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Preparation method of magnetic composite adsorbing material for Antarctic krill protein enzymolysis solution defluorination

The technology of composite adsorption material and protease hydrolyzate is applied in the field of preparation of composite adsorption material, which can solve the problems of difficulty in post-processing and increase the difficulty of separation of adsorbents, and achieves convenient separation, convenient separation, recovery and regeneration, and fluorine removal effect. excellent effect

Inactive Publication Date: 2015-08-05
DALIAN POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in order to achieve higher adsorption efficiency, finer adsorbents are often prepared to increase their specific surface area, which increases the difficulty of adsorbent separation and makes post-processing more difficult.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1. Weigh a certain mass of Fe 3 o 4 , slowly added to the concentration of 1.85wt% chitosan acetic acid solution (2wt%), Fe 3 o 4 The quality of: the volume of chitosan acetic acid solution is controlled at 13:1, unit g / L, then with the supersonic wave (frequency 120kHz) ultrasonic dispersion 30min of 300 watts;

[0020] 2. Add the above solution to 0.65 times the volume of Ca(NO 3 ) 2 solution, and stirred at 65°C for 20min;

[0021] 3. Under the condition of keeping stirring, use a constant flow pump to slowly drop the above solution into 0.24 times the volume of (NH 4 ) 2 HPO 4 In the solution, the molar ratio of Ca / P was kept at 1.62, during which the pH was adjusted with ammonia water to keep the value at 10, the stirring time continued for 2 hours, and then stood at room temperature for 26 hours;

[0022] 4. Vacuum filter the solution after standing, and repeatedly wash the solid matter with deionized water and absolute ethanol until neutral, then vacuum-d...

Embodiment 2

[0024] 1. Weigh a certain mass of Fe 3 o 4 , slowly added to the concentration of 1.90wt% chitosan acetic acid solution (2wt%), Fe 3 o 4 The quality of: the volume of chitosan acetic acid solution is controlled at 12:1, unit g / L, then with the supersonic wave (frequency 80kHz) ultrasonic dispersion 25min of 400 watts;

[0025] 2. Add the above solution to 0.70 times the volume of Ca(NO 3 ) 2 solution, and stirred at 70 ° C for 15 min;

[0026] 3. Under the condition of keeping stirring, use a constant flow pump to slowly drop the above solution into 0.25 times the volume of (NH 4 ) 2 HPO 4 In the solution, the molar ratio of Ca / P was kept at 1.64, during which the pH was adjusted with ammonia water to keep the value between 11, the stirring time continued for 2.5h, and then stood at room temperature for 28h;

[0027] 4. Vacuum filter the solution after standing, and wash the solid matter repeatedly with deionized water and absolute ethanol to neutrality, then vacuum-dr...

Embodiment 3

[0029] 1. Weigh a certain mass of Fe 3 o 4 , slowly added to the concentration of 1.95wt% chitosan acetic acid solution (2wt%), Fe 3 o 4 The quality: the volume of chitosan acetic acid solution is controlled at 11:1, unit g / L, then with the supersonic wave (frequency 70kHz) ultrasonic dispersion 30min of 500 watts;

[0030] 2. Add the above solution to 0.75 times the volume of Ca(NO 3 ) 2 solution, and stirred at 75 ° C for 10 min;

[0031]3. Under the condition of keeping stirring, use a constant flow pump to slowly drop the above solution into 0.16 times the volume of (NH 4 ) 2 HPO 4 In the solution, the molar ratio of Ca / P was kept at 1.65, during which the pH was adjusted with ammonia water to keep the value at 10, the stirring time continued for 3 hours, and then stood at room temperature for 30 hours;

[0032] 4. Vacuum filter the solution after standing, and wash the solid matter repeatedly with deionized water and absolute ethanol to neutrality, then vacuum-dry...

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PUM

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Abstract

The invention discloses a preparation method of a magnetic composite adsorbing material for Antarctic krill protein enzymolysis solution defluorination, which comprises the following steps: 1. adding Fe3O4 into a chitosan acetic acid solution, and carrying out ultrasonic dispersion; 2. adding the solution into a Ca(NO3)2 solution, and stirring; 3. under stirring conditions, slowly and dropwisely adding the solution into a (NH4)2HPO4 solution while keeping the Ca / P mole ratio at 1.60-1.80 and regulating the pH value at 10-11, and standing; and 4. carrying out vacuum filtration on the solution, repeatedly washing with deionized water and anhydrous ethanol until the solid becomes neutral, carrying out vacuum drying, pulverizing the dried product into powder, and screening to obtain the magnetic hydroxyapatite / chitosan (HA / CS) composite adsorbing material. The saturation magnetization of the magnetic composite adsorbing material is 18.0-20.0 emu / g. When the magnetic composite adsorbing material is used for defluorinating the Antarctic krill protein enzymolysis solution, the water-soluble fluorine removal rate can reach 90% above; and the adsorbing material after defluorination is more convenient for separation, recovery and regeneration due to the magnetism of the adsorbing material.

Description

technical field [0001] The invention relates to the preparation of a magnetic composite adsorption material, in particular to the preparation of a magnetic composite adsorption material which can be used for the removal of fluorine in antarctic krill protein enzymatic hydrolyzate. Background technique [0002] Chitosan (Chitosan, CS), the chemical name is poly 2-amino-2-deoxy-D-β-1,4-glucose, the product of chitin deacetylation, is a natural polymer compound, Its molecular structure contains a large number of free amino groups. These free amino groups can combine a proton in a weak acid solution system to form a cationic polymer, and adsorb anions such as fluoride ions through electrostatic attraction. However, due to the disadvantages of easy loss and low adsorption capacity, the simple use of chitosan for fluorine removal cannot achieve good results. In addition, chitosan's poor mechanical strength, insolubility in water, and gel-like precipitation under alkaline conditio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/24B01J20/30C02F1/28C02F1/58
Inventor 周大勇阴法文王力丽刘文涛万锈琳杨静峰温成荣朱蓓薇
Owner DALIAN POLYTECHNIC UNIVERSITY
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