CN108504302A - A kind of high molecular bonding film with water-proof function - Google Patents
A kind of high molecular bonding film with water-proof function Download PDFInfo
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- CN108504302A CN108504302A CN201810306371.0A CN201810306371A CN108504302A CN 108504302 A CN108504302 A CN 108504302A CN 201810306371 A CN201810306371 A CN 201810306371A CN 108504302 A CN108504302 A CN 108504302A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J105/00—Adhesives based on polysaccharides or on their derivatives, not provided for in groups C09J101/00 or C09J103/00
- C09J105/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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Abstract
The invention belongs to adhesive technical fields, and in particular to a kind of preparation method of the high molecular bonding film with water-proof function.The present invention includes the processing of substrate, the preparation of solution, the layer assembly of high molecular bonding film, the preparation of macromolecule layer assembly self-supporting film.The bonding film that the method for the present invention provides can be bonded and be stretched in water.After film forming, self-supporting film can be made by adopting stripping with machinery method.For macromolecule self-supporting bonding film obtained after pigskin bonding experiment, it is 44.48 ± 9.79kPa to measure tensile strength.And the high molecular bonding film prepared surveys its transmitance after bonding, with ultraviolet specrophotometer and is more than 60%.The thickness for growing the film in a period is 0.01-50 μm, and the thickness of film increases with being incremented by for period.
Description
Technical field
The invention belongs to field of adhesive technology, and in particular to a kind of system of the high molecular bonding film with water-proof function
Method.
Background technology
In order to solve the prior art it is harsh there are de-alkali additives and not environmentally, the use of bonding film is by shapes of substrates and kind
The limiting of class, non-water-tight problem.The present invention provides a kind of preparation method of the high molecular bonding film with water-proof function.This bonding
Film has preparation process simple and environmentally-friendly, is not limited by substrate, can assemble and can bond etc. in water in aqueous solution
Advantage.In tissue adhesion, clinical medicine etc. has a good application prospect.
Invention content
In order to solve existing technical problem, the present invention provides a kind of system of the high molecular bonding film with water-proof function
Method.The technical solution of use is as follows:
Construct the selection of primitive:
The cation that the present invention uses constructs primitive as the macromolecule containing amino, and mass-volume concentration is 0.5-15mg/
ML, pH value of solution are 4-7;It is the macromolecule containing carboxyl that anion, which constructs primitive, and mass-volume concentration is 0.5-15mg/mL, molten
Liquid pH is 4-7;Catechol group is grafted to by 1- (3- dimethylamino-propyls) -3- ethyl-carbodiimide hydrochlorides (EDC)
On the strand of chitosan (CHI) and Sodium Hyaluronate (HA).
The preparation of bonding film:
(1) cation constructs the preparation of primitive CHI-C solution.
At room temperature, 0.1-15mg CHI are placed in beaker, 10-200mL H is added2O, to dissolving, adjusting pH is for stirring
4-7, it is denoted as solution A.0.01-1g 3,4- dihydroxyphenyl propionic acid is dissolved in 10-200mL H2In O, 0.01-1g is then added
EDC, reaction 0.5-for 24 hours, are denoted as solution B, finally mix A and B solution, and it is 4-7 to adjust pH, and reaction 0.5-is for 24 hours, you can is made
Cation constructs primitive CHI-C solution.The molecular weight ranges of above-mentioned CHI used are 200000-300000.
Further, the mass-volume concentration that cation constructs primitive CHI-C is 0.5-15 mg/mL.
(2) anion constructs the preparation of primitive HA-D solution.
At room temperature, 0.1-15mg HA are dissolved in 10-200mL PBS buffer solution, it is 4-7 to adjust pH, is then added
0.01-1g EDC, reaction 0.5-for 24 hours, are eventually adding 0.01-1g dopamine hydrochlorides, so that pH value of solution is remained 4-7, reaction
0.5–24h.The molecular weight of above-mentioned HA used is 1630000, and the pH of phosphate buffer is 6-8, a concentration of 0.01-0.2mol/
L。
Further, the mass-volume concentration that anion constructs primitive HA-D is 0.5-15 mg/mL.
