CN108653799B - Preparation method of hydrophilic antibacterial silicone rubber medical dressing - Google Patents
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- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
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- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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Abstract
The invention discloses a preparation method of a hydrophilic antibacterial silicone rubber medical dressing, which specifically comprises the following steps: firstly, preparing a mixed solution of chitosan-coated nano titanium oxide, and then treating silicon rubber by adopting plasma to prepare activated silicon rubber; adding activated silicon rubber into an ethanol solution of a silane coupling agent for treatment, and then placing the treated activated silicon rubber into a succinic acid diimide water solution for stirring treatment to prepare surface modified silicon rubber; and finally, placing the surface modified silicone rubber in a mixed solution of chitosan-coated nano titanium oxide for ultrasonic treatment, taking out, and drying to obtain the medical dressing. The medical dressing prepared by the invention has good hydrophilicity, can effectively promote the healing of the wound surface and the healing quality, has good antibacterial performance, and is simple to prepare and low in preparation cost.
Description
The technical field is as follows:
the invention relates to the field of medical materials, in particular to a preparation method of a hydrophilic antibacterial silicone rubber medical dressing.
Background art:
the medical dressing is used as a covering of a wound, can replace damaged skin to play a role of temporary barrier in the process of wound healing, avoids or controls wound infection, and provides an environment beneficial to wound healing. The market of medical dressings at home and abroad is huge, and the medical dressings in China are greatly increased due to skin injuries caused by accidents or operations for tens of millions of people every year, chronic skin injuries caused by pressure sores, diabetes, varicose veins and other diseases due to aging population and the like.
The traditional dressings are traditional gauze dressings, and the modern dressings are also classified into synthetic fiber dressings, polymeric film dressings and foaming polymer dressings. However, the traditional dressing can cause dehydration on the surface of the wound, easy penetration of bacteria and easy adhesion to the wound during the use process. Therefore, modern dressings are more widely applied, but the modern dressings adopted at present have high preparation cost, poor air permeability and poor functionality.
The invention content is as follows:
the invention aims to provide a preparation method of a hydrophilic antibacterial silicone rubber medical dressing aiming at the defects of the prior art, the medical dressing prepared by the method has a certain protection effect on a wound, can effectively improve the healing speed of the wound, improves the healing quality, and has good antibacterial and anti-inflammatory effects.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a hydrophilic antibacterial silicone rubber medical dressing comprises the following steps:
(1) preparing titanium-containing cyclohexane sol by adopting a sol-gel method; then dissolving chitosan in deionized water to prepare a chitosan solution, slowly dripping the prepared chitosan solution into the prepared titanium-containing cyclohexane sol, stirring while dripping, continuing to stir at the rotating speed of 800 plus one 1500 rpm for 30min after finishing dripping, and preparing a mixed solution of the chitosan-coated nano titanium oxide after stirring;
(2) treating silicon rubber by adopting plasma to prepare activated silicon rubber;
(3) adding the prepared activated silicon rubber into an ethanol solution of a silane coupling agent for surface treatment, then placing the silicon rubber subjected to surface treatment into an aqueous solution of succinic acid diimide, stirring and treating for 1-2 hours at 40-60 ℃, taking out, and drying to prepare surface modified silicon rubber;
(4) and (2) placing the surface modified silicon rubber into the mixed solution of the chitosan-coated nano titanium oxide prepared in the step (1), performing ultrasonic treatment for 1-6min under the power of 500-1000W, taking out, washing to be neutral, and drying to prepare the medical dressing.
Preferably, in the step (1), the specific process of preparing the titanium-containing cyclohexane sol by the sol-gel method comprises the following steps: mixing cyclohexane and absolute ethyl alcohol, stirring uniformly, adding triethylamine dropwise, stirring continuously, adding tetrabutyl titanate dropwise, stirring uniformly, placing the mixed solution in a reaction kettle, sealing, and reacting at 150 ℃ for 20 hours to obtain the catalyst.
Preferably, in the technical scheme, the volume ratio of the cyclohexane to the absolute ethyl alcohol to the triethylamine to the tetrabutyl titanate is 50:5: 1: 1.
preferably, in the step (1), the chitosan aqueous solution has a mass concentration of 7-22%.
Preferably, the mass ratio of the chitosan to the nano titanium oxide is (1.33-2.06): 1.
preferably, in the step (2), the plasma treatment conditions are as follows: the vacuum degree is 10-12Pa, and the treatment time is 10-15 min.
Preferably, in the step (3), the mass ratio of the activated silicone rubber to the silane coupling agent is (6-11): 1.
preferably, in the above technical solution, the mass ratio of the silicone rubber after surface treatment to the succinic acid diimide is 1: (0.03-0.06).
