Preparatory work/about to start work
(1) Wash and dry the distillation bottle, weigh it to 0. 1g, and then put it in the oven for later use.
(2) Wash, dry and number the 150m 1 or 250m 1 conical flask, weigh its mass to the accuracy of 1mg, and then put it into a dryer for later use.
(3) Cleaning and drying all parts of the cooling device, wherein the sand core filter funnel is soaked in the washing liquid, distilled and cleaned until neutral, and then dried for later use.
(4) Prepare asphalt samples.
(5) When distilling in a high-temperature furnace, preheating is needed, and the constant temperature in the furnace is controlled at 550℃ and 10℃.
(6) Prepare ice water in a beaker.
Test steps
1) Weigh the quality of asphalt samples in distillation bottles (mb is (50&; p 1 usmn； 1)g, accurate to 0. 1g, use a cork with a conical cork as a receiver and put it in a beaker filled with ice water.
(2) When using a high-temperature electric furnace, set the distillation bottle containing the sample at a constant temperature (550&:p1usmn; 10)℃
If a gas stove is used, adjust the flame height to surround the distillation bottle.
(3) Adjust the heating intensity (that is, adjust the distance between the distillation bottle and the high-temperature furnace or the flame size of the gas furnace), so that the initial distillation starts within 5-8min after the heating starts (the first drop of distillate flows out from the branch nozzle). After that, distillation is continued at the outflow rate of two drops per second (4-5m 1/min) until no oil escapes, and then the bottom of the distillation bottle is burned red within 1min (i.e. the distillation residue in the bottle is coked).
The whole distillation process must be completed within 25 minutes. After distillation, the remaining distillate in the branch pipe should flow into the receiver.
(4) Take out the conical bottle containing distillate oil from the ice water, dry the water outside the bottle, cool it at room temperature, and weigh its mass to obtain the total mass of distillate oil (m 1), accurate to 0.05g.
(5) heating and melting the distillate oil in the conical flask, and uniformly stirring. When heating, the temperature should not be too high to avoid evaporation loss. Then pour the melted distillate into another conical flask (250m 1) with known quality, and weigh the mass (m2) of the distillate for wax removal, accurate to 1mg, and the quantity should ensure that 0.05-0. 1g wax can be obtained after freezing and filtering, but the sampling amount should not exceed/kloc.
(6) Install the cooling and filtering device, and connect the rubber tube of the filter bottle branch pipe with the water pump (or vacuum pump) and the U-shaped mercury column pressure gauge. Inject an appropriate amount of cold liquid (industrial alcohol) into the cold bath, and the liquid level of the cold bath is about 70mm higher than that of the sample cooling cylinder (ether-alcohol), so that dry ice added into the cold bath will not splash on the sample cooling cylinder, and stir the cold liquid with appropriate tools to keep the temperature at (-20 soil 0.5)℃. The cryogenic water tank can also be used as a cold water bath. At this time, the cold liquid can be 1: 1 methanol aqueous solution, and the low-temperature water tank should be able to automatically control the temperature to (-20 soil 0.5)℃.
(7) Inject 10 1 ether into the conical flask filled with distillate oil to fully dissolve it, then inject it into the sample cooling cylinder, and then wash the oil-containing conical flask twice with 15 1 ether, pour the washing liquid into the sample cooling cylinder and inject 25m 1 into the sample cooling cylinder. From the time of adding ether, the wax was cooled for several minutes to completely crystallize and separate out.
(8) Measure 50nI 1 ether-ethanol 1: 1 mixed solution in another conical flask or test tube (50m 1) in advance, and cool it to -20℃ for at least 15 minutes before use.
(9) When the solution in the sample cooling cylinder is cooled and crystallized, pull out the plug, filter the wax precipitated by crystallization, hang the plug in the sample cooling cylinder by an appropriate method, and keep natural filtering for 30 minutes.
(10) When no liquid can be seen in the sand core filter funnel, start the water flow pump (or vacuum pump) and adjust the vacuum degree of the U-shaped mercury column manometer, so that the filtering speed of the filtrate is about one drop per second until the liquid drops. ) Then carefully turn off the water pump (or vacuum pump) and restore the manometer to normal pressure. Then add 30m 1 into the cooled ether-ethanol mixture at one time, wash off the wax layer, and clean the plug and the inner wall of the sample cooling cylinder. Continue to filter, when the solvent is not visible on the wax layer, continue to filter for 5 minutes, discharge the solvent in the wax and remove the solution in the wax.
(1 1) Take out the sample from the cold bath, cool the filter device, remove the suction filter bottle, and pour the solution into the recovery bottle. The suction filter bottle was also washed with the mixed solution of ether and ethanol for three times, each time with 10- 15m 1, and the washing liquid was poured into the recovery bottle.
(12) Reinstall the sample cooling cylinder, plug and suction filter bottle, and then preheat it to (50-60)℃ with.
(13) Pour the wax liquid in the suction filter bottle into the weighed conical bottle.) Wash the suction filter bottle with normal temperature petroleum ether for three times, with the dosage of 10- 15m 1 each time. Pour the lotion into the wax solution in the conical flask.
(14) Put the conical flask with wax solution on a suitable heat source to collect the solvent or evaporate it completely. Then put the conical flask into an oven with a temperature of 105℃ and a soil temperature of 5℃ to remove petroleum ether, then put it into a vacuum drying oven (105℃ and a residual pressure of 2 1-35kPa) 1h, and then put it into a dryer to cool it/kloc-0.
After distilling the same asphalt sample, three samples were taken from the distillate for testing.
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