Germanium-containing non-ferrous metal oxide or sulfide ore material, prior to recovery of the main metal to volatilize germanium sublimed into dust, and further the process of obtaining pure GeO 2. Most of the main metals in the raw materials are lead , zinc , copper and the like. The process of this method is short, and it is not necessary to go through the treatment steps of leaching, filtration, tannin precipitation, calcination, etc., and directly obtain the cerium concentrate containing more than 10% cerium. The recovery rate of cerium is high, but only the raw materials can be recovered. The antimony sulfide and antimony oxide are not subject to promotion due to the constraints of the main metal production process.
The principle of sulphide and suboxides has a high vapor pressure at lower temperatures. For example, the vapor pressure of GeS is 1386Pa at 997K, the vapor pressure of GeS 2 at 956K is 380Pa, and the vapor pressure of GeO at 166K is 1662.5Pa. . In addition, they also have the property of being sublimated and volatilized at a lower temperature in a neutral or weak reducing atmosphere. These characteristics of bismuth sulfide and suboxide can be utilized to control the furnace atmosphere and temperature so that they first sublimate and volatilize. The main metal sulfides or oxides such as lead, zinc and copper in the raw materials are rarely volatilized under these conditions. According to this, in the early stage of recovering the main metal lead, zinc, copper, and the like of the raw material, the ruthenium in the raw material is preferentially volatilized and concentrated in the soot to be recovered.
Process Belgium Hoboken Ovipet Metallurgical Company (MH0) used a single volatilization method to recover plutonium from vermiculite in 1952. China also used similar two-volatility method to recover plutonium from lead-zinc ore in the 1960s.
The primary volatiles raw material is vermiculite concentrate, and the main components (mass fraction w/%) are: Ge 0.25, Cu 27.8, Zn 7.92, Pb 25.0, As 7.5 and the like. After the raw materials are dried, the charcoal or 10% coke with a mass of 4% is added to make a pellet (see the charge group). The aggregate is periodically added to the shaft furnace with a cross-sectional area of ​​0.23m×0.58m, and the reducing gas containing C0 30%, H 2 1%～2% and the remaining nitrogen is sent from the upper part of the furnace to the volatilization temperature. Control is between 1143 and 1253K. Under these conditions, bismuth sulfides and suboxides in the furnace, as well as impurities such as arsenic , sublime into the flue gas. The temperature of the flue gas discharged from the shaft furnace is above 973K, and it is necessary to recover 80% of the crucible by the condenser first, and then collect the dust with a cloth bag. Calcine is sent to recover the main metal. During the process, the enthalpy of volatilization is 92% to 93%, while PbS is only volatilized by 5% to 10%. The collected cerium-containing sulfide dust is blown into the air in an electric furnace at a temperature of 823 K for oxygen roasting to remove arsenic and sulfur. The calcined product (antimony concentrate) is purified by chlorination distillation, hydrolyzed, and finally a GeO 2 -containing antimony concentrate is obtained (see classic chlorination method).
The raw material of the two volatilization method is lead-zinc concentrate, and the main component (mass fraction w/%) is Ge 0.005-0.008, Pb2.4, Zn 40-42.2, etc.
Two volatile extraction processes
The process is shown in the figure. One volatilization is the raw material is blended into petroleum slag (or charcoal, or coke), and after being formed into a pellet, it is added into a rotary kiln, and is reduced and volatilized in a reducing atmosphere at a temperature of 1223 to 1273 K for 1 h. The gas of the reducing atmosphere generally contains CO 3 %, C0 2 17%, O 2 1%, and the balance is N 2 . The volatilization rate is 98%, the soot rate is 8%, and the dust content is 0.05% to 0.06%. The calcine obtained by volatilization is sent to recover the main metal. Since the primary volatile dust is mostly mechanical dust and the niobium grade is low, it needs to be granulated and then subjected to secondary volatilization. The second volatilization was carried out in a shaft furnace and volatilized at a temperature of 1223 K for 0.5 h. In order to suppress the volatilization of lead, a high column and low level temperature (less than 873K) operating system are used. The enthalpy evaporation rate is 98%, and the secondary volatile dust rate is 2% of the pellets. After the secondary volatile dust collected is oxidized and dearsenized, the antimony concentrate containing more than 10% of antimony is obtained. The cerium concentrate is subjected to chlorination distillation, double distillation, and hydrolysis to obtain a pure GeO 2 product containing cerium 68% to 69%. The direct recovery of hydrazine is greater than 70% and the total recovery is 85%.
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