CN103724654A - Preparation methods of pentachlorophenol molecularly imprinted polymer microspheres and solid phase extraction column thereof - Google Patents
Preparation methods of pentachlorophenol molecularly imprinted polymer microspheres and solid phase extraction column thereof Download PDFInfo
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- CN103724654A CN103724654A CN201210389144.1A CN201210389144A CN103724654A CN 103724654 A CN103724654 A CN 103724654A CN 201210389144 A CN201210389144 A CN 201210389144A CN 103724654 A CN103724654 A CN 103724654A
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Abstract
The invention provides a preparation method of pentachlorophenol molecularly imprinted polymer microspheres, which comprises the following steps: (1) dissolving template molecules of pentachlorophenol and functional monomers with a molar ratio of 1.5:1-2:1 in an acetonitrile solution containing a cross-linking agent and an initiator to prepare a mixed solution; (2) sealing the mixed solution, performing a polymerization reaction under a heating stirring condition to generate white powdery polymer; (3) extracting the synthesized white powdery polymer by using a mixed solution of methanol and acetic acid as an extraction liquid, removing the template molecules, continuing to extract with pure methanol to remove acetic acid molecules; (4) when extraction is finished, putting the polymer in a vacuum drying box, drying to reach a constant weight, crushing and sieving to obtain pentachlorophenol molecularly imprinted polymer microspheres. Meanwhile, the invention also discloses a preparation method of a solid phase extraction column of the pentachlorophenol molecularly imprinted polymer microspheres. The advantages of the methods of the invention are simple preparation process, high adsorption selectivity, and rapid adsorption speed.
Description
Technical field
The invention belongs to pollutent sorbing material synthesis technical field in environmental analysis, be specifically related to the preparation method of a kind of pentachlorophenol molecular blotting polymer microsphere and solid-phase extraction column thereof.
Background technology
Molecular imprinting just refers to take specific molecule as template, and preparation has the technology of specific identification function and high selectivity material to this molecule.This technology is very rapid in development recent years.By thering is molecule that specified shape and big or small needs identify as template molecule using one, this template molecule is dissolved in linking agent, add again after specific function monomer initiated polymerization the polymkeric substance that height of formation is crosslinked, its inner embedding and the interactional template molecule of function monomer.Then utilize the method for physics or chemistry by template molecule wash-out, on polymeric matrix, just left like this hole similar to template molecule shape, and in hole, the position of each functional group and template molecule used are complementary, can there is special keying action with template molecule, thereby realize the identification to template molecule.The preparation method of the molecular blotting polymer microsphere of development in recent years (MIPMs), has and makes the advantages such as simple, with low cost and sturdy and durable, applied widely, and is described as " omnipotent molecular recognition material ".The preparation of molecular blotting polymer microsphere and applied research have obtained certain achievement, and are at present the high speed development stage.Molecularly imprinted polymer is application to some extent in the real lifes such as separation, catalysis.But also there are many problems that need solution at present.Subject matter comprises that preparing craft is comparatively complicated, needs to add plurality of reagents, and adsorption selectivity is poor, and rate of adsorption is slow etc.These deficiencies and problem, to prepare pentachlorophenol molecular blotting polymer microsphere more obvious.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, and the preparation method of a kind of pentachlorophenol molecular blotting polymer microsphere and solid-phase extraction column thereof is provided, and the method preparation process is simple, and adsorption selectivity is high, and rate of adsorption is fast.
The present invention solves the problems of the technologies described above taked technical scheme: a kind of preparation method of pentachlorophenol molecular blotting polymer microsphere, comprise the steps: that (1) is dissolved into template molecule pentachlorophenol and the function monomer ratio of 1.5: 1 in molar ratio～2: 1 in the acetonitrile solution that contains linking agent and initiator, is prepared into mixed solution; (2) by after mixed solution sealing, under condition of heating and stirring, polymerization reaction take place generates white powder shaped polymer; (3) take the mixing solutions white powder shaped polymer synthetic as extracting solution extracts of methyl alcohol and acetic acid, remove template molecule, then continue with pure methanol extraction removal molecular acid; (4) after extraction finishes, polymkeric substance is placed in to vacuum drying oven and is dried to weight, after pulverizing and sieving, obtain pentachlorophenol molecular blotting polymer microsphere.
