CN105732992A - Preparation method of polyvinyl alcohol-poly trimethylene carbonate-polydioxanone double-graft copolymer - Google Patents
Preparation method of polyvinyl alcohol-poly trimethylene carbonate-polydioxanone double-graft copolymer Download PDFInfo
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- CN105732992A CN105732992A CN201610108639.0A CN201610108639A CN105732992A CN 105732992 A CN105732992 A CN 105732992A CN 201610108639 A CN201610108639 A CN 201610108639A CN 105732992 A CN105732992 A CN 105732992A
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- Prior art keywords
- polyvinyl alcohol
- preparation
- ptmc
- ppdo
- graft copolymer
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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
Abstract
The invention discloses a preparation method of a polyvinyl alcohol-poly trimethylene carbonate-polydioxanone double-graft copolymer. The preparation method comprises the following steps: adding polyvinyl alcohol, carboxyl-terminated poly trimethylene carbonate monododecyl ether, carboxyl-terminated polydioxanone monotridecyl ether, a solvent and a condensing agent into a dry reactor, stirring for reaction for 2-4 days at a temperature of 28-32 DEG C under inert atmosphere, terminating the reaction, and carrying out filtering, dialysis and drying to obtain a target object. The preparation method disclosed by the invention has the advantages that the preparation process is simple, and easy to master, and the target object obtained is a novel degradable biomaterial.
Description
Technical field
The present invention relates to the preparation method of a kind of polyvinyl alcohol-PTMC-PPDO dual graft copolymer, belong 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 and pharmacology aspect.PTMC and PPDO are to have the biomaterial of excellent biocompatibility and biodegradability, have good hydrophobicity, have a wide range of applications at medicine.PTMC segment, PPDO segment are grafted on polyvinyl alcohol molecule chain obtained polyvinyl alcohol-PTMC-PPDO dual graft copolymer set polyvinyl alcohol, PTMC and the advantage of PPDO three simultaneously, it is a kind of to there is amphipathic novel degradable biomaterial, certainly will have a good application prospect in terms of 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 preparation method of the preferable polyvinyl alcohol-PTMC of effect-PPDO dual graft copolymer.Its technical scheme is:
A kind of preparation method of polyvinyl alcohol-PTMC-PPDO dual graft copolymer, it is characterized in that: in copolymer, the molecular weight of polyvinyl alcohol segments is 43000～52000, the molecular weight of PTMC segment is 2200～2300, and the molecular weight of PPDO segment is 2200～2300；Its preparation method is as follows:
Polyvinyl alcohol, the PTMC monododecyl ether of carboxy blocking, PPDO list tridecyl ether, solvent and the condensing agent of carboxy blocking is added in dry reactor, under inert atmosphere, in 28～32 DEG C of stirring reactions 2～4 days, terminate reaction, by filtering, dialysing, it is dried, obtains object.
The preparation method of described a kind of polyvinyl alcohol-PTMC-PPDO dual graft copolymer, PTMC monododecyl ether is 15～25:1 with the mol ratio of polyvinyl alcohol, and PPDO list tridecyl ether is 15～25:1 with the mol ratio of polyvinyl alcohol.
The preparation method of described a kind of polyvinyl alcohol-PTMC-PPDO dual graft copolymer, condensing agent usesN,N ’-dicyclohexylcarbodiimide,N,N ’-DIC or 3-ethyl-1-(3-dimethylaminopropyl) carbodiimide, condensing agent is 1.08～1.8:1 with the mol ratio of polyvinyl alcohol, and solvent uses dimethyl sulfoxide, and reactant solution concentration is 5～15 g:100 ml.
Compared with prior art, its advantage is the present invention:
1, the preparation method of described a kind of polyvinyl alcohol-PTMC-PPDO dual graft copolymer, uses 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-PTMC-PPDO dual graft copolymer is a kind of novel degradable biomaterial.
Detailed description of the invention
Embodiment
1
12.2 grams of polyvinyl alcohol (molecular weight is 43000), the PTMC monododecyl ether (molecular weight is 2200) of 11.5 grams of carboxy blockings and the PPDO list tridecyl ether (molecular weight is 2200) of 11.5 grams of carboxy blockings is added at dry reactor, add 325 ml dimethyl sulfoxide, add 0.075 gramN,N ’-dicyclohexylcarbodiimide, under inert atmosphere, in 28 DEG C of stirring reactions 2 days, terminates reaction, by filtering, dialysing, is dried, obtains object.
Embodiment
2
13.3 grams of polyvinyl alcohol (molecular weight is 47000), the PTMC monododecyl ether (molecular weight is 2200) of 11.6 grams of carboxy blockings and the PPDO list tridecyl ether (molecular weight is 2200) of 11.6 grams of carboxy blockings is added at dry reactor, add 335 ml dimethyl sulfoxide, add 0.044 gramN,N ’-DIC, under inert atmosphere, in 30 DEG C of stirring reactions 3 days, terminates reaction, by filtering, dialysing, is dried, obtains object.
