CN102898569A - Preparation method of ion exchange resin - Google Patents
Preparation method of ion exchange resin Download PDFInfo
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- CN102898569A CN102898569A CN2012104082270A CN201210408227A CN102898569A CN 102898569 A CN102898569 A CN 102898569A CN 2012104082270 A CN2012104082270 A CN 2012104082270A CN 201210408227 A CN201210408227 A CN 201210408227A CN 102898569 A CN102898569 A CN 102898569A
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Abstract
The invention provides a preparation method of an ion exchange resin, which comprises the following steps: (1) mixing a dispersant solution and an organic phase, and gradually heating to carry out polymerization reaction; (2) adding chloromethyl ether into the obtained white ball, and adding a catalyst zinc chloride to carry out chloromethylation reaction; and (3) adding methanol into the obtained chlorine ball, dropwisely adding a trimethylamine water solution, adding a 10% sodium chloride solution, adding hydrochloric acid for neutralization, and washing with water to obtain the resin. The ion exchange resin provided by the invention has the advantages of favorable selectivity, high uranium adsorption capacity and high exchange speed.
Description
Technical field
The present invention relates to Uranium Mining smelting tech field, be specifically related to a kind of preparation method of ion exchange resin.
Background technology
Along with the development of uranium mining technology, Situ Leaching technique is not owing to needing ore extraction is out carried out molten soaking, production process is simple, less investment, found the factory fast, production cost is low, therefore as the main development direction.Because it is low that ground soaks the leach liquor uranium content, carry out enrichment with extraction process and be difficult for realizing, can only adsorb by spent ion exchange resin.Available have resin and anionite-exchange resin.The resin immunity from interference is strong, and its weak point is the drip washing difficulty, and itself is expensive, can only use under given conditions.The uranium ore leach liquor is when adopting ion exchange process to extract uranium, and ion exchange resin is had higher requirement: selectivity is good, and the uranium loading capacity is high, and exchange velocity is fast.
From present case, being used for the higher anionite-exchange resin of ground soaking technology uranium loading capacity has Pyridine Resin, all pass resin (such as Dowex21K, U.S. Dow company commercial resin).The Pyridine Resin that Ukraine produces is because the characteristic (chemical instability under alkaline condition) of its pyridine ring can only be used for acid system and carry uranium; And Dowex21K is to acid system, and alkaline process is all applicable.So-called high adsorption uranium capacity, reason are that resin adsorbs the highly selective of uranium in the use system, and highly selective is that the physical structure of resin uniqueness determines.Obtain selectivity good, loading capacity is high, and exchange velocity is fast is used for the ion exchange resin that uranium ore ground soaks, and the physical structure of studying resin is one of the most effective approach.
Summary of the invention
The object of the present invention is to provide a kind of selectivity for uranium ore ground soaking technology good, the uranium loading capacity is high, the preparation method of the basic anion resin that exchange velocity is fast.
