DD143250A1 - METHOD FOR PRODUCING METAL SALT SOLUTIONS OF ALIPHATIC CARBON ACIDS - Google Patents

Abstract

The invention relates to a process for the preparation of metal salt solutions aliphatic, preferably branched, carboxylic acids the elements potassium and zinc, primarily as activators find use in the foaming process of PVC pastes. Goal and Task of the invention are, by changing the technological conditions as well as modifying additives the dam The state of the art adhering defects, resulting in particular from the Compromise solution between quality parameters and space-time Zmsbeute in the preparation of such metal salt solutions as well as the increased Requirements of the processors revealed to avoid. According to the invention become high-quality metal salt solutions aliphatic, preferably branched chain, carboxylic acids of the elements potassium and Zinc obtained in high space-time yield when during the reaction ■ Alkanediol, preferably 20 to 25% ethylene glycol, and after removal of the reactivated water and cooling to at least 100 ° C 25 to 35% of a combination consisting of urea, glycol partial ether. and alkanetriol partial esters.

Description

invention registration

Title of the invention

Process for the preparation of metal salt solutions of aliphatic carboxylic acids

Applicant of the invention

The invention relates to a process for the preparation of metal salt solutions of aliphatic, preferably branched, carboxylic acids of the elements potassium and zinc, which find various other uses as PVC stabilizers, catalysts, siccatives etc. In particular, the use of such metal salt solutions for foaming PVC pastes has become increasingly important obtained because they strongly activating the decomposition of the chemical blowing agent einviirken.

Characteristic of the "known tectonic solutions

It is already widely known to carry out the preparation of metal salts of aliphatic branched-chain, preferably carboxylic acids, in the presence of customary solvents or additives such as Vi / sichmacher, aliphatic cycloaliphatic or aromatic hydrocarbons, higher alcohols, esters or ethers.

In this context it has also been described to prepare storage-stable, highly concentrated, low-viscosity metal salt solutions which are suitable in particular as activators for the foaming process, in such a way that the reaction mixture

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mixed both small amount-η substituted ketones and small amounts of substituted ether added (DD-EB 95 365).

Furthermore, it is known, especially in combinations of metal salt solutions of elements of the 1st and 2nd group of the periodic table, especially potassium and zinc, urea or urea derivatives to add to the reaction still to eliminate any remaining disadvantages. Although metal salt solutions which despite high concentration and relatively low viscosity have a good storage stability but whose production is predominantly a compromise solution between the relevant quality features and space-time yield, are obtained by the above-mentioned procedure. Thus, an interaction manifests itself as advantageous quality parameters on various occasions At the expense of space-time yield go, while on the other hand, the preference of the Raurn-time yield. Some qualitative properties of Hetallsalzlösungen - especially in conjunction with the growing claims of processors - in question. This is particularly true of the viscosity, the reduction of which is already clearly limited in DD-EB 110 647, and its effect on the spreadability and cold resistance as well as on the plasticizer compatibility and effectiveness of the metal salt solution.

In contrast, the space-time yield is determined in particular by material losses in the wastewater and the problems associated therewith, as well as by faster solubility of the reaction components and synergists.

At the DD-EB 110 647 closest to the invention criteria of space-time yield were discriminated in favor of qualitative features; Nevertheless, the increased demands of users for very low viscosity and excellent plasticizer compatibility could not always be taken into account ·

Z _- JeI the invention

The aim of the invention is to adhere to the state of the art inherent shortcomings, in particular from the compromise solution

between Qualitätsparametera and space-time yield in the production of metal salt solutions of the elements potassium and zinc, turn off or largely eliminate »·,. A further object of the invention is to further improve the viscosity and plasticizer compatibility of such metal salt solutions so that they, in particular as activators in the foaming process of PVC pastes, meet the growing requirements of Weitervererbeiter sides,

Explanation of the essence of the invention

According to the objective of the invention, the object of the invention to provide a process for the preparation of metal salt solutions of aliphatic, preferably branched chain, carboxylic acids of the elements potassium and zinc to develop, in which by changing the technological conditions and the modifying additives in high space-time yield and be obtained at low wastewater pollution metal salt solutions, which are characterized by very low viscosity and excellent plasticizer compatibility and activity with good storage stability.

