CN107033605A - A kind of method being improved with MPEGPLA and polycaprolactone to polypropylene sorrel water resistance and compliance - Google Patents
A kind of method being improved with MPEGPLA and polycaprolactone to polypropylene sorrel water resistance and compliance Download PDFInfo
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- CN107033605A CN107033605A CN201710362681.XA CN201710362681A CN107033605A CN 107033605 A CN107033605 A CN 107033605A CN 201710362681 A CN201710362681 A CN 201710362681A CN 107033605 A CN107033605 A CN 107033605A
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- mpegpla
- polycaprolactone
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- water resistance
- polypropylene sorrel
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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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- C—CHEMISTRY; METALLURGY
- 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
- 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
- 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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- C—CHEMISTRY; METALLURGY
- 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
- C08J2487/00—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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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Abstract
The present invention discloses a kind of method being improved with MPEGPLA and polycaprolactone to polypropylene sorrel water resistance and compliance, using following steps：1）The synthesis of polyacrylic acid polycaprolactone graft copolymer：Add hydroxy-end capped polycaprolactone monododecyl ether, solvent, condensing agent and polyacrylic acid in dry reactor, stirring reaction 2~3 days, terminating reaction obtains object；2）MPEGPLA and Polycaprolactone modified polypropylene sorrel preparation：Polyacrylic acid polycaprolactone graft copolymer, MPEGPLA and solvent are added in dry reactor, after stirring is mixed 50~60 minutes, with the tape casting film forming and drying, object of the present invention is obtained.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 and polycaprolactone are with excellent biocompatibility and biodegradability
Biomaterial, with good hydrophobicity and compliance.Polycaprolactone segment introducing polyacrylic acid segment is first formed poly- third
Olefin(e) acid-polycaprolactone graft copolymer, then adds poly acrylic acid-poly caprolactone graft copolymer shape by MPEGPLA segments again
Into blend, modified polypropene sorrel is made, 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 method being improved with MPEGPLA and polycaprolactone to polypropylene sorrel water resistance and compliance, its feature exists
In：The molecular weight of polyacrylic acid segment is 82000~90000 in Modified Membrane, the molecular weight of polycaprolactone segment for 2000~
The molecular weight of 2400, MPEGPLA segments is 4500~5000；Its method of modifying uses following steps：
1）The synthesis of poly acrylic acid-poly caprolactone graft copolymer：Hydroxy-end capped polycaprolactone is added in dry reactor
Under monododecyl ether, solvent, condensing agent and polyacrylic acid, inert atmosphere, in 26~33 DEG C of stirring reactions 2~3 days, terminate anti-
Should, by filtering, dialysis, dry, obtain object；
2）MPEGPLA and Polycaprolactone modified polypropylene sorrel preparation：In dry reactor add poly acrylic acid-poly oneself
Under interior ester graft copolymer, MPEGPLA and solvent, inert atmosphere, after 46~50 DEG C of stirrings are mixed 50~60 minutes, with curtain coating
Method film forming and drying, obtain object.
A kind of described side being improved with MPEGPLA and polycaprolactone to polypropylene sorrel water resistance and compliance
Method, step 1）In, the mol ratio of polycaprolactone monododecyl ether and polyacrylic acid is 15~25:1.
A kind of described side being improved with MPEGPLA and polycaprolactone to 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 1.07~1.8:1, solvent is sub- using dimethyl
Sulfone, reactant solution concentration is 5~15 g:100 ml.
A kind of described side being improved with MPEGPLA and polycaprolactone to polypropylene sorrel water resistance and compliance
Method, step 2）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）, mass percents of the MPEGPLA in Modified Membrane is 1~3%, and solvent uses dimethyl sulfoxide (DMSO), and mixture is molten
Liquid concentration is 25~30 g:100 ml.
