CN106977945A - A kind of method that polypropylene glycol improves polypropylene sorrel water resistance and compliance with PTMC - Google Patents
A kind of method that polypropylene glycol improves polypropylene sorrel water resistance and compliance with PTMC Download PDFInfo
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- CN106977945A CN106977945A CN201710376544.1A CN201710376544A CN106977945A CN 106977945 A CN106977945 A CN 106977945A CN 201710376544 A CN201710376544 A CN 201710376544A CN 106977945 A CN106977945 A CN 106977945A
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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
- C08J2469/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
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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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Abstract
The present invention discloses a kind of method that polypropylene glycol improves polypropylene sorrel water resistance and compliance with PTMC, using following steps：1）Hydroxy-end capped polypropylene glycol monobutyl ether, solvent, condensing agent and polyacrylic acid is added in dry reactor, reacts 2~4 days, obtains polyacrylic acid polypropylene glycol graft copolymer；2）Graft copolymer, hydroxy-end capped PTMC monododecyl ether, solvent and condensing agent are added in dry reactor, reacts 2~4 days, obtains polyacrylic acid polypropylene glycol PTMC dual graft copolymer；3）Dual graft copolymer, PTMC monododecyl 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.Polypropylene glycol（Molecular weight more than 2000）It is with excellent with PTMC
The biomaterial of biocompatibility and biodegradability, with hydrophobicity and compliance.First polypropylene glycol segment is grafted to
Poly acrylic acid-poly propane diols graft copolymer is obtained on polyacrylic acid strand, then PTMC segment is grafted
Poly acrylic acid-poly propane diols-poly- three methylene is formed on to the polyacrylic acid segment in poly acrylic acid-poly propane diols graft copolymer
Base carbonic ester dual graft copolymer, then adds poly acrylic acid-poly propane diols-poly- Sanya by PTMC segment again
Methyl carbonic dual graft copolymer formation blend, is made modified polypropene sorrel, so as to drastically increase polyacrylic acid
The water resistance and compliance of film.
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 that polypropylene glycol improves polypropylene sorrel water resistance and compliance with PTMC, its feature exists
In：The molecular weight of polyacrylic acid segment is 80000~91000 in Modified Membrane, the molecular weight of polypropylene glycol segment for 2500~
2700, the molecular weight of PTMC segment is 2300~2500；Its method of modifying uses following steps：
1）The synthesis of poly acrylic acid-poly propane diols graft copolymer：Hydroxy-end capped polypropylene glycol is added in dry reactor
Under monobutyl ether, solvent, condensing agent and polyacrylic acid, inert atmosphere, in 25~35 DEG C of stirring reactions 2~4 days, terminating reaction was led to
Filter, dialyse, dry, obtain object；
2）The synthesis of poly acrylic acid-poly propane diols-PTMC dual graft copolymer：Added in dry reactor
Poly acrylic acid-poly propane diols graft copolymer, hydroxy-end capped PTMC monododecyl ether, solvent and condensation
Under agent, inert atmosphere, in 25~33 DEG C of stirring reactions 2~4 days, terminating reaction by filtering, dialysis, was dried, obtains target
Thing；
3）The preparation for the polypropylene sorrel that polypropylene glycol is improved with PTMC：Poly- third is added in dry reactor
Olefin(e) acid-polypropylene glycol-PTMC dual graft copolymer, PTMC monododecyl ether and molten
Under agent, inert atmosphere, after 46~52 DEG C of stirrings are mixed 50~60 minutes, with the tape casting film forming and drying, object is obtained.
A kind of described polypropylene glycol improves the side of polypropylene sorrel water resistance and compliance with PTMC
Method, step 1）In, the mol ratio of polypropylene glycol monobutyl ether and polyacrylic acid is 15~25:1.
A kind of described polypropylene glycol improves the side of polypropylene sorrel water resistance and compliance with PTMC
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 1.06~1.8:1, solvent is sub- using dimethyl
Sulfone, reactant solution concentration is 5~15 g:100 ml.
