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A method for the enrichment of p-chlorophenol organic pollutants in titanium dioxide self-assembled microcapsules

An organic pollutant, titanium dioxide technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, water pollutants, etc., can solve the problems of long treatment period, complex matrix interference, complicated operation, etc., to achieve a good enrichment index, enrichment short time effect

Active Publication Date: 2020-12-01
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the pollution of environmental chlorophenol organic pollutants is becoming more and more serious, generally speaking, its concentration in the environment is still relatively low (ppt-ppb level), and there is interference from complex matrix, the pretreatment is trace environmental It is an indispensable and important link in the analysis of endocrine disruptors, which needs to be enriched for the needs of high sensitivity and high efficiency detection of trace endocrine disruptors
Traditional sample pretreatment methods, such as Soxhlet extraction, liquid-liquid extraction, etc., mostly have the disadvantages of complicated operation, high work intensity, long processing cycle, large loss of organic solvent, and low extraction efficiency.

Method used

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  • A method for the enrichment of p-chlorophenol organic pollutants in titanium dioxide self-assembled microcapsules
  • A method for the enrichment of p-chlorophenol organic pollutants in titanium dioxide self-assembled microcapsules
  • A method for the enrichment of p-chlorophenol organic pollutants in titanium dioxide self-assembled microcapsules

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Embodiment 1 (product preparation):

[0047] A titanium dioxide self-assembled microcapsule, the preparation steps of which are as follows:

[0048] (1) Preparation of amphiphilic titanium dioxide particles:

[0049] 2g TiO 2 Dissolved in 8g of 1mol / L hydrochloric acid solution to prepare 20wt% TiO 2 Suspension, then add 50mL of methanol solvent to it, stir evenly and heat up to 45°C, called solution A; dissolve 0.98g of hexadecyltrimethoxysilane and 12.73mL of silane coupling agent KH-792 in 10mL of methanol solvent After stirring evenly, add it dropwise to the solution A which has been heated to 45°C, keep the temperature at 45°C, and continue the magnetic stirring reaction for 16h. After the reaction was completed, it was centrifuged, and the obtained solid was washed three times with toluene, and vacuum-dried at 60° C. for 48 hours to obtain amphiphilic titanium dioxide particles.

[0050] (2) Preparation of titanium dioxide self-assembled microcapsules:

[0051]...

Embodiment 2

[0056] Embodiment 2 (microcapsule morphology observation):

[0057] A self-assembled microcapsule of amphiphilic titanium dioxide, the preparation steps of which are as follows:

[0058] (1) Preparation of amphiphilic titanium dioxide particles:

[0059] The preparation method is the same as step (1) of Example 1.

[0060] (2) Preparation of titanium dioxide self-assembled microcapsules:

[0061] Take 5 mg of the amphiphilic titanium dioxide particles obtained in step (1) and put them in a test tube, add 2 ml of water, and disperse fully by ultrasonic; then add 200 μl of dodecane to the test tube, place it in a tumbler and turn it at a speed of 80 rad / min for 2 hours.

[0062] Observing the microcapsule morphology formed in step (2) under a fluorescence microscope, obtained Figure 5 It is found that its size is between 100 μm and 500 μm, and the position of the microcapsule formed by it is on the water surface and is a white emulsion. It is observed through a microscope th...

Embodiment 3

[0063] Embodiment 3 (simulation application experiment): the application experiment of titanium dioxide self-assembled microcapsules enriching low concentration 2-CP in simulated sewage

[0064] Get eight parts of 5 mg of amphiphilic titanium dioxide particles prepared by the step (1) of Example 1, place them in eight test tubes respectively, add 2 ml of o-chlorophenol (2-CP) solution with a concentration of 20 mg / L, and fully ultrasonically Disperse; then add 200μl cyclohexane, n-hexane, n-heptane, dodecane, n-hexanol, n-octanol, oleic acid and no oil phase to the eight test tubes respectively, and place them in a tumbler at 80rad / min The speed is turned over for 24 hours, and the enrichment reaches equilibrium.

[0065] High performance liquid chromatography was used to detect the concentration of 2-CP in the organic phase and the residual water phase to evaluate the enrichment effect.

[0066] Figure 6 It is a comparison chart of the enrichment effect of low-concentratio...

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Abstract

The invention belongs to the technical field of enrichment of low-concentration organic pollutants and particularly relates to a method of enriching chlorophenol organic pollutants by amphiphilic titanium dioxide self-assembled microcapsules. The method includes: with titanium dioxide as a precursor, modifying with hexadecyltrimethoxysilane (referred to as HDTMS) and N-aminoethyl-gamma-aminopropyltrimethoxysilane (KH-792) to obtain amphiphilic titanium dioxide particles, dispersing the amphiphilic titanium dioxide particles as a membrane material in wastewater containing chlorophenol organic pollutants, adding little alcohol or alkane or vegetable oil as an oil phase, and carrying out self-assembly to form oil-in-water structural microcapsules. The microcapsule extraction method herein enables low-concentration chlorophenol nonpolar organics in wastewater to be enriched in the microcapsules; high concentration is reached; subsequent treatment is facilitated. Compared with traditional liquid-liquid microextraction and solid-liquid microextraction, the method herein is simple to perform, good in enrichment effect, and high in enrichment speed; the membrane material is rescuable, andsubsequent analysis and detoxifying treatment are facilitated.

Description

technical field [0001] The invention relates to the technical field of enrichment of low-concentration chlorophenol organic pollutants, in particular to a method for enrichment of chlorophenol organic pollutants in titanium dioxide self-assembled microcapsules. Background technique [0002] Chlorophenols (CPs) are a typical class of refractory organic pollutants. It has broad-spectrum antibacterial, bactericidal and insecticidal effects. It is mainly used for antisepsis and disinfection of wood, vegetables, leather, paint, etc. It is also an intermediate product of many industrial synthesis, and also used as a raw material for fungicides, pesticides, and pharmaceutical industries. use. Experiments confirmed that all CPs have bactericidal activity, phytotoxicity and bioaccumulation. Many have obvious "three-induced" effects, especially for fish, shellfish and other aquatic organisms. Although the pollution of environmental chlorophenol organic pollutants is becoming more a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G23/047B01J13/02C02F1/26C02F1/40
CPCB01J13/02C01G23/047C01P2002/72C01P2002/82C02F1/26C02F1/40C02F2101/345C02F2101/36
Inventor 孙杰喻玲玲范顶进尹杉杉张云宋陈程
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES