CN106977946A - A kind of method that polypropylene glycol is improved with PPDO to polypropylene sorrel water resistance and compliance - Google Patents
A kind of method that polypropylene glycol is improved with PPDO to polypropylene sorrel water resistance and compliance Download PDFInfo
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- CN106977946A CN106977946A CN201710376555.XA CN201710376555A CN106977946A CN 106977946 A CN106977946 A CN 106977946A CN 201710376555 A CN201710376555 A CN 201710376555A CN 106977946 A CN106977946 A CN 106977946A
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- polypropylene glycol
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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
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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
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- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
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Abstract
The present invention discloses a kind of method that polypropylene glycol is improved with PPDO to polypropylene sorrel water resistance and compliance, using following steps：1）Hydroxy-end capped PPDO monododecyl ether, solvent, condensing agent and polyacrylic acid is added in dry reactor, reacts 2~4 days, obtains polyacrylic acid PPDO graft copolymer；2）Graft copolymer, amino-terminated polypropylene glycol monobutyl ether, solvent and condensing agent are added in dry reactor, reacts 2~4 days, obtains polyacrylic acid polypropylene glycol PPDO dual graft copolymer；3）Dual graft copolymer, polypropylene glycol monobutyl 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 life with PPDO
The biomaterial of thing compatibility and biodegradability, with hydrophobicity and compliance.First PPDO segment is connect
Branch is to obtaining poly acrylic acid-poly Lanthanum Isopropoxide graft copolymer on polyacrylic acid strand, then polypropylene glycol segment is connect
Branch to formed on the polyacrylic acid segment in poly acrylic acid-poly Lanthanum Isopropoxide graft copolymer poly acrylic acid-poly propane diols-
PPDO dual graft copolymer, then adds poly acrylic acid-poly propane diols-poly- to dioxy by polypropylene glycol segment again
Cyclohexanone dual graft copolymer formation blend, is made modified polypropene sorrel, so as to drastically increase polypropylene sorrel
Water resistance and compliance.
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 is improved with PPDO to polypropylene sorrel water resistance and compliance, it is special
Levy and be：The molecular weight of polyacrylic acid segment is 81000~94000, the molecular weight of PPDO segment in Modified Membrane
For 2600~2700, the molecular weight of polypropylene glycol segment is 2300~2400；Its method of modifying uses following steps：
1）The synthesis of poly acrylic acid-poly Lanthanum Isopropoxide graft copolymer：Hydroxy-end capped gather is added in dry reactor
Under Lanthanum Isopropoxide monododecyl ether, solvent, condensing agent and polyacrylic acid, inert atmosphere, in 28~33 DEG C of stirring reactions 2
~4 days, terminating reaction by filtering, dialysis, was dried, obtains object；
2）The synthesis of poly acrylic acid-poly propane diols-PPDO dual graft copolymer：Added in dry reactor poly-
Acrylic acid-PPDO graft copolymer, amino-terminated polypropylene glycol monobutyl ether, solvent and condensing agent, indifferent gas
Under atmosphere, in 27~33 DEG C of stirring reactions 2~4 days, terminating reaction by filtering, dialysis, was dried, obtains object；
3）The preparation for the polypropylene sorrel that polypropylene glycol is improved with PPDO：Polypropylene is added in dry reactor
Under acid-polypropylene glycol-PPDO dual graft copolymer, polypropylene glycol monobutyl ether and solvent, inert atmosphere, in 48~
After 53 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 is improved with PPDO to polypropylene sorrel water resistance and compliance
Method, step 1）In, the mol ratio of PPDO monododecyl ether and polyacrylic acid is 15~25:1.
A kind of described polypropylene glycol is improved with PPDO to polypropylene sorrel water resistance and compliance
Method, step 1）In, condensing agent is usedN,N’- dicyclohexylcarbodiimide,N,N’- DIC or 3- second
Base -1-（3- dimethylaminopropyls）The mol ratio of carbodiimide, condensing agent and polyacrylic acid is 1.06~1.9:1, solvent uses two
Methyl sulfoxide, reactant solution concentration is 5~15 g:100 ml.
A kind of described polypropylene glycol is improved with PPDO to polypropylene sorrel water resistance and compliance
Method, step 2）In, polypropylene glycol monobutyl ether and polyacrylic acid chain in poly acrylic acid-poly Lanthanum Isopropoxide graft copolymer
The mol ratio of section is 15~25:1.
A kind of described polypropylene glycol is improved with PPDO to polypropylene sorrel water resistance and compliance
Method, step 2）In, condensing agent is usedN,N’- dicyclohexylcarbodiimide,N,N’- DIC or 3- second
Base -1-（3- dimethylaminopropyls）Carbodiimide, condensing agent and polypropylene in poly acrylic acid-poly Lanthanum Isopropoxide graft copolymer
The mol ratio of sour 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 polypropylene glycol is improved with PPDO to polypropylene sorrel water resistance and compliance
Method, step 3）In, mass percent of the polypropylene glycol monobutyl ether in Modified Membrane is 2~3%, and solvent is sub- using dimethyl
Sulfone, mixture solution concentration is 25~30 g:100 ml.
