CN105694057A - Method for preparing polyving akohol-polycaprolactone-poly(p-dioxanone) double graft copolymer - Google Patents
Method for preparing polyving akohol-polycaprolactone-poly(p-dioxanone) double graft copolymer Download PDFInfo
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- CN105694057A CN105694057A CN201610108630.XA CN201610108630A CN105694057A CN 105694057 A CN105694057 A CN 105694057A CN 201610108630 A CN201610108630 A CN 201610108630A CN 105694057 A CN105694057 A CN 105694057A
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- Prior art keywords
- polycaprolactone
- polyvinyl alcohol
- ppdo
- graft copolymer
- preparation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
- C08G81/02—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers at least one of the polymers being obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C08G81/024—Block or graft polymers containing sequences of polymers of C08C or C08F and of polymers of C08G
- C08G81/027—Block or graft polymers containing sequences of polymers of C08C or C08F and of polymers of C08G containing polyester or polycarbonate sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2230/00—Compositions for preparing biodegradable polymers
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Biological Depolymerization Polymers (AREA)
- Graft Or Block Polymers (AREA)
Abstract
The invention discloses a method for preparing a polyving akohol-polycaprolactone-poly(p-dioxanone) double graft copolymer. The method comprises the steps of adding polyving akohol, carboxyl end capped polycaprolactone mono dodecyl ether, carboxyl end capped poly(p-dioxanone) mono undecyl ether, solvent and condensing agent into a dry reactor for stirring reaction lasting 2-3 days at 28-34 DEG C in the inert atmosphere, stopping reaction, and obtaining the target product through filtration, dialysis and drying. The preparing process is simple and easy to grasp, and the target product is a novel degradable biological material.
Description
Technical field
The preparation method that the present invention relates to a kind of polyvinyl alcohol-polycaprolactone-PPDO dual graft copolymer, belongs to biodegradated polymer materal preparing technical field。
Background technology
Polyvinyl alcohol is a kind of biomaterial with good biocompatibility and biodegradability, has excellent hydrophilic, is widely used in medicine。Polycaprolactone and PPDO are to have the biomaterial of good biocompatibility and biodegradability, have good hydrophobicity, have a wide range of applications at medicine。Polyvinyl alcohol-polycaprolactone-PPDO dual graft copolymer set that to be grafted on polyvinyl alcohol molecule chain by polycaprolactone segment, PPDO segment obtained simultaneously advantage of polyvinyl alcohol, polycaprolactone and PPDO three, it is a kind of there is amphipathic novel degradable biomaterial, certainly will have a good application prospect in preparing sustained-release drug carrier。
Summary of the invention
It is an object of the invention to provide a kind of simple to operate and the good polyvinyl alcohol-polycaprolactone of effect-PPDO dual graft copolymer preparation method。Its technical scheme is:
A kind of preparation method of polyvinyl alcohol-polycaprolactone-PPDO dual graft copolymer, it is characterized in that: in copolymer, the molecular weight of polyvinyl alcohol segments is 42000～51000, the molecular weight of polycaprolactone segment is 2100～2400, and the molecular weight of PPDO segment is 2100～2400；Its preparation method is as follows:
Polyvinyl alcohol, the polycaprolactone monododecyl ether of carboxy blocking, the PPDO list undecyl ether of carboxy blocking, solvent and condensing agent is added in dry reactor, under inert atmosphere, in 28～34 DEG C of stirring reactions 2～3 days, terminate reaction, by filtering, dialyse, drying, obtain object。
The preparation method of described a kind of polyvinyl alcohol-polycaprolactone-PPDO dual graft copolymer, the mol ratio of polycaprolactone monododecyl ether and polyvinyl alcohol is 15～25:1, and the mol ratio of PPDO list undecyl ether and polyvinyl alcohol is 15～25:1。
The preparation method of described a kind of polyvinyl alcohol-polycaprolactone-PPDO dual graft copolymer, condensing agent adoptsN,N’-dicyclohexylcarbodiimide,N,N’-DIC or 3-ethyl-1-(3-dimethylaminopropyl) carbodiimide, the mol ratio of condensing agent and polyvinyl alcohol is 1.07～1.8:1, and solvent adopts dimethyl sulfoxide, and reactant solution concentration is 5～15g:100ml。
Compared with prior art, its advantage is the present invention:
1, the preparation method of described a kind of polyvinyl alcohol-polycaprolactone-PPDO dual graft copolymer, adopts a kind of polymer and two kinds of different polymeric monomer to carry out the means of esterification simultaneously, simple to operate, be prone to grasp；
2, described a kind of polyvinyl alcohol-polycaprolactone-PPDO dual graft copolymer is a kind of novel degradable biomaterial。
Detailed description of the invention
