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Saponifying method for rare-earth organic extracting agent

A rare earth organic and extraction agent technology, applied in the direction of improving process efficiency, etc., can solve the problems of large volume of water phase, lack of operability, loss of organic phase, etc., achieve volume reduction of water phase, broad application prospects, and low ammonia nitrogen content Effect

Inactive Publication Date: 2019-08-16
DEQING XINGBANG RARE EARTH NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the saponification is completed, the volume of the aqueous phase is too large, which will lead to a large loss of the organic phase discharged with the discarded water
Therefore, using clarified lime water for saponification also lacks operability in actual production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of saponification method of rare earth organic extractant, concrete steps are as follows:

[0026] Step 1, raw ore dissolution: burn and pulverize the rare earth raw ore to obtain rare earth raw ore powder, mix the rare earth raw ore powder with hydrochloric acid with a mass fraction of 32%, and the molar ratio of rare earth ions and chloride ions when the rare earth raw ore powder is mixed with hydrochloric acid with a mass fraction of 32% The ratio is 1:2, heated to 52°C in the reactor and stirred for 2.4h, and then continued to add 32% hydrochloric acid until the solid no longer decreased, and after cooling to room temperature, the solid-liquid separation was carried out by means of pressure filtration to obtain a mixed Rare earth chloride solution;

[0027] Step 2, adjusting the enrichment liquid: adding ammonia water to the mixed rare earth chloride solution, adjusting the pH to neutral, adding pure water until the rare earth ion concentration in the solutio...

Embodiment 2

[0031] A kind of saponification method of rare earth organic extractant, concrete steps are as follows:

[0032] Step 1, raw ore dissolution: burn and pulverize the rare earth raw ore to obtain rare earth raw ore powder, mix the rare earth raw ore powder with hydrochloric acid with a mass fraction of 38%, and the molar ratio of rare earth ions and chloride ions when the rare earth raw ore powder is mixed with hydrochloric acid with a mass fraction of 38% The ratio is 1:3.2, heating and stirring in the reaction kettle, and then continue to add hydrochloric acid with a mass fraction of 38% until the solid no longer decreases, and then carry out solid-liquid separation after cooling to normal temperature to obtain a mixed rare earth chloride solution;

[0033] Step 2, adjust the enrichment liquid: add ammonia water to the mixed rare earth chloride solution, adjust the pH to neutral, the molar ratio of the rare earth ion to the ammonium ion in the ammonia water is 1:0.1, add pure w...

Embodiment 3

[0037] A kind of saponification method of rare earth organic extractant, concrete steps are as follows:

[0038] Step 1, raw ore dissolution: burn and pulverize the rare earth raw ore to obtain rare earth raw ore powder, mix the rare earth raw ore powder with hydrochloric acid with a mass fraction of 35%, and the molar ratio of rare earth ions and chloride ions when the rare earth raw ore powder is mixed with hydrochloric acid with a mass fraction of 35% The ratio is 1:4, heated to 55°C in the reactor and stirred for 3 hours, then continued to add hydrochloric acid with a mass fraction of 35% until the solid was no longer reduced, and after cooling to room temperature, the solid-liquid separation was carried out by means of pressure filtration to obtain mixed rare earth Chloride solution;

[0039] Step 2, adjust the enrichment liquid: add ammonia water to the mixed rare earth chloride solution, the molar ratio of the rare earth ion to the ammonium ion in the ammonia water is 1...

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Abstract

The invention discloses a saponifying method for a rare-earth organic extracting agent, relates to the field of rare-earth organic extracting agent saponifying, and aims to solve the problem that operability is absent for saponifying clear limewater. The saponifying method comprises the following steps: step I, dissolving raw ores; step II, regulating enrichment liquor; step III, preparing an extracting agent solution; and step IV, saponifying. Sodium ions which are difficult to remove are introduced into process flow, ammonia water achieves the effect of regulating the pH value, and is not the source of saponification lye, so that ammonia-nitrogen content in wastewater is extremely low, and product purity is high. 92% or more of active calcium hydroxide powder is adopted to replace conventional clear limewater to saponify, the water phase size is reduced by about one half, discharge of ammonia-nitrogen wastewater is reduced, and saponifying cost of the calcium hydroxide powder is lower than that of soda and ammonia base. Calcium chloride in wastewater can be recycled, and environmental pollution is small. Moreover, the saponifying method has an economic value.

Description

technical field [0001] The invention relates to the field of saponification of rare earth organic extractants, in particular to a saponification method of rare earth organic extractants. Background technique [0002] The rare earth raw ore extraction and separation process is to dissolve the mixed rare earth chloride solution obtained after the raw ore is acid-dissolved, use P507 as the extraction agent, kerosene as the dispersant, and extract the rare earth after saponification with ammonia water. After extraction and separation, each rare earth element is gradually separated to obtain a single high-purity rare earth chloride enrichment solution. [0003] In the old production process, ammonia water is used as a saponification raw material, which has the advantages of high saponification efficiency and no introduction of new impurities, but the cost of raw materials is high, and ammonia nitrogen wastewater causes serious environmental pollution. Therefore, the ammonia water...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/38C22B59/00C22B26/20
CPCC22B26/20C22B59/00C22B3/3844Y02P10/20
Inventor 张江华罗棋邵方舟潘慧华钟竞德李恒华
Owner DEQING XINGBANG RARE EARTH NEW MATERIALS
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