groups, polyisocyanates comprising uretdione groups, polyisocyanates comprising biuret groups, polyisocyanates comprising urethane or allophanate groups, polyisocyanates comprising oxadiazinetrione groups or iminooxadiazinedione groups and/or uretonimine-modified polyisocyanates produced by the process according to claim 13 .
15 . In a process for producing plastics comprising urethane, thiourethane, isocyanurate, amide and/or urea groups by the polyisocyanate polyaddition process or for producing light-stable polyurethane lacquers and coatings, the improvement comprising including the organic isocyanate according to claim 12 .
16 . method according to claim 10 , wherein the organic amine is selected from the group consisting of pure isomers or isomeric mixtures of diaminotoluene, diaminodimethylbenzene, diaminonaphthalene, diaminobenzene, diaminodiphenylmethane and mixtures thereof.
17 . The method according to claim 10 , wherein the organic amine an aliphatic, cycloaliphatic or araliphatic amine selected from the group consisting of 1,4-diaminobutane, 1,5-diaminopentane (PDA), 1,6-diaminohexane (HDA), 1,11-diaminoundecane, 1-amino-3,5,5-trimethyl-5-aminomethylcyclohexane (IPDA), bis(p-aminocyclohexyl)methane (PACM), 1,5-diamino -2-methylpentane, 2,5-diamino-2,5-dimethylhexane, 1,4-diaminocyclohexane, 2,4-hexahydrotoluylenediamine, 2,6-hexahydrotoluylenediamine (H6TDA), 1,3-bis(aminomethyl)benzene (m-XDA), 1,4-bis(aminomethyl)benzene (p-XDA), isomers of bis(aminomethyl)cyclohexane (H6-XDA), tetramethylxylylenediamine (TMXDA), isomers of bis(aminomethyl)norbornane (NBDA), neopentanediamine, 2,4,4-trimethylhexamethylenediamine, 2,2,4-trimethylhexamethylenediamine and mixtures thereof