CN106947265A - A kind of method that PPDO is improved with PTMC to polypropylene sorrel water resistance and compliance - Google Patents
A kind of method that PPDO is improved with PTMC to polypropylene sorrel water resistance and compliance Download PDFInfo
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- CN106947265A CN106947265A CN201710376541.8A CN201710376541A CN106947265A CN 106947265 A CN106947265 A CN 106947265A CN 201710376541 A CN201710376541 A CN 201710376541A CN 106947265 A CN106947265 A CN 106947265A
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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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- 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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- 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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- C—CHEMISTRY; METALLURGY
- 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 method that PPDO is improved with PTMC to polypropylene sorrel water resistance and compliance, using following steps：1）Hydroxy-end capped PTMC monododecyl ether, solvent, condensing agent and polyacrylic acid is added in dry reactor, reacts 2~4 days, obtains polyacrylic acid PTMC graft copolymer；2）Graft copolymer, amino-terminated PPDO list tridecyl ether, solvent and condensing agent are added in dry reactor, reacts 2~4 days, obtains polyacrylic acid PPDO PTMC dual graft copolymer；3）Dual graft copolymer, PPDO list tridecyl ether and solvent are added in dry reactor, after mixing 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 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.PPDO and PTMC are with excellent biocompatibility
With the biomaterial of biodegradability, with good hydrophobicity and compliance.First PTMC segment is connect
Branch, then will be poly- to dioxocyclohex to obtaining poly acrylic acid-poly trimethylene carbonate graft copolymer on polyacrylic acid strand
Polypropylene is formed on the polyacrylic acid segment that ketone segment is grafted in poly acrylic acid-poly trimethylene carbonate graft copolymer
Acid-PPDO-PTMC dual graft copolymer, then again adds PPDO segment
Poly acrylic acid-poly Lanthanum Isopropoxide-PTMC dual graft copolymer 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：
What a kind of PPDO was improved with PTMC to polypropylene sorrel water resistance and compliance
Method, it is characterised in that：The molecular weight of polyacrylic acid segment is 82000~91000, PTMC chain in Modified Membrane
The molecular weight of section is 2600~2700, and the molecular weight of PPDO segment is 2300~2400；Its method of modifying is used
Following steps：
1）The synthesis of poly acrylic acid-poly trimethylene carbonate graft copolymer：Added in dry reactor hydroxy-end capped
Under PTMC monododecyl ether, solvent, condensing agent and polyacrylic acid, inert atmosphere, in 27~33 DEG C of stirrings
Reaction 2~4 days, terminating reaction by filtering, dialysis, is dried, obtains object；
2）The synthesis of poly acrylic acid-poly Lanthanum Isopropoxide-PTMC dual graft copolymer：In dry reactor
Interior addition poly acrylic acid-poly trimethylene carbonate graft copolymer, amino-terminated PPDO list tridecyl
Under ether, solvent and condensing agent, inert atmosphere, in 26~33 DEG C of stirring reactions 2~4 days, terminating reaction, by filtering, dialysis, dry
It is dry, obtain object；
3）The preparation for the polypropylene sorrel that PPDO is improved with PTMC：Add in dry reactor
Enter poly acrylic acid-poly Lanthanum Isopropoxide-PTMC dual graft copolymer, PPDO list tridecane
Under base ether and solvent, inert atmosphere, after 46~52 DEG C of stirrings are mixed 50~60 minutes, with the tape casting film forming and drying, obtain
Object.
A kind of described PPDO is with PTMC to polypropylene sorrel water resistance and compliance
The method improved, step 1）In, the mol ratio of PTMC monododecyl ether and polyacrylic acid for 15~
25:1。
A kind of described PPDO is with PTMC to polypropylene sorrel water resistance and compliance
The method improved, 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 1.06~1.9:1, solvent
Using dimethyl sulfoxide (DMSO), reactant solution concentration is 5~15 g:100 ml.
A kind of described PPDO is with PTMC to polypropylene sorrel water resistance and compliance
The method improved, step 2）In, PPDO list tridecyl ether and poly acrylic acid-poly trimethylene carbonate
The mol ratio of polyacrylic acid segment is 15~25 in graft copolymer:1.