It has been found that high-quality metal salt solutions of aliphatic, preferably branched, carboxylic acids by reaction of basic compounds of the elements potassium and zinc with aliphatic, preferably branched chain), carboxylic acids using urea or urea derivatives and organic solvents in high space-time yield can be prepared if during the reaction alkanediol, preferably ethylene glycol, and after removal of the water of reaction and cooling to at least 100 ⁰ C, a combination consisting of urea, Glykolpartialather and alkanetriol partial ester, are added.

In this connection, it was further found that it is favorable to add alkanediol, preferably ethylene glycol, only after completion of the reaction of basic potassium compounds and before the beginning of the reaction of basic zinc compounds, in each case with aliphatic carboxylic acids

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The proportion of alkanediol, preferably Äthylenglykolf 20-25%, based on the metal salt solution. Furthermore, it has been found to be advantageous that the added after the process of cooling combination should suitably from 30 - 4% urea, 50 - 65% glycol partial and 2 - 15% alkanetriol partial ester should exist. The combination itself is purchased in an amount of 25 - 35%> to the metal salt solution, added «

As Glykolpartialäther are particularly compounds with a boiling point of about 16O ⁰ G, such as ethylene glykolrnonobutyläther or Diäthylenglykolmonoäthylather suitable, while have proven particularly suitable as alkanetriol partial esters Glyzerinmonoöleat and Glyzerinmonooctoat.

Execution; sb ei s pi e le_

1. In a reaction vessel 367 g of 2-A'thylhexansäure and 20 ml of water were introduced and added at 60 ⁰ C 36 g of 96% potassium carbonate. After completion of the reaction, the reaction water was removed by distillation, and 202.5 g of ethylene glycol was added. This was followed by the addition of 81.5 g of zinc oxide at about 90 ⁰ C under vigorous stirring. After completion of the second reaction, dehydration was again carried out and the mixture was cooled to 100.degree. Subsequently, a combination consisting of 90 g of urea, 157> 5 g Äthylenglykolmonobutyläther and 27 g Glyzerinmonooleat, registered, After completion of the stirring or dissolution process was a final Eiltration.

The preparation was carried out in 4 ₅ 5 hrs, while a yield of 920 g, that is 99 _S 25% of theory, was obtained.

The viscosity at 25 ⁰ C was 319 cP, the pour point was -27 ⁰ C _e

The product was clear and showed no crystalline or oily deposits after 6 months of storage. When mixed with plasticizers good compatibility was found *

The reaction of 2-ethylhexanoic acid with potassium carbonate was carried out analogously to Example 1. The resulting potassium 2-ethylhexoate were then added to 225 S hexylene glycol. This was followed by the addition of 81.5 S zinc oxide at about 90 ° C with vigorous stirring * Wake the second reaction was dehydrated and 'cooled the mixture to 9O ⁰ C.

Subsequently, a combination consisting of 81 g urea, 112 g Diäthylenglykolmonoäthylather and 31j5 g Glyzerinmonooctoat entered. After completion of the approximately 5 minutes of stirring or dissolving process was followed by filtration, The preparation was carried out in 4-, I Std., This was a yield of 895 Sj that are 99.5% of theory, preserved.

The viscosity at 25 ⁰ O was 285 cP, the pour point was -28 ⁰ C.

The product was clear and showed neither crystalline nor oil-like deposits even after several months of storage. When blended with plasticizers, a good compatibility was found

Claims (5)

invention claims 1 «Process for the preparation of metal salt solutions of aliphatic carboxylic acids by reaction of basic compounds of the elements potassium and zinc with aliphatic, preferably branched, carboxylic acids using urea or, urea derivatives and organic solvents, characterized in that during the reaction alkanediol, preferably Ä'thylenglykol, and after removal of the water of reaction and cooling to at least 100 ⁰ C, a combination consisting of urea, Glykolpartialather and alkanetriol Partialiester, added vi / earth. 2. The method according to item 1, characterized in that alkanediol preferably ethylene glycol, after completion of the reaction of basic potassium compounds and before, beginning of the reaction of basic zinc compounds, each with aliphatic carboxylic acids, are added. 3 · Method according to items 1 and 2, characterized in that. The proportion of alkanediol, preferably ethylene glycol, 20-25%, based on the metal salt solution. 4. The method according to item 1, characterized in that the combination of 30 - 40% urea, 50 - 65% Glykolpartialäther and 2 - 15% alkanetriol partial ester consists. 5 · The method of item 1 and 4, characterized in that the combination in an amount of 25 - 35% is _obtained} to the metal salt solution was added.