Tobacco smoke filter material and process for the preparation thereof
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example 1
Preparation of Acetoacetate-Functional Cellulose Acetate Tow
[0023]A sample of cellulose acetate filter tow (25.2 g) was added to a 1 L, round-bottom flask equipped with a thermowell, a rod shaped magnetic stirring bar under argon, a vigereux column, and a distillation take off head. The cellulose acetate of the filter tow has an acetyl degree of substitution (DS) of 2.45 providing an expected free hydroxyl content of 52 millimoles (mmol). The filter tow consisted of cellulose acetate filaments having a denier per filament of 2.7 and a total denier of 35,000. To the flask was charged toluene (502.7 g) and the mixture was heated to reflux (pot temperature=109° C.) and maintained at reflux for 30 minutes. The resulting distillate (8 g) was removed until it was no longer cloudy; the distillate was found to contain about 1 ml of water. Over a 30 to 60 minute period the mixture was permitted to cool to 60° C. using a heating mantel as an insulator. 4-(Dimethylamino)pyridine (DMAP; 0.47 g)...
example 2
Preparation of Acetoacetate-Functional Cellulose Acetate Tow
[0026]In this example a large excess of diketene was used to obtain a higher degree of acetoacetate substitution. The cellulose acetate of the filter tow utilized has an acetyl DS of 2.45 providing an expected free hydroxyl content of 53 mmol. Cellulose acetate filter tow (25.77 g) was added to a 1 L, round-bottom flask equipped with a thermowell, a glass mechanical stirrer under argon, a vigereux column, and a distillation take off head. The filter tow consisted of cellulose acetate filaments having a denier per filament of 2.7 and a total denier of 35,000. To the flask was charged toluene (503.00 g) and the mixture was heated to reflux (pot temperature=109° C.) and maintained at reflux for 30 minutes. The resulting distillate (5 g) was removed until it was no longer cloudy; the distillate was found to contain about 1 ml of water. Over a 30 to 60 minute period the mixture was permitted to cool to 60° C. using a heating man...
example 3
Preparation of Acetoacetate-Functional Cellulose Acetate Filter Rod
[0028]This example illustrates the reaction of gaseous diketene with cellulose acetate in the form of a filter rod 12.5 cm in length having an outside diameter of 8 mm). The filter rod (approximately 0.8 g weight) is produced from cellulose acetate filter tow and paper wrap wherein the cellulose acetate of the filter tow utilized has an acetyl DS of 2.45 providing an expected free hydroxyl content of 1.7 mmol. The filter tow consisted of cellulose acetate filaments having a denier per filament of 2.7 and a total denier of 35,000. The filter rod was inserted tightly into a glass tube equipped with vacuum tubing and vacuum meters on both ends. To one end was attached a vacuum pump with trap filled with dry ice. To the other end was attached a 15-mL round-bottom vacuum flask charged with diketene (5.0 g). The pump then was turned on to yield a vacuum of about 3 mm-Hg on the pump side and 8 mm-Hg on the flask side. This ...
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