Process for producing oligoamines or polyamines

Compositions – Preservative agents – Anti-corrosion

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252332, 252340, 252344, 252358, 528421, 528422, 528492, 525406, 525504, B01D 1704

Patent

active

058464530

DESCRIPTION:

BRIEF SUMMARY
This application is a 371 of PCT/EP95/03809 filed Sep. 26, 1995.


BACKGROUND OF THE INVENTION

1. Field of the Invention
The present invention relates to an improved process for preparing alkoxylates of oligoamines or polyamines by a two-stage procedure where, in the first stage, one molecule of alkylene oxide per NH group is added onto the oligoamines or polyamines in the presence of water, alcohols or acids or a mixture thereof in the absence of a neutral or basic catalyst and, in the second stage, after removal of water and acids reaction with further alkylene oxide is carried out in the presence of a conventional neutral or basic catalyst.
2. Description of the Background Art
DE-B 22 27 546 discloses a two-stage process for preparing alkoxylated polyalkyleneimines in which, in the first stage, a polyalkylenepolyamine is exposed, in the presence of from 1 to 50% by weight of water, to sufficient alkylene oxide for the corresponding amino alcohol to be produced with saturation of all the valencies bonding hydrogen atoms to the nitrogen atoms and, in the second stage, after removal of the water an alkaline catalyst is added, followed by further alkoxylation.
It is known that the further reaction of the amino alcohol in the second stage must be carried out in the absence of water, because otherwise there is excessive formation of many unwanted byproducts with a glycol or polyglycol structure. However, further alkoxylation of pure polymeric amino alcohol, for example in the melt, takes place only very slowly. In particular, states of high viscosity occur at the start of this further reaction and are difficult to control and overcome, which leads to great variations in the reaction times and products which differ greatly in their viscosity.


SUMMARY OF THE INVENTION

It is an object of the present invention to find reaction conditions under which the polymeric amino alcohols from the first stage of the described preparation process can be alkoxylated in an economic and efficient manner with short reaction times to give reproducible products.
We have found that this object is achieved by a process as defined at the outset, wherein, before the second stage is carried out, an organic solvent or diluent or a mixture thereof from the group of or a mixture thereof,


DETAILED DESCRIPTION OF THE INVENTION

Said solvent or diluent is preferably added in an amount of from 2 to 400 parts by weight, in particular 5 to 200 parts by weight, especially 10 to 100 parts by weight, based on the weight of the adduct from the first stage.
Examples of suitable alcohols and phenols or their alkoxylates (a) are C.sub.1 -C.sub.8 -alkanols, in particular C.sub.1 -C.sub.4 -alkanols, such as ethanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, sec-butanol, tert-butanol, n-pentanol, n-hexanol, n-heptanol, n-octanol or 2-ethylhexanol, cyclohexanol, benzyl alcohol, polyhydric alcohols such as ethylene glycols or propylene glycol, phenols such as unsubstituted phenol, cresols or naphthols and, especially in the case of phenols, products of the reaction thereof with from 1 to 30 mol, in particular 2 to 15 mol, per hydroxyl group of ethylene oxide, propylene oxide, butylene oxide or a mixture thereof.
Examples of polyglycols (b) are diethylene glycol, triethylene glycol, tetraethylene glycol and polyethylene glycols with average molecular weights of from 200 to 2000, in particular 300 to 1000, furthermore dipropylene glycol, tripropylene glycol, tetrapropylene glycol and polypropylene glycols with average molecular weights of from 270 to 2000, in particular 350 to 1000, and furthermore dibutylene glycol, tributylene glycol, tetrabutylene glycol and polybutylene glycols with average molecular weights of from 320 to 2000, in particular 400 to 1000.
Particularly suitable N-substituted open-chain or cyclic carboxamides (c) are N,N-dimethylformamide, N,N-dibutylformamide, N,N-dimethylacetamide and N-methylpyrrolidone.
Examples of suitable alkanolmono- and -polyamines or their alkoxylates (d) are monoethanolamine, diethanolamine,

REFERENCES:
patent: 3907701 (1975-09-01), Liebold et al.
patent: 4147724 (1979-04-01), Knofel et al.
patent: 4705834 (1987-11-01), Baur et al.
patent: 5445765 (1995-08-01), Elfers et al.

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