SU411095A1 - - Google Patents

Description

one

A known method for the production of Cyanethylcellulose by nitrating cyaethylcellulose with a nitrous mixture consisting of 56% nitric acid, phosphoric anhydride and tetrachloride carbon at 24 ° C for 2 hours. The final products are soluble only in dimethylformamide and in mixtures of acetic acid with rhodium and potassium iodide.

In order to obtain from cellulose with a high degree of polymerization of esters soluble in commonly available solvents x-acetone, acetopitrile, methylene chloride-methanol mixture in a ratio of 9: 1, etc., it was proposed to carry out the esterification of free hydroxyl cyanoethylcellulose with 100% nitric acid.

Example 1. 1 g of cyapethylcellulose (Y 256), synthesized from cotton linters, is placed in nitric acid cooled to -10 ° C (d4 1.513). Bath module 1:15. After 1 hour, the reaction mass was poured into a 50% aqueous solution of acetic acid, cooled to -15 ° C and washed several times. Subsequently, washing with distilled water is carried out until neutrality by methyl orange. Sample height2

Sew in a vacuum oven at 50 ° C. The product has the following elemental composition (%): C- 51.68; N - 12.8; P 5.65; O - 29.88, which corresponds to the degree of substitution (y) for pyrogrune 14, cyanate groups 256. The infrared spectra of this ether show the bands absorbed in the region of 2248 corresponding to the stretching vibrations of the triple bond of CN-group, the absorption bands in the region of 2880-2940 cm are characteristic of the CH bond of the methylene groups of cyanoethoxy. The absorption bands in the 1640 and 1260 cm regions correspond to oscillations of the nitro groups. The main dielectric characteristics of nitrated tsanethyl cellulose at 20 ° C and a frequency of an electric field of 1000 Hz are 0.02 and 12, respectively. The specific volume resistance at 20 ° C is 10 ohm-cm. The intrinsic viscosity of the nitrated sample, determined in acetone, is 4.05, (i of the initial cyanoethylcellulose-4, 9). The sample is dissolved in the solvents listed above.

Example 2. Cyanethyl cellulose (7,249) obtained from sulphite wood pulp is treated with nitric acid under conditions similar to Prnmer I. The final product has the following elementary composition 3 (%): N -13.25; O -52.64; H is 5.59, which corresponds to the degree of substitution (y) for the n-trog groups 29, for the cytotoxic groups of 249. The sample is dissolved in 11 above and 11 times higher solvents. The characteristic 5 viscosity of an imitated sample, definitelein in acetone, is equal to 3.2 (i starting ethanol cellulose 4,1 j. 4 Subject of the invention The method of producing cyapethyl nitrocellulose by nitrating cyan cellulose cellulose acid, with the aim of obtaining from cellulose with a high degree of polymerization of soluble esters, nitration is carried out with 100% nitric acid.