Realize the technical scheme of the object of the invention: a kind of preparation method of ion exchange resin, it comprises the steps:
(1) suspension polymerization
Preparation dispersant solution: gelatin is added to the water, stirs and obtain gelatin solution, wherein the add-on 5g/L of gelatin ~ 10g/L; Then adding mass percent concentration in every liter of gelatin solution is 0.1% ~ 0.2% methylene blue aqueous solution 10ml ~ 20ml again;
The preparation organic phase: divinylbenzene, vinylbenzene are mixed, and wherein the mass percent of divinylbenzene is 15% ~ 30%, and cinnamic mass percent is 70% ~ 85%; Then in divinylbenzene and cinnamic mixture, add dibenzoyl peroxide and pore-creating agent, the adding quality of dibenzoyl peroxide is 0.5% ~ 1% of divinylbenzene and styrene mixture total mass, and the adding quality of pore-creating agent is 30% ~ 110% of divinylbenzene and styrene mixture total mass;
Described pore-creating agent comprises A component and B component, and the A component is whiteruss or white oil, and the B component is toluene or dimethylbenzene, and wherein the mass ratio of A component and B component is for being 4:(0.5 ~ 2);
Dispersant solution and the organic phase of above-mentioned preparation are mixed at 45 ℃~50 ℃, and wherein the volume ratio of dispersant solution and organic phase is 2 ~ 3:1; And progressively heat up and carry out polyreaction: 0.5h and rise to 60 ℃, insulation 1h; 0.5h rises to 70 ℃ again, insulation 2h; 0.5h rises to 80 ℃ again, insulation 6h; 0.5h rises to 85 ℃ again, insulation 4h; To the products therefrom suction filtration, wash at last, drying, screening obtains Archon pearl body;
(2) chloromethylation
Add chloromethyl ether in step (1) gained Archon pearl body, the quality of chloromethyl ether is 2 ~ 3 times of Archon pearl weight; Leave standstill the 2 ~ 3h that expands, then add the catalyzer zinc chloride, carry out chloromethylation at 40 ~ 42 ℃, reaction times 14 ~ 18h obtains the chlorine ball;
(3) amination reaction
In step (2) gained chlorine ball, add methyl alcohol, start stirring, the 2h that expands under the room temperature, the add-on of methyl alcohol is 0.3 ~ 0.5 times of chlorine ball quality;
Then be cooled to 15 ℃, drip trimethylamine aqueous solution, regulate the pH value greater than 9 with liquid caustic soda, at 18 ~ 25 ℃ of reaction 5 ~ 10h; The concentration of trimethylamine aqueous solution is 30% ~ 50%, and add-on is 2 ~ 4 times of chlorine ball quality;
Suction filtration amination mother liquor adds 10% sodium chloride solution again, starts stirring.
Adding at last hydrochloric acid, to be neutralized to pH be 2 ~ 5, stirs 6h, and holding temperature is not higher than 25 ℃; Being washed to pH is 6 ~ 7, obtains resin.
The preparation method of aforesaid a kind of ion exchange resin, the adding quality of the described pore-creating agent of its step (1) is 40% ~ 70% of divinylbenzene and styrene mixture total mass.
The preparation method of aforesaid a kind of ion exchange resin, the A component of the pore-creating agent described in its step (1) and the mass ratio of B component are for being 4:(0.7 ~ 1).
The degree of crosslinking scope of linking agent divinylbenzene is 5% ~ 15% among the preparation method of aforesaid a kind of ion exchange resin, its step (1).
The degree of crosslinking scope of linking agent divinylbenzene is 7% ~ 10% among the preparation method of aforesaid a kind of ion exchange resin, its step (1).
Beneficial effect of the present invention is: the basic anion resin of the present invention's preparation has following premium properties: (a) dynamic performance of good adsorption uranium can adapt to the ADSORPTION IN A FIXED BED operation of large flow, high flow rate; (b) to HCO
3-Lower adsorption rate has avoided consuming too much HCO when adsorption uranium
3-And to underground leaching generation detrimentally affect; (c) in the leach liquor absorbing process, all present the low higher uranium loading capacity of uranium concentration leach liquor; (d) have preferably drip washing performance, the qualifying liquid bed volume can be controlled at 3 ~ 4 times of bed volumes, and the qualifying liquid uranium concentration is high, and this reduces the reagent consumption of post precipitation operation significantly; (e) in actual motion, the absorption saturated capacity of uranium surpasses the wet R of 100mgU/mL, obviously is better than commercial resin of the same type.
Description of drawings
Fig. 1 is preparation method's schema of a kind of ion exchange resin of the present invention.
Embodiment
Preparation method to a kind of ion exchange resin of the present invention is further described below in conjunction with the drawings and specific embodiments.
