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Preparation method of iron ion croscarmellose in-situ growing Prussian-blue microsphere adsorbing material

A technology of carboxymethyl cellulose and cross-linked carboxymethyl, which is applied in the field of preparation of iron ion cross-linked carboxymethyl cellulose in-situ grown Prussian blue microsphere adsorption material, achieving simple preparation process, low energy consumption, and easy synthesis The effect of simple process

Inactive Publication Date: 2016-10-26
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After searching, there is no report on the extraction of rare element cesium from salt lake brine by synthesizing Prussian blue gel microspheres by cross-linking carboxymethyl cellulose with iron ions through in situ growth method

Method used

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  • Preparation method of iron ion croscarmellose in-situ growing Prussian-blue microsphere adsorbing material
  • Preparation method of iron ion croscarmellose in-situ growing Prussian-blue microsphere adsorbing material
  • Preparation method of iron ion croscarmellose in-situ growing Prussian-blue microsphere adsorbing material

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Embodiment 1

[0040] A preparation method for iron ion cross-linked carboxymethyl cellulose in-situ growth Prussian blue microsphere adsorption material, comprising the following steps:

[0041] Step 1, dissolving carboxymethyl cellulose in ultrapure water, stirring for 6 hours to obtain a sol with a concentration of 3 wt%, and ultrasonically degassing the sol for 10 minutes; the ultrasonic power of the ultrasonic degassing is 150W, and the ultrasonic frequency is 20KHz; The viscosity of the carboxymethyl cellulose is 1400mpa.s;

[0042] Step 2, use the electrospray device to electrospray the ultrasonically degassed sol into the receiving device with a concentration of 6wt% iron ion solution, and stir the iron ion solution during the electrospraying process; Add 2 mL of glutaraldehyde dropwise, stir for 12 h at a speed of 350 r / min, and filter to obtain iron ion-loaded gel microspheres;

[0043] Step 3. Place 7 g of the gel microspheres prepared in step 2 in a circulating water type vacuum...

Embodiment 2

[0045] A preparation method for iron ion cross-linked carboxymethyl cellulose in-situ growth Prussian blue microsphere adsorption material, comprising the following steps:

[0046] Step 1, dissolving carboxymethyl cellulose in ultrapure water, stirring for 5 hours to obtain a sol with a concentration of 3 wt%, and ultrasonically degassing the sol for 12 minutes; the ultrasonic power of the ultrasonic degassing is 1000W, and the ultrasonic frequency is 24KHz; The viscosity of the carboxymethyl cellulose is 1000mpa.s;

[0047] Step 2, use the electrospray device to electrospray the ultrasonically degassed sol into the receiving device with a concentration of 7wt% iron ion solution, and stir the iron ion solution during the electrospraying process; Add 0.2 mL of glutaraldehyde dropwise, stir for 13 h at a speed of 250 r / min, and filter to obtain iron ion-loaded gel microspheres;

[0048] Step 3: Place 8 g of the gel microspheres prepared in step 2 in a circulating water vacuum f...

Embodiment 3

[0050] A preparation method for iron ion cross-linked carboxymethyl cellulose in-situ growth Prussian blue microsphere adsorption material, comprising the following steps:

[0051] Step 1, dissolving carboxymethyl cellulose in ultrapure water, stirring for 6 hours to obtain a sol with a concentration of 5 wt%, and ultrasonically degassing the sol for 14 minutes; the ultrasonic power of the ultrasonic degassing is 800W, and the ultrasonic frequency is 20KHz; The viscosity of the carboxymethyl cellulose is 1200mpa.s;

[0052] Step 2, use the electrospray device to electrospray the ultrasonically degassed sol into the receiving device with a concentration of 9wt% iron ion solution, and stir the iron ion solution during the electrospraying process; Add 0.5 mL of glutaraldehyde dropwise, stir for 18 h at a speed of 200 r / min, and filter to obtain gel microspheres loaded with iron ions; the electrospray device includes a high-voltage power supply, a syringe pump, a syringe and a rec...

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Abstract

The invention discloses a preparation method of an iron ion croscarmellose in-situ growing Prussian-blue microsphere adsorbing material. The method comprises the following steps of (1) dissolving carboxymethylcellulose into ultrapure water, stirring to obtain a concentrated sol, and performing ultrasonic defoaming on the sol; (2) electrically injecting the ultrasonic defoamed sol into a receiving device containing iron ions by using an electric injector; during electric injecting procedure, dropwise adding a cross-linking agent into the receiving device; stirring, filtering to obtain gel microspheres loading iron ions; (3) washing the prepared gel microspheres; soaking the gel microspheres into a potassium ferrocyanide solution; stirring and filtering; drip washing the obtained gel microspheres; and drying to obtain the Prussian-blue microsphere adsorbing material. The preparation method of the Prussian-blue microsphere adsorbing material disclosed by the invention has the characteristics of simple synthetic process, less energy consumption, good mechanical stability, good selectivity, reusability and the like; therefore the preparation method can be widely used for processing cesium containing Saline Lake brine, mother liquor of salt production, mother liquor after extracting lithium, nuclear waste liquid and the like.

Description

technical field [0001] The invention belongs to the technical field of utilization of biomass material resources, and in particular relates to a preparation method of iron ion cross-linked carboxymethyl cellulose in-situ grown Prussian blue microsphere adsorption material. Background technique [0002] As the first artificially synthesized coordination compound, Prussian blue is a face-centered cubic structure lattice with octahedral ligands, and its structural formula is Fe 4 [Fe(CN) 6 ] 3 ·XH 2 O(X=14-16), which has the advantages of non-toxicity, acid resistance, chemical stability, radiation resistance and strong binding ability to cesium. According to whether there are monovalent ions in the crystal lattice, it can be divided into soluble and insoluble Prussian blue, but the Prussian blue prepared by the general method has irregular shape or too fine particles, poor mechanical strength, and cannot be used for continuous column operation. Difficult to achieve large-s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/24B01J20/28B01J20/30C22B26/10
CPCB01J20/24B01J20/28019C22B26/10
Inventor 张永德宗有莉乔丹欧敏华张思月杨辉
Owner SOUTHWEAT UNIV OF SCI & TECH
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