(3) preparation of the n-layer CHI-C/HA-D multilayer films with water-proof function.
At room temperature, by the processed substrate to be bonded in surface immerse successively the CHI-C solution prepared, deionized water,
0.5-20min is impregnated in deionized water, HA-D solution, deionized water, deionized water obtains one layer as a growth cycle
The waterproof high molecular bonding film that thickness is 0.01-50 μm, is denoted as CHI-C/HA-D;Often increase a growth cycle, bonding film
Thickness increases by 0.01-50 μm, and growth cycle is repeated several times, you can obtaining n-layer has the high molecular bonding film of water-proof function, is denoted as
(CHI-C/HA-D) * n, wherein n are natural number.
(4) base treatment
Water-resistant binder film prepared by the present invention is not limited by shapes of substrates and type, such as glass, plastics, metal
Deng.Wherein, metallic substrates are scrubbed with ethyl alcohol, remove surface impurity;Substrate of glass first cleans 10-20min with EtOH Sonicate,
Then it is 7 to use volume ratio:3 dense H2SO4And H2O2Mixed liquor heating, which is boiled to bubble-free, to be generated, finally by substrate deionization
Water is spare with air blow drying after rinsing.Plastic-substrates use ethyl alcohol, water to be cleaned by ultrasonic respectively.The purpose that substrate is handled is
Increase its surface hydrophilicity, is conducive to constructing for bonding film.
The feasibility of bonding film can be further proved by following two experiments:
1, the bonding of the substrate to be bonded containing bonding film.
This adhesion process can both carry out in air, can also be carried out in water.The growth for taking two panels to be bonded has (CHI-
C/HA-D) the substrate of different shapes of * n bonding films, one drop water of on piece dropwise addition wherein, then by the two substrates to be bonded
It puts well face-to-face, or there is the substrate of different shapes of (CHI-C/HA-D) * n bonding films to be placed directly in water two panels growth,
It is bonded in water, then applies the 1-30min of continuous of 0.01-0.2MPa, keep two substrate bondings to be bonded secured.
Certainly, pressure applied can be with bigger, but excessive pressure may treat certain properties of bonded substrate
It has an impact, or even substrate can be damaged.
2, the stretching of the substrate to be bonded containing bonding film.
Sample after bonding is completed to bond with iron plate in air by commercialized AB glue, this operating process 0-
30min is placed on 0.1-3h in the container of saturated humidity 100RH% after bonding, to ensure that AB glue is fully cured.Then sample is soaked
2-4h under the conditions of 100RH% are ducked in drink or are placed on, to ensure sample by water complete wetting.To finally put in water or
Sample in 100RH% containers takes out, and completes to stretch in air.Time used in entire drawing process is 0.1-2min, with to the greatest extent
Amount ensures that stretching environment is consistent with sample placement environment.
Advantageous effect:
The present invention provides a kind of preparation methods of the high molecular bonding film with water-proof function.Using the method for layer by layer deposition,
It is grafted catechol group in the high polymer main chain with biocompatibility, thickness is made at 0.01-50 μm, can be glued in water
The high molecular bonding film with water-proof function for closing and stretching.It after film forming, adopts and removes with machinery method, self-supporting can be made
Film.
Figure of description:
Fig. 1 is high molecular bonding film parameters prepared by the present invention.
Specific implementation mode:
Carry out the specific implementation that the present invention is furture elucidated below by way of some examples and as a result, rather than with these examples
To limit the present invention.
Embodiment 1:The preparation of 100 layers of CHI-C/HA-D multilayer films with water-proof function.
(1) preparation of cationic primitive CHI-C solution.
