GB/T 480-2010Test of low temperature distillation of coal by aluminum retort (English PDF)

4.1 Xylene or toluene: chemically pure.

4.2 Lubricating oil and selected flake graphite powder.

5.1 Aluminum retort

5.1.1 Aluminum retort body (Figure 1), made of aluminum;

5.1.2 Aluminum retort cover (Figure 2), made of aluminum;

5.1.3 Delivery line (Figure 3), made of copper;

5.1.4 Connecting nut (Figure 4), made of steel.

5.2 Heating device: with temperature control device; specifications and

performance shall meet the following requirements:

a) The temperature shall be increased to 260 °C within the first (15 ~ 20) min;

b) During (260 ~ 510) °C, the heating rate is 5 °C/min. The total temperature

rise error is ±10 °C;

c) The final temperature can reach above 510 °C.

6.3 Coal sample

The coal sample is an air-dried coal sample, whose particle size is less than

0.2 mm, that is prepared according to GB 474 or GB/T 19494.2.

6.4 Instrument assembly

6.4.1 Cover the retort cover. Use a small wooden hammer to lightly tap the retort

cover tightly. Use a tight airtight cork stopper to connect the aluminum retort

delivery line to the conical flask. Extend the aluminum retort delivery line into

the bottle; the length of the extension shall not be less than half the height of

the bottle, but shall not be in contact with the bottom of the bottle. Insert a

slightly curved glass air duct from another small hole of the cork stopper for gas

discharge. All junctions shall be airtight. The conical flask shall be washed, dried

and weighed, to 0.01 g, in advance before it is connected to the aluminum retort.

6.4.2 Put the aluminum retort into the electric furnace; at the same time, put the

conical flask into the cooling bath. Close the furnace cover; insert the

thermocouple or thermometer into the temperature measuring hole of the

aluminum retort.

6.4.3 Put a certain amount of water and ice cubes in the cooling bath; the

conical flask shall be immersed in the water as much as possible, but the bottle

mouth shall be higher than the water surface. Circulating water below 15 °C

can also be used; but the circulating water flow shall be able to make tar and

water vapor condense.

6.4.4 The test device shall be placed in a fume hood; otherwise, a rubber tube

shall be connected to the air duct on the conical flask, so as to lead the gas out

of the room.

7.1 Fully stir the coal samples; take (20 ± 0.5) g of coal sample (weigh to 0.01

g) from 4 ~ 5 different parts of the coal sample container; put it in a watch glass;

then, transfer all the coal samples to the aluminum retort.

Note: If the preliminary test which is conducted with reference to Appendix D

shows that the coal sample is very expandable, an appropriate amount

of sand can be added to prevent it from expanding. Coal sample and

sand shall be mixed evenly, and put in the retort; make the surface

smooth.

7.2 After everything is prepared, it can be heated by electricity. The sides and

bottom of the aluminum retort shall be heated at the same time, to keep the

temperature of each part of the bottle body uniform. Within the first (15 ~ 20)

min, the temperature shall be raised to 260 °C; after reaching 260 °C, the

heating rate shall be strictly controlled to 5 °C/min; the actual temperature shall

be checked every 10 min, to keep the difference from the to-be-reached

temperature within 10 °C. When it reaches 510 °C, keep it warm for 20 min and

stop heating.

7.3 During the test, the tar, water vapor and coal gas which are produced after

the coal sample is heated enter the conical flask through the delivery line. The

tar and water vapor shall be condensed in the conical flask. The coal gas is led

outside by the rubber tube.

7.4 After the heating is stopped, use an alcohol lamp or other heat source to

slightly heat the aluminum retort delivery line, so that the tar that is attached to

the delivery line wall flows into the conical flask.

7.5 After the tar that is attached to the delivery line wall flows out, drain the cold

water in the cooling bath or remove the cooling bath; remove the thermocouple

or thermometer; remove the cork stopper that connects the conical flask to the

retort body; remove the aluminum retort; put it in the shade place to cool. In

order to prevent the coke residue from absorbing moisture in the air, the delivery

line of the aluminum retort shall be sealed at this time.

7.6 Dry the outer wall of the conical flask that contains the coolant; weigh it after

placing it for about 5 min (weigh to 0.01 g). The difference between the mass

of the conical flask that contains the condensate and the mass of the conical

flask before dry distillation is the mass of the dry distillation condensate.

7.7 Determine the water content in the condensate (dry distillation total moisture)

as described in 8. The difference between the mass of condensate and the

mass of water is the mass of tar.

7.8 After the aluminum retort cools, remove the retort cover; pour the coke

residue into the weighing bottle and weigh it (weigh to 0.01 g). Be careful not to

scrape the retort body when scraping the coke residue on the retort wall.

7.9 The total coal sample minus the sum of the condensate mass and the coke

residue mass is the mass and loss of coal gas. The mass fraction of each

product to the mass fraction of the coal sample is the air-dried basis yield.

7.10 The pyrolysis water yield is obtained by subtracting the air-dried basis

moisture Mad (measured according to GB/T 212) from the dry distillation total

moisture (7.6).

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