N-Heptane CAS 142-82-5

(1) Increase n-heptane, a basic material with a purity of regarding 98%, over the silica gel adsorption column. The specs of the adsorption column are: size 1.5 m, internal size 3.2 centimeters, the quantity of silica gel filled up is 4/5 of the column length, in addition to circulation right into the column by gravity Inside, control the circulation rate of 50mL-80mL/ minutes, make the all-natural solvent fully contact with the silica gel, and also take in the alkane and additionally fragrant hydrocarbon pollutants in it, and also remove the very first effluent (relating to 200-500ml), because the pollutants in the silica gel will absolutely be hauled with the Come out, assess the liquid out.
( 2) Circulation the uncovered n-heptane effluent right into the diatomite adsorption column, the diatomite adsorption column is the same as the silica gel adsorption column, as well as make use of the diatomite adsorption column to contact with the natural solvent, which can take in impurities such as carbonyl substances and also different from them Breaking up, the flow cost is 50mL-80mL/ minutes, and also the absorbance of the outflow examination is close to the index. For the adsorption columns (silica gel, diatomaceous world) utilized in the above 2 steps, the candidate has actually executed numerous examinations. The results disclose that the integrated use both adsorbents has a better impact. After being adsorbed by two-stage adsorption columns, the product of n-heptane is ≥ 99%.
( 3) The n-heptane effluent of step (2) is dried by means of a drying out column, the desiccant in the drying column is anhydrous calcium chloride or calcium hydride, as well as also the moisture material of the drying out effluent is 0.01% to 0.05%, over 0.05% Assuming that the desiccant is filled with water, replace the desiccant prior to drying. After drying with anhydrous calcium chloride or calcium hydride, the water content gets to 0.01% to 0.05%.
( 4) Put the dried effluent right into the reaction pot for adjustment, and likewise utilize electrical house heating to manage the home heating temperature level at 140 ° C to 200 ° C, the temperature degree of the n-heptane fluid in the kettle is 100 ° C to 110 ° C, as well as likewise the temperature level of the result liquid is 98 ° C to 99 ° C; The reflux proportion is 10:5 ~ 8, gradually transform the reflux percentage to 10:12 ~ 15, as well as lastly acquire the chromatographic high quality n-heptane thing; repair according to the figured out process conditions, handle the rectification temperature level and reflux proportion, and additionally remove the previous portion, and prepare The n-heptane created all pleased the chromatographic index demands.
( 5) After passing the test, the ended up item is filteringed system with a 0.45 μm microporous membrane layer, bottled, as well as also conserved under nitrogen protection.