CN105601846B - Chitosan surface molecule print club-shaped material - Google Patents
Chitosan surface molecule print club-shaped material Download PDFInfo
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- CN105601846B CN105601846B CN201510572025.3A CN201510572025A CN105601846B CN 105601846 B CN105601846 B CN 105601846B CN 201510572025 A CN201510572025 A CN 201510572025A CN 105601846 B CN105601846 B CN 105601846B
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Abstract
The present invention is prepared for a kind of chitosan surface molecule print club-shaped material, and solvent, chitosan, monomer I, initiator are sufficiently mixed, and the volume ratio of solvent and monomer I is 1:1~1:25, initiator content is the 0.001~20% of monomer mass, leads to N2, 1~30h is polymerize under 10~150 DEG C of reaction temperature, the atmospheric pressure of pressure 1~100, is precipitated out in the calm agent of polymer that chitosan polymerize to obtain with monomer, forms nano-scale chitosan polymer microballoon 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, it is sufficiently mixed, sealing, sonic oscillation, is put into 5~100h of polymerization in insulating box, obtains the good surface molecule print club-shaped material of memory performance.Club-shaped material prepared by this method is widely used in terms of the specific recognition to target molecule.
Description
Technical field
The present invention relates to a kind of method for preparing chitosan molecule trace shape memory club-shaped material.
Background technology
Molecularly imprinted polymer is a kind of adsorbing separation material to To Template molecule with specific selectivity recognition capability
Material, in liquid chromatogram, biology sensor, SPE, the good application prospect that many fields have such as catalyze and synthesize.Wherein
Molecular engram microsphere (MIMs) due to prepare and using relatively convenient, chromatographic efficiency is high and is easy to Functional Design, in recent years gradually into
For the focus of research.Surface grafting technology is that the imprinted layer with recognition site is incorporated in stromal surface by occur in recent years a kind of
Novel surface engram technology, using chitose graft copolymer as carrier, utilize the biocompatibility and readily degradable of chitosan
Can, life science and environment scientific research is more suitable for, the report of this respect is less.
The present invention carries out radical polymerization using two step blending methods, has no report.
The content of the invention
The purpose of the present invention is to prepare chitosan surface molecule print club-shaped material, and method is simple, and can prepare shape
The good material of memory performance, it is a kind of economic, efficient preparation method.
The present invention is carried out free-radical polymerized using two step blending methods：(1) preparation of chitosan polymer microballoon：By solvent,
Chitosan, monomer I, initiator are sufficiently mixed, and the volume ratio of solvent and monomer I is 1:1~1:25, initiator content is monomer matter
The 0.001~20% of amount, lead to N2, 1~30h, chitosan are polymerize under 10~150 DEG C of reaction temperature, the atmospheric pressure of pressure 1~100
It is precipitated out in the calm agent of polymer for polymerizeing to obtain with monomer, forms nano-scale chitosan polymer microballoon emulsion；(2) surface
The preparation of molecular engram club-shaped material：The volume ratio of addition monomer II, template molecule into emulsion, emulsion and monomer II is 1:5
~10:1, the mass ratio of template molecule and monomer II is 1:1~1:30, it is sufficiently mixed, sealing, sonic oscillation, is put into insulating box
5~100h of middle polymerization, obtain the good surface molecule print club-shaped material of memory performance；
The one kind of the solvent in formic acid, acetic acid solution；
One kind in methyl methacrylate, EMA or butyl methacrylate of the monomer I or
More than one mixtures；
The monomer II is selected from phosphoric acid ester and methyl methacrylate, EMA or butyl methacrylate
Mixture；
The initiator is azodiisobutyronitrile, ABVN, persulfuric acid salt initiator or their mixture；
The one kind of the template molecule 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 reaction time of chitosan polymer microballoon in the present invention is 2~20h；The molecular engram club-shaped material
The preparation reaction time be 10~80h.
The mass ratio of template molecule and monomer II in the present invention is 1:1~1:15.
Brief description of the drawings
Fig. 1 bar-like shape memory material samples
The Recovery Process of Fig. 2 bar-like shape memory materials
Embodiment
Embodiment 1
1.00g chitosans, 30mL3% acetic acid aqueous solutions, stirring dissolve chitosan, lead to N2, sequentially add 8mL
0.01g/mL ammonium persulfate solutions and 4mL methyl methacrylates, copolyreaction 4h at 60 DEG C, cool down to obtain white emulsion.Again
0.2g/L bovine serum albumin 10mL, 5mL tributyl phosphates and 10mL methyl methacrylates are added, sealing, supersonic oscillations, is put
Enter 70 DEG C of water-baths, constant temperature copolymerization 48h, it is shape-memory material to obtain bar polymers.
Embodiment 2
1.00g chitosans, 30mL3% acetic acid aqueous solutions, stirring dissolve chitosan, lead to N2, sequentially add 15mL
0.01g/mL ammonium persulfate solutions and 10mL methyl methacrylates, copolyreaction 10h at 80 DEG C, cool down to obtain white emulsion.
