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Self recycling method of waste water in rare earth carbonate precipitation

A rare earth carbonate self-recycling technology, applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as unacceptable by enterprises, environmental pollution, and large equipment needs, so as to improve the effective utilization rate and improve the rare earth Yield, the effect of reducing waste of resources

Inactive Publication Date: 2011-02-09
BAOTOU JINGRUI NEW MATERIAL
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

[0003] Ammonium bicarbonate has low price and large output. It has been widely used in the rare earth industry since the 1990s. The concentration of ammonium chloride in the rare earth carbonate precipitation mother liquor is relatively high. It can be concentrated and crystallized by multi-effect falling film or heat transfer oil heating equipment. Recovering ammonium chloride, rare earth carbonate entrains or adsorbs certain chloride ions and ammonium ions in the precipitation process. In order to prepare pure rare earth carbonate, a large amount of new water is required for multiple cross-flow washing to wash off these ions, and the washing of rare earth carbonate The ammonium chloride concentration in the filtrate decreases with the increase of the number of washes. After the first washing, the ammonium chloride concentration in the filtrate is lower than that of the mother liquor. After the second washing, the ammonium chloride concentration in the filtrate is lower than that of the first filtrate. After multiple washings, the ammonium chloride content in the filtrate is very low. These filtrates cannot be directly recovered by simple concentration and crystallization processes like the mother liquor, and cannot be discharged directly. This problem has always plagued the development of enterprises, (patent: CN101088935A And CN1331055A) high-concentration ammonium salt waste water is reclaimed ammonium chloride with concentration method, and low-concentration ammonium salt waste water adopts air stripping method to prepare ammoniacal liquor, but low-concentration ammonium salt waste water produces a large amount, and air stripping method needs equipment big, and the energy consumption is big, High cost, unacceptable for enterprises
Sodium carbonate is used as a precipitant to prepare rare earth carbonate. Although the wastewater does not contain ammonia nitrogen, it contains sodium chloride. If it is discharged, it will also pollute the environment.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0017] Feed liquid: the mixed rare earth chloride is extracted and separated by two stages of neodymium samarium and cerium praseodymium, and the residual liquid of the cerium praseodymium extraction and separation section is a praseodymium neodymium chloride solution, which is used as a praseodymium neodymium carbonate precipitation liquid, and its composition includes PR 6 o 11 Content is 25%, Nd 2 o 3 The content is 75%, the rare earth concentration is 1.27mol / L, pH=2, and the precipitation of praseodymium and neodymium carbonate is 5700 tons per year.

[0018] Precipitating agent: ammonium bicarbonate solution.

[0019] The concentration of praseodymium neodymium chloride solution before the precipitation of praseodymium carbonate is 1.27mol / L, and the solution volume is 40M 3 / day, use 50M 3 4 settling tanks, each settling 2 times a day, a total of 8 settling; in one 50M 3 Add praseodymium and neodymium chloride solution 5M in the precipitation tank 3 , join 21.5M...

Embodiment 2

[0021] Raw material: The rare earth chloride solution is extracted and separated by two stages of gadolinium, terbium and europium and gadolinium, and the back-extracted raffinate in the europium and gadolinium extraction and separation stage is a gadolinium chloride solution, which is used as a gadolinium carbonate precipitation feed solution. The rare earth concentration is 1.23mol / L, and the pH= 2. The precipitation of gadolinium carbonate is 300 tons / year.

[0022] Precipitating agent: sodium carbonate solution.

[0023] The concentration of feed solution before gadolinium carbonate precipitation is 1.23mol / L, and the volume of feed solution is 2M 3 / day, use 12M 3 1 settling tank, settling once a day; add gadolinium chloride solution 2M to the settling tank 3 , adding 3.6M 3 Gadolinium carbonate precipitation wastewater dilutes the concentration of gadolinium chloride solution to 0.44mol / L, and the volume of gadolinium chloride solution is 5.6M 3 , heat the gadoliniu...

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Abstract

The invention relates to a self recycling method of waste water in rare earth carbonate precipitation, which belongs to the field of rare earth hydrometallurgy. The method comprises the following steps: part of mother liquor, which is generated in the rare earth carbonate precipitation production process, is directly transmitted into a rare earth carbonate recycling pool to be clarified, and concentrating and crystallization equipment is used for recyling ammonium chloride or sodium chloride; the rest of the mother liquor is transmitted into a mother liquor storage tank, and is used for adjusting the concentration of carbonate precipitation liquor and dissolving the precipitant; the rare earth carbonate precipitate is washed in a reverse flow mode to obtain a first filtrate; the first filtrate and the mother liquor are recycled to the rare earth carbonate precipitation technique to dissolve the precipitant and dilute the liquor; and the residual waste water after recycling is concentrated and crystallized to recycle ammonium chloride or sodium chloride. The precipitation waste water is recycled, thereby reducing waste water discharge amount and the consumption of new water, increasing the concentration of ammonium chloride or sodium chloride in waste water and lowering the energy consumption for concentration and crystallization.

Description

technical field [0001] The invention relates to a method for self-recycling of rare earth carbonate precipitation wastewater, which belongs to the field of rare earth hydrometallurgy. Background technique [0002] In industrial production, ammonium bicarbonate and sodium carbonate are mainly used as precipitants for rare earth carbonate, and the pH value of the mother liquor after precipitation is both 7; Contains ammonium chloride, the mother liquor and filtrate are concentrated and crystallized to recover ammonium chloride, ammonium chloride is mainly used to prepare agricultural fertilizers; sodium carbonate solution is used as the precipitant, the mother liquor after precipitation and the filtrate of washing rare earth carbonate contain sodium chloride, The mother liquor and filtrate are concentrated and crystallized to recover sodium chloride, and sodium chloride is prepared by electrolysis to prepare sodium hydroxide and hydrochloric acid. [0003] Ammonium bicarbonat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C22B59/00C22B3/26
CPCY02P10/20
Inventor 郝先库张瑞祥刘海旺王士智斯琴毕力格许宗泽马显东吴英陈敏璇胡珊珊
Owner BAOTOU JINGRUI NEW MATERIAL
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