Preferably, the mass ratio of the surface-modified silicone rubber to the chitosan is 1: (0.1-0.5).
The invention has the following beneficial effects:
the silicon rubber is used as a matrix of the medical dressing, the surface of the silicon rubber is provided with some reactive active points after plasma treatment, then the silicon rubber is treated in an absolute ethyl alcohol solution of a silane coupling agent, so that the silane coupling agent is grafted on the surface of the silicon rubber, a reactive group is introduced on the surface of the silicon rubber, finally the silicon rubber is added into an aqueous solution of succinic acid diimide to react at a certain temperature, and the surface of the modified silicon rubber is provided with more active groups;
according to the invention, firstly, a sol-gel method is adopted to prepare titanium-containing sol, then the prepared chitosan solution is dripped, stirred and precipitated, chitosan can be effectively coated on the surface of nano titanium oxide, the dispersibility of the nano titanium oxide is effectively improved, and the chitosan can be grafted on the surface of modified silicon rubber, so that the hydrophilicity and antibacterial performance of a matrix are effectively improved, the healing of a wound surface can be effectively promoted, and the quality of wound healing of the wound surface is improved.
The specific implementation mode is as follows:
in order to better understand the present invention, the following examples further illustrate the invention, the examples are only used for explaining the invention, not to constitute any limitation of the invention.
Example 1
A preparation method of a hydrophilic antibacterial silicone rubber medical dressing comprises the following steps:
(1) preparing titanium-containing cyclohexane sol by adopting a sol-gel method; then dissolving chitosan in deionized water to prepare a chitosan solution with the mass concentration of 7%, slowly dripping the prepared chitosan solution into the prepared titanium-containing cyclohexane sol, stirring while dripping, continuing to stir at the rotating speed of 800 rpm for 30min after dripping is finished, and preparing a mixed solution of chitosan-coated nano titanium oxide after stirring is finished; wherein the mass ratio of the chitosan to the nano titanium oxide is 1.33: 1;
(2) treating silicon rubber by adopting plasma to prepare activated silicon rubber;
(3) adding the prepared activated silicon rubber into an ethanol solution of a silane coupling agent for surface treatment, then placing the silicon rubber subjected to surface treatment into an aqueous solution of succinic acid diimide, stirring and treating for 1h at 40 ℃, taking out, and drying to prepare surface modified silicon rubber; wherein the mass ratio of the activated silicon rubber to the silane coupling agent is 6: 1; the mass ratio of the silicone rubber subjected to surface treatment to the succinic acid diimide is 1: 0.03;
(4) placing the surface-modified silicone rubber into the mixed solution of the chitosan-coated nano titanium oxide prepared in the step (1), performing ultrasonic treatment for 1-6min at the power of 500W, taking out, washing to be neutral, and drying to prepare the medical dressing; wherein the mass ratio of the surface modified silicone rubber to the chitosan is 1: 0.1.
example 2
A preparation method of a hydrophilic antibacterial silicone rubber medical dressing comprises the following steps:
(1) preparing titanium-containing cyclohexane sol by adopting a sol-gel method; then dissolving chitosan in deionized water to prepare a chitosan solution with the mass concentration of 22%, slowly dripping the prepared chitosan solution into the prepared titanium-containing cyclohexane sol, stirring while dripping, continuing to stir at the rotating speed of 1500 rpm for 30min after finishing dripping, and preparing a mixed solution of chitosan-coated nano titanium oxide after stirring; wherein the mass ratio of the chitosan to the nano titanium oxide is 2.06: 1;
(2) treating silicon rubber by adopting plasma to prepare activated silicon rubber;
(3) adding the prepared activated silicon rubber into an ethanol solution of a silane coupling agent for surface treatment, then placing the silicon rubber subjected to surface treatment into an aqueous solution of succinic acid diimide, stirring and treating for 2 hours at 60 ℃, taking out, and drying to prepare surface modified silicon rubber; wherein the mass ratio of the activated silicon rubber to the silane coupling agent is 11: 1; the mass ratio of the silicone rubber subjected to surface treatment to the succinic acid diimide is 1: 0.06;
(4) placing the surface-modified silicone rubber into the mixed solution of the chitosan-coated nano titanium oxide prepared in the step (1), performing ultrasonic treatment for 1-6min at the power of 1000W, taking out, washing to be neutral, and drying to prepare the medical dressing; wherein the mass ratio of the surface modified silicone rubber to the chitosan is 1: 0.5.