A kind of described PPDO is with PTMC to polypropylene sorrel water resistance and compliance
The method improved, step 2）In, condensing agent is usedN,N’- dicyclohexylcarbodiimide,N,N’- DIC
Or 3- ethyls -1-（3- dimethylaminopropyls）Carbodiimide, condensing agent and poly acrylic acid-poly trimethylene carbonate graft copolymer
The mol ratio of middle polyacrylic acid segment is 1.06~1.9:1, solvent uses dimethyl sulfoxide (DMSO), and reactant solution concentration is 5~15
g:100 ml。
A kind of described PPDO is with PTMC to polypropylene sorrel water resistance and compliance
The method improved, step 3）In, mass percent of the PPDO list tridecyl ether in Modified Membrane be 2~
3%, 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 PPDO and PTMC enter to polypropylene sorrel water resistance and compliance
Row improvement method, using esterification, amidation process and blending three kinds of means, it is simple to operate, be easy to grasp；
2nd, described polyacrylic acid improvement film water resistance and compliance are enhanced.
Embodiment
Embodiment 1
1）The preparation of poly acrylic acid-poly trimethylene carbonate graft copolymer
15.7 grams of polyacrylic acid are added in dry reactor（Molecular weight is 82000）, 9.3 grams of hydroxy-end capped polytrimethylenes
Carbonic ester monododecyl ether（Molecular weight is 2600）, 248 ml dimethyl sulfoxide (DMSO)s are added, 0.049 gram is addedN,N’- two rings
Under hexyl carbodiimide, inert atmosphere, in 27 DEG C of stirring reactions 2 days, terminating reaction by filtering, dialysis, was dried, obtains mesh
Mark thing；
2）The preparation of poly acrylic acid-poly Lanthanum Isopropoxide-PTMC dual graft copolymer
Added in dry reactor 12 grams of poly acrylic acid-poly trimethylene carbonate graft copolymers, 6.5 grams it is amino-terminated
PPDO list tridecyl ether（Molecular weight is 2300）, 186 ml dimethyl sulfoxide (DMSO)s are added, 0.036 gram is addedN, N’Under-dicyclohexylcarbodiimide, inert atmosphere, in 26 DEG C of stirring reactions 2 days, terminating reaction by filtering, dialysis, was dried,
Obtain object；
3）The preparation for the polypropylene sorrel that PPDO is improved with PTMC
10 grams of poly acrylic acid-poly Lanthanum Isopropoxide-PTMC dual graft copolymerization are added in dry reactor
Thing and 37 ml dimethyl sulfoxide solvents, it is another to add the PPDO list tridecyl ether for accounting for Modified Membrane gross weight 2%（Point
Son amount is 2300）, under inert atmosphere, in 46 DEG C of stirring mixing 50 minutes, the tape casting film forming is used, is done in 50 DEG C of vacuum drying chambers
It is dry to obtain object.
After tested：The surface contact angle and its elongation at break of object and water of the present invention respectively than improving before modified
11.7 ° and 9.5%.
Embodiment 2
1）The preparation of poly acrylic acid-poly trimethylene carbonate graft copolymer
15 grams of polyacrylic acid are added in dry reactor（Molecular weight is 87000）, 8.6 grams of hydroxy-end capped polytrimethylene carbon
Acid esters monododecyl ether（Molecular weight is 2600）, 236 ml dimethyl sulfoxide (DMSO)s are added, 0.028 gram is addedN,N’- diisopropyl
Under base carbodiimide, inert atmosphere, in 30 DEG C of stirring reactions 3 days, terminating reaction by filtering, dialysis, was dried, obtains target
Thing；
2）The preparation of poly acrylic acid-poly Lanthanum Isopropoxide-PTMC dual graft copolymer
Added in dry reactor 12.2 grams of poly acrylic acid-poly trimethylene carbonate graft copolymers, 6.4 grams it is amino-terminated
PPDO list tridecyl ether（Molecular weight is 2400）, 185 ml dimethyl sulfoxide (DMSO)s are added, 0.021 gram is addedN,N’Under-DIC, inert atmosphere, in 30 DEG C of stirring reactions 3 days, terminating reaction, by filtering, dialysis, dry
It is dry, obtain object；
3）The preparation for the polypropylene sorrel that PPDO is improved with PTMC
9.9 grams of poly acrylic acid-poly Lanthanum Isopropoxide-PTMC dual graft copolymerization are added in dry reactor
Thing and 36 ml dimethyl sulfoxide solvents, it is another to add the PPDO list tridecyl ether for accounting for Modified Membrane gross weight 3%（Point
Son amount is 2400）, under inert atmosphere, in 48 DEG C of stirring mixing 55 minutes, the tape casting film forming is used, is done in 50 DEG C of vacuum drying chambers
It is dry to obtain object.