At room temperature, 0.1g CHI are placed in beaker, 50mL H is added2O, to dissolving, it is 6.2 to adjust pH, is denoted as stirring
Solution A.0.04g 3,4- dihydroxyphenyl propionic acid is dissolved in 50mL H2In O, 0.0717g EDC are then added, react 3h, note
For solution B.Finally A and B solution are mixed, it is 5 to adjust pH, reacts 3h, you can it is molten that obtained cation constructs primitive CHI-C
Liquid.The molecular weight ranges of above-mentioned CHI used are 200000-300000.
Further, the mass-volume concentration that cation constructs primitive CHI-C is 1mg/mL.
(2) anion constructs the preparation of primitive HA-D solution.
At room temperature, 0.1g HA are dissolved in 100mL PBS buffer solution, it is 5 to reconcile pH, and 0.0433g is then added
EDC reacts 3h, is eventually adding 0.0527g dopamine hydrochlorides, and pH value of solution is made to remain 5, reacts 3h.Point of above-mentioned HA used
Son amount is 1630000, and the pH of phosphate buffer is 6, a concentration of 0.01mol/L.
Further, the mass-volume concentration that anion constructs primitive HA-D is 1mg/mL.
(3) preparation of 100 layers of CHI-C/HA-D multilayer films with water-proof function.
At room temperature, by the processed substrate to be bonded in surface immerse successively the CHI-C solution prepared, deionized water,
5min, 1min, 1min, 5min, 1min, 1min are impregnated in deionized water, HA-D solution, deionized water, deionized water.As one
A growth cycle is denoted as CHI-C/HA-D, and growth cycle is repeated several times, you can obtains 100 layers of macromolecule with water-proof function
Bonding film is denoted as (CHI-C/HA-D) * 100.
(4) base treatment:
The growth for taking two panels to be bonded has the sheet glass of (CHI-C/HA-D) * 100 bonding film, is cut into 5*6mm2, then exist
Two sheet glass intersections are put well in water, it is 5*5mm to make contact area2, then apply the continuous 10min of 0.2MPa, make
Two sheet glass bondings to be bonded are secured.Sample after bonding is impregnated into 4d in deionized water, then passes through commercialized AB
Glue is completed to bond in air with iron plate, and placing 10min in air makes AB glue cure, and then impregnates sample in water
2h, to ensure sample by water complete wetting.To finally sample taking-up in water be put, completes to stretch in air, it is entire to stretch
Time used in process is 2min, and it is 0.68 ± 0.09MPa to measure tensile strength, this is compared with the intensity of hydrogel kPa ranks, tool
There is preferable mechanical performance.
Embodiment 2:The preparation of 150 layers of CHI-C/HA-D multilayer films with water-proof function.
(1) preparation of cationic primitive solution.
At room temperature, 0.1g CHI are placed in beaker, 50mL H is added2O, to dissolving, it is 6.2 to adjust pH, is denoted as stirring
Solution A.0.04g 3,4- dihydroxyphenyl propionic acid is dissolved in 50mL H2In O, 0.0717g EDC are then added, react 3h, note
For solution B, finally A and B solution are mixed, it is 5 to adjust pH, reacts 3h, you can it is molten that obtained cation constructs primitive CHI-C
Liquid.The molecular weight ranges of above-mentioned CHI used are 200000-300000.
Further, the mass-volume concentration that cation constructs primitive CHI-C is 1mg/mL.
(2) anion constructs the preparation of primitive solution.
At room temperature, 0.1g HA are dissolved in 100mL PBS buffer solution, it is 5 to reconcile pH, and 0.0433g is then added
EDC reacts 3h, is eventually adding 0.0527g dopamine hydrochlorides, and pH value of solution is made to remain 5, reacts 3h.Point of above-mentioned HA used
Son amount is 1630000, and the pH of phosphate buffer is 6, a concentration of 0.01mol/L.
Further, the mass-volume concentration that anion constructs primitive HA-D is 1mg/mL.
(3) preparation of 150 layers of CHI-C/HA-D multilayer films with water-proof function.