example 3
A preparation method of a hydrophilic antibacterial silicone rubber medical dressing comprises the following steps:
(1) preparing titanium-containing cyclohexane sol by adopting a sol-gel method; then dissolving chitosan in deionized water to prepare a chitosan solution with the mass concentration of 10%, slowly dripping the prepared chitosan solution into the prepared titanium-containing cyclohexane sol, stirring while dripping, continuing to stir at the rotating speed of 900 revolutions per minute for 30min after dripping is finished, and preparing a mixed solution of chitosan-coated nano titanium oxide after stirring is finished; wherein the mass ratio of the chitosan to the nano titanium oxide is 1.53: 1;
(2) treating silicon rubber by adopting plasma to prepare activated silicon rubber;
(3) adding the prepared activated silicon rubber into an ethanol solution of a silane coupling agent for surface treatment, then placing the silicon rubber subjected to surface treatment into an aqueous solution of succinic acid diimide, stirring and treating for 1.2 hours at the temperature of 45 ℃, taking out, and drying to prepare surface modified silicon rubber; wherein the mass ratio of the activated silicon rubber to the silane coupling agent is 7: 1; the mass ratio of the silicone rubber subjected to surface treatment to the succinic acid diimide is 1: 0.035;
(4) placing the surface-modified silicone rubber into the mixed solution of the chitosan-coated nano titanium oxide prepared in the step (1), performing ultrasonic treatment for 1-6min at the power of 600W, taking out, washing to be neutral, and drying to prepare the medical dressing; wherein the mass ratio of the surface modified silicone rubber to the chitosan is 1: 0.2.
example 4
A preparation method of a hydrophilic antibacterial silicone rubber medical dressing comprises the following steps:
(1) preparing titanium-containing cyclohexane sol by adopting a sol-gel method; then dissolving chitosan in deionized water to prepare a chitosan solution with the mass concentration of 13%, slowly dripping the prepared chitosan solution into the prepared titanium-containing cyclohexane sol, stirring while dripping, continuing to stir at the rotating speed of 1000 rpm for 30min after dripping is finished, and preparing a mixed solution of chitosan-coated nano titanium oxide after stirring is finished; wherein the mass ratio of the chitosan to the nano titanium oxide is 1.75: 1;
(2) treating silicon rubber by adopting plasma to prepare activated silicon rubber;
(3) adding the prepared activated silicon rubber into an ethanol solution of a silane coupling agent for surface treatment, then placing the silicon rubber subjected to surface treatment into an aqueous solution of succinic acid diimide, stirring and treating for 1.4 hours at 50 ℃, taking out, and drying to prepare surface modified silicon rubber; wherein the mass ratio of the activated silicon rubber to the silane coupling agent is 8: 1; the mass ratio of the silicone rubber subjected to surface treatment to the succinic acid diimide is 1: 0.04;
(4) placing the surface-modified silicone rubber into the mixed solution of the chitosan-coated nano titanium oxide prepared in the step (1), performing ultrasonic treatment for 1-6min at the power of 700W, taking out, washing to be neutral, and drying to prepare the medical dressing; wherein the mass ratio of the surface modified silicone rubber to the chitosan is 1: 0.02.
example 5
A preparation method of a hydrophilic antibacterial silicone rubber medical dressing comprises the following steps:
(1) preparing titanium-containing cyclohexane sol by adopting a sol-gel method; then dissolving chitosan in deionized water to prepare a chitosan solution with the mass concentration of 15%, slowly dripping the prepared chitosan solution into the prepared titanium-containing cyclohexane sol, stirring while dripping, continuing to stir at the rotating speed of 1100 rpm for 30min after finishing dripping, and preparing a mixed solution of chitosan-coated nano titanium oxide after finishing stirring; wherein the mass ratio of the chitosan to the nano titanium oxide is 1.86: 1;
(2) treating silicon rubber by adopting plasma to prepare activated silicon rubber;
(3) adding the prepared activated silicon rubber into an ethanol solution of a silane coupling agent for surface treatment, then placing the silicon rubber subjected to surface treatment into an aqueous solution of succinic acid diimide, stirring and treating for 1.6 hours at 50 ℃, taking out, and drying to prepare surface modified silicon rubber; wherein the mass ratio of the activated silicon rubber to the silane coupling agent is 9: 1; the mass ratio of the silicone rubber subjected to surface treatment to the succinic acid diimide is 1: 0.045;
(4) placing the surface-modified silicone rubber into the mixed solution of the chitosan-coated nano titanium oxide prepared in the step (1), performing ultrasonic treatment for 1-6min at the power of 800W, taking out, washing to be neutral, and drying to prepare the medical dressing; wherein the mass ratio of the surface modified silicone rubber to the chitosan is 1: 0.04.