As preferably; described function monomer comprises methacrylic acid, acrylamide, 2-acrylamide-2-methyl isophthalic acid-propanesulfonic acid, N-acryl L-Ala, 4-vinylstyrene; described linking agent is N; N '-methylene-bisacrylamide, ethyleneglycol dimethyacrylate, described initiator is Diisopropyl azodicarboxylate, Potassium Persulphate.
As preferably, described acetonitrile solution is 50ml, and contained linking agent and initiator are 10～20mmol; Described polymerization temperature is 55～70 ℃, and the reaction times is 12～24h.
A kind of method of preparing solid-phase extraction column with pentachlorophenol molecular blotting polymer microsphere, comprise the steps: to weigh pentachlorophenol molecular blotting polymer microsphere, be filled in polypropylene solid phase extraction column, polyethylene sieve plate is loaded onto respectively in the top of filler and bottom; Adopt methyl alcohol: Virahol volume ratio=2: 1 as dress post homogenate liquid, vacuumizes under state, packs homogenate into polypropylene solid phase extraction column, finally covers tightly sieve plate, obtains pentachlorophenol molecularly imprinted solid phase extraction column.
Compared with the existing technology, the present invention be take pentachlorophenol as template molecule, and acetonitrile is solvent, under the condition of linking agent and initiator existence, is prepared, and step is simple, easy to operate; Prepared polymer beads is even, and specific surface area and pore volume are large, and adsorption selectivity is high, and rate of adsorption is fast; Polymkeric substance can directly be tested in water surrounding, without too much other organic reagent, and environmental friendliness.
Embodiment
Below in conjunction with embodiment, to of the present invention, be further elaborated.
Embodiment 1: a kind of pentachlorophenol molecular blotting polymer microsphere, make as follows: (1) is dissolved into template molecule pentachlorophenol and the function monomer amount of 1.5: 1 in molar ratio～2: 1 in the acetonitrile solution that contains 10～20mmol linking agent and catalytic amount of initiator that is no less than 50ml, be prepared into mixed solution, wherein function monomer comprises methacrylic acid, acrylamide, 2-acrylamide-2-methyl isophthalic acid-propanesulfonic acid, N-acryl L-Ala, 4-vinylstyrene, linking agent is N, N '-methylene-bisacrylamide, ethyleneglycol dimethyacrylate, initiator is Diisopropyl azodicarboxylate, Potassium Persulphate, (2) by after mixed solution sealing, under condition of heating and stirring, polymerization reaction take place generates white powder shaped polymer, and polymerization temperature is 55～70 ℃, and the reaction times is 12～24h, (3) take the mixing solutions white powder shaped polymer synthetic as extracting solution extracts of methyl alcohol and acetic acid, remove template molecule, then continue with pure methanol extraction removal molecular acid, (4) after extraction finishes, polymkeric substance is placed in to vacuum drying oven and is dried to weight, after pulverizing and sieving, obtain pentachlorophenol molecular blotting polymer microsphere.
Embodiment 2: a kind of pentachlorophenol molecular blotting polymer microsphere solid-phase extraction column, make as follows: weigh pentachlorophenol molecular blotting polymer microsphere, be filled in polypropylene solid phase extraction column, polyethylene sieve plate is loaded onto respectively in the top of filler and bottom; Adopt methyl alcohol: Virahol volume ratio=2: 1 as dress post homogenate liquid, vacuumizes under state, packs homogenate into polypropylene solid phase extraction column, finally covers tightly sieve plate, obtains pentachlorophenol molecularly imprinted solid phase extraction column.
Though it is pointed out that above-described embodiment is to the present invention's detailed text description of contrasting, these text descriptions are the simple description to mentality of designing of the present invention just, rather than the restriction to thinking of the present invention.Any combination, increase or modification that is no more than mentality of designing of the present invention, all falls within the scope of protection of the present invention.