Embodiment 1
As shown in Figure 1, the preparation method of a kind of ion exchange resin of the present invention comprises the steps:
(1) suspension polymerization
Preparation dispersant solution: gelatin is added in the 1L water, stir and obtain gelatin solution, wherein the add-on 8g/L of gelatin; Then adding mass percent concentration in every liter of gelatin solution is 0.1% methylene blue aqueous solution 16ml again.
The preparation organic phase: divinylbenzene (DVB), vinylbenzene (ST) are mixed, and wherein the mass percent of divinylbenzene is 25%, and cinnamic mass percent is 75%; Then in divinylbenzene and cinnamic mixture, add dibenzoyl peroxide (BPO) and pore-creating agent, the adding quality of dibenzoyl peroxide is 0.8% of divinylbenzene and styrene mixture total mass, and the adding quality of pore-creating agent is 60% of divinylbenzene and styrene mixture total mass;
Described pore-creating agent comprises A component and B component, and the A component is whiteruss, and the B component is toluene, and wherein the mass ratio of A component and B component is for being 4:1.The degree of crosslinking scope of linking agent divinylbenzene is 8%.
Dispersant solution and the organic phase of above-mentioned preparation are mixed at 45 ℃, and wherein the volume ratio of dispersant solution and organic phase is 3:1; And progressively heat up and carry out polyreaction: 0.5h and rise to 60 ℃, insulation 1h; 0.5h rises to 70 ℃ again, insulation 2h; 0.5h rises to 80 ℃ again, insulation 6h; 0.5h rises to 85 ℃ again, insulation 4h; To the products therefrom suction filtration, wash at last, drying, screening obtains Archon pearl body.
(2) chloromethylation
Add chloromethyl ether in step (1) gained Archon pearl body, the quality of chloromethyl ether is 3 times of Archon pearl weight; Leave standstill expansion 2h, then add the catalyzer zinc chloride, carry out chloromethylation at 40 ℃, reaction times 15h obtains the chlorine ball.
(3) amination reaction
In step (2) gained chlorine ball, add methyl alcohol, start stirring, the 2h that expands under the room temperature, the add-on of methyl alcohol is 0.4 times of chlorine ball quality;
Then be cooled to 15 ℃, drip trimethylamine aqueous solution, guarantee the pH value greater than 9, at 25 ℃ of reaction 6h; The concentration of trimethylamine aqueous solution is 40%, and add-on is 4 times of chlorine ball quality;
Suction filtration amination mother liquor adds 10% sodium chloride solution again, starts stirring.
Adding at last hydrochloric acid, to be neutralized to pH be 2, stirs 6h, and being washed to pH is 6, obtains resin.
The equation of above-mentioned reaction is as follows:
Embodiment 2
As shown in Figure 1, the preparation method of a kind of ion exchange resin of the present invention comprises the steps:
(1) suspension polymerization
Preparation dispersant solution: gelatin is added in the 1L water, stir and obtain gelatin solution, wherein the add-on 5g/L of gelatin; Then adding mass percent concentration in every liter of gelatin solution is 0.1% methylene blue aqueous solution 10ml again.
The preparation organic phase: divinylbenzene (DVB), vinylbenzene (ST) are mixed, and wherein the mass percent of divinylbenzene is 15%, and cinnamic mass percent is 85%; Then in divinylbenzene and cinnamic mixture, add dibenzoyl peroxide (BPO) and pore-creating agent, the adding quality of dibenzoyl peroxide is 0.5% of divinylbenzene and styrene mixture total mass, and the adding quality of pore-creating agent is 40% of divinylbenzene and styrene mixture total mass;
Described pore-creating agent comprises A component and B component, and the A component is whiteruss, and the B component is toluene, and wherein the mass ratio of A component and B component is for being 4:0.7.The degree of crosslinking scope of linking agent divinylbenzene is 7%.
