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A thermosensitive hydrogel adsorbent and its preparation method and application

A temperature-sensitive hydrogel and adsorbent technology, which can be used in chemical instruments and methods, other chemical processes, and the improvement of process efficiency. The effect of cyclic adsorption performance, high adsorption rate, and small amount of eluent

Active Publication Date: 2020-11-03
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, traditional hydrogel adsorbents are designed to only adsorb rare earth metal ions, and there is not much research on the subsequent enrichment and recovery.

Method used

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  • A thermosensitive hydrogel adsorbent and its preparation method and application
  • A thermosensitive hydrogel adsorbent and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Get 0.6433g NIPAM, 0.066g MA, 0.028g crosslinking agent MBAM, 0.070g initiator APS and join in the sample bottle, add 9.35mL deionized water to dissolve, then add 0.65mL 1g / L GO solution and stir, pass After entering argon for 20 minutes, 50 μL TEMED was added, and after standing at 25°C for 3 minutes, it was transferred to a -25°C refrigerator and sealed for reaction for 24 hours. After the reaction was completed, the hydrogel was thawed at room temperature, cut into pieces, soaked, and vacuum-dried to obtain the adsorbent. The SEM photo is as follows: figure 1 As shown, the hydrogel adsorbent has an obvious hierarchical network structure inside, which is interconnected by large pores with a pore size of 10-100 μm and small pores of 1-50 μm.

[0050] The rare earth metal salt LaCl 3 Prepare an aqueous solution with a concentration of 360 mg / L and pH=5.0 for later use.

[0051] Mix 0.055g of the above-mentioned prepared hydrogel adsorbent with 20mL of the above-mentio...

Embodiment 2

[0059] Get 0.6433g NIPAM, 0.066g MA, 0.028g crosslinking agent MBAM, 0.070g initiator APS and join in the sample bottle, add 9.35mL deionized water to dissolve, then add 0.65mL 1g / L GO solution and stir, pass After entering argon for 20 minutes, add 50 μL TEMED, react at 25°C for 24 hours, cut the hydrogel into pieces, soak, and vacuum-dry to obtain the adsorbent. The SEM photo is as follows: figure 2 As shown, the pore size of the hydrogel is mainly continuously distributed between 0.05 and 100 μm.

[0060] The rare earth metal salt LaCl 3 Prepare an aqueous solution with a concentration of 360 mg / L and pH=5.0 for later use.

[0061] Mix 0.055g of the prepared hydrogel adsorbent with 20mL of the above solution, place it at room temperature at 25°C for 12h, and then use ICP-MS to measure the content of lanthanum ions in the aqueous solution before and after adsorption. After measurement and calculation, its equilibrium adsorption capacity is 20.29±0.395mg / g.

[0062] Take ...

Embodiment 3

[0064] Get 0.6433g NIPAM, 0.033g MA, 0.028g crosslinking agent MBAM, 0.070g initiator APS and join in the sample bottle, add 9.35mL deionized water to dissolve, then add 0.65mL 1g / L GO solution and stir, pass After entering argon for 20 minutes, add 50 μL TEMED, react at 25° C. for 3 minutes, transfer to a refrigerator at -25° C., seal and react for 24 hours. After the reaction is completed, the freeze-polymerized hydrogel is cut into pieces, soaked, and vacuum-dried to obtain the adsorbent.

[0065] The rare earth metal salt LaCl 3 Prepare an aqueous solution with a concentration of 360 mg / L and pH=5.0 for later use.

[0066] Mix 0.055g of the prepared hydrogel adsorbent with 20mL of the above solution, place it at room temperature at 25°C for 12h, and then use ICP-MS to measure the content of lanthanum ions in the aqueous solution before and after adsorption. After measurement and calculation, its equilibrium adsorption capacity is 19.53±0.403mg / g.

[0067] Take out the h...

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Abstract

The invention discloses a thermosensitive hydrogel adsorbent and a preparation method thereof. The preparation method of the thermosensitive hydrogel adsorbent comprises dissolving thermosensitive monomers, carboxyl-containing monomers, graphene, crosslinking agent and initiator into water, inletting inert gas to remove dissolved oxygen, adding in initiator accelerant, and performing sealed reaction at -25-60 DEG C to obtain hydrogel; unfreezing, slicing, soaking and vacuum-drying the obtained hydrogel to obtain the thermosensitive hydrogel adsorbent. The thermosensitive hydrogel adsorbent prepared through the method above can efficiently separate and recover rare earth metal ions in aqueous solution. The invention also discloses a method for selectively adsorbing, separating and recovering rare earth metal ions. The method comprises mixing the thermosensitive hydrogel adsorbent with solution containing the rare earth metal ions for selective adsorption and separation; contracting anddehydrating the post-adsorption thermosensitive hydrogel adsorbent at 40-70 DEG C; eluting the contracted thermosensitive hydrogel adsorbent to recover the rare earth metal ions.

Description

technical field [0001] The invention relates to the technical field of enrichment and recovery of rare earth metals, in particular to a temperature-sensitive hydrogel adsorbent and its preparation method and application. Background technique [0002] Rare Earth Elements (REEs) refers to the general term for 15 lanthanide elements in Group IIIB of the periodic table and 17 elements including scandium and yttrium. Because of its unique performance in catalysis, optics and magnetism, it is considered as magnetic material (driver), hydrogen storage alloy secondary material (power battery), exhaust gas purifier (gasoline, diesel additive), petrochemical purifier (oil production) , Luminescent materials (LED TV, display), polishing powder (energy-saving lamps, chips) and many other ideal materials. However, unlike ordinary metals or precious metals, rare earth elements are often dispersed as rare earth minerals all over the world, and now there are few mineable deposits rich in r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30C22B3/24C22B59/00C08F220/54C08F222/02C08F222/38C08F220/06
CPCB01J20/262B01J20/28047C08F220/54C08F222/385C22B3/24C22B59/00C08F222/02C08F220/06Y02P10/20
Inventor 单国荣杨新蔚
Owner ZHEJIANG UNIV
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