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Preparation method for zirconium-contained rare-earth composite oxide

A rare earth composite and oxide technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, chemical/physical processes, etc., can solve problems such as cost increase, high-concentration sodium salt wastewater pollution, etc. achieve good performance

Active Publication Date: 2012-04-18
GRIREM ADVANCED MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For this reason, many factories (such as rare earth separation plants, etc.) cancel the ammonia nitrogen precipitation system preparation technology, and use sodium carbonate or sodium hydroxide instead of ammonia water and ammonium bicarbonate as precipitants to produce metal carbonates, hydroxides or metal oxides, but the cost The increase is about 1 times, and it also brings high-concentration sodium salt wastewater pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Dolomite (Si content 2.5wt%, Fe content 0.9wt%, Al content 0.5wt%) was calcined at 1000°C for 3 hours to obtain lightly burned dolomite, the weight-liquid-solid ratio of water and magnesium oxide / calcium was 3:1 Add water and digest at 80°C for 2 hours, then adjust the slurry with water at a liquid-solid ratio of 40:1 based on the weight of water and magnesium oxide / calcium, then pass in carbon dioxide gas (90vt%), react at 20°C for 30 minutes, and clarify Filtration gave a magnesium bicarbonate / calcium aqueous solution (MgO: 6.8 g / L, CaO: 1.3 g / L, Fe: 4.1 ppm, Al: 1.0 ppm).

[0034] Dosing according to the Ce / Zr molar ratio of 1:1 to obtain 3M 3 A mixed solution of cerium nitrate and zirconium nitrate (0.50mol / L) was added to the reactor. Then 9.9M 3 The above-mentioned aqueous solution of magnesium bicarbonate is added into a reactor for precipitation reaction, the amount of alkali used is 90% of the theoretical amount, the reaction time is 2 hours, the reaction tem...

Embodiment 2

[0037] The light-burned magnesia obtained by roasting magnesite at 900°C for 2 hours (Si content 3.2wt%, Fe content 0.7wt%, Al content 0.37wt%), the liquid-solid ratio calculated by water and magnesia weight is 2:1 Add water to digest at 80°C for 2 hours, calculate the liquid-solid ratio based on the weight of water and magnesium oxide to be 57:1, add water to adjust the slurry, feed carbon dioxide gas (80vt%), react at 25°C for 2 hours, and filter to obtain pure Aqueous solution of magnesium bicarbonate (MgO: 15.3 g / L, Fe: 12.8 ppm, Al: 1.7 ppm).

[0038] Dosing according to the Ce / Zr / La molar ratio of 1:1:0.1 to obtain 1.6M 3 Cerium nitrate, zirconium nitrate, lanthanum nitrate mixed solution (1.0mol / L), and join in the reactor, then use 4.2M 3 The above-mentioned aqueous solution of magnesium bicarbonate is subjected to precipitation reaction, the amount of alkali is 80% of the theoretical amount, the reaction time is 2 hours, the reaction temperature is 50°C, and the pH v...

Embodiment 3

[0041] The magnesium oxide and calcium oxide mixture obtained by roasting dolomite (Si content 2.5wt%, Fe content 0.9wt%, Al content 0.5wt%) at 1000 °C for 2 hours, added water and digested at 80 °C for 1 hour, according to water and oxidation The liquid-solid ratio calculated by magnesium / calcium weight is 5: 1; add an appropriate amount of magnesium chloride solution for alkali conversion, then filter and wash to obtain magnesium hydroxide filter cake; add water to adjust the slurry, and calculate the liquid-solid ratio according to the weight of water and magnesium oxide to be 190: 1, then pass into carbon dioxide gas (70vt%), react at 25 ℃ for 2 hours, through clarification and filtration, obtain pure magnesium bicarbonate aqueous solution (MgO: 4.7g / L, Fe: 1.1ppm, Al: 0.7ppm).

[0042] According to the molar ratio of Ce / Zr / La / Nd is 1:1:0.1:0.1, to obtain 1.0M 3 Cerium nitrate, zirconium nitrate, lanthanum nitrate, neodymium nitrate mixed solution (2.0mol / L), then added to...

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Abstract

The invention relates to a preparation method for a zirconium-contained rare-earth composite oxide. At a certain ratio, rare earth (cerium, yttrium, praseodymium or terbium) is mixed with zirconium to burden, or rare earth (cerium, yttrium, praseodymium or terbium) and zirconium are mixed with at least one of other metal ions (aluminum, barium, magnesium, strontium, titanium, manganese, ferrum, copper and hafnium) to burden. A magnesium bicarbonate or / and calcium bicarbonate aqueous solution prepared from raw materials of magnesium or / and calcium minerals or oxides and hydroxides by at least one working procedure of roasting, digesting, mixing size, carbonizing and the like can serve as a precipitator to carry out precipitation so as to obtain at least one of rare earth and zirconium composite carbonate and subcarbonate, and the at least one of rare earth and zirconium composite carbonate and subcarbonate is further roasted to obtain a zirconium-contained rare-earth composite oxide product. In the preparation method, cheap calcium or / and magnesium minerals or low-purity oxides and hydroxides can serve as initial raw materials to replace common chemical industry precipitators, such as ammonia water, ammonium bicarbonate, sodium carbonate, sodium hydroxide and the like, substances, such as magnesium, calcium, carbon dioxide and the like can be effectively circulated and utilized so as to greatly lower the production cost of the zirconium-contained rare-earth composite oxide, such as ceria-zirconia, yttrium zirconium, praseodymium zirconium, terbium zirconium and the like. In addition, in the production technology disclosed by the invention, no ammonia nitrogen wastewater, high-salinity wastewater and the like are generated, carbon dioxide greenhouse gas emission amount is reduced, the preparation technology is environmentally-friendly, and environment pollution is avoided.

Description

technical field [0001] The invention relates to a preparation method of a zirconium-containing rare earth composite oxide. Specifically, the magnesium bicarbonate and / or calcium bicarbonate aqueous solution prepared by at least one step of roasting, digestion, pulping and carbonization from magnesium or / and calcium minerals or oxides and hydroxides is used as a precipitating agent Precipitating rare earth, zirconium ions in the solution or rare earth, zirconium and other metal ions in the solution to obtain at least one of rare earth and zirconium composite carbonate and basic carbonate, and further roasting to obtain zirconium-containing Rare earth composite oxide products. The zirconium-containing rare earth composite oxides in the present invention include but are not limited to cerium-zirconium composite oxides, yttrium-zirconium composite oxides, praseodymium-zirconium, terbium-zirconium composite oxides, and the like. The obtained cerium-zirconium composite oxide is an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/48C04B35/50B01J23/10B01J23/83B01J23/34B01J32/00
Inventor 崔梅生黄小卫侯永可冯宗玉于瀛赵娜龙志奇李红卫
Owner GRIREM ADVANCED MATERIALS CO LTD
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