CN106987129A - A kind of MPEGPLA is with gathering（Lactide glycolide）The method for improving polypropylene sorrel water resistance and compliance - Google Patents
A kind of MPEGPLA is with gathering（Lactide glycolide）The method for improving polypropylene sorrel water resistance and compliance Download PDFInfo
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- CN106987129A CN106987129A CN201710362664.6A CN201710362664A CN106987129A CN 106987129 A CN106987129 A CN 106987129A CN 201710362664 A CN201710362664 A CN 201710362664A CN 106987129 A CN106987129 A CN 106987129A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L87/00—Compositions of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
- C08L87/005—Block or graft polymers not provided for in groups C08L1/00 - C08L85/04
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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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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2387/00—Characterised by the use of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The present invention discloses a kind of MPEGPLA with gathering（Lactide glycolide）The method for improving polypropylene sorrel water resistance and compliance, using following steps：1）The synthesis of polyacrylic acid MPEGPLA graft copolymers：Add hydroxy-end capped MPEGPLA, solvent, condensing agent and polyacrylic acid in dry reactor, stirring reaction 2~3 days, terminating reaction obtains object；2）MPEGPLA is with gathering（Lactide glycolide）The preparation of modified polypropylene sorrel：Polyacrylic acid MPEGPLA graft copolymers are added in dry reactor, are gathered（Lactide glycolide）Monododecyl ether and solvent, after stirring is mixed 50~60 minutes, with the tape casting film forming and drying, obtain object of the present invention.Preparation technology of the present invention is simple, be easy to grasp, and gained Modified Membrane water resistance and compliance are greatly improved.
Description
Technical field
The present invention relates to a kind of method being improved to polypropylene sorrel water resistance and compliance, belong to thin polymer film
Preparing technical field.
Background technology
Polyacrylic acid is a kind of biomaterial with good biocompatibility and biodegradability, polypropylene sorrel
It can be used as artificial skin etc., but polypropylene sorrel hydrophily is too strong and more stiff, lacks preferable water resistance and compliance, so that
Its application is limited to a certain extent.MPEGPLA（The weight ratio of polyethylene glycol and PLA is 10/90）With it is poly-（D, L- third is handed over
Ester-glycolide）（The weight ratio of lactide and glycolide is 90/10）It is with excellent biocompatibility and biodegradability
Biomaterial, with good hydrophobicity and compliance.MPEGPLA segments are first introduced into polyacrylic acid segment formation polypropylene
Acid-MPEGPLA graft copolymers, then again will be poly-（Lactide coglycolide）Segment adds polyacrylic acid-MPEGPLA grafting altogether
Polymers formation blend, is made modified polypropene sorrel, so as to drastically increase the water resistance and compliance of polypropylene sorrel.
The content of the invention
It is preferable to polypropylene sorrel water resistance and submissive it is an object of the invention to provide a kind of simple to operate and effect
The method that property is improved.Its technical scheme is：
A kind of MPEGPLA is with gathering（Lactide coglycolide）The method for improving polypropylene sorrel water resistance and compliance, its feature exists
In：In Modified Membrane the molecular weight of polyacrylic acid segment be the molecular weight of 81000~89000, MPEGPLA segments be 2400~
2500, gather（Lactide coglycolide）The molecular weight of segment is 5200~6000；Its method of modifying uses following steps：
1）The synthesis of polyacrylic acid-MPEGPLA graft copolymers：Hydroxy-end capped MPEGPLA is added in dry reactor, it is molten
Under agent, condensing agent and polyacrylic acid, inert atmosphere, in 28~34 DEG C of stirring reactions 2~3 days, terminating reaction, by filtering, thoroughly
Analyse, dry, obtain object；
2）MPEGPLA is with gathering（Lactide coglycolide）The preparation of modified polypropylene sorrel：Poly- third is added in dry reactor
It is olefin(e) acid-MPEGPLA graft copolymers, poly-（Lactide coglycolide）Under monododecyl ether and solvent, inert atmosphere, in 46~
After 52 DEG C of stirrings are mixed 50~60 minutes, with the tape casting film forming and drying, object is obtained.
A kind of described MPEGPLA is with gathering（Lactide coglycolide）Improve the side of polypropylene sorrel water resistance and compliance
Method, step 1）In, MPEGPLA is poly- using mono methoxy polyethylene glycol（D,L）Lactic acid copolymer（The weight of polyethylene glycol and PLA
Amount is than being 10/90）, the mol ratio of MPEGPLA and polyacrylic acid is 15~25:1.
