CN109550073A - A kind of photo-thermal anti-bacterial hydrogel dressing and preparation method thereof - Google Patents

A kind of photo-thermal anti-bacterial hydrogel dressing and preparation method thereof Download PDF

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CN109550073A
CN109550073A CN201811166462.5A CN201811166462A CN109550073A CN 109550073 A CN109550073 A CN 109550073A CN 201811166462 A CN201811166462 A CN 201811166462A CN 109550073 A CN109550073 A CN 109550073A
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sodium alginate
preparation
bacterial hydrogel
acrylamide
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宁成云
张珂嘉
周正难
王珍高
代聪
姚甜甜
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Foshan Huajian Technology Co Ltd
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Foshan Huajian Technology Co Ltd
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Abstract

The invention belongs to the technical field of medical material, a kind of photo-thermal anti-bacterial hydrogel dressing and preparation method thereof is disclosed.Method: (1) by tungsten disulfide ultrasonic disperse in sodium alginate soln in, mixed solution is obtained;(2) mixed solution is mixed with acrylamide, crosslinking agent, initiator, obtains pre-polymerization liquid;(3) pre-polymerization liquid is subjected to plastic, obtains photo-thermal anti-bacterial hydrogel dressing.Present invention ultrasound removing tungsten disulfide, effect for removing dispersion in sodium alginate soln is good;By being used in combination tungsten disulfide and sodium alginate and acrylamide, obtained aerogel dressing not only has excellent mechanical property, while having excellent photo-thermal antibacterial effect.Method of the invention is simple, and aerogel dressing yield is big and stablizes.