At room temperature, by the processed substrate to be bonded in surface immerse successively the CHI-C solution prepared, deionized water,
5min, 1min, 1min, 5min, 1min, 1min are impregnated in deionized water, HA-D solution, deionized water, deionized water, as one
A growth cycle is denoted as CHI-C/HA-D, and growth cycle is repeated several times, you can obtains 150 layers of macromolecule with water-proof function
Bonding film is denoted as (CHI-C/HA-D) * 150.
The growth for taking two panels to be bonded has the sheet glass of (CHI-C/HA-D) * 150 bonding film, is cut into 5*6mm2, then exist
Two sheet glass intersections are put well in water, it is 5*5mm to make contact area2, then apply the continuous 10min of 0.2MPa, make
Two sheet glass bondings to be bonded are secured.Sample after bonding is impregnated into 4d in deionized water, the sample after bonding is passed through
Commercialized AB glue is completed to bond in air with iron plate, and placing 10min in air makes AB glue cure.Then it is immersed in
2h in water, makes film fully soak, and the tensile strength of survey is 0.75 ± 0.41 MPa.With blade directly by bonding film (CHI-C/HA-
D it) * 150 peels off from the substrate and has just obtained self-supporting film.
(4) pigskin adhesive test.
In order to prove that self-supporting bonding film has good biocompatibility, we select and pigskin similar in tissue
As experimental subjects.Prepared (CHI-C/HA-D) * 100 self-supporting bonding film is cut into 5*5mm by us2Size, in water and
Pigskin is bonded together under the continuous of 0.2MPa, it is 44.48 ± 9.79kPa then to measure its tensile strength, is more than quotient
Adhesive strength (the Int.J.Adhes. of Fibrin Glue (fibrin glues) 0.002-0.040MPa of industry
Adhes.1997,17:127.)。
The above-mentioned high molecular bonding film prepared is surveyed its transmitance after bonding, with ultraviolet specrophotometer and is more than
60%.
Embodiment 3:The preparation of 200 layers of CHI-C/HA-D multilayer films with water-proof function.
(1) preparation of cationic primitive solution.
At room temperature, 0.1g CHI are placed in beaker, 50mL H is added2O, to dissolving, it is 6.2 to adjust pH, is denoted as stirring
Solution A.0.04g 3,4- dihydroxyphenyl propionic acid is dissolved in 50mL H2In O, 0.0717g EDC are then added, react 3h, note
For solution B, finally A and B solution are mixed, it is 5 to adjust pH, reacts 3h, you can it is molten that obtained cation constructs primitive CHI-C
Liquid.The molecular weight ranges of above-mentioned CHI used are 200000-300000.
Further, the mass-volume concentration that cation constructs primitive CHI-C is 1mg/mL.
(2) anion constructs the preparation of primitive solution.
At room temperature, 0.1g HA are dissolved in 100mL PBS buffer solution, it is 5 to reconcile pH, and 0.0433g is then added
EDC reacts 3h, is eventually adding 0.0527g dopamine hydrochlorides, and pH value of solution is made to remain 5, reacts 3h.Point of above-mentioned HA used
Son amount is 1630000, and the pH of phosphate buffer is 6, a concentration of 0.01mol/L.
Further, the mass-volume concentration that anion constructs primitive HA-D is 1mg/mL.
(3) preparation of 200 layers of CHI-C/HA-D multilayer films with water-proof function.
At room temperature, by the processed substrate to be bonded in surface immerse successively the CHI-C solution prepared, deionized water,
5min, 1min, 1min, 5min, 1min, 1min are impregnated in deionized water, HA-D solution, deionized water, deionized water.As one
A growth cycle is denoted as CHI-C/HA-D, and growth cycle is repeated several times, you can obtains 200 layers of macromolecule with water-proof function
Bonding film is denoted as (CHI-C/HA-D) * 200.