Embodiment
3
14.3 grams of polyvinyl alcohol (molecular weight is 52000), the PTMC monododecyl ether (molecular weight is 2300) of 11.9 grams of carboxy blockings and the PPDO list tridecyl ether (molecular weight is 2300) of 11.9 grams of carboxy blockings is added at dry reactor, add 348 ml dimethyl sulfoxide, add 0.067 gram of 3-ethyl-1-(3-dimethylaminopropyl) carbodiimide, under inert atmosphere, in 32 DEG C of stirring reactions 4 days, terminate reaction, by filtering, dialysing, it is dried, obtains object.
Claims (3)
1. the preparation method of polyvinyl alcohol-PTMC-PPDO dual graft copolymer, it is characterized in that: in copolymer, the molecular weight of polyvinyl alcohol segments is 43000～52000, the molecular weight of PTMC segment is 2200～2300, and the molecular weight of PPDO segment is 2200～2300；Its preparation method is as follows:
Polyvinyl alcohol, the PTMC monododecyl ether of carboxy blocking, PPDO list tridecyl ether, solvent and the condensing agent of carboxy blocking is added in dry reactor, under inert atmosphere, in 28～32 DEG C of stirring reactions 2～4 days, terminate reaction, by filtering, dialysing, it is dried, obtains object.
The preparation method of a kind of polyvinyl alcohol-PTMC-PPDO dual graft copolymer the most according to claim 1, it is characterized in that: PTMC monododecyl ether is 15～25:1 with the mol ratio of polyvinyl alcohol, PPDO list tridecyl ether is 15～25:1 with the mol ratio of polyvinyl alcohol.
The preparation method of a kind of polyvinyl alcohol-PTMC-PPDO dual graft copolymer the most according to claim 1, it is characterised in that: condensing agent usesN,N’-dicyclohexylcarbodiimide,N,N’-DIC or 3-ethyl-1-(3-dimethylaminopropyl) carbodiimide, condensing agent is 1.08～1.8:1 with the mol ratio of polyvinyl alcohol, and solvent uses dimethyl sulfoxide, and reactant solution concentration is 5～15 g:100 ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610108639.0A CN105732992B (en) | 2016-02-29 | 2016-02-29 | A kind of preparation method of polyvinyl alcohol-polytrimethylene carbonate-polydioxanone dual graft copolymer |
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| CN201610108639.0A CN105732992B (en) | 2016-02-29 | 2016-02-29 | A kind of preparation method of polyvinyl alcohol-polytrimethylene carbonate-polydioxanone dual graft copolymer |
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| CN105732992A true CN105732992A (en) | 2016-07-06 |
| CN105732992B CN105732992B (en) | 2019-02-19 |
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| CN201610108639.0A Expired - Fee Related CN105732992B (en) | 2016-02-29 | 2016-02-29 | A kind of preparation method of polyvinyl alcohol-polytrimethylene carbonate-polydioxanone dual graft copolymer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107011673A (en) * | 2017-05-22 | 2017-08-04 | 山东理工大学 | A kind of method that PTMC improves polypropylene sorrel water resistance and compliance with PPDO |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881398A (en) * | 2014-03-24 | 2014-06-25 | 山东理工大学 | Method for improving water resistance of polyvinyl alcohol film by using poly(trimethylene carbonate) and poly(p-dioxanone) |
| 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 |
| CN104559213A (en) * | 2015-01-06 | 2015-04-29 | 山东理工大学 | Method for improving hydrophily and flexibility of polypeptide membrane by poly(trimethylene carbonate) and polyethylene glycol |
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2016
- 2016-02-29 CN CN201610108639.0A patent/CN105732992B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881398A (en) * | 2014-03-24 | 2014-06-25 | 山东理工大学 | Method for improving water resistance of polyvinyl alcohol film by using poly(trimethylene carbonate) and poly(p-dioxanone) |
| 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 |
| CN104559213A (en) * | 2015-01-06 | 2015-04-29 | 山东理工大学 | Method for improving hydrophily and flexibility of polypeptide membrane by poly(trimethylene carbonate) and polyethylene glycol |
Non-Patent Citations (1)
| Title |
|---|
| 朱国全等: "《聚乙烯醇／聚氨酯共混薄膜制备及性能研究》", 《山东理工大学学报（自然科学版）》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107011673A (en) * | 2017-05-22 | 2017-08-04 | 山东理工大学 | A kind of method that PTMC improves polypropylene sorrel water resistance and compliance with PPDO |
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