Compared with prior art, its advantage is the present invention：
1st, a kind of described polypropylene glycol and PPDO are improved to polypropylene sorrel water resistance and compliance
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 Lanthanum Isopropoxide graft copolymer
15.5 grams of polyacrylic acid are added in dry reactor（Molecular weight is 81000）, 9.4 grams it is hydroxy-end capped poly- to dioxy ring
Hexanone monododecyl ether（Molecular weight is 2600）, 248 ml dimethyl sulfoxide (DMSO)s are added, 0.049 gram is addedN,N’- two hexamethylenes
Under base carbodiimide, inert atmosphere, in 28 DEG C of stirring reactions 2 days, terminating reaction by filtering, dialysis, was dried, obtains target
Thing；
2）The preparation of poly acrylic acid-poly propane diols-PPDO dual graft copolymer
Added in dry reactor 12.1 grams of poly acrylic acid-poly Lanthanum Isopropoxide graft copolymers, 6.5 grams it is amino-terminated
Polypropylene glycol monobutyl ether（Molecular weight is 2300）, 187 ml dimethyl sulfoxide (DMSO)s are added, 0.036 gram is addedN,N’- dicyclohexyl
Under carbodiimide, inert atmosphere, in 27 DEG C of stirring reactions 2 days, terminating reaction by filtering, dialysis, was dried, obtains object；
3）The preparation for the polypropylene sorrel that polypropylene glycol is improved with PPDO
10.1 grams of poly acrylic acid-poly propane diols-PPDO dual graft copolymers and 37 are added in dry reactor
Ml dimethyl sulfoxide solvents, it is another to add the polypropylene glycol monobutyl ether for accounting for Modified Membrane gross weight 2%（Molecular weight is 2300）, indifferent gas
Under atmosphere, mixed 50 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
11.6 ° and 9.1%.
Embodiment 2
1）The preparation of poly acrylic acid-poly Lanthanum Isopropoxide graft copolymer
15 grams of polyacrylic acid are added in dry reactor（Molecular weight is 87000）, 8.9 grams it is hydroxy-end capped poly- to dioxocyclohex
Ketone monododecyl ether（Molecular weight is 2700）, 238 ml dimethyl sulfoxide (DMSO)s are added, 0.028 gram is addedN,N’- diisopropyl
Under carbodiimide, inert 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-PPDO dual graft copolymer
Added in dry reactor 12.2 grams of poly acrylic acid-poly Lanthanum Isopropoxide graft copolymers, 6.4 grams it is amino-terminated
Polypropylene glycol monobutyl ether（Molecular weight is 2400）, 185 ml dimethyl sulfoxide (DMSO)s are added, 0.021 gram is addedN,N’- diisopropyl
Under carbodiimide, inert atmosphere, in 30 DEG C of stirring reactions 3 days, terminating reaction by filtering, dialysis, was dried, obtains object；
3）The preparation for the polypropylene sorrel that polypropylene glycol is improved with PPDO
9.9 grams of poly acrylic acid-poly propane diols-PPDO dual graft copolymers and 36 are added in dry reactor
Ml dimethyl sulfoxide solvents, it is another to add the polypropylene glycol monobutyl ether for accounting for Modified Membrane gross weight 3%（Molecular weight is 2400）, indifferent gas
Under atmosphere, mixed 55 minutes in 50 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
12.5 ° and 10.1%.
Embodiment 3
1）The preparation of poly acrylic acid-poly Lanthanum Isopropoxide graft copolymer
16 grams of polyacrylic acid are added in dry reactor（Molecular weight is 94000）, 8.4 grams it is hydroxy-end capped poly- to dioxocyclohex
Ketone monododecyl ether（Molecular weight is 2700）, 244 ml dimethyl sulfoxide (DMSO)s are added, 0.041 gram of 3- ethyls -1- is added（3- bis-
First aminopropyl）Under carbodiimide, inert atmosphere, in 33 DEG C of stirring reactions 4 days, terminating reaction by filtering, dialysis, was dried, obtained
To object；
2）The preparation of poly acrylic acid-poly propane diols-PPDO dual graft copolymer
Added in dry reactor 11.6 grams of poly acrylic acid-poly Lanthanum Isopropoxide graft copolymers, 5.5 grams it is amino-terminated
Polypropylene glycol monobutyl ether（Molecular weight is 2400）, 173 ml dimethyl sulfoxide (DMSO)s are added, 0.028 gram of 3- ethyls -1- is added（3- bis-
First aminopropyl）Under carbodiimide, inert atmosphere, in 33 DEG C of stirring reactions 4 days, terminating reaction by filtering, dialysis, was dried, obtained
To object；
3）The preparation for the polypropylene sorrel that polypropylene glycol is improved with PPDO
9.5 grams of poly acrylic acid-poly propane diols-PPDO dual graft copolymers and 35 are added in dry reactor
Ml dimethyl sulfoxide solvents, it is another to add the polypropylene glycol monobutyl ether for accounting for Modified Membrane gross weight 2%（Molecular weight is 2400）, indifferent gas
Under atmosphere, mixed 60 minutes in 53 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
13.4 ° and 11.1%.