Compared with prior art, its advantage is the present invention：
1st, a kind of described method being improved with MPEGPLA and polycaprolactone to 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 poly acrylic acid-poly caprolactone graft copolymer
20 grams of polyacrylic acid are added in dry reactor（Molecular weight is 82000）With 8.9 grams of hydroxy-end capped polycaprolactone lists
Lauryl ether（Molecular weight is 2000）, 285 ml dimethyl sulfoxide (DMSO)s are added, 0.062 gram is addedN,N’- dicyclohexyl carbon two
Under imines, inert atmosphere, in 26 DEG C of stirring reactions 2 days, terminating reaction by filtering, dialysis, was dried, obtains object；
2）MPEGPLA and Polycaprolactone modified polypropylene sorrel preparation
10 grams of poly acrylic acid-poly caprolactone graft copolymers and 37 ml dimethyl sulfoxide solvents are added in dry reactor, separately
Add the MPEGPLA for accounting for Modified Membrane gross weight 1%（Molecular weight is 4500）, under inert atmosphere, in 46 DEG C of stirring mixing 50 minutes,
The tape casting film forming is used, 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
12.7 ° and 9.2%.
Embodiment 2
1）The preparation of poly acrylic acid-poly caprolactone graft copolymer
21 grams of polyacrylic acid are added in dry reactor（Molecular weight is 85000）With 10.2 grams of hydroxy-end capped polycaprolactone lists
Lauryl ether（Molecular weight is 2200）, 311 ml dimethyl sulfoxide (DMSO)s are added, 0.039 gram is addedN,N’- diisopropyl carbon two
Under imines, inert atmosphere, in 30 DEG C of stirring reactions 3 days, terminating reaction by filtering, dialysis, was dried, obtains object；
2）MPEGPLA and Polycaprolactone modified polypropylene sorrel preparation
10.1 grams of poly acrylic acid-poly caprolactone graft copolymers are added in dry reactor and 36.5 ml dimethyl sulfoxide (DMSO)s are molten
Agent, it is another to add the MPEGPLA for accounting for Modified Membrane gross weight 2%（Molecular weight is 4700）, under inert atmosphere, in 48 DEG C of stirring mixing 55
Minute, the tape casting film forming is used, 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 9.5%.
Embodiment 3
1）The preparation of poly acrylic acid-poly caprolactone graft copolymer
22 grams of polyacrylic acid are added in dry reactor（Molecular weight is 90000）With 10.8 grams of hydroxy-end capped polycaprolactone lists
Lauryl ether（Molecular weight is 2400）, 333 ml dimethyl sulfoxide (DMSO)s are added, 0.058 gram of 3- ethyls -1- is added（3- diformazan ammonia
Propyl group）Under carbodiimide, inert atmosphere, in 33 DEG C of stirring reactions 2 days, terminating reaction by filtering, dialysis, was dried, obtains mesh
Mark thing；
2）MPEGPLA and Polycaprolactone modified polypropylene sorrel preparation
9.5 grams of poly acrylic acid-poly caprolactone graft copolymers and 35 ml dimethyl sulfoxide solvents are added in dry reactor,
It is another to add the MPEGPLA for accounting for Modified Membrane gross weight 3%（Molecular weight is 5000）, under inert atmosphere, in 50 DEG C of 60 points of stirring mixing
Clock, uses the tape casting film forming, and 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
13.6 ° and 10.3%.
Claims (4)
1. a kind of method being improved with MPEGPLA and polycaprolactone to polypropylene sorrel water resistance and compliance, its feature
It is：The molecular weight of polyacrylic acid segment is 82000~90000 in Modified Membrane, the molecular weight of polycaprolactone segment for 2000~
The molecular weight of 2400, MPEGPLA segments is 4500~5000；Its method of modifying uses following steps：
1）The synthesis of poly acrylic acid-poly caprolactone graft copolymer：Hydroxy-end capped polycaprolactone is added in dry reactor
Under monododecyl ether, solvent, condensing agent and polyacrylic acid, inert atmosphere, in 26~33 DEG C of stirring reactions 2~3 days, terminate anti-
Should, by filtering, dialysis, dry, obtain object；
2）MPEGPLA and Polycaprolactone modified polypropylene sorrel preparation：In dry reactor add poly acrylic acid-poly oneself
Under interior ester graft copolymer, MPEGPLA and solvent, inert atmosphere, after 46~50 DEG C of stirrings are mixed 50~60 minutes, with curtain coating
Method film forming and drying, obtain object.
