SU1643562A1 - Cellulose oligomer as binder for lacquers and method for its production - Google Patents

Abstract

The invention relates to the preparation of a binder for paints and varnishes based on cellulose oligomer, by the reaction of ethyl, acetyl or nitrocellulose with phenyl or chlorohexyl isocyanate in the presence of boron etherate fluoride. Cellulose oligomer provides a drying time for a varnish film (up to 0.3 hours), an increase in elasticity, adhesion, water resistance (up to 24 sou. Tons) and light resistance. 2 sp.f-ly, 4 tab.

Description

The invention relates to the field of film-forming, namely, a urethane binder based on cellulose for paints and varnishes, -. fishing intended for protective and decorative coatings of metal, wood and other substrates.

The aim of the invention is to obtain a cellulose oligomer having a structure that provides an increase in solubility and an improvement in the performance of coatings based on it.

The resulting cellulose oligomer, a solid that decomposes when heated, is soluble in carbon tetrachloride, perchlorethylene or their mixtures, has a mol.m.1627-4261 and is characterized by the presence in the structure of octacyclyurethane units and urethane groups in the 1,4-glucose group position

The composition and structure of the new compound is confirmed by IR and NMR C-spectroscopy.

The formation of a substituted urethane bond as a result of the reaction is confirmed by the absence in the IR and NMR spectra of the absorption bands caused by the presence of hydrogen at the nitrogen atom, as is characteristic of the urethane bond.

The NMR spectra of solutions of the reaction products thoroughly purified from impurities of the initial reagents are removed on a Bruker spectrometer in deuterochloroform at an operating frequency for carbon resonance of 62.9 MHz in the Fourier transform mode with broadband

 A

from protons, H ..

The incorporation of monoisocyanate into the macromolecule chain along the 1,4-glucosidic bond in the glucopyran ring is proved by the presence in the product spectrum of the action of triethylcellulose with phenylisocyanate signals: from the phenyl fragment, ment - 119, 123, 129, .139 ppm in the chain and 118.5; 123.5; 129; 137.5 ppm (in the ring; from carbonyl carbon

(L

WITH

O5 4

WITH

ate

oz

No

ppm, also according to I

316

isocyanate group - $ 157 chain of about 153 ppm in the ring, and the appearance of an additional broadened g signal from the (Ј -carbon atom of the glucopyranic ring associated with the phenyl isocyanate fragment, at V 1 01 ppm) The ratio of monoisocyanate in the chain and in the ring is 1: 1, and the ratio of the number of glucopyranic cycles per phenyl or chlorohexyl urethane group (i.e. the degree of urethanization) is easily calculated from the integral curve of NMR spectra C and the ratio m: n: p is 1j1: 1-8.

The method for preparing cellulose oligomer is carried out as follows.

Perchlorethylene or a mixture of perchlorethylene with tetrachloride is poured into the reaction flask with a stirrer, a cooler, a calcium chloride tube, an addition funnel when injecting an inert gas.

Q

0

five

carbon, load pre-dried azeotropic distillation with benzene ethyl, acetyl or nitrocellulose, boron trifluoride etherate, the mixture is heated to 80 ° C with stirring for 2.0-2.5 hours, then phenyl is added dropwise over 20-40 minutes; or chlorhexyl isocyanate, incubated for 0.5-2 hours until completion of the reaction (disappearance of free monoisocyanate), cooled, filtered, washed with petroleum ether, the solvent is distilled off. The resulting urethane-containing product is analyzed.

Data on the synthesis of binders are given in Table. 1 and 2, and the composition and properties of paints and varnishes - in table 3 and 4.

Claims (2)

Claims 1. Cellulose oligomer of general formula R1 O I II N-C-0 where R is C2H5 - C - CH3, - N02; about K1 - C1 (CIS) b-; m: n: p 1: 1: 1-8, H OR OR H K-RJ Choor V with mol.m. 1627-4261 as a bond for paints and varnishes. 45 2. A method for producing a cellulose oligomer of the general formula CH9OR R1 0 n I Я Чг-N-C-0 + HNl DR P where R - CjHj--; - С - CH3; -NO g; R sbH5-C1 (CHg) 6-; m: n: p 1: 1: 1-8, Mol.1627-4261, characterized in that ethyl, acetyl or nitrocellulose as a solution in 20 notable groups. Cellulose Chemicals Cellulose Acetate Nitrocellulose phenyl isocyanate Chlorhexyl isocyanate Ether of boron trifluoride Dibutyl tin urine Dimethylformamide Perchlorethylene Carbon tetrachloride N0 J sneso C1 (CH2) b Temperature stage I, ° C 80 H. OR perchlorethylene or its mixtures with carbon tetrachloride are treated with boron trifluoride etherate at 80–90 ° C for 1.5–2.0 h, and then a solution of phenyl or chlorohexyl isocyanate is added over 25–30 min. Isoci Disappearance Table 1 18.34 37.5-42.7 43.1 13.6 0.4 47.421.4 41, 184 27.45 -48.0 21.5 sneso H2) b 13.7 CaHe- fCfiHf ICKCH H Ws Hgс6н5 85 85 80 80 1643562 Appearance Bleach- Clear solution Purity No mechanical impurities at 62.7 52.6 57.1 58.85 14.9986 52 25 Full full Oh oh thirty 22 20 nr 95 Does not combine Does not combine Oh oh ABOUT about 1: 1: 8 1627 1: 1: 1 4261 1: 1: 4 2300 1: 1: 2 3850 eight Continuation of table 1 Muddy Colorless solution transparent salt-color Observations- Mechanical additives of the mixture are absent. 20 nr 95 Does not combine Does not combine ABOUT about 1: 1: 2 3850 Components Content of components, mash, c. compositions one but with lay y 40 65 0.01 12.00 52 0.03 18.97 0.015 7.5 7.5 20,511,014,0 24,485 11.99 Varnish delivery form Mono-component composition Transparent homogeneous gloss film; texture is well developed. 40 48 44 164356210 Table 3 T 52 0.03 18.97 The composition of the composition is uniform gloss, texture proosho 48 44 24 five thirty 24 24 thirty thirty No change I 1 1 24 ten Yellowing 3