抄録
After studying the effects of allylation condition on the degree of reaction and the solubility of the reaction product in a solvent, a preparation method of the completely soluble allylcellulose in a solvent by using a kneader designed for this purpose is described. Also allylation processes are analysed.
The allylcellulose was prepared from allylating the alkalicellulose, treated with a 50% NaOHaq, with a liquid allylhalide in a glass ampoul agitated by electromagnetic means. Its iodine value (I. V.) was levelled off to ca. 180. The levelling-off of I. V. was not affected by the allylation temperature, addition of the solvents and permeating the allylhalide into alkalicellulose by high pressure of N2 gas, but the I. V. rose to ca. 200 by addition of a free NaOH. However these allycelluloses were not completely soluble in a solvent.
The allylcellulose prepared with the above described kneader of 2 liters under the condition that alkalicellulose treated with 50% NaOH; 170g, free NaOH; 120g, allylbromide; 800cc, allylation temperature; 80°C, allylation time; 2hrs, had 203.5 of levelling-off I. V. and is completely soluble in such solvents as benzene, toluene, xylene, cyclohexane, dimethylformamide, dimethylsulfoxide, etc. It is interesting that the above allylcellulose is also soluble in the various vinyl monomers such as styrene, P-vinyltoluene, α-methylstyrene, methylmethacrylate, methylacrylate, vinylacetate, acrylonitrile, etc.
ENaOH, efficiency of the allylation, may be defined as follows:
ENaOH=(NaOH mol equivalent to degree of allylation)/(NaOH mol consumed in practice) then ENaOH increases with the D. S. and decreases with the allylation temperature and the NaOH concentration for steeping pulp at a certain D. S.
It was found that the relation between D. S. and Z, consumed NaOH per cellulose in alkalicellulose, was Z=K[D. S.]n
where n; constant and n was independent of the NaOH concentration for steeping pulp and increases with the allylation temperature.