After tested：The surface contact angle and its elongation at break of object and water of the present invention respectively than improving before modified
12.5 ° and 10.5%.
Embodiment 3
1）The preparation of poly acrylic acid-poly trimethylene carbonate graft copolymer
15.2 grams of polyacrylic acid are added in dry reactor（Molecular weight is 91000）, 8.3 grams of hydroxy-end capped polytrimethylenes
Carbonic ester monododecyl ether（Molecular weight is 2700）, 236 ml dimethyl sulfoxide (DMSO)s are added, 0.041 gram of 3- ethyls -1- is added
（3- dimethylaminopropyls）Under carbodiimide, inert atmosphere, in 33 DEG C of stirring reactions 4 days, terminating reaction, by filtering, dialysis, dry
It is dry, obtain object；
2）The preparation of poly acrylic acid-poly Lanthanum Isopropoxide-PTMC dual graft copolymer
Added in dry reactor 11.4 grams of poly acrylic acid-poly trimethylene carbonate graft copolymers, 5.6 grams it is amino-terminated
PPDO list tridecyl ether（Molecular weight is 2400）, 173 ml dimethyl sulfoxide (DMSO)s are added, 0.028 gram is added
3- ethyls -1-（3- dimethylaminopropyls）Under carbodiimide, inert atmosphere, in 33 DEG C of stirring reactions 4 days, terminating reaction passed through mistake
Filter, dialyse, dry, obtain object；
3）The preparation for the polypropylene sorrel that PPDO is improved with PTMC
9.5 grams of poly acrylic acid-poly Lanthanum Isopropoxide-PTMC dual graft copolymerization are added in dry reactor
Thing and 35 ml dimethyl sulfoxide solvents, it is another to add the PPDO list tridecyl ether for accounting for Modified Membrane gross weight 2%（Point
Son amount is 2400）, under inert atmosphere, in 52 DEG C of stirring mixing 60 minutes, the tape casting film forming is used, is done in 50 DEG C of vacuum drying chambers
It is dry to obtain object.
After tested：The surface contact angle and its elongation at break of object and water of the present invention respectively than improving before modified
13.4 ° and 11.1%.
Claims (6)
1. a kind of PPDO is improved with PTMC to polypropylene sorrel water resistance and compliance
Method, it is characterised in that：The molecular weight of polyacrylic acid segment is 82000~91000, PTMC in Modified Membrane
The molecular weight of segment is 2600~2700, and the molecular weight of PPDO segment is 2300~2400；Its modification method is adopted
Use following steps：
1）The synthesis of poly acrylic acid-poly trimethylene carbonate graft copolymer：Added in dry reactor hydroxy-end capped
Under PTMC monododecyl ether, solvent, condensing agent and polyacrylic acid, inert atmosphere, in 27~33 DEG C of stirrings
Reaction 2~4 days, terminating reaction by filtering, dialysis, is dried, obtains object；
2）The synthesis of poly acrylic acid-poly Lanthanum Isopropoxide-PTMC dual graft copolymer：In dry reactor
Interior addition poly acrylic acid-poly trimethylene carbonate graft copolymer, amino-terminated PPDO list tridecyl
Under ether, solvent and condensing agent, inert atmosphere, in 26~33 DEG C of stirring reactions 2~4 days, terminating reaction, by filtering, dialysis, dry
It is dry, obtain object；
3）The preparation for the polypropylene sorrel that PPDO is improved with PTMC：Add in dry reactor
Enter poly acrylic acid-poly Lanthanum Isopropoxide-PTMC dual graft copolymer, PPDO list tridecane
Under base ether and solvent, inert atmosphere, after 46~52 DEG C of stirrings are mixed 50~60 minutes, with the tape casting film forming and drying, obtain
Object.
