CS241565B1 - A method for producing a thixotropic dispersion of oligomeric polyester ether - Google Patents

Abstract

The invention provides a method for two-stage production of a thixotropic dispersion of oligomeric polyester of terephthalic acid, ethylene glycol and polyethylene glycol with its subsequent dispersion in water. The product achieves favorable dirt removal, lower static charge formation and improved hygienic properties on mixed polyester textile materials.

Description

241565

BACKGROUND OF THE INVENTION The present invention relates to a process for the preparation of a thixotropic dispersion of polyester ether of terephthalic acid, ethylene glycol and polyethylene glycol as a textile auxiliary, which makes it easy to spin and reduce the formation of static charge of polyester and / or mixed polyester textiles. materials.

Acrylic acid copolymers with esters of acrylic and / or methacrylic acids (Roessler E., SandnerB .: Melliand Textilber. 50, 836 (1969)] are used to treat spin easy to wash. for the same purpose, double-acting perfluorinated compounds are used with hydrophilic polymer blocks interspersed with the other perfluorinated chain [Tessoro GC, Willard JJ: Tenside 6, 258 (1969)].

Polyester ethers, especially for polyester and / or mixed polyester textile materials (Brit. Pat. No. 1088 984), are also preferably used for this purpose.

A disadvantage of formulations based on esters of α-caprylic and / or methacrylic acids is that their activity is bound to the ionized form of the alkaline sodium salts of polyacrylic copolymers which, in the repeated washing process due to the present water hardness, pass to the non-ionized calcium and magnesium salts, losing their activity after five to seven cycles.

The use of perfluorinated compounds has been hampered by the high cost of formulations prepared by telomerization of tetrafluoroethylene and superficial reactions, as well as by the electrolysis of higher carboxylic acids in a liquid hydrofluoric acid environment.

Tixotropic dissociation types produced so far! based on polyester ethers (Brit. Pat. No. 1088 984), characterized in that the polyesters are always prepared by a one-stage process of terephthalic acid dimethyl ester, ethylene glycol and polyethylene glycol in the presence of a catalyst, which leads to the formation of products with linear alternation. polyglycol chains.

It has been found that if the preparation of the polyester ether is carried out according to the invention, ie the primary preparation of the polyester oligomer and subsequent reaction with polyethylene glycol, with an average molecular weight of 300 to 1500, preferably 600, at a temperature of 200 to 260 ° C and a pressure of 200 to 10,000 Pa obtains a product which is characterized by the localization of the polyglycol ether chain at the ends of the resulting oligomer, which, among other things, occurs! increased saponification number of the product.

The product thus prepared can then be dispersed in water using a mechanical ejector-type mechanical device, a high speed stirrer, a colloid mill, a bead mill, and the like. and / or with an effective dispersant.

This type of preparation allows a higher degree of cohesive forces between fiber and segmentaml containing acid terephthalic acid with ethylene glycol in the co-crystallization and a more effective hydrophilizing effect of the polyglycol ether chain.

When applying the subject product to a polyester polyester and / or mixed polyester fabric, an increased level of soil wettability, lower static build up, and improved hygienic properties due to increased water vapor sorption and water uptake while maintaining the physico-mechanical properties of the fabric treated material are achieved.

The process for the production of the thixotropic di-dispersion of terephthalic acid esters of ethylene glycol and polyethylene glycol is described below by way of example without being limited thereto. Přikladl

1320 liters of ethylene glycol, which is heated to 115 ° C, are added to the reactor, 1880 kg of molten dimethyl ester terephthalic acid are added, the mixture is further heated and at a temperature of 150 ° C to 170 ° C, 23.4 liters are added. zinc acetate in the form of a 2.5% solution in ethylene glycol.

The mixture was further heated until methanol was distilled off. Thereafter, the reaction mixture was gradually heated up to 210 ° C, adding 1830 kg of polyethylene glycol with a reactive average molecular weight of 600, followed by successive heating while distilling off the ethylene glycol at 260 ° C and 200 Pa. 3800 kg of polyesterether melt with a viscosity of 9.3 ml / g are obtained. Example 1

The melt of 360 kg of the polyester ether prepared according to Example 1 at 180 ° C to 220 ° C is slowly discharged into 1800 liters of water at 15 ° C to the turbine agitator mouth, forming a thixotropic stable dispersion which after dispensing the entire amount of melt to a temperature of 40 ° C and not further agitating to obtain a 200 kg dispersion containing 18% polyester ether. Example 3

The polyester ether melt prepared by Example 1 is pressed with a heated pump at a rate of 600 kg / h into a cyclone mixer, to which it simultaneously tangentially feeds 3,000 kg / h of a thixotropic dispersion of the oligomeric polyester ether containing 16.5% dry matter. Example 4

Polyester melt prepared by

Claims (1)

The 120 kg of warmed to 180 ° C is gradually added to 500 1 of 30 ° C water with vigorous stirring. The dispersion having a temperature of 38 ° C is then fed into a flow-through pearl mill by means of a metering pump, whereupon 620 kg of a constant thixotropic dispersion of polyether ether in water with a dry matter content of 18.2 percent is obtained. EXAMPLE 5 100 kg of the polyester ether melt prepared according to Example 1, heated to 190 DEG C., are added for 10 minutes with stirring to 400 l of a 0.1% by weight solution of ethanolamine salt of sulfated alcohol. C10 to C16 at 19 ° C. 500 kg of thixotropic polyesterether dispersion is obtained with a dry matter content of 20%. OBJECT OF THE INVENTION A method of producing a thixotropic dispersion of olefin terephthalic acid polyester ether, ethylene glycol, and polyethylene glycol, characterized in that polyester is reacted with lyethylene glycol having an average molecular weight of 300-1,500, preferably 600, by pre-esterification of dimethyl terephthalate with ethylene glycol prepared by polyester. , a temperature of 200 ° C to 260 ° C and a pressure of 200 Pa to 10,000 Pa, and the thus prepared polyester ester is dispersed in water.