Claims (6)
1. a kind of method that polypropylene glycol is improved with PPDO to polypropylene sorrel water resistance and compliance, its
It is characterised by：The molecular weight of polyacrylic acid segment is 81000~94000, the molecule of PPDO segment in Modified Membrane
Measure as 2600~2700, the molecular weight of polypropylene glycol segment is 2300~2400；Its modification method uses following steps：
1）The synthesis of poly acrylic acid-poly Lanthanum Isopropoxide graft copolymer：Hydroxy-end capped gather is added in dry reactor
Under Lanthanum Isopropoxide monododecyl ether, solvent, condensing agent and polyacrylic acid, inert atmosphere, in 28~33 DEG C of stirring reactions 2
~4 days, terminating reaction by filtering, dialysis, was dried, obtains object；
2）The synthesis of poly acrylic acid-poly propane diols-PPDO dual graft copolymer：Added in dry reactor poly-
Acrylic acid-PPDO graft copolymer, amino-terminated polypropylene glycol monobutyl ether, solvent and condensing agent, indifferent gas
Under atmosphere, in 27~33 DEG C of stirring reactions 2~4 days, terminating reaction by filtering, dialysis, was dried, obtains object；
3）The preparation for the polypropylene sorrel that polypropylene glycol is improved with PPDO：Polypropylene is added in dry reactor
Under acid-polypropylene glycol-PPDO dual graft copolymer, polypropylene glycol monobutyl ether and solvent, inert atmosphere, in 48~
After 53 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 PPDO are to polypropylene sorrel water resistance and submissive
The method that property is improved, it is characterised in that：Step 1）In, PPDO monododecyl ether and polyacrylic acid rub
You are than being 15~25:1.
3. a kind of polypropylene glycol according to claim 1 and PPDO are to polypropylene sorrel water resistance and soft
The pliable method improved, it is characterised in that：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 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 PPDO are to polypropylene sorrel water resistance and submissive
The method that property is improved, it is characterised in that：Step 2）In, polypropylene glycol monobutyl ether and poly acrylic acid-poly Lanthanum Isopropoxide
The mol ratio of polyacrylic acid segment is 15~25 in graft copolymer:1.
5. a kind of polypropylene glycol according to claim 1 and PPDO are to polypropylene sorrel water resistance and soft
The pliable method improved, it is characterised in that：Step 2）In, condensing agent is usedN,N’- dicyclohexylcarbodiimide,N,N’-
DIC or 3- ethyls -1-（3- dimethylaminopropyls）Carbodiimide, condensing agent is with poly acrylic acid-poly to dioxy ring
The mol ratio of polyacrylic acid segment is 1.06~1.9 in hexanone graft copolymer:1, solvent uses dimethyl sulfoxide (DMSO), and reactant is molten
Liquid concentration is 5~15 g:100 ml.
6. a kind of polypropylene glycol according to claim 1 and PPDO are to polypropylene sorrel water resistance and submissive
The method that property is improved, it is characterised in that：Step 3）In, mass percent of the polypropylene glycol monobutyl ether in Modified Membrane is 2
~3%, solvent uses dimethyl sulfoxide (DMSO), and mixture solution concentration is 25~30 g:100 ml.
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| CN201710376555.XA CN106977946A (en) | 2017-05-25 | 2017-05-25 | A kind of method that polypropylene glycol is improved with PPDO to polypropylene sorrel water resistance and compliance |
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| CN201710376555.XA CN106977946A (en) | 2017-05-25 | 2017-05-25 | A kind of method that polypropylene glycol is improved with PPDO to polypropylene sorrel water resistance and compliance |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486806A (en) * | 2009-02-17 | 2009-07-22 | 四川大学 | Natural polymer / degradable polymer composite material and preparation thereof |
| CN105542207A (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 polypropylene glycol and polypeptide-polyvinylpyrrolidone |
| CN105542482A (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(p-dioxanone) and poly(lactic acid-glycolic acid) |
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- 2017-05-25 CN CN201710376555.XA patent/CN106977946A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486806A (en) * | 2009-02-17 | 2009-07-22 | 四川大学 | Natural polymer / degradable polymer composite material and preparation thereof |
| CN105542207A (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 polypropylene glycol and polypeptide-polyvinylpyrrolidone |
| CN105542482A (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(p-dioxanone) and poly(lactic acid-glycolic acid) |
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Application publication date: 20170725 |