Description

A kind of photo-thermal anti-bacterial hydrogel dressing and preparation method thereof
Technical field
The invention belongs to the technical fields of biomaterial for medical purpose, and in particular to a kind of photo-thermal antiseptic dressing and its preparation side Method.
Background technique
Skin is to protect internal organ from external environmental interference and the important natural barrier organ for preventing from being dehydrated in vivo, after damage Its protection mechanism can be lost.The wound infection as caused by bacterium is one of postoperative most common complication.In case of this feelings Condition, microorganism are easy to invade and initially form bacterium colony, so as to cause serious wound infection, hinder agglutination, or even cause The complication of threat to life.In addition, serious wounds dehydration can interfere preferably wet healing environment and delay wound healing.Cause This, is making great efforts to develop for protecting damaged skin from the new material that infects and be dehydrated.Traditional dry dressing such as cotton, day So or bandage and gauze are synthesized for being initially important wound healing phase, but they are dry and cannot provide tide Wet environment, and they are also often susceptible to adhere to dry wound surface and finally cause wound after its removal.In order to gram These disadvantages are taken, have been grown up various wet dressings by the researcher that wet wound healing concept inspires.Wherein, it especially closes Gel is filled the water, because they can keep moist environment in wound interface, allows gas exchanges, plays the barrier to microorganism Effect, removes excessive exudate, has excellent biocompatibility, promotes the quick healing of wound, easily remove hurtless measure.
Conventional hydrogel is made of natural or synthetic polymer, and typically exhibits the mechanical performance of relative mistake and small Balance-swelling ratio, which has limited their practical applications as dressing.
Dressing of the invention is aerogel dressing, has excellent elasticity and tensile property, can be bonded wound well, and Synchronous body movement;And under the irradiation of near infrared light, good photo-thermal antibacterial effect is shown, prevents the bacterium sense of wound Dye.The present invention causes plastic using heat, and process is simple, easy to operate, and yield is big and stablizes, excellent in mechanical performance, photo-thermal antibacterial Effect is obvious, solves defect and deficiency of the existing technology.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art, the purpose of the present invention is to provide a kind of photo-thermal anti-bacterial hydrogels to apply The preparation method of material.The present invention is obtained two-dimensional material and is uniformly dispersed by the thinned tungsten disulfide of ultrasound in sodium alginate soln Sodium alginate soln, by heat cause, preparation doping tungsten disulfide two-dimensional material sodium alginate-acrylamide gel apply Material.Prepared aerogel dressing has good mechanical property and good light thermal property.Aerogel dressing pair of the invention Wound has extraordinary antibacterial effect, while having excellent biocompatibility, promotes the quick healing of wound, easily removes Hurtless measure, and there is excellent mechanical property.
Another object of the present invention is to provide the hydrogels prepared by the above method with photo-thermal anti-microbial property Dressing.Hydrogel of the invention has elasticity and tensile property well, can be bonded wound, and synchronous body movement well, Under the irradiation of near infrared light, good photo-thermal antibacterial effect is shown, the bacterium infection of wound is prevented.Photo-thermal of the invention is anti- Bacterium aerogel dressing can prevent wound postoperative infection.
In order to achieve the purpose that invention, the technical solution adopted by the present invention is that:
A kind of preparation method of photo-thermal anti-bacterial hydrogel dressing, includes the following steps:
(1) by tungsten disulfide ultrasonic disperse in sodium alginate soln, mixed solution is obtained;
(2) mixed solution is mixed with acrylamide, crosslinking agent, initiator, obtains pre-polymerization liquid;
(3) pre-polymerization liquid is subjected to plastic, obtains photo-thermal anti-bacterial hydrogel dressing.
Ultrasonic condition described in step (1) is 80~800W, and 20~100Hz, ultrasonic time is 1~100h.
The dosage of tungsten disulfide described in step (1) meets the following conditions: tungsten disulfide accounts for mixed solution gross mass 0.075%~1.5%.
The concentration of sodium alginate is 0.02wt%~5wt% in sodium alginate soln described in step (1).
Mixed solution described in step (1) specifically refers to tungsten disulfide ultrasound removing the low speed in sodium alginate soln Centrifugation, removes unstripped material, then high speed centrifugation, disperses precipitating in sodium alginate soln again, obtains mixed solution; The concentration of sodium alginate of the tungsten disulfide ultrasound removing in sodium alginate soln is 0.02wt%~0.2wt%;By precipitating weight The concentration for being newly scattered in the sodium alginate soln in sodium alginate soln is 1.5wt%~4.8wt%.
The revolving speed of the low-speed centrifugal is 800-2000r/min;The ultracentrifugal revolving speed is 5000-12000r/ Min, the time of low-speed centrifugal are 10-60min, and the ultracentrifugal time is 10~60min.
The dosage of acrylamide described in step (2) is the 6%~18.7% of mixed solution and acrylamide gross mass.
Crosslinking agent described in step (2) is N, N- methylene-bisacrylamide, N hydroxymethyl acrylamide, the initiator For ammonium persulfate or potassium peroxydisulfate.
The dosage of crosslinking agent described in step (2) is the 0.04%~1.2% of acrylamide quality;The dosage of initiator is The 0.05%~0.2% of acrylamide quality.
The temperature of plastic described in step (3) is 40~70 DEG C, and gelation time is 1~5h.
Hydrogel described in step (3) forms in a mold, and plastic is after demoulding with a thickness of 1~3 millimeter.
The photo-thermal anti-bacterial hydrogel dressing is prepared by above-mentioned method.
Photo-thermal antibacterial effect may be implemented in the photo-thermal antiseptic dressing under the conditions of near-infrared, is used for wound dressing.
Present invention ultrasound removing tungsten disulfide, effect for removing dispersion in sodium alginate soln is good;By by curing Tungsten and sodium alginate and acrylamide are used in combination, and obtained aerogel dressing not only has excellent mechanical property, simultaneously With excellent photo-thermal antibacterial effect.Hydrogel of the invention has elasticity and tensile property well, can be bonded wound well Mouthful, and synchronous body movement, under conditions of near-infrared, antibacterial prevents the bacterium infection of wound.Method of the invention is simple, Aerogel dressing yield is big and stablizes, excellent in mechanical performance, and photo-thermal antibacterial effect is obvious.
