SU146036A1 - Method for producing monomeric compounds from furfural and ketone derivatives - Google Patents

Description

It is known that polymer compounds obtained on the basis of furfural and its derivatives possess high heat resistance, and therefore are of considerable practical interest.

5-hydroxymethylfurfurol, produced by hydrolysis of cellulose, is a highly reactive compound that is able to form spatially cross-linked polymers under the action of a number of acidic agents.

However, this high reactivity of 5-hydroxymethylfurfural does not allow the polymerization of this compound to be controlled, and is a reason that it does not allow it to obtain technically suitable materials.

When studying the course of polymerization of some derivatives of 5-hydroxymethylfurfural, it was found that their reactivity is lower than that of the original 5-hydroxymethylfurfural and allows their use as a starting material for the production of heat-resistant polymers.

On the basis of these observations, a new method has been developed for the preparation of monomeric compounds from furfural derivatives, and ketones / in which. In order to obtain polymers with high heat resistance, 5-hydroxymethylfurfural is used as a starting material.

A general method for the preparation of monomeric compounds consists in the condensation of 5-hydroxymethylfurfurol with ketones in various molar ratios, in the presence of bases at temperatures of 16-88 ° C. The reaction proceeds with a large release of heat and is carried out in an aqueous medium with vigorous cooling. The course of the reaction is controlled by the sequence and amount of the reactants introduced, in parts. After completion of the condensation, the product is neutralized with a mineral no. 146Ш6-2 with an oral or organic acid, separated from water, washed and dried.

The formation of polymers from the obtained compounds is carried out by heating in the presence of catalysts.

The resulting monomeric compounds, as well as fusible and soluble resins, are capable of forming copolymers with various resins, rubbers and cellulose ethers.

Example. Preparation of Monomeric Compounds of 5-hydroxymethylfurfural with acetone (FAO grade).

The monomeric compound 5-hydroxymethylfurfural with acetone is a (5-hydroxymethyl-a-furyl-p-Binyl) ketone mixed with a bis (5-hydroxy-vinyl-a-furyl-p-vinyl) -ketone and products with a deeper degree of compaction.

An equimolar mixture of 5-hydroxymethyl-furfural and acetone and a double weight amount of water are charged into a flask equipped with a stirrer, a cooler and a thermometer and, after switching on the stirrer, in portions of 2%, based on the weight of 5-hydroxymethylfurfural caustic soda in the form solution. After the termination of the exothermic reaction phase, the temperature at which should not exceed 80 °, the reaction mass is heated for another 1-2 hours at 96-100 °, neutralized with sulfuric acid, the product is separated from the aqueous salt solution, washed and dried at 105 °. The resulting monomer brand FAO has the following indicators. The specific gravity is 1.12; pH-7; solubility in acetone is complete.

In the presence of 0.6% sulfonic acid and heating at 20–25 ° C for 20–30 hours, FAO monomer forms a non-combustible polymer, which has water resistance, Kanavz heat resistance of 490 °, and high chemical resistance.

On the basis of the FAO monomer, plastoconcrete with temporary resistance is also obtained (in kg / cm} compression 800-1200, stretching 70-180 and bending 360-320 and heat resistance up to 500 °.

The subject invention was also invented. The method for producing monomeric compounds from furfural derivatives and ketones subjected to polymerization, characterized in that, in order to obtain polymers having a high thermal stability, 5-about-half-methyl-furrode is used as the starting material.