The growth for taking two panels to be bonded has the sheet glass of (CHI-C/HA-D) * 200 bonding film, is cut into 5*6mm2, then exist
Two sheet glass intersections are put well in water, it is 5*5mm to make contact area2, then apply the continuous 10min of 0.2MPa, make
Two sheet glass bondings to be bonded are secured.Sample after bonding is impregnated into 4d in deionized water, then passes through commercialized AB
Glue is completed to bond in air with iron plate, and placing 10min in air makes AB glue cure.Then 2h in water is impregnated, film is made
Fully wetting, it is 0.73 ± 0.24MPa to measure tensile strength.
Claims (9)
1. a kind of high molecular bonding film with water-proof function, in tissue adhesion, clinical medicine etc. has good application
Foreground.It is characterized in that:The structure of high molecular bonding film contains catechol group, and the structure being further grafted is 3,4- dihydroxyphenyls
Base propionic acid and dopamine.
2. the high molecular bonding film with water-proof function as described in claim 1, it is characterised in that:Preparing has water-proof function
The method of high molecular bonding film be layer by layer deposition.
3. the high molecular bonding film with water-proof function as described in claim 1, it is characterised in that:The cation constructs base
Member is the macromolecule containing amino, and mass-volume concentration is 0.5-15mg/mL, and pH value of solution is 4-7;Anion construct primitive be containing
It is 0.5-15mg/mL to have the macromolecule of carboxyl, mass-volume concentration, and pH value of solution is 4-7.
4. the high molecular bonding film with water-proof function as described in claim 1, it is characterised in that:Grow the film in a period
Thickness is 0.05-10 μm, and the thickness of film increases with being incremented by for period.
5. the high molecular bonding film with water-proof function as described in claim 1, it is characterised in that:Pass through 1- (3- diformazan ammonia
Base propyl) catechol group is grafted to chitosan (CHI) and Sodium Hyaluronate by -3- ethyl-carbodiimide hydrochlorides (EDC)
(HA) on strand.
6. the high molecular bonding film with water-proof function as described in claim 1, it is characterised in that:What is prepared has waterproof work(
The high molecular bonding film of energy can be bonded and be stretched in water.
7. the high molecular bonding film with water-proof function as described in claim 1, it is characterised in that:The processing of substrate, metal
Substrate is scrubbed with ethyl alcohol, removes surface impurity;Substrate of glass is first cleaned 10-20 minutes with EtOH Sonicate, and volume is then used
Than being 7:3 dense H2SO4And H2O2Mixed liquor heating, which is boiled to bubble-free, to be generated, and is used after finally rinsing substrate with deionized water
Air blow drying is spare;Plastic-substrates use ethyl alcohol, water to be cleaned by ultrasonic respectively.
8. the high molecular bonding film with water-proof function as described in claim 1, it is characterised in that:It is carried out using mechanical means
Stripping, can be made self-supporting bonding film.
9. the high molecular bonding film with water-proof function as described in claim 1, it is characterised in that:When film is grown, every layer
Film all contains catechol group.
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CN109485882A (en) * | 2018-10-08 | 2019-03-19 | 长春理工大学 | A kind of preparation method of self-supporting film |
CN110903411A (en) * | 2019-12-10 | 2020-03-24 | 中国科学院兰州化学物理研究所 | Adhesive hydroxybutyl chitosan, preparation method thereof, reversible adhesive wound dressing applicable to aged skin and preparation method thereof |
CN111411384A (en) * | 2019-01-07 | 2020-07-14 | 长春理工大学 | Method for preparing transparent self-supporting film |
CN111411385A (en) * | 2019-01-07 | 2020-07-14 | 长春理工大学 | Preparation method of self-supporting latex film |
CN112062985A (en) * | 2019-06-10 | 2020-12-11 | 长春理工大学 | Method for preparing self-supporting film |
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CN111411385A (en) * | 2019-01-07 | 2020-07-14 | 长春理工大学 | Preparation method of self-supporting latex film |
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CN110903411A (en) * | 2019-12-10 | 2020-03-24 | 中国科学院兰州化学物理研究所 | Adhesive hydroxybutyl chitosan, preparation method thereof, reversible adhesive wound dressing applicable to aged skin and preparation method thereof |
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