Dispersant solution and the organic phase of above-mentioned preparation are mixed at 45 ℃, and wherein the volume ratio of dispersant solution and organic phase is 2.5:1; And progressively heat up and carry out polyreaction: 0.5h and rise to 60 ℃, insulation 1h; 0.5h rises to 70 ℃ again, insulation 2h; 0.5h rises to 80 ℃ again, insulation 6h; 0.5h rises to 85 ℃ again, insulation 4h; To the products therefrom suction filtration, wash at last, drying, screening obtains Archon pearl body.
(2) chloromethylation
Add chloromethyl ether in step (1) gained Archon pearl body, the quality of chloromethyl ether is 2 times of Archon pearl weight; Leave standstill expansion 3h, then add the catalyzer zinc chloride, carry out chloromethylation at 40 ℃, reaction times 14h obtains the chlorine ball.
(3) amination reaction
In step (2) gained chlorine ball, add methyl alcohol, start stirring, the 2h that expands under the room temperature, the add-on of methyl alcohol is 0.5 times of chlorine ball quality;
Then be cooled to 15 ℃, drip trimethylamine aqueous solution, guarantee the pH value greater than 9, at 20 ℃ of reaction 8h; The concentration of trimethylamine aqueous solution is 35%, and add-on is 3 times of chlorine ball quality;
Suction filtration amination mother liquor adds 10% sodium chloride solution again, starts stirring.
Adding at last hydrochloric acid, to be neutralized to pH be 2, stirs 6h, and being washed to pH is 6, obtains resin.
Embodiment 3
As shown in Figure 1, the preparation method of a kind of ion exchange resin of the present invention comprises the steps:
(1) suspension polymerization
Preparation dispersant solution: gelatin is added in the 1L water, stir and obtain gelatin solution, wherein the add-on 10g/L of gelatin; Then adding mass percent concentration in every liter of gelatin solution is 0.1% methylene blue aqueous solution 20ml again.
The preparation organic phase: divinylbenzene (DVB), vinylbenzene (ST) are mixed, and wherein the mass percent of divinylbenzene is 20%, and cinnamic mass percent is 80%; Then in divinylbenzene and cinnamic mixture, add dibenzoyl peroxide (BPO) and pore-creating agent, the adding quality of dibenzoyl peroxide is 1% of divinylbenzene and styrene mixture total mass, and the adding quality of pore-creating agent is 70% of divinylbenzene and styrene mixture total mass;
Described pore-creating agent comprises A component and B component, and the A component is whiteruss, and the B component is toluene, and wherein the mass ratio of A component and B component is for being 4:2.The degree of crosslinking scope of linking agent divinylbenzene is 10%.
Dispersant solution and the organic phase of above-mentioned preparation are mixed at 50 ℃, and wherein the volume ratio of dispersant solution and organic phase is 2:1; And progressively heat up and carry out polyreaction: 0.5h and rise to 60 ℃, insulation 1h; 0.5h rises to 70 ℃ again, insulation 2h; 0.5h rises to 80 ℃ again, insulation 6h; 0.5h rises to 85 ℃ again, insulation 4h; To the products therefrom suction filtration, wash at last, drying, screening obtains Archon pearl body.
(2) chloromethylation
Add chloromethyl ether in step (1) gained Archon pearl body, the quality of chloromethyl ether is 3 times of Archon pearl weight; Leave standstill expansion 3h, then add the catalyzer zinc chloride, carry out chloromethylation at 42 ℃, reaction times 18h obtains the chlorine ball.
(3) amination reaction
In step (2) gained chlorine ball, add methyl alcohol, start stirring, the 2h that expands under the room temperature, the add-on of methyl alcohol is 0.3 times of chlorine ball quality;
Then be cooled to 15 ℃, drip trimethylamine aqueous solution, guarantee the pH value greater than 9, at 18 ℃ of reaction 10h; The concentration of trimethylamine aqueous solution is 30%, and add-on is 3 times of chlorine ball quality;
Suction filtration amination mother liquor adds 10% sodium chloride solution again, starts stirring.
