CN105601846A - Chitosan surface molecularly imprinted rod-like material - Google Patents
Chitosan surface molecularly imprinted rod-like material Download PDFInfo
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- CN105601846A CN105601846A CN201510572025.3A CN201510572025A CN105601846A CN 105601846 A CN105601846 A CN 105601846A CN 201510572025 A CN201510572025 A CN 201510572025A CN 105601846 A CN105601846 A CN 105601846A
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Abstract
The invention relates to preparation of a chitosan surface molecularly imprinted rod-like material. The preparation method consists of: fully mixing a solvent, chitosan, a monomer I and an initiator, keeping the volume ratio of the solvent to the monomer I at 1:1-1:25, and an initiator content of 0.001-20%, introducing N2, conducting polymerization at a reaction temperature of 10-150DEG C and under 1-100 atmospheric pressure for 1-30h, precipitating a polymer obtained by polymerization of chitosan and the monomer out of the solvent to form a nanoscale chitosan polymer microsphere emulsion; then adding a monomer II and a template molecule, controlling the volume ratio of the emulsion to the monomer II at 1:5-10:1, and the mass ratio of the template molecule to the monomer II at 1:1-1:30, fully mixing the substances, conducting sealing and ultrasonic oscillation, then placing the product into a constant temperature box to carry out polymerization for 5-100h, thus obtaining the surface molecularly imprinted rod-like material with good memory performance. The rod-like material prepared by the method provided by the invention is widely applied in the aspect of specific recognition of target molecules.
Description
Technical field
The present invention relates to a kind of method of preparing chitosan molecule trace shape memory club-shaped material.
Background technology
Molecularly imprinted polymer is a kind of adsorption and separation material To Template molecule to specific selectivity recognition capability, in liquid chromatogram, biology sensor, SPE, the good application prospect that many fields have such as catalyze and synthesize. Wherein molecular engram microsphere (MIMs) facilitates because preparation is relative with application, chromatographic efficiency is high and be convenient to Functional Design, in recent years becomes gradually the focus of research. Surface grafting technology is the novel surface engram technology that imprinted layer that a kind of handle of in recent years occurring has a recognition site is combined in stromal surface, taking chitose graft copolymer as carrier, utilize biocompatibility and the readily degradable energy of shitosan, be more suitable for life science and environment scientific research, the report of this respect is less.
The present invention adopts two step blending methods to carry out radical polymerization, has no report.
Summary of the invention
The object of the invention is to prepare shitosan surface molecule print club-shaped material, method is simple, and can prepare the material that shape-memory properties is good, is a kind of economic, efficient preparation method.
The present invention adopts two step blending methods to carry out free-radical polymerized: the preparation of (1) chitosan polymer microballoon: solvent, shitosan, monomer I, initator are fully mixed, the volume ratio of solvent and monomer I is 1:1～1:25, initiator content is 0.001～20% of monomer mass, logical N2, polymerization 1～30h under 10～150 DEG C of reaction temperatures, pressure 1～100 atmospheric pressure, is precipitated out in the calm agent of polymer that shitosan and monomer polymerization obtain, and forms nano-scale chitosan polymer microballoon emulsion; (2) preparation of surface molecule print club-shaped material: add monomer II, template molecule in emulsion, the volume ratio of emulsion and monomer II is 1:5～10:1, the mass ratio of template molecule and monomer II is 1:1～1:30, fully mix, sealing, sonic oscillation, put into insulating box polymerization 5～100h, obtain the surface molecule print club-shaped material that memory performance is good;
Described solvent is selected from the one in formic acid, acetic acid solution;
Described monomer I is selected from one or more mixtures in methyl methacrylate, EMA or butyl methacrylate;
Described monomer II is selected from the mixture of phosphoric acid ester and methyl methacrylate, EMA or butyl methacrylate;
Described initator is azodiisobutyronitrile, ABVN, persulfuric acid salt initator or their mixture;
Described template molecule is selected from the one in bovine serum albumin, human albumin, amino acids.