A kind of described MPEGPLA is with gathering（Lactide coglycolide）Improve the side of polypropylene sorrel water resistance and compliance
Method, step 1）In, condensing agent is usedN,N’- dicyclohexylcarbodiimide,N,N’- DIC or 3- ethyls -1-
（3- dimethylaminopropyls）The mol ratio of carbodiimide, condensing agent and polyacrylic acid is 1.08~1.9:1, solvent is sub- using dimethyl
Sulfone, reactant solution concentration is 5~15 g:100 ml.
A kind of described MPEGPLA is with gathering（Lactide coglycolide）Improve the side of polypropylene sorrel water resistance and compliance
Method, step 2）In, gather（Lactide coglycolide）Monododecyl ether is using poly-（D, L- lactide coglycolide）Single dodecyl
Ether（The weight ratio of lactide and glycolide is 90/10）, gather（Lactide coglycolide）Matter of the monododecyl ether in Modified Membrane
It is 2~4% to measure percentage, and solvent uses dimethyl sulfoxide (DMSO), and mixture solution concentration is 25~30 g:100 ml.
Compared with prior art, its advantage is the present invention：
1st, a kind of described MPEGPLA is with gathering（Lactide coglycolide）The method for improving polypropylene sorrel water resistance and compliance,
Using esterification and blending two kinds of means, it is simple to operate, be easy to grasp；
2nd, described polyacrylic acid modified film water resistance and compliance are enhanced.
Embodiment
Embodiment 1
1）The preparation of polyacrylic acid-MPEGPLA graft copolymers
19.6 grams of polyacrylic acid are added in dry reactor（Molecular weight is 81000）With 10.8 grams of hydroxy-end capped MPEGPLA
（Molecular weight is 2400）, 293 ml dimethyl sulfoxide (DMSO)s are added, 0.063 gram is addedN,N’- dicyclohexylcarbodiimide, indifferent gas
Under atmosphere, in 28 DEG C of stirring reactions 2 days, terminating reaction by filtering, dialysis, was dried, obtains object；
2）MPEGPLA is with gathering（Lactide coglycolide）The preparation of modified polypropylene sorrel
10 grams of polyacrylic acid-MPEGPLA graft copolymers and 37 ml dimethyl sulfoxide solvents are added in dry reactor, separately
Add and account for the poly- of Modified Membrane gross weight 2%（Lactide coglycolide）Monododecyl ether（Molecular weight is 5200）, under inert atmosphere,
Mixed 50 minutes in 46 DEG C of stirrings, use the tape casting film forming, object is dried to obtain in 50 DEG C of vacuum drying chambers.
After tested：The surface contact angle and its elongation at break of object and water of the present invention respectively than improving before modified
12.4 ° and 9.1%.
Embodiment 2
1）The preparation of polyacrylic acid-MPEGPLA graft copolymers
21.1 grams of polyacrylic acid are added in dry reactor（Molecular weight is 85000）With 11.3 grams of hydroxy-end capped MPEGPLA
（Molecular weight is 2400）, 322 ml dimethyl sulfoxide (DMSO)s are added, 0.039 gram is addedN,N’- DIC, indifferent gas
Under atmosphere, in 30 DEG C of stirring reactions 3 days, terminating reaction by filtering, dialysis, was dried, obtains object；
2）MPEGPLA is with gathering（Lactide coglycolide）The preparation of modified polypropylene sorrel
9.9 grams of polyacrylic acid-MPEGPLA graft copolymers and 36.5 ml dimethyl sulfoxide solvents are added in dry reactor,
Another add accounts for the poly- of Modified Membrane gross weight 3%（Lactide coglycolide）Monododecyl ether（Molecular weight is 5500）, inert atmosphere
Under, mixed 55 minutes in 48 DEG C of stirrings, use the tape casting film forming, object is dried to obtain in 50 DEG C of vacuum drying chambers.
After tested：The surface contact angle and its elongation at break of object and water of the present invention respectively than improving before modified
12.8 ° and 9.5%.
Embodiment 3
1）The preparation of polyacrylic acid-MPEGPLA graft copolymers
21.4 grams of polyacrylic acid are added in dry reactor（Molecular weight is 89000）With 11.3 grams of hydroxy-end capped MPEGPLA
（Molecular weight is 2500）, 323 ml dimethyl sulfoxide (DMSO)s are added, 0.058 gram of 3- ethyls -1- is added（3- dimethylaminopropyls）Carbon two
Under imines, inert atmosphere, in 34 DEG C of stirring reactions 2 days, terminating reaction by filtering, dialysis, was dried, obtains object；
2）MPEGPLA is with gathering（Lactide coglycolide）The preparation of modified polypropylene sorrel
9.5 grams of polyacrylic acid-MPEGPLA graft copolymers and 35 ml dimethyl sulfoxide solvents are added in dry reactor, separately
Add and account for the poly- of Modified Membrane gross weight 4%（Lactide coglycolide）Monododecyl ether（Molecular weight is 6000）, under inert atmosphere,
Mixed 60 minutes in 52 DEG C of stirrings, use the tape casting film forming, object is dried to obtain in 50 DEG C of vacuum drying chambers.
