The method for extracting rare earth elements from phosphogypsum

 

(57) Abstract:

The invention relates to a process of producing compounds of rare earth elements (REE) by integrated processing of Apatite. Neutralization of the solution obtained after processing of phosphogypsum leachate solution containing 0.1-0.5 g-EQ/l of sulfuric acid, spend oxide or magnesium carbonate, and separating the precipitate REE filtering. As magnesium carbonate used magnesite. As the leach solution can be used a solution of magnesium sulfate after the precipitate containing REE, acidity which regulate the addition of sulfuric acid. The achieved result is to improve the filterability of precipitation, reducing their moisture and reusability of the leaching solution in circulation. 2 C.p. f-crystals.

The invention relates to the field of technology for compounds of rare earth elements (REE) by integrated processing of Apatite.

The method for extracting rare earth elements from phosphogypsum (see the patent of Russia No. 2104938, IPC6C 01 F 17/00, 1998) by leaching it with acidified solutions with subsequent neutralization of the mixture of gaseous amaknak conditions leaching ensure recovery of REE in quantities of only 15%. In addition, the method does not allow for reuse of the leach liquors.

There is also known a method for extracting rare earth elements from phosphogypsum (see ed.St. USSR N 1818304, IPC6C 01 F 17/00, 1993), including processing of source material with a solution of ammonium sulfate with a concentration of 10-50 g/l and acidity 0.1-0.5 g-EQ/l, neutralizing the resulting solution with ammonia emitting rare earth elements in the precipitate and separating the precipitate by filtration.

By a known method when the content of ammonium sulphate leaching solutions not more than 50 g/l achieved the recovery of REE 30-34%, however, the resulting precipitation is difficult filtered, and the humidity precipitations after filtering is about 85 wt.%, what hinders their further processing. When the concentration of ammonium sulfate in acidic leaching solutions more than 50 g/l recovery of REE into solution leaching sharply decreases due to the formation of the double sulphate of ammonium and REE, prevented REE into solution. In addition, when used for neutralization of leaching solutions of ammonia accumulates in them ammonium sulfate. This limits the ability to reuse solutions is not bol is divided into the task of improving the filterability of precipitation, reduce humidity and increase the frequency of use of the leaching solutions.

The problem is solved in that in the method for extracting rare earth elements from phosphogypsum, including processing of source material leaching solution containing 0.1-0.5 g-EQ/l of sulfuric acid, neutralizing the resulting solution with the extraction of rare earth elements in the precipitate and separating the precipitate by filtration, according to the invention the neutralization solution conducting oxide or magnesium carbonate.

The solution of this problem is achieved by the fact that as the magnesium carbonate used magnesite.

The problem is solved also by the fact that as the leach solution used solution of magnesium sulfate after the precipitate containing rare earth elements, acidity which regulate the addition of free sulphuric acid.

The use of magnesium oxide or magnesium carbonate (including in the form of magnesite) to neutralize the solution leaching allows you to get a well filterable precipitation, humidity, after which the filter does not exceed 50-54 wt.%.

Neutralised oxide or carbonate magic the presence of a high concentration (about 100 g/l) of magnesium sulfate has virtually no effect on the transition REE into solution.

The essence of the proposed method can be explained by the following examples.

Example 1. 1 kg of phosphogypsum containing of 0.54 wt.% the amount of REE, is treated with a solution of 10 g/l (0.2 g-EQ/l) H2SO4if T:W=1:5 for 0.5 hours. The solution is filtered and neutralized by the introduction of 20 g of magnesium oxide to a pH of 5.5 with stirring for 1 hour. The precipitate is filtered off and dried. The filtration rate is 1.3 m3/m2per hour, the weight of wet sediment is equal for 52.6 g, dry and 25.8 g, humidity equal to 51.8 wt.%. Dry sludge has to 7.0 wt.% (1.8 g) REE. Recovery of REE is 33.3%.

Example 2. The process is conducted under the conditions of example 1, but the neutralization is carried out 40 g of crushed magnesite. The filtration rate is 1.3 m3/m2per hour, the weight of wet sediment equal of 49.6 g, dry - 23,4 g, the humidity of 52.8 wt. %. The content of REE in the dry precipitate is equal to 7.7 wt.% (1.8 g). Recovery of REE is 33.3%.

Example 3. The process is conducted under the conditions of example 2, but for processing of phosphogypsum use a solution containing 96 g/l of magnesium sulfate (working solution of 8 cycles) with the addition of sulfuric acid to a concentration of 10 g/l (0.2 g-EQ/l). The filtration rate is 1.35 m3/m2per hour, the weight of wet sediment RA is t to 34.8%.

Example 4 (the prototype). 1 kg of phosphogypsum is treated with a solution of ammonium sulfate 50 g/l, containing 10 g/l (0.2 g-EQ/l) sulfuric acid, at T:W=1:5 for 1 hour. The solution is filtered and neutralized by ammonia water to pH 5. The formed precipitate was separated by filtration and dried. The filtration rate is 0.25 m3/m2per hour, the weight of wet sediment equal 130,4 g, dry - 20.6 g, humidity - 84,2 wt.%. The total content of REE in dry sediment - 8.0 wt.% (1.65 g). Recovery of REE is 30,5%.

Thus, from these examples it follows that the present invention allows to increase the filtration rate of precipitation in 5 times, to reduce their moisture content at 30-32 wt. %, and also provides reusability in circulation of the leaching solution.

1. The method for extracting rare earth elements from phosphogypsum, including processing of source material leaching solution containing 0.1 - 0.5 g-EQ/l of sulfuric acid, neutralizing the resulting solution with the extraction of rare earth elements in the precipitate and separating the precipitate by filtration, characterized in that the neutralization of the solution conducting oxide or magnesium carbonate.

2. The method according to p. 1, characterized in that as CT the surrounding solution using a solution of magnesium sulfate after separation of the precipitate, containing rare earth elements, the acidity of which is regulated addition of sulfuric acid.

 

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