CN108774389A - A kind of preparation method of antibacterial medical polymer material - Google Patents
A kind of preparation method of antibacterial medical polymer material Download PDFInfo
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- CN108774389A CN108774389A CN201810567049.3A CN201810567049A CN108774389A CN 108774389 A CN108774389 A CN 108774389A CN 201810567049 A CN201810567049 A CN 201810567049A CN 108774389 A CN108774389 A CN 108774389A
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- polymer material
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- polyurethane
- sodium alginate
- antibacterial medical
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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
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Materials For Medical Uses (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of antibacterial medical polymer material, specifically include following steps：Medical polyurethane is dissolved in tetrahydrofuran first, then acetum is added, sodium alginate soln and silane coupling agent is added dropwise, then nano-calcium carbonate is added, cellular Alginate microparticles are made, is attached to polyurethane surface, ethyl orthosilicate is then added dropwise, antibacterial medical polymer material is made in stirring hydrolysis at a certain temperature.Method disclosed by the invention is easy to operate, and medical macromolecular materials mechanical property obtained is good, and biocompatibility is good, and durability is good.
Description
Technical field：
The present invention relates to field of medical materials, are specifically related to a kind of preparation method of antibacterial medical polymer material.
Background technology：
For medical macromolecular materials also at polymer material, it is then to be equipped with other additions using high-molecular compound as matrix
The material that agent is constituted.High molecular material includes natural macromolecular material, such as cotton, fiber crops, silk, hair；By natural polymer raw material
By modified polymer material made of chemical process, such as viscose rayon, acetate fiber, modified starch；By small molecule chemical combination
The synthesis high molecular material that object is synthesized by polymerisation, as acrylic resin, polyurethane resin, butadiene rubber, acrylic acid apply
Material etc..
Medical macromolecular materials be by be directly used in human body or with health it is closely related for the purpose of, therefore to enter face
The material of bed service stage has strict requirements.Medical macromolecular materials generally have the following performance：Resistance to biodeterioration, object
Reason and stable mechanical property, easily processed into type；Material is easy to get, and price is appropriate.
Invention content：
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of preparation sides of antibacterial medical polymer material
Method, this method is easy to operate, and manufacturing cost is low, and medical macromolecular materials mechanical property obtained is good, and biocompatibility is good, durable
Property is good.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of antibacterial medical polymer material, includes the following steps：
(1) medical polyurethane is dissolved in tetrahydrofuran, polyurethane solutions is made, aqueous acetic acid is added, stirs evenly, made
Obtain mixed liquor；
(2) sodium alginate is dissolved in deionized water and sodium alginate soln is made；
(3) sodium alginate soln and silane coupling agent, 2000-5000 revs/min of shape are sequentially added into polyurethane solutions
It is stirred 15-35min under state, nano-calcium carbonate is then added, continues to stir 30min, emulsion is made after stirring；
(4) ethyl orthosilicate is added dropwise into above-mentioned emulsion, is then stirred to react at 80 DEG C, it after reaction, will be anti-
It answers liquid to be cooled to room temperature, is subsequently poured into vessel, solvent is volatilized, form a film, antibacterial medical high score is made in washing, vacuum drying
Sub- material.
As a preferred embodiment of the above technical solution, in step (1), the medical polyurethane, tetrahydrofuran mass ratio be 1：
(10-35)。
As a preferred embodiment of the above technical solution, in step (1), the mass concentration of the aqueous acetic acid is 5-15%.
As a preferred embodiment of the above technical solution, in step (2), the mass concentration of the sodium alginate soln is 3-6%.
As a preferred embodiment of the above technical solution, in step (3), polyurethane, sodium alginate, silane coupling agent, nano-calcium carbonate
The mass ratio of calcium is 8：(0.1-0.4)：0.03:0.1.
As a preferred embodiment of the above technical solution, in step (1), the polyurethane, acetic acid mass ratio 10：(0.5-1).
As a preferred embodiment of the above technical solution, in step (4), the rate of addition of ethyl orthosilicate is 3-5mL/min.
As a preferred embodiment of the above technical solution, in step (4), the rotating speed being stirred to react is 800-1500 revs/min, is stirred
The time for mixing reaction is 10-20h.
As a preferred embodiment of the above technical solution, ethyl orthosilicate, sodium alginate mass ratio be 0.1：(1-5).
