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Hydrophilic magnetic resin with high specific surface area and preparation method thereof and method for rapidly extracting phthalic acid ester in water body

A high specific surface area, magnetic resin technology, applied in the direction of extraction water/sewage treatment, water/sewage treatment, chemical instruments and methods, etc., can solve the problems of lack of detection methods and difficult detection of phthalates, and achieve improved Extraction efficiency, realize fast and efficient solid phase extraction and detection analysis, and enhance the effect of application range

Active Publication Date: 2013-12-11
NANJING UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problems that existing phthalates are difficult to detect and lack of effective detection means, the present invention provides a hydrophilic high specific surface area magnetic resin and its preparation method and its application in rapid extraction of phthalates in water The method developed a hydrophilic high specific surface area magnetic resin material, and modified hydroxyl groups on its surface, so that it can interact with phthalates in water through hydrogen bonding to enhance the ability to detect target substances. Selectivity, establishing a fast and efficient extraction method for trace phthalates in water based on magnetic solid-phase extraction

Method used

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  • Hydrophilic magnetic resin with high specific surface area and preparation method thereof and method for rapidly extracting phthalic acid ester in water body
  • Hydrophilic magnetic resin with high specific surface area and preparation method thereof and method for rapidly extracting phthalic acid ester in water body
  • Hydrophilic magnetic resin with high specific surface area and preparation method thereof and method for rapidly extracting phthalic acid ester in water body

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preparation example Construction

[0043] A preparation method of a hydrophilic high specific surface area magnetic resin, the steps of which are:

[0044] (a) Equipped with a water phase, in which 0.5% to 2% of gelatin and 5 to 20% of salt are added, accounting for the mass percentage of the water phase;

[0045] (b) Equipped with an oil phase, mix the reactant monomer and the porogen toluene, add the initiator benzoyl peroxide, and mix well to obtain the oil phase; the reactant monomers are divinylbenzene, vinyl benzoate and formaldehyde Glycidyl acrylate, wherein the mass ratio of vinyl benzoate to divinylbenzene is 1:0.5-2, and the mass ratio of glycidyl methacrylate to divinylbenzene is 1:1-9. The mass ratio of the porogen toluene to the reactant monomer is 1-2:1, and the mass ratio of the initiator benzoyl peroxide is 0.5-3% of the total amount of the reactant monomer and the porogen.

[0046] (c) Add oleic acid-coated and modified magnetic particles to the oil phase, and after mixing evenly, add the oil...

Embodiment 1

[0058] 500 g of the water phase was prepared using 5.0 g of gelatin and 100.0 g of table salt. The oil phase consisted of 21.0 g divinylbenzene, 11.7 g vinyl benzoate, 2.3 g glycidyl methacrylate, 35.0 g toluene and 1.4 g benzoyl peroxide. The oil phase was coated with 8.75g oleic acid Fe 3 o 4 After mixing evenly, add it into a three-necked flask to mix with the water phase (175g), control the stirring speed at 300rpm, raise the temperature to 60°C for 6h, and keep it at 85°C for 6h. Wash the obtained resin white balls (45.2g) with ethanol and pure water, dry them, swell in dichloroethane for 6 hours, add 22.6g of anhydrous ferric chloride and react at 80°C for 12 hours to obtain a highly cross-linked resin . Add highly cross-linked spheres (43.5g) into 261g of 5% sodium hydroxide solution, react at 60°C for 5 hours, and after cooling, centrifuge the resin, wash and dry with ethanol-pure water to obtain hydrophilic and high specific surface area magnetism resin. The resu...

Embodiment 2

[0063] 1000 g of the aqueous phase was prepared using 5.0 g of gelatin and 100.0 g of table salt. The oil phase consisted of 10.0 g divinylbenzene, 20.0 g vinyl benzoate, 3.3 g glycidyl methacrylate, 40.0 g toluene and 2.7 g benzoyl peroxide. The oil phase was coated with 2.7g oleic acid gamma-Fe 2 o 3 After mixing evenly, add it into a three-necked flask to mix with the water phase (696.4g), control the stirring speed at 400rpm, raise the temperature to 80°C for 3h, and keep at 90°C for 5h. Wash the obtained white ball resin (31.5g) with ethanol and pure water, dry it, swell it in dichloroethane for 9 hours, add 6.3g of anhydrous ferric chloride and react it at 80°C for 9 hours to obtain a highly cross-linked resin . Add highly cross-linked balls (30.2g) into 241.6g of 5% sodium hydroxide solution, react at 70°C for 5 hours, and after cooling, centrifuge the resin, wash and dry with ethanol-pure water to obtain hydrophilic and high specific surface area magnetic resin.

...

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Abstract

The invention discloses a hydrophilic magnetic resin with a high specific surface area and a preparation method thereof and a method for rapidly extracting phthalic acid ester in a water body, belonging to the technical filed of preparation of absorbent resins for rapid enrichment and separation of trace organic substances in the water body. A precursor resin is prepared through addition of magnetic particles and the copolymerization reaction of divinylbenzene, benzoic acid vinyl esters and glycidyl methacrylate, the specific surface area of the resin is improved by a post cross-linking reaction, an ester group on the surface of the resin is hydrolyzed in an alkaline solution, so that the magnetic resin rich in hydroxyl perssad with high specific surface area is prepared. The resin has higher extracting performance and selectivity to phthalic acid ester substances in the water body, and trace phthalic acid ester substances in large volume of water body can be rapidly and efficiently enriched and separated through a rapid separation technology based on a novel magnetic solid phase extraction rod.

Description

technical field [0001] The invention relates to the technical field of preparation of adsorption resins that can be used for rapid enrichment and separation of trace organic matter in water bodies, in particular, to a hydrophilic high specific surface area magnetic resin and its preparation method and its application in rapid extraction of phthalates in water bodies. Formate method. Background technique [0002] Phthalates, also known as phthalates, are widely used in daily life products and are ubiquitous in the environment. Studies have shown that phthalates can interfere with endocrine, reduce the number of sperm in men, lower their motility, and have abnormal shapes. In severe cases, they can also lead to dead sperm and testicular cancer. At present, this substance has been identified as a typical type of endocrine disruptor, and its existence in the environment and the process of migration and transformation need to be strictly monitored. Among them, the most importan...

Claims

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Application Information

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IPC IPC(8): C08F212/36C08F218/10C08F220/32C08F2/44C08F8/12C08J9/28C08J7/02C08J3/24B01J20/26B01J20/30C02F1/28C02F1/26
CPCC08F212/36C08F2/44B01J20/267C02F2101/305B01J20/223B01J20/3071C02F1/285C02F1/48B01J20/28009C08F218/10C08F220/286C02F1/288C02F2101/32
Inventor 周庆张满成李爱民双陈冬王梦乔王未黄从建江静怡李海波
Owner NANJING UNIV
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