Preparation method of magnetic KMS-1/Fe3O4 composite material and application of material for removing ciprofloxacin

A technology of ciprofloxacin and composite materials, which is applied in chemical instruments and methods, water/sludge/sewage treatment, alkali metal compounds, etc., to achieve the effects of high removal rate, low cost, and environmental protection

Active Publication Date: 2016-09-28
INST OF URBAN ENVIRONMENT CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The results of literature search show that: using cysteine ​​as coupling agent, adopting vibration-ultrasonic method, nano-Fe 3 o 4 Loaded on the KMS-1 material to prepare KMS-1 / Fe 3 o 4 Composite materials and methods for adsorbing ciprofloxacin and their applications have not been reported yet

Method used

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  • Preparation method of magnetic KMS-1/Fe3O4 composite material and application of material for removing ciprofloxacin
  • Preparation method of magnetic KMS-1/Fe3O4 composite material and application of material for removing ciprofloxacin
  • Preparation method of magnetic KMS-1/Fe3O4 composite material and application of material for removing ciprofloxacin

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Example 1 : This KMS-1 / Fe 3 o 4 Composite material preparation and characterization, the details are as follows:

[0034] (1) The layered chalcogenide KMS-1 was synthesized according to the method reported in the literature ( JACS , 2009, 131: 6599–6607): Sn (23 mmol), Mn (11.53 mmol), K 2 CO 3 (11.53 mmol), S (69 mmol) and H 2 O (15.38 mL), hydrothermally reacted in an oven at 200°C for 4 days, cooled to room temperature, 2 Wash with ethanol several times in sequence, and finally dry it in a vacuum oven at 60°C before use;

[0035] (2) Nano Fe 3 o 4 Synthetic method, 4.05 g FeCl 3 ·H 2 O, 3 g PEG 2000, 10.8 g NaAC and 120 mL ethylene glycol were placed in a 200 mL reactor, and hydrothermally reacted in an oven at 200 °C for 20 h. After cooling to room temperature, wash with ethanol several times with the aid of a magnet, and finally dry it in a vacuum oven at 60°C before use;

[0036] (3) KMS-1 / Fe 3 o 4 The preparation method is as follows: take 0.1g-0...

Embodiment 2

[0038] Example 2 : KMS-1 / Fe 3 o 4 Adsorption and removal of ciprofloxacin (CIP) in water under different reaction time conditions, the specific content is as follows:

[0039] (1) Prepare KMS-1 / Fe according to Example 1 3 o 4 composite materials;

[0040] (2) Use KMS-1 / Fe 3 o 4 Adsorb the CIP solution with an initial concentration of 10 mg / L, shake it in a shaker at 25°C at a speed of 300 r / min, and take samples at different time periods (10-180min). Then filter with filter paper, and the gained filtrate measures the concentration of CIP by high performance liquid chromatography;

[0041] (3) Draw the obtained data into a graph, such as image 3 As shown, when the reaction was carried out for 5 minutes, the equilibrium adsorption capacity of CIP was 6 mg / g. As the reaction time increased, the adsorption capacity of CIP also increased rapidly, and the adsorption was saturated at about 30 min, and the maximum adsorption capacity was 10 mg / g, continue to prolong the r...

Embodiment 3

[0042] Example 3 : initial pH vs. KMS-1 / Fe 3 o 4 Composite system adsorption removes the effect of ciprofloxacin (CIP) in water, the specific content is as follows:

[0043] (1) Prepare KMS-1 / Fe according to Example 1 3 o 4 composite materials;

[0044] (2) Prepare a solution with a concentration of 10 mg / LCIP, measure 20 mL of CIP target solution into 12 clean reaction bottles, and adjust the pH of the target solution to 0.86, 2.0, 3.05, 4.1, 5.09, 6.07, 7.0, 8.0, 9.0, 10.0, 11.0, and 12.0. Add a certain amount of KMS-1 / Fe to 12 reaction bottles respectively 3 o 4 Composite material, stirred at room temperature (300 rpm) for 3 hours, then sampled and analyzed;

[0045] (3) Draw the obtained data into a graph, such as Figure 4 As shown, when the pH is 1, the maximum adsorption capacity is 10 mg / g, when the pH = 2, the maximum adsorption capacity is slightly decreased, and in the range of pH 3-8, the adsorption capacity remains at 9 mg / g Above, when the pH was 9, t...

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Abstract

The invention provides a preparation method of a magnetic KMS-1 / Fe3O4 composite material and application of the material for removing ciprofloxacin. The method comprises the steps that 1, L-cysteine serves as a coupling agent, and the KMS-1 / Fe3O4 composite material is prepared under a specific condition; 2, a ciprofloxacin target solution of which the concentration ranges from 10 mg / L to 250 mg / L is prepared, and the pH is adjusted to be 1-12; 3, a certain amount of the KMS-1 / Fe3O4 composite material is added to the ciprofloxacin target solution, and the mixture is put at room temperature for a reaction. According to the preparation method of the magnetic KMS-1 / Fe3O4 composite material and the application of the material for removing ciprofloxacin, the preparation method of the magnetic KMS-1 / Fe3O4 composite material is found for the first time, it is found that the composite material can rapidly and efficiently remove ciprofloxacin, and a good adsorptive property can be maintained on the reaction condition that the change of the pH value is large (pH=1-11). According to the preparation method of the magnetic KMS-1 / Fe3O4 composite material and the application of the material for removing ciprofloxacin, the processes are easy to operate, the technology is simple, and the requirement on equipment is low; the material can be widely used for removal of antibiotic pollutants in a water environment and has a wide market application prospect.

Description

technical field [0001] The invention belongs to a magnetic chalcogenide composite material and a preparation method thereof, in particular to a chalcogenide adsorbent loaded with nano-ferric oxide, that is, KMS-1 / Fe 3 o 4 A magnetic composite material and a preparation method thereof, the adsorbent can efficiently adsorb ciprofloxacin, and can be used to treat waste water polluted by antibiotic pollutants. [0002] The invention belongs to the technical field of environmental functional materials and water pollution control, and relates to a method of using L-cysteine ​​as a coupling agent to combine nano-Fe 3 o 4 Prepare KMS-1 / Fe by Loading on KMS-1 3 o 4 A magnetic composite material method and a method for efficiently and quickly removing ciprofloxacin by using the composite material and its application. Background technique [0003] The presence of antibiotics in the environment can affect the evolution of community structures in nature, leading to the development o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/06B01J20/28B01J20/30C02F1/28C02F101/38C02F101/36
CPCB01J20/0251B01J20/06B01J20/28009C02F1/281C02F1/288C02F2101/36C02F2101/38
Inventor 付明来王云霞杨佳诚苑宝玲
Owner INST OF URBAN ENVIRONMENT CHINESE ACAD OF SCI
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