A kind of described polypropylene glycol improves the side of polypropylene sorrel water resistance and compliance with PTMC
Method, step 2）In, PTMC monododecyl ether and polypropylene in poly acrylic acid-poly propane diols graft copolymer
The mol ratio of sour segment is 15~25:1.
A kind of described polypropylene glycol improves the side of polypropylene sorrel water resistance and compliance with PTMC
Method, step 2）In, condensing agent is usedN,N’- dicyclohexylcarbodiimide,N,N’- DIC or 3- ethyls -1-
（3- dimethylaminopropyls）Carbodiimide, condensing agent rubs with polyacrylic acid segment in poly acrylic acid-poly propane diols graft copolymer
You are than being 1.06~1.8:1, solvent uses dimethyl sulfoxide (DMSO), and reactant solution concentration is 5~15 g:100 ml.
A kind of described polypropylene glycol improves the side of polypropylene sorrel water resistance and compliance with PTMC
Method, step 3）In, mass percent of the PTMC monododecyl ether in Modified Membrane is 2~4%, and solvent is adopted
With dimethyl sulfoxide (DMSO), mixture solution concentration is 25~30 g:100 ml.
Compared with prior art, its advantage is the present invention：
1st, the method for a kind of described polypropylene glycol and PTMC improvement polypropylene sorrel water resistance and compliance,
It is simple to operate, be easy to grasp using two step esterifications and the means that are combined of blending；
2nd, described polyacrylic acid improvement film water resistance and compliance are enhanced.
Embodiment
Embodiment 1
1）The preparation of poly acrylic acid-poly propane diols graft copolymer
15.4 grams of polyacrylic acid are added in dry reactor（Molecular weight is 80000）, 8.8 grams of hydroxy-end capped polypropylene glycol lists
Butyl ether（Molecular weight is 2500）, 243 ml dimethyl sulfoxide (DMSO)s are added, 0.049 gram is addedN,N’- dicyclohexylcarbodiimide, it is lazy
Property atmosphere under, in 25 DEG C of stirring reactions 2 days, terminating reaction by filtering, dialysis, was dried, and obtains object；
2）The preparation of poly acrylic acid-poly propane diols-PTMC dual graft copolymer
12.3 grams of poly acrylic acid-poly propane diols graft copolymers, 6.5 grams of hydroxy-end capped poly- three methylenes are added in dry reactor
Base carbonic ester monododecyl ether（Molecular weight is 2300）, 187 ml dimethyl sulfoxide (DMSO)s are added, 0.036 gram is addedN,N’- two
Under carbodicyclo hexylimide, inert atmosphere, in 25 DEG C of stirring reactions 2 days, terminating reaction by filtering, dialysis, was dried, obtained
Object；
3）The preparation for the polypropylene sorrel that polypropylene glycol is improved with PTMC
10 grams of poly acrylic acid-poly propane diols-PTMC dual graft copolymers and 37 are added in dry reactor
Ml dimethyl sulfoxide solvents, it is another to add the PTMC monododecyl ether for accounting for Modified Membrane gross weight 2%（Molecular weight
For 2300）, under inert atmosphere, in 46 DEG C of stirring mixing 50 minutes, the tape casting film forming is used, it is dry in 50 DEG C of vacuum drying chambers
To 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
12.4 ° and 9.7%.
Embodiment 2
1）The preparation of poly acrylic acid-poly propane diols graft copolymer
15 grams of polyacrylic acid are added in dry reactor（Molecular weight is 87000）, 8.6 grams of hydroxy-end capped polypropylene glycol monobutyls
Ether（Molecular weight is 2600）, 236 ml dimethyl sulfoxide (DMSO)s are added, 0.028 gram is addedN,N’- DIC, inertia
Under atmosphere, in 30 DEG C of stirring reactions 3 days, terminating reaction by filtering, dialysis, was dried, obtains object；
2）The preparation of poly acrylic acid-poly propane diols-PTMC dual graft copolymer
12.1 grams of poly acrylic acid-poly propane diols graft copolymers, 6.4 grams of hydroxy-end capped poly- three methylenes are added in dry reactor
Base carbonic ester monododecyl ether（Molecular weight is 2400）, 186 ml dimethyl sulfoxide (DMSO)s are added, 0.021 gram is addedN,N’- two
Under diisopropylcarbodiimide, inert atmosphere, in 30 DEG C of stirring reactions 3 days, terminating reaction by filtering, dialysis, was dried, obtained
Object；
3）The preparation for the polypropylene sorrel that polypropylene glycol is improved with PTMC
9.9 grams of poly acrylic acid-poly propane diols-PTMC dual graft copolymers and 36 are added in dry reactor
Ml dimethyl sulfoxide solvents, it is another to add the PTMC monododecyl ether for accounting for Modified Membrane gross weight 3%（Molecular weight
For 2400）, under inert atmosphere, in 48 DEG C of stirring mixing 55 minutes, the tape casting film forming is used, it is dry in 50 DEG C of vacuum drying chambers
To 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
13.1 ° and 10.5%.