Claims (4)
1. the preparation method of a pentachlorophenol molecular blotting polymer microsphere, it is characterized in that comprising the steps: that (1) is dissolved into template molecule pentachlorophenol and the function monomer ratio of 1.5: 1 in molar ratio～2: 1 in the acetonitrile solution that contains linking agent and initiator, be prepared into mixed solution; (2) by after mixed solution sealing, under condition of heating and stirring, polymerization reaction take place generates white powder shaped polymer; (3) take the mixing solutions white powder shaped polymer synthetic as extracting solution extracts of methyl alcohol and acetic acid, remove template molecule, then continue with pure methanol extraction removal molecular acid; (4) after extraction finishes, polymkeric substance is placed in to vacuum drying oven and is dried to weight, after pulverizing and sieving, obtain pentachlorophenol molecular blotting polymer microsphere.
2. the preparation method of pentachlorophenol molecular blotting polymer microsphere according to claim 1; it is characterized in that: described function monomer comprises methacrylic acid, acrylamide, 2-acrylamide-2-methyl isophthalic acid-propanesulfonic acid, N-acryl L-Ala, 4-vinylstyrene; described linking agent is N; N '-methylene-bisacrylamide, ethyleneglycol dimethyacrylate, described initiator is Diisopropyl azodicarboxylate, Potassium Persulphate.
3. the preparation method of pentachlorophenol molecular blotting polymer microsphere according to claim 1, is characterized in that: described acetonitrile solution is 50ml, and contained linking agent and initiator are 10～20mmol; Described polymerization temperature is 55～70 ℃, and the reaction times is 12～24h.
4. a pentachlorophenol molecular blotting polymer microsphere claimed in claim 1 is prepared the method for solid-phase extraction column, it is characterized in that comprising the steps: to weigh pentachlorophenol molecular blotting polymer microsphere, be filled in polypropylene solid phase extraction column, polyethylene sieve plate is loaded onto respectively in the top of filler and bottom; Adopt methyl alcohol: Virahol volume ratio=2: 1 as dress post homogenate liquid, vacuumizes under state, packs homogenate into polypropylene solid phase extraction column, finally covers tightly sieve plate, obtains pentachlorophenol molecularly imprinted solid phase extraction column.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105688444A (en) * | 2014-11-27 | 2016-06-22 | 宁波市疾病预防控制中心 | Chlorophenol graphene-based molecularly imprinted solid-phase extraction column and preparation method and application thereof |
| CN113209948A (en) * | 2021-05-19 | 2021-08-06 | 齐鲁工业大学 | Preparation method and application of multi-template molecularly imprinted composite material |
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| CN101497035A (en) * | 2008-12-30 | 2009-08-05 | 安徽农业大学 | Preparation method of solid-phase extraction small column for molecular imprinting of substituted carbamide pesticide |
| CN101907571A (en) * | 2010-06-28 | 2010-12-08 | 济南大学 | Mesoporous carbon molecular imprinting detector for detecting trace environment hormones and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101177500A (en) * | 2007-10-30 | 2008-05-14 | 湖北出入境检验检疫局检验检疫技术中心 | Method for preparing bisphenol A molecular engram polymer |
| CN101497035A (en) * | 2008-12-30 | 2009-08-05 | 安徽农业大学 | Preparation method of solid-phase extraction small column for molecular imprinting of substituted carbamide pesticide |
| CN101907571A (en) * | 2010-06-28 | 2010-12-08 | 济南大学 | Mesoporous carbon molecular imprinting detector for detecting trace environment hormones and application thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105688444A (en) * | 2014-11-27 | 2016-06-22 | 宁波市疾病预防控制中心 | Chlorophenol graphene-based molecularly imprinted solid-phase extraction column and preparation method and application thereof |
| CN113209948A (en) * | 2021-05-19 | 2021-08-06 | 齐鲁工业大学 | Preparation method and application of multi-template molecularly imprinted composite material |
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Application publication date: 20140416 |