Reaction temperature in the present invention is 30～120 DEG C.
Pressure in the present invention is 1～80 atmospheric pressure.
The preparation feedback time of the chitosan polymer microballoon in the present invention is 2～20h; The preparation feedback time of described molecular engram club-shaped material is 10～80h.
The mass ratio of the template molecule in the present invention and monomer II is 1:1～1:15.
Brief description of the drawings
Fig. 1 bar-like shape memory material sample
The Recovery Process of Fig. 2 bar-like shape memory material
Detailed description of the invention
Embodiment 1
1.00g shitosan, 30mL3% acetic acid aqueous solution, stirs shitosan is dissolved, logical N2, add successively 8mL0.01g/mL ammonium persulfate solution and 4mL methyl methacrylate, copolyreaction 4h at 60 DEG C, cooling white emulsion. Add again 0.2g/L bovine serum albumin 10mL, 5mL tributyl phosphate and 10mL methyl methacrylate, sealing, supersonic oscillations, put into 70 DEG C of water-baths, and constant temperature copolymerization 48h, obtains bar polymers and is shape-memory material.
Embodiment 2
1.00g shitosan, 30mL3% acetic acid aqueous solution, stirs shitosan is dissolved, logical N2, add successively 15mL0.01g/mL ammonium persulfate solution and 10mL methyl methacrylate, copolyreaction 10h at 80 DEG C, cooling white emulsion. Add again 0.2g/L bovine serum albumin 15mL, 10mL tributyl phosphate and 20mL methyl methacrylate, sealing, supersonic oscillations, put into 90 DEG C of water-baths, and constant temperature copolymerization 55h, obtains bar polymers and is shape-memory material.
Embodiment 3
1.00g shitosan, 30mL3% acetic acid aqueous solution, stirs shitosan is dissolved, logical N2, add successively 4mL0.01g/mL ammonium persulfate solution and 15mL methyl methacrylate, copolyreaction 20h at 40 DEG C, cooling white emulsion. Add again 0.2g/L bovine serum albumin 6mL, 15mL tributyl phosphate and 25mL methyl methacrylate, sealing, supersonic oscillations, put into 60 DEG C of water-baths, and constant temperature copolymerization 35h, obtains bar polymers and is shape-memory material.
Embodiment 4
1.00g shitosan, 30mL3% aqueous formic acid, stirs shitosan is dissolved, logical N2, add successively azodiisobutyronitrile and the 25mL methyl methacrylate of 1mg, copolyreaction 25h at 60 DEG C, cooling white emulsion. Add again 0.2g/L human albumin 8mL, 10mL tributyl phosphate and 22mL methyl methacrylate, sealing, supersonic oscillations, put into 80 DEG C of water-baths, and constant temperature copolymerization 60h, obtains bar polymers and is shape-memory material.
Embodiment 5
1.00g shitosan, 30mL3% aqueous formic acid, stirs shitosan is dissolved, logical N2, add successively ABVN and the 20mL methyl methacrylate of 1mg, copolyreaction 30h at 80 DEG C, cooling white emulsion. Add again 0.2g/L human albumin 13mL, 8mL tributyl phosphate and 16mL methyl methacrylate, sealing, supersonic oscillations, put into 70 DEG C of water-baths, and constant temperature copolymerization 65h, obtains bar polymers and is shape-memory material.
