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Preparation of magnetic hydrotalcite and determination method of trace F and Cl anions in phosphorus-rich sample

A magnetic hydrotalcite and anion technology, applied in chemical instruments and methods, measuring devices, material separation, etc., can solve the problems of magnetic hydrotalcite materials such as the repeated utilization efficiency of phosphate radical adsorption capacity

Pending Publication Date: 2020-11-06
SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But on F - and Cl - Under the premise of no adsorption, no magnetic hydrotalcite material with high phosphate adsorption capacity and good multiple reuse efficiency has been found so far.

Method used

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  • Preparation of magnetic hydrotalcite and determination method of trace F and Cl anions in phosphorus-rich sample
  • Preparation of magnetic hydrotalcite and determination method of trace F and Cl anions in phosphorus-rich sample
  • Preparation of magnetic hydrotalcite and determination method of trace F and Cl anions in phosphorus-rich sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] F, drawing of Cl anion standard curve:

[0041] (1) Absorb 1000mg·L -1 F standard solution and 1000mg·L -1 Cl standard solution 5.00mL each, dilute to 100mL with ultrapure water to obtain 50mg·L fluoride ion -1 , chloride ion 50mg·L -1 The mixed standard solution;

[0042] (2) 50mg·L -1 F, Cl mixed standard solution was diluted step by step with ultrapure water until the content of F and Cl was 0.1mg L -1 , 0.5mg·L -1 , 1mg·L -1 , 5mg·L -1 , 10mg·L -1 gradient standard solution;

[0043] (3) by ion chromatography analysis detection to each gradient standard solution, obtain the ion chromatography standard collection of illustrative plates of F, Cl anion, draw the standard curve Y=aX+b of F, Cl anion according to this collection of collection, wherein Y is peak area, unit is μS min; X is the anion concentration, the unit is mg L -1 ; a, b are dimensionless coefficients;

[0044] The standard curve for fluoride ion is: Y=0.4725X-0.0037; linear correlation coef...

Embodiment 2

[0047] Preparation and reuse of magnetic hydrotalcite materials:

[0048] A. Co-precipitation method and hydrothermal method to prepare magnetic hydrotalcite materials:

[0049] (1) Weigh 0.6g nanometer Fe 3 o 4 Powder, use 15mL 0.1mol·L -1 NaOH was ultrasonically dispersed for 10 min, then separated with a magnet, and set aside.

[0050] (2) Weigh 2.044g Mg(NO 3 ) 2 ·6H 2 O, 1.500g Al(NO 3 ) 3 9H 2 O and 1.68g CO(NH 2 ) 2 In 70mL of ultrapure water, place this mixture on a mixer and mix for 15 minutes for later use.

[0051] (3) Fe treated in (1) 3 o 4 The powder and the mixed salt solution in (2) were transferred to the liner of a 100mL tetrafluoroethylene reactor, placed on a mixer and mixed for 2 hours, then put into a high-pressure reactor and tightened.

[0052] (4) Put the reactor into an oven, and react at 120° C. for 12 hours.

[0053] (5) After the reaction kettle was cooled, the prepared product was washed three times with ultrapure water and absolute...

Embodiment 3

[0071] Detection of Anions in Phosphate Glass

[0072] A. Preparation of phosphate glass leaching solution: Take 0.2g of phosphate glass powder passed through a 400 mesh screen, add it into a 100mL polytetrafluoroethylene reactor liner filled with 80mL ultrapure water, tighten the autoclave, and place it at 80°C Heat in an oven for 24 hours, take it out after cooling, and filter with a 0.22 μm tetrafluoroethylene filter membrane to obtain a phosphate glass leachate;

[0073] B. Determination of anions in phosphate glass leachate:

[0074] (1) 80mL of phosphate glass leaching solution is placed in a beaker;

[0075] (2) Add 50 mg of magnetic hydrotalcite material to the beaker, place it on a mixer and mix for 5 minutes;

[0076] (3) Place the magnet on the outer wall of the beaker, the magnetic hydrotalcite material is immediately gathered to the side close to the magnet, the solution is poured out, filtered through a 0.22μm tetrafluoroethylene filter, passed through nitrogen...

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Abstract

The invention relates to preparation of a magnetic hydrotalcite material and a determination method of trace F and Cl anions in a phosphorus-rich sample. Phosphate radicals in the phosphorus-rich sample are adsorbed by utilizing the prepared magnetic hydrotalcite material, ion chromatographic analysis is performed on a sample solution, and the content of the trace F and Cl anions can be calculated. When trace anions in a high phosphate matrix are measured by ion chromatography, high-concentration phosphate can cause the chromatographic peaks of trace F and Cl anions to be covered or deformed on one hand, and can cause a chromatographic column to be overloaded on the other hand to influence the service life of the chromatographic column and even cause ghost peaks to influence the measurement result of the next needle. With the preparation of the magnetic hydrotalcite material and the determination method adopted, the above problems can be solved. The prepared magnetic hydrotalcite material does not adsorb the F and Cl anions while adsorbing the phosphate radicals, and therefore, the adsorption material can be separated from the original solution by virtue of a magnet, and the magnetic hydrotalcite material can be repeatedly and reliably used for measuring the content of trace F and Cl anions in phosphorus-rich samples such as phosphate glass and phosphorus-rich wastewater afterbeing subjected to desorption treatment.

Description

technical field [0001] The invention belongs to the technical field of magnetic adsorption material sample pretreatment, and more specifically utilizes the reusable magnetic hydrotalcite material to eliminate the phosphate radical matrix in the solution, and then uses ion chromatography to determine phosphorus-rich phosphate glass, phosphorus-containing wastewater, etc. The method of trace F and Cl anions in the sample. Background technique [0002] Anionic impurities such as fluorine and chlorine in phosphate laser glass originate from glass raw material and water removal process. Changes in the content and distribution of fluorine and chlorine impurity ions in laser glass or between batches of glass will cause changes in the refractive index, which will cause dynamic optical distortion of the laser glass, thereby affecting the beam quality of the output laser. The industrial wastewater produced by glass preparation contains pollutants such as fluorine, chlorine and phosph...

Claims

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Application Information

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IPC IPC(8): B01J20/28B01J20/06B01J20/30C02F1/28G01N30/96C02F101/10
CPCB01J20/28009B01J20/043B01J20/06C02F1/281G01N30/96C02F2101/105Y02P10/20
Inventor 陈思陈伟胡丽丽
Owner SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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