The invention has the advantages that：
The present invention uses medical polyurethane to prepare medical macromolecular materials for matrix, in order to improve its compatibility and antibiotic property
Can, medical polyurethane is dissolved in organic solvent by the present invention first, sodium alginate aqueous solution is then added, and nano-calcium carbonate is added
Calcium is crosslinked one layer of porous sodium alginate micro ball in polyurethane surface, can be effectively improved the biocompatibility of matrix；
Ethyl orthosilicate is added dropwise in the present invention, carries out in-situ hydrolysis reaction, silica obtained is in sodium alginate micro ball
Crosslinking and polyurethane surface in hole, medical macromolecular materials mechanical property obtained is good, and durability is good.
Specific implementation mode：
In order to better understand the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
The present invention is released, any restriction will not be constituted to the present invention.
Embodiment 1
A kind of preparation method of antibacterial medical polymer material, includes the following steps：
(1) medical polyurethane is dissolved in tetrahydrofuran, polyurethane solutions is made, the acetic acid water that mass concentration is 5% is added
Solution stirs evenly, and mixed liquor is made；Wherein, medical polyurethane, tetrahydrofuran mass ratio be 1：10；Polyurethane, acetic acid
Mass ratio 10：0.5；
(2) sodium alginate is dissolved in deionized water and the sodium alginate soln that mass concentration is 3-6% is made；
(3) sodium alginate soln and silane coupling agent are sequentially added into polyurethane solutions, are stirred in the state of 2000 revs/min
Mixing 15min is mixed, nano-calcium carbonate is then added, continues to stir 30min, emulsion is made after stirring；Wherein, poly- ammonia
Ester, sodium alginate, silane coupling agent, nano-calcium carbonate mass ratio be 8：0.1：0.03:0.1；
(4) ethyl orthosilicate is added dropwise into above-mentioned emulsion, 10h is then stirred to react under 80 DEG C, 800 revs/min, reacts
After, reaction solution is cooled to room temperature, is subsequently poured into vessel, solvent is volatilized, is formed a film, washing, vacuum drying are made anti-
Bacterium medical macromolecular materials；Wherein, the rate of addition of silester is 3mL/min.
Embodiment 2
A kind of preparation method of antibacterial medical polymer material, includes the following steps：
(1) medical polyurethane is dissolved in tetrahydrofuran, polyurethane solutions is made, the acetic acid water that mass concentration is 15% is added
Solution stirs evenly, and mixed liquor is made；Wherein, medical polyurethane, tetrahydrofuran mass ratio be 1：35；Polyurethane, acetic acid
Mass ratio 10：1；
(2) sodium alginate is dissolved in deionized water and the sodium alginate soln that mass concentration is 3-6% is made；
(3) sodium alginate soln and silane coupling agent are sequentially added into polyurethane solutions, are stirred in the state of 5000 revs/min
Mixing 35min is mixed, nano-calcium carbonate is then added, continues to stir 30min, emulsion is made after stirring；Wherein, poly- ammonia
Ester, sodium alginate, silane coupling agent, nano-calcium carbonate mass ratio be 8：0.4：0.03:0.1；
(4) ethyl orthosilicate is added dropwise into above-mentioned emulsion, 20h is then stirred to react under 80 DEG C, 1500 revs/min, instead
After answering, reaction solution is cooled to room temperature, is subsequently poured into vessel, solvent is volatilized, is formed a film, washing, vacuum drying are made
Antibacterial medical polymer material；Wherein, the rate of addition of silester is 5mL/min.
Embodiment 3
A kind of preparation method of antibacterial medical polymer material, includes the following steps：
(1) medical polyurethane is dissolved in tetrahydrofuran, polyurethane solutions is made, the acetic acid water that mass concentration is 7% is added
Solution stirs evenly, and mixed liquor is made；Wherein, medical polyurethane, tetrahydrofuran mass ratio be 1：15；Polyurethane, acetic acid
Mass ratio 10：0.6
(2) sodium alginate is dissolved in deionized water and the sodium alginate soln that mass concentration is 4% is made；
(3) sodium alginate soln and silane coupling agent are sequentially added into polyurethane solutions, are stirred in the state of 2500 revs/min
Mixing 20min is mixed, nano-calcium carbonate is then added, continues to stir 30min, emulsion is made after stirring；Wherein, poly- ammonia
Ester, sodium alginate, silane coupling agent, nano-calcium carbonate mass ratio be 8：0.2：0.03:0.1；
(4) ethyl orthosilicate is added dropwise into above-mentioned emulsion, 12h is then stirred to react under 80 DEG C, 100 revs/min, reacts
After, reaction solution is cooled to room temperature, is subsequently poured into vessel, solvent is volatilized, is formed a film, washing, vacuum drying are made anti-
Bacterium medical macromolecular materials；Wherein, the rate of addition of silester is 3.5mL/min.