Embodiment 3
1）The preparation of poly acrylic acid-poly propane diols graft copolymer
15.2 grams of polyacrylic acid are added in dry reactor（Molecular weight is 91000）, 8.6 grams of hydroxy-end capped polypropylene glycol lists
Butyl ether（Molecular weight is 2700）, 238 ml dimethyl sulfoxide (DMSO)s are added, 0.041 gram of 3- ethyls -1- is added（3- dimethylaminopropyls）
Under carbodiimide, inert atmosphere, in 35 DEG C of stirring reactions 4 days, terminating reaction by filtering, dialysis, was dried, obtains object；
2）The preparation of poly acrylic acid-poly propane diols-PTMC dual graft copolymer
11.5 grams of poly acrylic acid-poly propane diols graft copolymers, 5.8 grams of hydroxy-end capped poly- three methylenes are added in dry reactor
Base carbonic ester monododecyl ether（Molecular weight is 2500）, add 173 ml dimethyl sulfoxide (DMSO)s, add 0.028 gram of 3- ethyl-
1-（3- dimethylaminopropyls）Under carbodiimide, inert atmosphere, in 33 DEG C of stirring reactions 4 days, terminating reaction, by filtering, dialysis,
Dry, obtain object；
3）The preparation for the polypropylene sorrel that polypropylene glycol is improved with PTMC
9.5 grams of poly acrylic acid-poly propane diols-PTMC dual graft copolymers and 35 are added in dry reactor
Ml dimethyl sulfoxide solvents, it is another to add the PTMC monododecyl ether for accounting for Modified Membrane gross weight 4%（Molecular weight
For 2500）, under inert atmosphere, in 52 DEG C of stirring mixing 60 minutes, the tape casting film forming is used, it is dry in 50 DEG C of vacuum drying chambers
To 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
13.8 ° and 11.3%.
Claims (6)
1. a kind of polypropylene glycol improves the method for polypropylene sorrel water resistance and compliance, its feature with PTMC
It is：The molecular weight of polyacrylic acid segment is 80000~91000 in Modified Membrane, the molecular weight of polypropylene glycol segment for 2500~
2700, the molecular weight of PTMC segment is 2300~2500；Its modification method uses following steps：
1）The synthesis of poly acrylic acid-poly propane diols graft copolymer：Hydroxy-end capped polypropylene glycol is added in dry reactor
Under monobutyl ether, solvent, condensing agent and polyacrylic acid, inert atmosphere, in 25~35 DEG C of stirring reactions 2~4 days, terminating reaction was led to
Filter, dialyse, dry, obtain object；
2）The synthesis of poly acrylic acid-poly propane diols-PTMC dual graft copolymer：Added in dry reactor
Poly acrylic acid-poly propane diols graft copolymer, hydroxy-end capped PTMC monododecyl ether, solvent and condensation
Under agent, inert atmosphere, in 25~33 DEG C of stirring reactions 2~4 days, terminating reaction by filtering, dialysis, was dried, obtains target
Thing；
3）The preparation for the polypropylene sorrel that polypropylene glycol is improved with PTMC：Poly- third is added in dry reactor
Olefin(e) acid-polypropylene glycol-PTMC dual graft copolymer, PTMC monododecyl ether and molten
Under agent, inert atmosphere, after 46~52 DEG C of stirrings are mixed 50~60 minutes, with the tape casting film forming and drying, object is obtained.