Embodiment 1
The PPDO list undecyl ether (molecular weight is 2100) of 12.1 grams of polyvinyl alcohol (molecular weight is 42000), the polycaprolactone monododecyl ether (molecular weight is 2100) of 11.1 grams of carboxy blockings and 11.1 grams of carboxy blockings is added at dry reactor, add 315ml dimethyl sulfoxide, add 0.075 gramN,N’-dicyclohexylcarbodiimide, under inert atmosphere, in 28 DEG C of stirring reactions 2 days, terminates reaction, by filtering, dialysis, dry, obtains object。
Embodiment 2
The PPDO list undecyl ether (molecular weight is 2200) of 13.2 grams of polyvinyl alcohol (molecular weight is 47000), the polycaprolactone monododecyl ether (molecular weight is 2200) of 11.3 grams of carboxy blockings and 11.3 grams of carboxy blockings is added at dry reactor, add 328ml dimethyl sulfoxide, add 0.043 gramN,N’-DIC, under inert atmosphere, in 30 DEG C of stirring reactions 2 days, terminates reaction, by filtering, dialysis, dry, obtains object。
Embodiment 3
The PPDO list undecyl ether (molecular weight is 2400) of 14.1 grams of polyvinyl alcohol (molecular weight is 51000), the polycaprolactone monododecyl ether (molecular weight is 2400) of 12.2 grams of carboxy blockings and 12.2 grams of carboxy blockings is added at dry reactor, add 345ml dimethyl sulfoxide, add 0.065 gram of 3-ethyl-1-(3-dimethylaminopropyl) carbodiimide, under inert atmosphere, in 34 DEG C of stirring reactions 3 days, terminate reaction, by filtering, dialyse, drying, obtain object。
Claims (3)
1. the preparation method of polyvinyl alcohol-polycaprolactone-PPDO dual graft copolymer, it is characterized in that: in copolymer, the molecular weight of polyvinyl alcohol segments is 42000～51000, the molecular weight of polycaprolactone segment is 2100～2400, and the molecular weight of PPDO segment is 2100～2400；Its preparation method is as follows:
Polyvinyl alcohol, the polycaprolactone monododecyl ether of carboxy blocking, the PPDO list undecyl ether of carboxy blocking, solvent and condensing agent is added in dry reactor, under inert atmosphere, in 28～34 DEG C of stirring reactions 2～3 days, terminate reaction, by filtering, dialyse, drying, obtain object。
2. the preparation method of a kind of polyvinyl alcohol-polycaprolactone-PPDO dual graft copolymer according to claim 1, it is characterized in that: the mol ratio of polycaprolactone monododecyl ether and polyvinyl alcohol is 15～25:1, the mol ratio of PPDO list undecyl ether and polyvinyl alcohol is 15～25:1。
3. the preparation method of a kind of polyvinyl alcohol-polycaprolactone-PPDO dual graft copolymer according to claim 1, it is characterised in that: condensing agent adoptsN,N’-dicyclohexylcarbodiimide,N,N’-DIC or 3-ethyl-1-(3-dimethylaminopropyl) carbodiimide, the mol ratio of condensing agent and polyvinyl alcohol is 1.07～1.8:1, and solvent adopts dimethyl sulfoxide, and reactant solution concentration is 5～15g:100ml。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610108630.XA CN105694057A (en) | 2016-02-29 | 2016-02-29 | Method for preparing polyving akohol-polycaprolactone-poly(p-dioxanone) double graft copolymer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610108630.XA CN105694057A (en) | 2016-02-29 | 2016-02-29 | Method for preparing polyving akohol-polycaprolactone-poly(p-dioxanone) double graft copolymer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105694057A true CN105694057A (en) | 2016-06-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610108630.XA Pending CN105694057A (en) | 2016-02-29 | 2016-02-29 | Method for preparing polyving akohol-polycaprolactone-poly(p-dioxanone) double graft copolymer |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103865091A (en) * | 2014-03-24 | 2014-06-18 | 山东理工大学 | Method for improving water resisting performance of polyvinyl alcohol film from polycaprolactone and polylactic acid |
| CN104479158A (en) * | 2015-01-06 | 2015-04-01 | 山东理工大学 | Method for improving hydrophilia and flexibility of polypeptide membrane through polydioxanone and polyethylene glycol |
| CN104559219A (en) * | 2015-01-12 | 2015-04-29 | 山东理工大学 | Method for improving hydrophilicity and flexibility of polypeptide film by polycaprolactone and waterborne polyurethane |
-
2016
- 2016-02-29 CN CN201610108630.XA patent/CN105694057A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103865091A (en) * | 2014-03-24 | 2014-06-18 | 山东理工大学 | Method for improving water resisting performance of polyvinyl alcohol film from polycaprolactone and polylactic acid |
| CN104479158A (en) * | 2015-01-06 | 2015-04-01 | 山东理工大学 | Method for improving hydrophilia and flexibility of polypeptide membrane through polydioxanone and polyethylene glycol |
| CN104559219A (en) * | 2015-01-12 | 2015-04-29 | 山东理工大学 | Method for improving hydrophilicity and flexibility of polypeptide film by polycaprolactone and waterborne polyurethane |
Non-Patent Citations (1)
| Title |
|---|
| 胡跃飞等: "《现代有机合成试剂 性质、制备和反应》", 31 July 2006 * |
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Application publication date: 20160622 |