Embodiment 4
A kind of preparation method of antibacterial medical polymer material, includes the following steps：
(1) medical polyurethane is dissolved in tetrahydrofuran, polyurethane solutions is made, the acetic acid water that mass concentration is 9% is added
Solution stirs evenly, and mixed liquor is made；Wherein, medical polyurethane, tetrahydrofuran mass ratio be 1：20；Polyurethane, acetic acid
Mass ratio 10：0.7
(2) sodium alginate is dissolved in deionized water and the sodium alginate soln that mass concentration is 4.5% is made；
(3) sodium alginate soln and silane coupling agent are sequentially added into polyurethane solutions, are stirred in the state of 3000 revs/min
Mixing 20min is mixed, nano-calcium carbonate is then added, continues to stir 30min, emulsion is made after stirring；Wherein, poly- ammonia
Ester, sodium alginate, silane coupling agent, nano-calcium carbonate mass ratio be 8：0.2：0.03:0.1；
(4) ethyl orthosilicate is added dropwise into above-mentioned emulsion, 14h is then stirred to react under 80 DEG C, 1200 revs/min, instead
After answering, reaction solution is cooled to room temperature, is subsequently poured into vessel, solvent is volatilized, is formed a film, washing, vacuum drying are made
Antibacterial medical polymer material；Wherein, the rate of addition of silester is 4mL/min.
Embodiment 5
A kind of preparation method of antibacterial medical polymer material, includes the following steps：
(1) medical polyurethane is dissolved in tetrahydrofuran, polyurethane solutions is made, the acetic acid water that mass concentration is 9% is added
Solution stirs evenly, and mixed liquor is made；Wherein, medical polyurethane, tetrahydrofuran mass ratio be 1：20；Polyurethane, acetic acid
Mass ratio 10：0.7；
(2) sodium alginate is dissolved in deionized water and the sodium alginate soln that mass concentration is 5% is made；
(3) sodium alginate soln and silane coupling agent are sequentially added into polyurethane solutions, are stirred in the state of 4000 revs/min
Mixing 30min is mixed, nano-calcium carbonate is then added, continues to stir 30min, emulsion is made after stirring；Wherein, poly- ammonia
Ester, sodium alginate, silane coupling agent, nano-calcium carbonate mass ratio be 8：0.3：0.03:0.1；
(4) ethyl orthosilicate is added dropwise into above-mentioned emulsion, 16h is then stirred to react under 80 DEG C, 1300 revs/min, instead
After answering, reaction solution is cooled to room temperature, is subsequently poured into vessel, solvent is volatilized, is formed a film, washing, vacuum drying are made
Antibacterial medical polymer material；Wherein, the rate of addition of silester is 4mL/min.
Embodiment 6
A kind of preparation method of antibacterial medical polymer material, includes the following steps：
(1) medical polyurethane is dissolved in tetrahydrofuran, polyurethane solutions is made, the acetic acid water that mass concentration is 13% is added
Solution stirs evenly, and mixed liquor is made；Wherein, medical polyurethane, tetrahydrofuran mass ratio be 1：30；Polyurethane, acetic acid
Mass ratio 10：0.8；
(2) sodium alginate is dissolved in deionized water and the sodium alginate soln that mass concentration is 5.5% is made；
(3) sodium alginate soln and silane coupling agent are sequentially added into polyurethane solutions, are stirred in the state of 4500 revs/min
Mixing 30min is mixed, nano-calcium carbonate is then added, continues to stir 30min, emulsion is made after stirring；Wherein, poly- ammonia
Ester, sodium alginate, silane coupling agent, nano-calcium carbonate mass ratio be 8：0.35：0.03:0.1；
(4) ethyl orthosilicate is added dropwise into above-mentioned emulsion, 18h is then stirred to react under 80 DEG C, 1300 revs/min, instead
After answering, reaction solution is cooled to room temperature, is subsequently poured into vessel, solvent is volatilized, is formed a film, washing, vacuum drying are made
Antibacterial medical polymer material；Wherein, the rate of addition of silester is 4.5mL/min.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of antibacterial medical polymer material, which is characterized in that include the following steps：
(1) medical polyurethane is dissolved in tetrahydrofuran, polyurethane solutions is made, aqueous acetic acid is added, stirs evenly, be made mixed
Close liquid；
(2) sodium alginate is dissolved in deionized water and sodium alginate soln is made；
(3) sodium alginate soln and silane coupling agent are sequentially added into polyurethane solutions, in the state of 2000-5000 revs/min
It is stirred 15-35min, nano-calcium carbonate is then added, continues to stir 30min, emulsion is made after stirring；
(4) ethyl orthosilicate is added dropwise into above-mentioned emulsion, is then stirred to react at 80 DEG C, after reaction, by reaction solution
It is cooled to room temperature, is subsequently poured into vessel, solvent is volatilized, form a film, antibacterial medical macromolecule material is made in washing, vacuum drying
Material.