0.2g/L bovine serum albumin 15mL, 10mL tributyl phosphates and 20mL methyl methacrylates are added, is sealed, ultrasonic wave shakes
Swing, be put into 90 DEG C of water-baths, constant temperature copolymerization 55h, it is shape-memory material to obtain bar polymers.
Embodiment 3
1.00g chitosans, 30mL3% acetic acid aqueous solutions, stirring dissolve chitosan, lead to N2, sequentially add 4mL
0.01g/mL ammonium persulfate solutions and 15mL methyl methacrylates, copolyreaction 20h at 40 DEG C, cool down to obtain white emulsion.
0.2g/L bovine serum albumin 6mL, 15mL tributyl phosphates and 25mL methyl methacrylates are added, is sealed, supersonic oscillations,
60 DEG C of water-baths are put into, constant temperature copolymerization 35h, it is shape-memory material to obtain bar polymers.
Embodiment 4
1.00g chitosans, 30mL3% aqueous formic acids, stirring dissolve chitosan, lead to N2, sequentially add 1mg azo
Bis-isobutyronitrile and 25mL methyl methacrylates, copolyreaction 25h at 60 DEG C, cool down to obtain white emulsion.Add 0.2g/L
Human albumin 8mL, 10mL tributyl phosphate and 22mL methyl methacrylates, sealing, supersonic oscillations, are put into 80 DEG C of water-baths
Pot, constant temperature copolymerization 60h, it is shape-memory material to obtain bar polymers.
Embodiment 5
1.00g chitosans, 30mL3% aqueous formic acids, stirring dissolve chitosan, lead to N2, sequentially add 1mg azo
Two different heptonitrile and 20mL methyl methacrylates, copolyreaction 30h at 80 DEG C, cool down to obtain white emulsion.Add 0.2g/L
Human albumin 13mL, 8mL tributyl phosphate and 16mL methyl methacrylates, sealing, supersonic oscillations, are put into 70 DEG C of water-baths
Pot, constant temperature copolymerization 65h, it is shape-memory material to obtain bar polymers.
Claims (5)
- A kind of 1. method for preparing molecular engram club-shaped material, it is characterized in that legal system is blended using Raolical polymerizable and two steps Standby preferable molecular engram shape-memory material, specific preparation process are as follows：(1) preparation of chitosan polymer microballoonSolvent, chitosan, monomer I, initiator are sufficiently mixed, the volume ratio of solvent and monomer I is 1:1~1:25, initiator Content is the 0.001~20% of monomer mass, leads to N2, it polymerize 1 under 10~150 DEG C of reaction temperature, the atmospheric pressure of pressure 1~100 ~30h, the polymer that chitosan polymerize to obtain with monomer are precipitated out from solvent, form nano-scale chitosan polymer microballoon Emulsion；(2) preparation of surface molecule print club-shaped materialThe volume ratio of addition monomer II, template molecule into emulsion, emulsion and monomer II is 1:5~10:1, template molecule and list The mass ratio of body II is 1:1~1:30, it is sufficiently mixed, sealing, sonic oscillation, is put into 5~100h of polymerization in insulating box, is remembered Recall surface molecule print club-shaped material of good performance；The one kind of the solvent in formic acid, acetic acid solution；The one kind or one kind of the monomer I in methyl methacrylate, EMA or butyl methacrylate Thing mixed above；The monomer II be selected from phosphoric acid ester and methyl methacrylate, EMA or butyl methacrylate it is mixed Compound；The initiator is azodiisobutyronitrile, ABVN, persulfuric acid salt initiator or their mixture；The one kind of the template molecule in bovine serum albumin, human albumin, amino acids.
- 2. method according to claim 1, it is characterized in that：The reaction temperature is 30~120 DEG C.
- 3. method according to claim 1, it is characterized in that：The pressure is 1~80 atmospheric pressure.
- 4. method according to claim 1, it is characterized in that：The preparation reaction time of the chitosan polymer microballoon is 2~ 20h；The preparation reaction time of the molecular engram club-shaped material is 10~80h.
- 5. method according to claim 1, it is characterized in that：The mass ratio of the 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 |
|---|---|---|---|
| CN201510572025.3A CN105601846B (en) | 2015-09-10 | 2015-09-10 | Chitosan surface molecule print club-shaped material |
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| Publication Number | Publication Date |
|---|---|
| CN105601846A CN105601846A (en) | 2016-05-25 |
| CN105601846B true CN105601846B (en) | 2018-01-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510572025.3A Expired - Fee Related CN105601846B (en) | 2015-09-10 | 2015-09-10 | Chitosan surface molecule print club-shaped material |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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 |
-
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 |
|---|
| "Aggregation of magnetic chitosan based nanoparticles and their application in controlled drug release";Xuefang Zheng etal;《Russian jouranal of applied chemistry》;20150625;第88卷(第3期);524-528 * |
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| CN105601846A (en) | 2016-05-25 |
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