2. one kind according to claim 1 is entered with MPEGPLA with polycaprolactone to polypropylene sorrel water resistance and compliance
The improved method of row, it is characterised in that：Step 1）In, the mol ratio of polycaprolactone monododecyl ether and polyacrylic acid for 15~
25:1。
3. one kind according to claim 1 is entered with MPEGPLA with polycaprolactone to polypropylene sorrel water resistance and compliance
The improved method of row, 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 1.07~
1.8:1, solvent uses dimethyl sulfoxide (DMSO), and reactant solution concentration is 5~15 g:100 ml.
4. one kind according to claim 1 is entered with MPEGPLA with polycaprolactone to polypropylene sorrel water resistance and compliance
The improved method of row, it is characterised in that：Step 2）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）, mass percents of the MPEGPLA in Modified Membrane is 1~3%, and solvent is adopted
With dimethyl sulfoxide (DMSO), mixture solution concentration is 25~30 g:100 ml.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710362681.XA CN107033605A (en) | 2017-05-22 | 2017-05-22 | A kind of method being improved with MPEGPLA and polycaprolactone to polypropylene sorrel water resistance and compliance |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710362681.XA CN107033605A (en) | 2017-05-22 | 2017-05-22 | A kind of method being improved with MPEGPLA and polycaprolactone to polypropylene sorrel water resistance and compliance |
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| CN107033605A true CN107033605A (en) | 2017-08-11 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542480A (en) * | 2016-03-07 | 2016-05-04 | 山东理工大学 | Method for improving water resistance and flexibility of polyvinyl alcohol film through polycaprolactone and P(CPP-SA)-polyethylene glycol |
| CN105566648A (en) * | 2016-03-03 | 2016-05-11 | 山东理工大学 | Method for preparing polyving akohol-polycaprolactone-polypeptide double graft copolymer |
| CN105670305A (en) * | 2016-03-07 | 2016-06-15 | 山东理工大学 | Method for improving water resistance and flexibility of polyvinyl alcohol film by using polycaprolactone and polypeptide-polyethylene glycol |
| CN105670307A (en) * | 2016-03-16 | 2016-06-15 | 山东理工大学 | Method for improving water resistance and flexibility of polyvinyl alcohol membrane through polycaprolactone and poly(trimethylene carbonate)-polyvinylpyrrolidone |
-
2017
- 2017-05-22 CN CN201710362681.XA patent/CN107033605A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105566648A (en) * | 2016-03-03 | 2016-05-11 | 山东理工大学 | Method for preparing polyving akohol-polycaprolactone-polypeptide double graft copolymer |
| CN105542480A (en) * | 2016-03-07 | 2016-05-04 | 山东理工大学 | Method for improving water resistance and flexibility of polyvinyl alcohol film through polycaprolactone and P(CPP-SA)-polyethylene glycol |
| CN105670305A (en) * | 2016-03-07 | 2016-06-15 | 山东理工大学 | Method for improving water resistance and flexibility of polyvinyl alcohol film by using polycaprolactone and polypeptide-polyethylene glycol |
| CN105670307A (en) * | 2016-03-16 | 2016-06-15 | 山东理工大学 | Method for improving water resistance and flexibility of polyvinyl alcohol membrane through polycaprolactone and poly(trimethylene carbonate)-polyvinylpyrrolidone |
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Application publication date: 20170811 |