Adding at last hydrochloric acid, to be neutralized to pH be 2, stirs 6h, and being washed to pH is 6, obtains resin.
Claims (5)
1. the preparation method of an ion exchange resin, it is characterized in that: the method comprises the steps:
(1) suspension polymerization
Preparation dispersant solution: gelatin is added to the water, stirs and obtain gelatin solution, wherein the add-on 5g/L of gelatin ~ 10g/L; Then adding mass percent concentration in every liter of gelatin solution is 0.1% ~ 0.2% methylene blue aqueous solution 10ml ~ 20ml again;
The preparation organic phase: divinylbenzene, vinylbenzene are mixed, and wherein the mass percent of divinylbenzene is 15% ~ 30%, and cinnamic mass percent is 70% ~ 85%; Then in divinylbenzene and cinnamic mixture, add dibenzoyl peroxide and pore-creating agent, the adding quality of dibenzoyl peroxide is 0.5% ~ 1% of divinylbenzene and styrene mixture total mass, and the adding quality of pore-creating agent is 30% ~ 110% of divinylbenzene and styrene mixture total mass;
Described pore-creating agent comprises A component and B component, and the A component is whiteruss or white oil, and the B component is toluene or dimethylbenzene, and wherein the mass ratio of A component and B component is for being 4:(0.5 ~ 2);
Dispersant solution and the organic phase of above-mentioned preparation are mixed at 45 ℃~50 ℃, and wherein the volume ratio of dispersant solution and organic phase is 2 ~ 3:1; And progressively heat up and carry out polyreaction: 0.5h and rise to 60 ℃, insulation 1h; 0.5h rises to 70 ℃ again, insulation 2h; 0.5h rises to 80 ℃ again, insulation 6h; 0.5h rises to 85 ℃ again, insulation 4h; To the products therefrom suction filtration, wash at last, drying, screening obtains Archon pearl body;
(2) chloromethylation
Add chloromethyl ether in step (1) gained Archon pearl body, the quality of chloromethyl ether is 2 ~ 3 times of Archon pearl weight; Leave standstill the 2 ~ 3h that expands, then add the catalyzer zinc chloride, carry out chloromethylation at 40 ~ 42 ℃, reaction times 14 ~ 18h obtains the chlorine ball;
(3) amination reaction
In step (2) gained chlorine ball, add methyl alcohol, start stirring, the 2h that expands under the room temperature, the add-on of methyl alcohol is 0.3 ~ 0.5 times of chlorine ball quality;
Then be cooled to 15 ℃, drip trimethylamine aqueous solution, regulate the pH value greater than 9 with liquid caustic soda, at 18 ~ 25 ℃ of reaction 5 ~ 10h; The concentration of trimethylamine aqueous solution is 30% ~ 50%, and add-on is 2 ~ 4 times of chlorine ball quality;
Suction filtration amination mother liquor adds 10% sodium chloride solution again, starts stirring.
Adding at last hydrochloric acid, to be neutralized to pH be 2 ~ 5, stirs 6h, and holding temperature is not higher than 25 ℃; Being washed to pH is 6 ~ 7, obtains resin.
2. the preparation method of a kind of ion exchange resin according to claim 1, it is characterized in that: the adding quality of the described pore-creating agent of step (1) is 40% ~ 70% of divinylbenzene and styrene mixture total mass.
3. the preparation method of a kind of ion exchange resin according to claim 1, it is characterized in that: the A component of the pore-creating agent described in the step (1) and the mass ratio of B component are for being 4:(0.7 ~ 1).
4. the preparation method of a kind of ion exchange resin according to claim 1 is characterized in that: the degree of crosslinking scope of linking agent divinylbenzene is 5% ~ 15% in the step (1).
5. the preparation method of a kind of ion exchange resin according to claim 4 is characterized in that: the degree of crosslinking scope of linking agent divinylbenzene is 7% ~ 10% in the step (1).
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