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 present disclosure relates to a method of extracting germanium, which belongs to the field of metallurgy technologies of nonferrous metal, and particularly relates to a method of extracting germanium from a germanium deposit through thermal reduction, volatilization and concentration using sodium monophosphate as a reducing agent. The method of the present disclosure includes: adding sodium monophosphate to a germanium deposit; isolating from air; increasing the temperature and baking the germanium deposit; and obtaining a germanium concentrate after volatilization and concentration of the germanium deposit. Through baking the germanium deposit at 1,000 C., volatilization and concentration of the germanium deposit, the germanium recycling rate exceeds 96% when sodium monophosphate weighing 2.5% of the germanium depositis added. The present disclosure solves the following problems in the prior arts: existing pyrogenic methods for concentrating and extracting germanium from germanium deposits can hardly achieve a germanium recycling rate of greater than 75%; secondary pyrogenic recycling methods for extracting germanium slag have excessively high production cost and yield low germanium recycling rates; and the cost of hydrometallurgical treatment methods for low-grade germanium concentrates is too high.

Claims

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

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0024] FIG. 1 shows the flowchart of the process of the present disclosure.

DETAILED DESCRIPTION

Embodiment 1

[0025] The components of the raw materials are shown in Table 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

[0026] Step 1: weigh10 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.

[0027] Step 2: add the above mixture in the novel 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.

[0028] 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%.

[0029] 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

[0030] The components of the raw materials are shown in Table 2.

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

[0031] 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.

[0032] 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.

[0033] 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.

[0034] 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%.