example 6
A preparation method of a hydrophilic antibacterial silicone rubber medical dressing comprises the following steps:
(1) preparing titanium-containing cyclohexane sol by adopting a sol-gel method; then dissolving chitosan in deionized water to prepare a chitosan solution with the mass concentration of 19%, slowly dripping the prepared chitosan solution into the prepared titanium-containing cyclohexane sol, stirring while dripping, continuing to stir at the rotating speed of 1300 rpm for 30min after finishing dripping, and preparing a mixed solution of chitosan-coated nano titanium oxide after finishing stirring; wherein the mass ratio of the chitosan to the nano titanium oxide is 2.02: 1;
(2) treating silicon rubber by adopting plasma to prepare activated silicon rubber;
(3) adding the prepared activated silicon rubber into an ethanol solution of a silane coupling agent for surface treatment, then placing the silicon rubber subjected to surface treatment into an aqueous solution of succinic acid diimide, stirring and treating for 1.8 hours at 55 ℃, taking out, and drying to prepare surface modified silicon rubber; wherein the mass ratio of the activated silicon rubber to the silane coupling agent is 10: 1; the mass ratio of the silicone rubber subjected to surface treatment to the succinic acid diimide is 1: 0.05;
(4) placing the surface-modified silicone rubber into the mixed solution of the chitosan-coated nano titanium oxide prepared in the step (1), performing ultrasonic treatment for 1-6min at 900W, taking out, washing to be neutral, and drying to prepare the medical dressing; wherein the mass ratio of the surface modified silicone rubber to the chitosan is 1: 0.45.
the above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. A preparation method of a hydrophilic antibacterial silicone rubber medical dressing is characterized by comprising the following steps:
(1) preparing titanium-containing cyclohexane sol by adopting a sol-gel method; then dissolving chitosan in deionized water to prepare a chitosan solution, slowly dripping the prepared chitosan solution into the prepared titanium-containing cyclohexane sol, stirring while dripping, continuing to stir at the rotating speed of 800 plus one 1500 rpm for 30min after finishing dripping, and preparing a mixed solution of the chitosan-coated nano titanium oxide after stirring; the mass ratio of the chitosan to the nano titanium oxide is (1.33-2.06): 1;
(2) treating silicon rubber by adopting plasma to prepare activated silicon rubber; the plasma treatment conditions were: the vacuum degree is 10-12Pa, and the processing time is 10-15 min;
(3) adding the prepared activated silicon rubber into an ethanol solution of a silane coupling agent for surface treatment, then placing the silicon rubber subjected to surface treatment into an aqueous solution of succinic acid diimide, stirring and treating for 1-2 hours at 40-60 ℃, taking out, and drying to prepare surface modified silicon rubber; the mass ratio of the silicone rubber subjected to surface treatment to the succinic acid diimide is 1: (0.03-0.06);
(4) and (2) placing the surface modified silicon rubber into the mixed solution of the chitosan-coated nano titanium oxide prepared in the step (1), performing ultrasonic treatment for 1-6min under the power of 500-1000W, taking out, washing to be neutral, and drying to prepare the medical dressing.
2. The preparation method of the hydrophilic antibacterial silicone rubber medical dressing as claimed in claim 1, wherein in step (1), the specific process of preparing the titanium-containing cyclohexane sol by the sol-gel method comprises: mixing cyclohexane and absolute ethyl alcohol, stirring uniformly, adding triethylamine dropwise, stirring continuously, adding tetrabutyl titanate dropwise, stirring uniformly, placing the mixed solution in a reaction kettle, sealing, and reacting at 150 ℃ for 20 hours to obtain the catalyst.
3. The method for preparing a hydrophilic antibacterial silicone rubber medical dressing as claimed in claim 2, wherein: the volume ratio of the cyclohexane to the absolute ethyl alcohol to the triethylamine to the tetrabutyl titanate is (50: 5: 1): 1.
4. the method for preparing a hydrophilic antibacterial silicone rubber medical dressing as claimed in claim 1, wherein: in the step (1), the mass concentration of the chitosan aqueous solution is 7-22%.
5. The method for preparing a hydrophilic antibacterial silicone rubber medical dressing as claimed in claim 1, wherein: in the step (3), the mass ratio of the activated silicon rubber to the silane coupling agent is (6-11): 1.
6. the method for preparing a hydrophilic antibacterial silicone rubber medical dressing as claimed in claim 1, wherein: the mass ratio of the surface modified silicon rubber to the chitosan is 1: (0.1-0.5).
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| WO2017075320A1 (en) * | 2015-10-31 | 2017-05-04 | Dermalink Technologies, Inc. | Skin adhesives, antimicrobial compositions, articles, and methods for the use thereof |
| CN105831154A (en) * | 2016-04-07 | 2016-08-10 | 济南钛盾生物科技有限公司 | Titanium dioxide antibacterial sol and preparation method thereof |
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