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Magnesium-containing rare earth oxygen storage material and preparation method thereof

An oxygen storage material and rare earth technology, which is applied in separation methods, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problems of cost increase, high-concentration sodium salt wastewater pollution, etc., to avoid production and discharge, and eliminate environmental impacts Contamination, high stability effect

Inactive 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

At present, the preparation technology of ammonia nitrogen system has been subject to huge application restrictions. Some factories (such as rare earth separation plants, etc.) have canceled the preparation technology of ammonia nitrogen precipitation system, and use sodium carbonate or sodium hydroxide instead of ammonia water and ammonium bicarbonate as precipitants to produce metal carbonates. , hydroxide or metal oxide, but the cost is doubled, and it brings high-concentration sodium salt wastewater pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 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).

[0035] Press Ce 0.5 Zr 0.5 o 2 The chemical formula is compounded to get 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 re...

Embodiment 2

[0038] 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).

[0039] Press Ce 0.45 La 0.1 Zr 0.45 o 2 The chemical formula is compounded 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 magnesium bicarbonate aqueous solution 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, the pH va...

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] Press Ce 0.4 La 0.1 Nd 0.1 Zr 0.4 o 2 For batching, get 1.0M 3 Cerium nitrate, zirconium nitrate, lanthanum nitrate, neodymium nitrate mixed solution (2.0mol / L), then added to the 21.6...

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Abstract

The invention relates to a magnesium-containing rare earth oxygen storage material and a preparation method thereof. The expression of the magnesium-containing rare earth oxygen storage material is RExZryMzO2, wherein M represents Mg or other metal which comprises cerium zirconium composite oxide, praseodymium zirconium composite oxide, terbium zirconium composite oxide, and the like. The content of magnesium oxide is 0.001 wt% -5 wt%. The magnesium-containing rare earth oxygen storage material is prepared by using magnesium bicarbonate as a precipitant. The preparation method comprises the following steps: mixing rare earth (cerium, praseodymium or terbium) and zirconium, or mixing rare earth (cerium, praseodymium or terbium), zirconium and at least one of other rare earth ions (lanthanum, praseodymium, neodymium, samarium, gadolinium, yttrium) and / or other metal ions (aluminium, barium, strontium, titanium, manganese, iron, copper, hafnium); performing precipitation by using a magnesium bicarbonate or / and calcium bicarbonate aqueous solution as a precipitant, wherein the magnesium bicarbonate or / and calcium bicarbonate aqueous solution is prepared by at least one procedure of roasting, digestion, slurry mixing, and carbonization of raw materials of minerals or oxides or hydroxides of magnesium or / and calcium, then performing at least one procedure of filtration, washing, drying, and the like, and finally roasting at a certain temperature to obtain the product. The preparation method of the invention adopts a cheap routine chemical precipitant, realizes the effective recycling of magnesium, calcium, carbon dioxide and the like, and greatly reduces the production cost of the rare earth oxygen storage material. On the other hand, the production process in the invention does not generate ammonia nitrogen waste water, or waste water with high salinity, and reduces the discharge of carbon dioxide greenhouse gas; the preparation process is green and environment-friendly, and eliminates environment pollution.

Description

technical field [0001] The invention relates to a magnesium-containing rare earth oxygen storage material and a preparation method thereof. Specifically, the rare earth oxygen storage material contains a certain amount of magnesium oxide. The rare earth oxygen storage material uses calcium or / and magnesium minerals or oxides and hydroxides as raw materials, and magnesium bicarbonate and / or calcium aqueous solutions prepared by at least one step of roasting, digestion, pulping and carbonization are used as precipitating agents , while preparing. The magnesium-containing rare earth oxygen storage material in the present invention includes but is not limited to cerium-zirconium composite oxides, and may also be praseodymium-zirconium composite oxides and terbium-zirconium composite oxides. The magnesium-containing rare-earth oxygen storage material is an excellent catalyst carrier or additive material, and can be applied to catalytic purification of motor vehicle tail gas, indu...

Claims

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Application Information

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IPC IPC(8): B01J23/10B01J37/03B01D53/94
Inventor 黄小卫崔梅生冯宗玉于瀛侯永可赵娜龙志奇李红卫
Owner GRIREM ADVANCED MATERIALS CO LTD
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