After tested：The surface contact angle and its elongation at break of object and water of the present invention respectively than improving before modified
13.1 ° and 10.3%.
Claims (4)
1. a kind of MPEGPLA is with gathering（Lactide coglycolide）The method for improving polypropylene sorrel water resistance and compliance, its feature
It is：In Modified Membrane the molecular weight of polyacrylic acid segment be the molecular weight of 81000~89000, MPEGPLA segments be 2400~
2500, gather（Lactide coglycolide）The molecular weight of segment is 5200~6000；Its method of modifying uses following steps：
1）The synthesis of polyacrylic acid-MPEGPLA graft copolymers：Hydroxy-end capped MPEGPLA is added in dry reactor, it is molten
Under agent, condensing agent and polyacrylic acid, inert atmosphere, in 28~34 DEG C of stirring reactions 2~3 days, terminating reaction, by filtering, thoroughly
Analyse, dry, obtain object；
2）MPEGPLA is with gathering（Lactide coglycolide）The preparation of modified polypropylene sorrel：Poly- third is added in dry reactor
It is olefin(e) acid-MPEGPLA graft copolymers, poly-（Lactide coglycolide）Under monododecyl ether and solvent, inert atmosphere, in 46~
After 52 DEG C of stirrings are mixed 50~60 minutes, with the tape casting film forming and drying, object is obtained.
2. a kind of MPEGPLA according to claim 1 is with gathering（Lactide coglycolide）Improve polypropylene sorrel water resistance and
The method of compliance, it is characterised in that：Step 1）In, MPEGPLA is poly- using mono methoxy polyethylene glycol（D,L）Lactic acid copolymer
（The weight ratio of polyethylene glycol and PLA is 10/90）, the mol ratio of MPEGPLA and polyacrylic acid is 15~25:1.
3. a kind of MPEGPLA according to claim 1 is with gathering（Lactide coglycolide）Improve polypropylene sorrel water resistance and
The method of compliance, it is characterised in that：Step 1）In, condensing agent is usedN,N’- dicyclohexylcarbodiimide,N,N’- diisopropyl
Base carbodiimide or 3- ethyls -1-（3- dimethylaminopropyls）The mol ratio of carbodiimide, condensing agent and polyacrylic acid be 1.08~
1.9:1, solvent uses dimethyl sulfoxide (DMSO), and reactant solution concentration is 5~15 g:100 ml.
4. a kind of MPEGPLA according to claim 1 is with gathering（Lactide coglycolide）Improve polypropylene sorrel water resistance and
The method of compliance, it is characterised in that：Step 2）In, gather（Lactide coglycolide）Monododecyl ether is using poly-（D, L- third is handed over
Ester-glycolide）Monododecyl ether（The weight ratio of lactide and glycolide is 90/10）, gather（Lactide coglycolide）Single 12
Mass percent of the alkyl ether in Modified Membrane is 2~4%, and solvent uses dimethyl sulfoxide (DMSO), and mixture solution concentration is 25~30
g:100 ml。
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| CN201710362664.6A CN106987129A (en) | 2017-05-22 | 2017-05-22 | A kind of MPEGPLA is with gathering（Lactide glycolide）The method for improving polypropylene sorrel water resistance and compliance |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710362664.6A CN106987129A (en) | 2017-05-22 | 2017-05-22 | A kind of MPEGPLA is with gathering（Lactide glycolide）The method for improving polypropylene sorrel water resistance and compliance |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103865074A (en) * | 2014-04-11 | 2014-06-18 | 山东理工大学 | Preparation method of polypeptide-poly(caprolactone-lactide)-MPEGPLA double-graft copolymer |
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- 2017-05-22 CN CN201710362664.6A patent/CN106987129A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103865074A (en) * | 2014-04-11 | 2014-06-18 | 山东理工大学 | Preparation method of polypeptide-poly(caprolactone-lactide)-MPEGPLA double-graft copolymer |
Non-Patent Citations (1)
| Title |
|---|
| 蔡邦肖等: "高分离性能聚丙烯酸膜制备工艺的初步研究", 《第一届全国化学工程与生物化工年会论文摘要集（上）》 * |
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Application publication date: 20170728 |