Preparation method of molybdenum separation resin

A resin and synthetic resin technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of molybdenum loss, poor fastness of extraction color layer, etc., and achieve the effect of stable structure, good fastness and improved selectivity

Active Publication Date: 2013-10-09
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The extraction chromatographic layer prepared by this meth

Method used

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  • Preparation method of molybdenum separation resin

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Embodiment 1

[0022] (1) Prepare dispersant solution: add 0.8g dispersant (polyvinyl alcohol) into 50mL deionized water under stirring, raise the temperature to 50°C to completely dissolve the dispersant, and obtain a dispersant solution;

[0023] (2) Prepare the organic phase containing α-benzoin oxime: add 1g of α-benzoin oxime to 25mL organic solvent mixture of acetone and chloroform (2:1 volume ratio), stir to dissolve α-benzoin oxime, then add 0.1g Tackifier polystyrene, ultrasonically dispersed for 30-40 minutes to obtain an organic phase containing α-benzoin oxime;

[0024] (3) Preparation of styrene-divinylbenzene prepolymer: Mix 40g of styrene, 10g of divinylbenzene and 2g of initiator (dibenzoyl peroxide), stir evenly, heat up to 65-70°C, and make The reactant undergoes a prepolymerization reaction for 30-40 minutes to obtain a styrene-divinylbenzene prepolymer;

[0025] (4) Synthetic resin: Add 50mL of the styrene-divinylbenzene prepolymer obtained in step (3) into 50mL of the d...

Embodiment 2

[0027] Preparation method is the same as embodiment 1, and difference is:

[0028] In the dispersant solution of step (1), oxidized polyvinyl alcohol is used as the dispersant; in step (2), 25 mL of ethyl acetate and acetone (2:1 by volume) are used as organic solvents to dissolve 1 g of α-benzoin oxime, a tackifier Polystyrene is adopted; in the step (3), dibenzoyl peroxide is used as an initiator, and in the step (4), the styrene-divinylbenzene prepolymer, the dispersant solution and the organic phase containing α-benzoin oxime The volumes are 50 mL, 50 mL and 30 mL respectively, and the reaction temperature of the styrene-divinylbenzene prepolymer and the organic phase containing α-benzoin oxime is 85° C. for 15 hours.

Embodiment 3

[0030] Preparation method is the same as embodiment 1, and difference is:

[0031] In the dispersant solution of step (1), polymaleic acid is used as a dispersant; in the organic phase of step (2), ethanol and acetone are used as organic solvents to dissolve α-benzoin oxime, and the tackifier is polyethylene glycol distearic acid Esters; in step (3), potassium persulfate is used as the initiator, and the volumes of the styrene-divinylbenzene prepolymer, the dispersant solution and the organic phase containing α-benzoin oxime in the step (4) are 50mL and 50mL respectively , 30 mL, and the reaction temperature of the styrene-divinylbenzene prepolymer and the extract phase containing α-benzoin oxime is 85° C., and the reaction time is 15 hours.

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Abstract

The invention relates to a preparation method of molybdenum separation resin. The preparation method comprises the following steps of: (1) preparing a dispersing agent solution; (2) preparing an alpha-benzoinoxime contained organic phase; (3) preparing a styrene-divinylbenzene prepolymer; and (4) synthesizing the resin: adding the styrene-divinylbenzene prepolymer into the dispersing agent solution, stirring the mixture so that the styrene-divinylbenzene prepolymer is dispersed into bead bodiese, and slowly heating to 65-70 DEG C; adding the alpha-benzoinoxime contained organic phase, continuing to heat to 80-85 DEG C, reacting for 10-15h, stopping heating and naturally cooling the alpha-benzoinoxime contained organic phase; and when the temperature is reduced to 40-50 DEG C, filtering a reaction mixture, cleaning a sediment and naturally airing the sediment. The molybdenum separation resin obtained by using the method provided by the invention is stable in structure, firmness of an extraction color layer is good when the molybdenum separation resin is used for molybdenum extraction, and the selectivity of the alpha-benzoinoxime to molybdenum is greatly improved; and experiments and tests prove that the molybdenum separation resin provided by the invention has the saturation adsorption capacity as follows: 36-43mg of molybdenum is contained in each gram of dry resin.

Description

technical field [0001] The invention belongs to the technical field of molybdenum extraction, and in particular relates to a preparation method of molybdenum separation resin. Background technique [0002] α-benzoin oxime is a reagent with special chemoselectivity to molybdenum. There are two traditional methods of use: one is to dissolve α-benzoin oxime in ethanol, and mix it with the solution containing molybdenum to form a precipitate of molybdenum; One method is to dissolve α-benzoin oxime in chloroform or ethyl acetate, and fully shake with the solution containing trace molybdenum to realize the extraction of trace molybdenum. In microanalysis, it is hoped that molybdenum can be quickly and selectively separated. Diatomaceous earth or kel-F (chemical name: polychlorotrifluoroethylene) powder is often used as a support. After silanization, α-benzoin The oxime is physically adsorbed on it, dried and packed into a column for use. The extraction chromatographic layer prep...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F212/36C08F8/30B01J20/26C22B34/34
Inventor 丁有钱宿延涛杨金玲梁小虎
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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