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Phospho modified cellulose adsorbent and preparation method thereof, and application of adsorbent in rare-earth recovery

A cellulose and phosphoric acid-based technology, which is applied in the preparation of cellulose adsorbents and the adsorption of low-concentration scandium ions, can solve the problems of hindering industrial applications, poly-ammonia-nitrogen wastewater environment, and high synthesis costs, and achieve good separation and enrichment effects. The effect of high separation and enrichment efficiency and reduced processing cost

Active Publication Date: 2016-06-01
LIAONING UNIVERSITY
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  • Claims
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Problems solved by technology

At present, the commonly used extraction agents in the rare earth industry in my country mainly include neutral TBP, P305, Cyanex923 and acidic extraction agent P507. These extraction agents are widely used in the rare earth industry, but they also have some shortcomings: TBP’s effect on metal ions The extraction distribution ratio is relatively low, and it usually needs to be extracted under the condition of strong acid and salting-out agent; although P305 has a high extraction rate and a large separation factor, but P305 contains a large amount of reducing impurities that are not easy to eliminate, and Its synthesis cost is high, which limits its application to a certain extent; Cyanex923 is difficult to synthesize and its price is high, which hinders the pace of its industrial application; acidic extractant P507 has high acidity in the stripping of heavy rare earth elements, and it is difficult to strip completely , it takes a long time for the extraction to reach equilibrium, and more ammonia nitrogen wastewater is produced after saponification, causing environmental pollution
The concentration of rare earths in the leach solution obtained by the widely used in-situ leaching process is not high, and the concentration limit of rare earths recovered by the ammonium bicarbonate precipitation transformation process is within REO ～ 0.3g / L, which leads to great waste of valuable medium and heavy rare earth resources and environmental pollution

Method used

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  • Phospho modified cellulose adsorbent and preparation method thereof, and application of adsorbent in rare-earth recovery
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  • Phospho modified cellulose adsorbent and preparation method thereof, and application of adsorbent in rare-earth recovery

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1 Preparation of a phosphoric acid-based modified cellulose adsorbent (P-OCS)

[0032] 1) Using straw as raw material, first wash the straw with water to remove impurities such as sludge on the surface, put it in a constant temperature drying box to dry at 50°C, take it out and pulverize it into powder, then add 20g of straw powder to 80mL of concentrated sulfuric acid, and put it in a water bath Heating, controlling the temperature at about 80°C, stirring for 12 hours and filtering, using 0.1mol / L NaHCO 3 Wash, then wash with deionized water until neutral, filter again, put it in a constant temperature drying oven, dry at 60°C for 24 hours, grind and sieve, and finally get a powder with a particle size of 100–150 μm, which is sulfuric acid acidification The straw, denoted as OCS, provides raw materials for the synthesis of adsorbents.

[0033] 2) Weigh 60.5g of 1,3-dibromopropane and 25g of tributyl phosphite, add them into a three-neck round bottom flask, ...

Embodiment 2

[0038] Embodiment 2 Preparation of a phosphate-based cellulose adsorbent (P-OCS)

[0039] 1) Weigh 60.5g of 1,3-dibromopropane and add 25g of tributyl phosphite into a three-necked round bottom flask, stir, react at 140°C for 20h, and steam under reduced pressure at 115°C to obtain a colorless transparent liquid. Intermediate I was obtained.

[0040] 2) Add 35 mL of DMF, add 1 g of sulfuric acid-acidified straw OCS and 0.35 g of NaH under nitrogen protection, stir in an ice-water bath for 1 h, remove the ice-water bath, heat up to 40 ° C for 4 h, add 1 g of intermediate product I, mix and stir at room temperature for 24 h, pump filtered, washed several times with 1mol / L HCl and distilled water, and dried to obtain the intermediate product II.

[0041] 3) In the nitrogen protection system, mix the intermediate product II with 20 mL of ethanol, add 1 mL of 4.9 mol / L KOH solution, stir and reflux at 75 ° C for 24 h, filter with suction, wash with 1 mol / L HCl and distilled water ...

Embodiment 3

[0043] Example 3 The separation effect of a phosphoric acid-based modified cellulose adsorbent (P-OCS) on scandium in mixed rare earth metal ion solutions at different acidities

[0044] Take 100mL of solutions containing 20ppm Sc, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y ions respectively, adjust the acidity of the solutions, and then add 100mg of phosphoric acid-based modified cellulose adsorbent, oscillating and adsorbing for 24 hours, and measuring the concentration of each ion in the solution, such as figure 2 As shown, it can be seen from the figure that as the pH value increases, the adsorption rate of P-OCS to scandium gradually increases. When pH=5.25-5.75, the adsorption rate of P-OCS to scandium can reach nearly 100%. However, it basically does not adsorb other rare earth metal ions except scandium, and the adsorption rates are all less than 20%.

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Abstract

The invention relates to a phospho modified cellulose adsorbent, and a preparation method and application thereof. The technical scheme is as follows: the preparation method comprises the following steps: taking 1,3-dibromopropane and tributyl phosphite, carrying out reaction at 138-142 DEG C for 18-22 hours, and carrying out rotary evaporation at 115 DEG C under reduced pressure to obtain an intermediate product I; taking DMF (N,N-dimethylformamide), adding OCS and NaH in a nitrogen protective atmosphere, stirring in an ice water bath for 1 hour, removing the ice water bath, heating to 40-45 DEG C, reacting for 4 hours or so, adding the intermediate product I, mixing and stirring to react at room temperature for 24 hours, carrying out vacuum filtration, washing respectively with HCl and distilled water, and drying to obtain an intermediate product II; and in a nitrogen protective system, mixing the intermediate product II with ethanol, adding a KOH solution, stirring under reflux at 75 DEG C for 24-50 hours, carrying out vacuum filtration, washing respectively with HCl and distilled water to a neutral state, and drying. The adsorbent provided by the invention has high separation and enrichment efficiency, and can be used for selectively adsorbing scandium from a mixed rare earth ion solution.

Description

technical field [0001] The invention belongs to the technical field of preparation of green adsorbent and extraction of rare earth metals, and in particular relates to the preparation of a phosphoric acid-modified cellulose adsorbent and its adsorption to low-concentration scandium ions. Background technique [0002] my country is rich in rare earth resources. In recent years, the consumption and consumption of rare earths in new technologies and new material industries in my country have increased rapidly. In order to obtain high-quality pure rare earths, extraction and separation are one of the commonly used methods. At present, the commonly used extraction agents in the rare earth industry in my country mainly include neutral TBP, P305, Cyanex923 and acidic extraction agent P507. These extraction agents are widely used in the rare earth industry, but they also have some shortcomings: TBP’s effect on metal ions The extraction distribution ratio is relatively low, and it usu...

Claims

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Application Information

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IPC IPC(8): C08B11/10B01J20/24C22B3/24C22B59/00
CPCB01J20/24C08B11/10C22B3/24C22B59/00Y02P10/20
Inventor 熊英宣靖廖伍平李艳玲张志峰
Owner LIAONING UNIVERSITY
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