2. a kind of PPDO according to claim 1 and PTMC are water-fast to polypropylene sorrel
The method that property and compliance are improved, it is characterised in that：Step 1）In, PTMC monododecyl ether is with gathering
The mol ratio of acrylic acid is 15~25:1.
3. a kind of PPDO according to claim 1 and PTMC are resistance to polypropylene sorrel
The method that aqueous and compliance is improved, it is characterised in that：Step 1）In, condensing agent is usedN,N’- dicyclohexyl carbon two is sub-
Amine,N,N’- DIC or 3- ethyls -1-（3- dimethylaminopropyls）Carbodiimide, condensing agent and polyacrylic acid
Mol ratio is 1.06~1.9:1, solvent uses dimethyl sulfoxide (DMSO), and reactant solution concentration is 5~15 g:100 ml.
4. a kind of PPDO according to claim 1 and PTMC are water-fast to polypropylene sorrel
The method that property and compliance are improved, it is characterised in that：Step 2）In, PPDO list tridecyl ether and poly- third
The mol ratio of polyacrylic acid segment is 15~25 in olefin(e) acid-PTMC graft copolymer:1.
5. a kind of PPDO according to claim 1 and PTMC are resistance to polypropylene sorrel
The method that aqueous and compliance is improved, it is characterised in that：Step 2）In, condensing agent is usedN,N’- dicyclohexyl carbon two is sub-
Amine,N,N’- DIC or 3- ethyls -1-（3- dimethylaminopropyls）Carbodiimide, condensing agent and poly acrylic acid-poly
The mol ratio of polyacrylic acid segment is 1.06~1.9 in trimethylene carbonate graft copolymer:1, solvent is sub- using dimethyl
Sulfone, reactant solution concentration is 5~15 g:100 ml.
6. a kind of PPDO according to claim 1 and PTMC are water-fast to polypropylene sorrel
The method that property and compliance are improved, it is characterised in that：Step 3）In, PPDO list tridecyl ether is in modification
Mass percent in film is 2~3%, and solvent uses dimethyl sulfoxide (DMSO), and mixture solution concentration is 25~30 g:100 ml.
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| CN201710376541.8A CN106947265A (en) | 2017-05-25 | 2017-05-25 | A kind of method that PPDO is improved with PTMC to polypropylene sorrel water resistance and compliance |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105504322A (en) * | 2016-03-07 | 2016-04-20 | 山东理工大学 | Method for improving water resistance and flexibility of polyvinyl alcohol films by aid of poly-trimethylene carbonate and poly-p-dioxanone |
| CN105542178A (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 poly(trimethylene carbonate) and polypeptide |
| CN105694474A (en) * | 2016-03-07 | 2016-06-22 | 山东理工大学 | Method for improving water resisting property and flexibility of polyvinyl alcohol film by means of poly trimethylene carbonate and poly lactic acid-glycolic acid |
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- 2017-05-25 CN CN201710376541.8A patent/CN106947265A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105504322A (en) * | 2016-03-07 | 2016-04-20 | 山东理工大学 | Method for improving water resistance and flexibility of polyvinyl alcohol films by aid of poly-trimethylene carbonate and poly-p-dioxanone |
| CN105542178A (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 poly(trimethylene carbonate) and polypeptide |
| CN105694474A (en) * | 2016-03-07 | 2016-06-22 | 山东理工大学 | Method for improving water resisting property and flexibility of polyvinyl alcohol film by means of poly trimethylene carbonate and poly lactic acid-glycolic acid |
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