2. a kind of polypropylene glycol according to claim 1 and PTMC improve polypropylene sorrel water resistance and
The method of compliance, it is characterised in that：Step 1）In, the mol ratio of polypropylene glycol monobutyl ether and polyacrylic acid is 15~25:1.
3. a kind of polypropylene glycol according to claim 1 improves polypropylene sorrel water resistance with PTMC
And the method for compliance, it is characterised in that：Step 1）In, condensing agent is usedN,N’- dicyclohexylcarbodiimide,N,N’- two is different
Propyl group carbodiimide or 3- ethyls -1-（3- dimethylaminopropyls）The mol ratio of carbodiimide, condensing agent and polyacrylic acid is 1.06
~1.8:1, solvent uses dimethyl sulfoxide (DMSO), and reactant solution concentration is 5~15 g:100 ml.
4. a kind of polypropylene glycol according to claim 1 and PTMC improve polypropylene sorrel water resistance and
The method of compliance, it is characterised in that：Step 2）In, PTMC monododecyl ether and poly acrylic acid-poly third
The mol ratio of polyacrylic acid segment is 15~25 in glycol graft copolymer:1.
5. a kind of polypropylene glycol according to claim 1 improves polypropylene sorrel water resistance with PTMC
And the method for compliance, it is characterised in that：Step 2）In, condensing agent is usedN,N’- dicyclohexylcarbodiimide,N,N’- two is different
Propyl group carbodiimide or 3- ethyls -1-（3- dimethylaminopropyls）Carbodiimide, condensing agent and the grafting of poly acrylic acid-poly propane diols are common
The mol ratio of polyacrylic acid segment is 1.06~1.8 in polymers:1, solvent uses dimethyl sulfoxide (DMSO), and reactant solution concentration is 5
~15 g:100 ml.
6. a kind of polypropylene glycol according to claim 1 and PTMC improve polypropylene sorrel water resistance and
The method of compliance, it is characterised in that：Step 3）In, quality of the PTMC monododecyl ether in Modified Membrane
Percentage is 2~4%, and solvent uses dimethyl sulfoxide (DMSO), and mixture solution concentration is 25~30 g:100 ml.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710376544.1A CN106977945A (en) | 2017-05-25 | 2017-05-25 | A kind of method that polypropylene glycol improves polypropylene sorrel water resistance and compliance with PTMC |
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| CN201710376544.1A CN106977945A (en) | 2017-05-25 | 2017-05-25 | A kind of method that polypropylene glycol improves polypropylene sorrel water resistance and compliance with PTMC |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819906A (en) * | 2014-03-10 | 2014-05-28 | 山东理工大学 | Method for improving polypeptide membrane flexibility by adopting polypropylene glycol and poly trimethylene carbonate |
| CN103865273A (en) * | 2014-03-10 | 2014-06-18 | 山东理工大学 | Method for improving flexibility of polypeptide membrane by polypropylene glycol and poly-trimethylene carbonate |
| CN105542483A (en) * | 2016-03-16 | 2016-05-04 | 山东理工大学 | Method for modifying water resistance and flexibility of polyvinyl alcohol membrane through poly(trimethylene carbonate) and poly(p-dioxanone) |
-
2017
- 2017-05-25 CN CN201710376544.1A patent/CN106977945A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819906A (en) * | 2014-03-10 | 2014-05-28 | 山东理工大学 | Method for improving polypeptide membrane flexibility by adopting polypropylene glycol and poly trimethylene carbonate |
| CN103865273A (en) * | 2014-03-10 | 2014-06-18 | 山东理工大学 | Method for improving flexibility of polypeptide membrane by polypropylene glycol and poly-trimethylene carbonate |
| CN105542483A (en) * | 2016-03-16 | 2016-05-04 | 山东理工大学 | Method for modifying water resistance and flexibility of polyvinyl alcohol membrane through poly(trimethylene carbonate) and poly(p-dioxanone) |
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: 20170725 |