Claims (5)
1. prepare a method for molecular engram club-shaped material, it is characterized in that adopting Raolical polymerizable and two step blending methods to prepare desirable molecular engram shape-memory material, concrete preparation process is as follows:
(1) preparation of chitosan polymer microballoon
Solvent, shitosan, monomer I, initator are fully mixed, and the volume ratio of solvent and monomer I is 1:1～1:25, and initiator content is 0.001～20% of monomer mass, logical N2, polymerization 1～30h under 10～150 DEG C of reaction temperatures, pressure 1～100 atmospheric pressure, is precipitated out in the calm agent of polymer that shitosan and monomer polymerization obtain, and forms nano-scale chitosan polymer microballoon emulsion;
(2) preparation of surface molecule print club-shaped material
In emulsion, add monomer II, template molecule, the volume ratio of emulsion and monomer II is 1:5～10:1, the mass ratio of template molecule and monomer II is 1:1～1:30, fully mix, sealing, sonic oscillation, put into insulating box polymerization 5～100h, obtain the surface molecule print club-shaped material that memory performance is good;
Described solvent is selected from the one in formic acid, acetic acid solution;
Described monomer I is selected from one or more mixtures in methyl methacrylate, EMA or butyl methacrylate;
Described monomer II is selected from the mixture of phosphoric acid ester and methyl methacrylate, EMA or butyl methacrylate;
Described initator is azodiisobutyronitrile, ABVN, persulfuric acid salt initator or their mixture;
Described template molecule is selected from the one in bovine serum albumin, human albumin, amino acids.
2. method according to claim 1, is characterized in that: described reaction temperature is 30～120 DEG C.
3. method according to claim 1, is characterized in that: described pressure is 1～80 atmospheric pressure.
4. method according to claim 1, is characterized in that: the preparation feedback time of described chitosan polymer microballoon is 2～20h; The preparation feedback time of described molecular engram club-shaped material is 10～80h.
5. method according to claim 1, is characterized in that: the mass ratio of described template molecule and monomer II is 1:1～1:15.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510572025.3A CN105601846B (en) | 2015-09-10 | 2015-09-10 | Chitosan surface molecule print club-shaped material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510572025.3A CN105601846B (en) | 2015-09-10 | 2015-09-10 | Chitosan surface molecule print club-shaped material |
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| CN105601846A true CN105601846A (en) | 2016-05-25 |
| CN105601846B CN105601846B (en) | 2018-01-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040003A (en) * | 2019-12-20 | 2020-04-21 | 扬州工业职业技术学院 | Chitosan oligosaccharide derivative molecular imprinting functional monomer and preparation method thereof |
| CN111732805A (en) * | 2020-06-28 | 2020-10-02 | 宣城市创道智能技术开发有限责任公司 | Chitosan-doped polyester material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101298039A (en) * | 2008-01-18 | 2008-11-05 | 清华大学 | Preparation of chitosan molecular imprinting adsorbing agent |
| CN102977334A (en) * | 2012-12-31 | 2013-03-20 | 贵州大学 | Molecularly imprinted polymer and preparation method and application thereof |
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2015
- 2015-09-10 CN CN201510572025.3A patent/CN105601846B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101298039A (en) * | 2008-01-18 | 2008-11-05 | 清华大学 | Preparation of chitosan molecular imprinting adsorbing agent |
| CN102977334A (en) * | 2012-12-31 | 2013-03-20 | 贵州大学 | Molecularly imprinted polymer and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| XUEFANG ZHENG ETAL: ""Aggregation of magnetic chitosan based nanoparticles and their application in controlled drug release"", 《RUSSIAN JOURANAL OF APPLIED CHEMISTRY》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040003A (en) * | 2019-12-20 | 2020-04-21 | 扬州工业职业技术学院 | Chitosan oligosaccharide derivative molecular imprinting functional monomer and preparation method thereof |
| CN111040003B (en) * | 2019-12-20 | 2023-03-14 | 扬州工业职业技术学院 | Chitosan oligosaccharide derivative molecular imprinting functional monomer and preparation method thereof |
| CN111732805A (en) * | 2020-06-28 | 2020-10-02 | 宣城市创道智能技术开发有限责任公司 | Chitosan-doped polyester material and preparation method thereof |
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| CN105601846B (en) | 2018-01-12 |
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Granted publication date: 20180112 Termination date: 20180910 |