2. a kind of preparation method of antibacterial medical polymer material as described in claim 1, it is characterised in that：In step (1),
The medical polyurethane, tetrahydrofuran mass ratio be 1：(10-35).
3. a kind of preparation method of antibacterial medical polymer material as described in claim 1, it is characterised in that：In step (1),
The mass concentration of the aqueous acetic acid is 5-15%.
4. a kind of preparation method of antibacterial medical polymer material as described in claim 1, it is characterised in that：In step (2),
The mass concentration of the sodium alginate soln is 3-6%.
5. a kind of preparation method of antibacterial medical polymer material as described in claim 1, it is characterised in that：In step (3),
Polyurethane, sodium alginate, silane coupling agent, nano-calcium carbonate mass ratio be 8：(0.1-0.4)：0.03:0.1.
6. a kind of preparation method of antibacterial medical polymer material as described in claim 1, it is characterised in that：In step (1),
The mass ratio 10 of the polyurethane, acetic acid：(0.5-1).
7. a kind of preparation method of antibacterial medical polymer material as described in claim 1, it is characterised in that：In step (4),
The rate of addition of ethyl orthosilicate is 3-5mL/min.
8. a kind of preparation method of antibacterial medical polymer material as described in claim 1, it is characterised in that：In step (4),
The rotating speed being stirred to react is 800-1500 revs/min, and the time being stirred to react is 10-20h.
9. a kind of preparation method of antibacterial medical polymer material as described in claim 1, it is characterised in that：Positive silicic acid second
Ester, sodium alginate mass ratio be 0.1：(1-5).
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| CN201810567049.3A CN108774389A (en) | 2018-06-05 | 2018-06-05 | A kind of preparation method of antibacterial medical polymer material |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980697A (en) * | 2013-06-07 | 2014-08-13 | 安徽大学 | Nanosilicon dioxide modified polyurethane elastomer and preparation method thereof |
| CN104151465A (en) * | 2014-07-26 | 2014-11-19 | 哈尔滨工业大学 | Method for preparing PAN (polyacrylonitrile)-g-SiO2 polymer based on synchronous in-situ hydrolysis of PAN and TEOS (tetraethyl orthosilicate) |
| CN106563398A (en) * | 2016-10-28 | 2017-04-19 | 佛山科学技术学院 | Preparation method of organic/inorganic composite microspheres with raspberry-like structures and application thereof |
| CN107793743A (en) * | 2017-11-14 | 2018-03-13 | 安徽省健源医疗器械设备有限公司 | A kind of antibacterial medical polymer material and preparation method thereof |
| CN107880532A (en) * | 2017-11-23 | 2018-04-06 | 马鞍山菌菌食品科技有限公司 | A kind of sodium alginate cross-linking dendritic macromole/aqueous polyurethane preservative film and preparation method thereof |
-
2018
- 2018-06-05 CN CN201810567049.3A patent/CN108774389A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980697A (en) * | 2013-06-07 | 2014-08-13 | 安徽大学 | Nanosilicon dioxide modified polyurethane elastomer and preparation method thereof |
| CN104151465A (en) * | 2014-07-26 | 2014-11-19 | 哈尔滨工业大学 | Method for preparing PAN (polyacrylonitrile)-g-SiO2 polymer based on synchronous in-situ hydrolysis of PAN and TEOS (tetraethyl orthosilicate) |
| CN106563398A (en) * | 2016-10-28 | 2017-04-19 | 佛山科学技术学院 | Preparation method of organic/inorganic composite microspheres with raspberry-like structures and application thereof |
| CN107793743A (en) * | 2017-11-14 | 2018-03-13 | 安徽省健源医疗器械设备有限公司 | A kind of antibacterial medical polymer material and preparation method thereof |
| CN107880532A (en) * | 2017-11-23 | 2018-04-06 | 马鞍山菌菌食品科技有限公司 | A kind of sodium alginate cross-linking dendritic macromole/aqueous polyurethane preservative film and preparation method thereof |
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