SU412207A1 - METHOD OF OBTAINING CARBOTSEP OLYGOMER WITH END FUNCTIONAL GROUPS - Google Patents

Description

This invention relates to the synthesis of terminal functionalized chain-chain oligomers.

A known method for producing chain-chain oligomers with terminal carboxyl, ether and hydroxyl groups is aqueous emulsion or solution polymerization or copolymerization of diene and / or vinyl monomers using initiators containing appropriate functional groups, such as hydrogen peroxide.

The aim of the invention is to obtain chain-chain oligomers with terminal hydrazide groups.

For this purpose, azo-bis-isobutyric acid dihydrazide is used as the initiator.

SNDS

1I 0

C-C-N-N-C-C

NH., NH / 1I NHNH2

BUT

CH,

The polymerization process is carried out according to conventional methods for the preparation of oligomers by radical polymerization in bulk, solution, emulsion. The molecular weight of oligomers depends on the monomer irirodes and synthesis conditions. The presence of hydrazide groups in oligomers was proved by acetylation by the Ver. Method and confirmed by IR spectra (5).

The proposed method is technologically advanced, and it allows to obtain oligomers in one stage with a good yield.

The resulting oligomers are intermediates for the synthesis of new polymeric materials by crosslinking them with dinosocyanatamp, diepoxides and other polyfunctional compounds.

LR and meer. 8 ml of isoprene and 0.63 g of azobisisobutyric acid dihydrazide in 20 ml of methanol are heated in a sealed ampoule at 80 ° C for 15 hours. Obtain 1.5 g of oligomer mol. weight. 3250, determined ebuliokscopically in benzene and containing 1.78% hydrazide groups. In the infrared spectra of the oligomer there are intense stretching vibration bands of 1660 3300 cm, corresponding to C-O and N-P groups in hydrazides.

PRI mme R 2. 4.4 ml of butadiene, 1.4 ml of 2-methyl-5-vinyl-pyridine (2M5WP) and 0.5 g of azo-bis-isobutyric acid dihydrazide in 20 ml of dioxane are heated in a sealed ampoule at 80 ° C for 20 hours. Obtain 1.2 g of cooligomer with mol ... weight. 2100 and the content of terminal hydrazide groups 5.6%. The composition of cooligomer butadiene: 2M5VP 80: 20 weight. %

Example 3. 4.5 g of styrene and 0.25 g of azo-bis-isobutyric acid digandrazide in 20 ml of methanol are heated in an indicated ampoule and 80 ° C for 10 hours. Obtain 1.3 g of oligostirol mol. weight. 5000 and the content of terminal hydrazide groups of 2.15%.

Example 4. 10 ml of isoprene, 0.58 g of azo-bis-iso-butyric acid dihydrazide and 0.3 g of OP-10 emulsifier in 10 ml of distilled water are heated in a sealed ampoule at 85 ° C for 17 hours. Get 2.3 g of oligoisoprene, mol. weight. 3200 and hydrazide content of 3.6%.

Subject invention

A method for the preparation of chain-chain oligomers with terminal functional groups by aqueous emulsion or solution polymerization or - isobutyric acid.