SU1549970A1 - Method of obtaining alcoxy-substituted alumoxane resins - Google Patents

Abstract

The invention relates to methods for producing alumoxane resins with trimethylsiloxy or chelating alkoxy substituents, which can be used in the preparation of ceramic and composite materials for the modification of polymers. The invention makes it possible to increase the aluminum content in the resin to 15.8-25.3 wt.% And reduce the consumption of trimethylsilanol or a chelating hydroxy compound to 50%. The method is carried out by the interaction of an aluminum alkoxide with trimethylsilanol or a chelating hydroxy compound, followed by hydrolysis of the resulting mixture. Alcohols of any alcohols can be used as an aluminum alkoxide, but it is preferable to use ethylates, propylates, butylates. Β-hydroxyketones, β-diketones, β-oxo- and β-hydroxycarboxylic acids and their esters can be used as a chelating hydroxy compound. 1 tab.

Description

The invention relates to methods for producing alkoxy-substituted alumoxane resins, in particular to a method for producing alumoxane resins with trimethylsiloxy or chelating alkoxy substituents, which can be used in the preparation of ceramic and composite materials for modifying polymers.

The purpose of the invention is to increase the aluminum content in the resin and reduce the consumption of the organic hydroxy compound.

Alcohols of any alcohols can be used as alcohols of aluminum, but it is preferable to use ethylates, propylates and butylates.

As chelating hydroxy compounds, y-hydroxyketones, ft-diketones, (3-ox-and-hydroxycarboxylic acids and their β-oxoketones and / 3-oxo-acid esters) are hydroxy compounds in the tautomeric enol form can be used. Acetylacetone and acetoacetic ester are the most accessible.

Example 1. A 1 L four-necked flask with an elective agitator, a dropping funnel, a recalcator with a calcium chloride tube and an internal thermometer was charged with 408 g of a 25% toluene solution of aluminum isopropylate. 30 g of acetoacetic elira are poured in and heated for 1 hour.

sd

at 50 ° C. Cool the reaction mixture to 20 ° C and for 2 h with intensive stirring a solution of 11.2 g of water in 125 ml of isopropanol is added dropwise. Heat the reaction mixture in an oil bath for 2 hours at JOO ° C. The volatile products are distilled off with a gradual increase in the bath temperature to 150 ° C for 2 hours. The obtained dry resin is finally dried under vacuum to 1 kPa at J20 ° C for 2 hours. 64.5 g of a white solid resin is obtained that is soluble in aromatic hydrocarbons. , ketones and esters. The aluminum content is 20.6%.

The synthesis of alumoxane resins is carried out in a similar manner according to other examples.

The conditions for the preparation of alumoxane resins and their properties are listed in the table.

The structural formula of the resulting resins can be represented as

OR I

R OJ AI-O AI-OVJR1,

where R is H or alkyl;

R is trimethylsilyl or the residue of a chelating agent;

0.5 p 1;

Claims (1)

Go fa 5-7. Invention Formula The method of producing alkoxy-substituted alumoxane resins by the interaction of aluminum alkoxide with an organic hydroxy compound, followed by hydrolysis of the resulting mixture, characterized in that, to increase the aluminum content in the resin and reduce the consumption of the organic hydroxy compound, 1 mol of aluminum hydroxide takes a mole of organic hydroxy resin and a decrease in organic hydroxy compound consumption; (3-p) / 2 mol of water, where 0, while the organic hydroxy compound is trimethylsilyl anol or a chelating hydroxy compound. In examples 1-8 - isopropyl A, in example 9 - ethnlat A1, in example EB examples 1-5 - acetoxenus air, in example 8 - acetylacetone, trimethylsilanol. M, 6 102nd solution in isopropanol (examples 1-8), ethanol (example 9), measure 10). Gelation during hydrolysis. According to the description of the known method. Determined by crystalline in tsclohexane.