Method of extracting germanium from germanium deposit using thermal reduction process

Abstract

A method of extracting germanium from a germanium deposit using a thermal reduction process is disclosed. The method includes: adding sodium monophosphate to a germanium deposit to obtain a mixed germanium deposit; isolating the mixed germanium deposit from air; increasing the temperature and then baking the mixed germanium deposit; and obtaining a germanium concentrate after volatilization of the mixed germanium deposit.

Claims

1. A method of extracting germanium from a germanium deposit using a thermal reduction and volatilization process, comprising: Step 1): weighing a germanium deposit having a particulate diameter of less than 1 cm to obtain a weight of the germanium deposit, weighing sodium monophosphate crushed to 120 meshes or more in an amount of 2.5%-7.5% by weight of the germanium deposit, dissolving the sodium monophosphate with water at a weight that is 0.1-0.5 times the weight of the germanium deposit to obtain a solution, and uniformly mixing the solution with the germanium deposit to obtain a mixed germanium deposit; and Step 2): placing the mixed germanium deposit in a Muffle furnace or a pyrogenic germanium extracting device preheated to 900 C.-1,000 C., closing the Muffle furnace or the pyrogenic germanium extracting device to isolate the mixed germanium deposit from air, increasing a temperature in the Muffle furnace or the pyrogenic germanium extracting device to 1,000 C.-1,100 C., baking the mixed germanium deposit for 1-2 hour(s) for volatilizing and concentrating so that germanium is concentrated in volatilized smog, and collecting the volatilized smog that enters into a smog-collecting bag to obtain a germanium concentrate.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIG. 1 shows the flowchart of the process of the present disclosure.

DETAILED DESCRIPTION

Embodiment 1

(2) The components of the raw materials are shown in Table 3.

(3) TABLE-US-00002 TABLE 3 Components of the raw materials Germanium/ Ash/ Fixed carbon/ Water/ Calcium/ Magnesium/ Aluminum/ Silicon/ Arsenic/ Phosphorous/ % % % % % % % % % % Germanium 0.0321 42.20 25.6 17.32 2.41 0.53 2.56 12.17 0.03 0.02 deposit

(4) Step 1: weigh 10 tons of germanium deposits crushed to have a granularity of 1 cm or less and shown in Table 3; weigh 250 kg of sodium monophosphate (accounting for 2.5 wt % of the germanium deposits); add 1,000 kg water to dissolve the sodium monophosphate; and uniformly mix an obtained sodium monophosphate solution and the germanium deposits using a mixing machine.

(5) Step 2: add the above mixture in the pyrogenic germanium extracting device preheated to 900 C. or above, wherein industrial coal with a thickness of 5 cm-8 cm is used as primer in the furnace; maintain the thickness of the coal layer to be 50 cm-70 cm; cover a layer of domestic coal on the germanium deposits; close the furnace door; increase airing to raise the temperature in the furnace to 1,000 C.-1,100 C. for baking and volatizing for 1 hour at a constant temperature; turn the coal layer 2-3 times to ensure complete burning during the baking and volatizing period; maintain a negative pressure state in the furnace by adjusting the flow rate of induced air during the baking and volatizing period, which may be performed by observing a pressure gauge or observing that flames do not come out of the furnace door.

(6) Step 3: after the baking and volatizing period is completed, lower the temperature in the furnace to 500 C.; start a slag discharging device to discharge the slag; cool the slag to room temperature; weigh the slag to obtain a weight of 5.83 tons; and calculate the loss on ignition rate of the germanium deposits to be 42.10%.

(7) Step 4: sample the slag left after volatilization; calculate the germanium grade in the slag left after volatilization to be 0.0021%; calculate the germanium volatilization rate of the germanium deposits to be 96.30%.

Embodiment 2

(8) The components of the raw materials are shown in Table 2.

(9) TABLE-US-00003 TABLE 2 Components of the raw materials Germanium/ Ash/ Fixed carbon/ Water/ Calcium/ Magnesium/ Aluminum/ Silicon/ Arsenic/ Phosphorous/ % % % % % % % % % % Germanium 0.0448 59.9 18.68 15.2 3.42 0.39 3.00 14.97 0.04 0.03 deposit

(10) Step 1: weigh 50 g of germanium deposits shown in Table 2 and put the germanium deposits in a cupel; weigh 2.5 g of sodium monophosphate (accounting for 5 wt % of the germanium deposits) and put the sodium monophosphate in a small beaker; take 25 mL of water to dissolve the sodium monophosphate; add an obtained sodium monophosphate solution to the germanium deposits sample; mix uniformly the monophosphate solution and the germanium deposits sample using a glass bar; take 10 mL of water to wash the small beaker and the glass bar, and add the used water to the germanium deposits sample; put the sample in a baking oven preheated to 90 C. for 30 minutes to evaporate water until the sample is almost dry.

(11) Step 2: take the sample out of the baking oven; put the sample in a Muffle furnace preheated to 900 C.; and increase the temperature in the Muffle furnace to 1,000 C. for baking and volatizing at a constant temperature for 1 hour.

(12) Step 3: after the baking and volatizing are completed, lower the temperature to 500 C.; take the cupel out of the Muffle furnace and cool the cupel to room temperature; weigh the baked slag left after volatilization to obtain a weight of 28.7 g; calculate a loss on ignition rate of the germanium deposits to be 42.6%; take out the slag and grind the same to be 120 meshes or above.

(13) Step 4: take certain amount of the slag left after volatilization for analysis; and calculate a germanium grade of the slag left after volatilization to be 0.0033%; calculate the germanium volatilization rate of the germanium deposits to be 95.50%.