The invention has the following advantages that
(1) aerogel dressing of the invention has excellent photo-thermal antibacterial effect, realizes the quick antibacterial of wound surface;
(2) method of the invention is simple, and cost is relatively low, can be with large scale preparation and production;
(3) aerogel dressing stable components prepared by, quickly, method safety, yield is big and stablizes, and mechanical property is excellent for sterilization Different, photo-thermal effect is obvious, durable antibacterial effect.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture in embodiment 1 with photo-thermal anti-bacterial hydrogel dressing;
Fig. 2 is the cyclic tension figure in embodiment 1 with photo-thermal anti-bacterial hydrogel dressing;
Fig. 3 is that sodium alginate-acrylamide gel (left side) is added and has photo-thermal in embodiment 1 under illumination condition The optical photograph that anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after bacterium co-cultivation afterwards;
Fig. 4 is that sodium alginate-acrylamide gel (left side) is added and has photo-thermal in embodiment 2 under illumination condition The optical photograph that anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after bacterium co-cultivation afterwards;
Fig. 5 is that sodium alginate-acrylamide gel (left side) is added and has photo-thermal in embodiment 3 under illumination condition The optical photograph that anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after bacterium co-cultivation afterwards;
Fig. 6 is that sodium alginate-acrylamide gel (left side) is added and has photo-thermal in embodiment 4 under illumination condition The optical photograph that anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after bacterium co-cultivation afterwards.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited In this.
Embodiment 1
(1) tungsten disulfide is added in the sodium alginate soln that concentration is 0.025wt% and is mixed, it is then ultrasonic 12h (power 300W, frequency 45Hz) is centrifuged 30min with 1500 revs/min of revolving speeds, takes supernatant, then with 8000 revs/min Clock revolving speed is centrifuged 30min, collects precipitating;Then it disperses precipitating in the sodium alginate soln that concentration is 1.5wt%, is mixed Close solution;Tungsten disulfide concentration in mixed solution is 0.075wt%;
(2) acrylamide is added into mixed solution (acrylamide accounts for mixed solution and acrylamide gross mass 12.5%), be uniformly mixed, be added relative acrylamide's mass 0.06% crosslinking agent N, N- methylene-bisacrylamide and 0.09% thermal initiator ammonium persulfate is uniformly mixed, and obtains pre-polymerization liquid;
(3) pre-polymerization liquid is poured into 5 centimetres of length, it is 5 centimetres wide, with a thickness of in 2 millimeters of molds, the mold of pre-polymerization liquid will be poured into Be put into baking oven, at 50 DEG C, react 2.5 hours plastics, demoulding obtain good mechanical properties with photo-thermal anti-microbial property Aerogel dressing.
Fig. 1 is the low power scanning electron microscope (SEM) photograph in embodiment 1 with photo-thermal anti-bacterial hydrogel dressing;Fig. 2 is light in embodiment 1 The mechanical property of hot anti-bacterial hydrogel dressing is assessed, the cyclic tension figure of aerogel dressing.Fig. 3 is in embodiment 1 in illumination item Under part, sodium alginate-acrylamide gel (left side) is added and has photo-thermal anti-bacterial hydrogel dressing (right side) afterwards and Escherichia coli The optical photograph of the plate coating of bacterium solution after co-cultivation.
Photo-thermal anti-bacterial hydrogel dressing manufactured in the present embodiment is under conditions of illumination, antibiotic rate 100%;And alginic acid Antibiotic rate is 0% to sodium-acrylamide gel (no tungsten disulfide) under light illumination.Two in aerogel dressing manufactured in the present embodiment Tungsten sulfide extent of exfoliation is high, evenly dispersed in aerogel dressing matrix, and performance, which is stablized, has long acting antibiotic effect.
The mechanical experimental results of aerogel dressing manufactured in the present embodiment are as shown in table 1.
The mechanical property parameters of the aerogel dressing of 1 embodiment 1 of table preparation
Embodiment 2
(1) tungsten disulfide is added in the sodium alginate soln that concentration is 0.05wt% and is mixed, then ultrasound 10h (power 500W, frequency 45Hz) is centrifuged 30min with 1500 revs/min of revolving speeds, takes supernatant, then turn with 8000 revs/min Speed centrifugation 30min, collects precipitating;Then it disperses precipitating in the sodium alginate soln that concentration is 1.75wt%, is mixed Solution;Tungsten disulfide concentration in mixed solution is 0.1wt%;
(2) acrylamide is added into mixed solution (acrylamide accounts for mixed solution and acrylamide gross mass 15%) it, is uniformly mixed, crosslinking agent N, the N- methylene-bisacrylamide and 0.09% of relative acrylamide's mass 0.06% is added Thermal initiator ammonium persulfate, be uniformly mixed, obtain pre-polymerization liquid;
(3) pre-polymerization liquid is poured into 5 centimetres of length, it is 5 centimetres wide, with a thickness of in 2 millimeters of molds, the mold of pre-polymerization liquid will be poured into Be put into baking oven, at 50 DEG C, react 2.5 hours plastics, demoulding obtain good mechanical properties with photo-thermal anti-microbial property Aerogel dressing.Fig. 4 is that sodium alginate-acrylamide gel (left side) is added and has light in embodiment 2 under illumination condition The optical photograph that hot anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after Escherichia coli co-cultivation afterwards.
Photo-thermal anti-bacterial hydrogel dressing manufactured in the present embodiment is under conditions of illumination, antibiotic rate 100%;And alginic acid Antibiotic rate is 0% to sodium-acrylamide gel (no tungsten disulfide) under light illumination.Two in aerogel dressing manufactured in the present embodiment Tungsten sulfide extent of exfoliation is high, evenly dispersed in aerogel dressing matrix, and performance, which is stablized, has long acting antibiotic effect.
The mechanical experimental results of aerogel dressing manufactured in the present embodiment are as shown in table 2.
The mechanical property parameters of the aerogel dressing of 2 embodiment 2 of table preparation
Embodiment 3
(1) tungsten disulfide is added in the sodium alginate soln that concentration is 0.1wt% and is mixed, then ultrasound 8h (power 600W, frequency 45Hz) is centrifuged 30min with 1500 revs/min of revolving speeds, takes supernatant, then turn with 8500 revs/min Speed centrifugation 30min, collects precipitating;Then it disperses precipitating in the sodium alginate soln that concentration is 2wt%, it is molten to obtain mixing Liquid;Tungsten disulfide concentration in mixed solution is 0.125wt%;
(2) acrylamide is added into mixed solution (acrylamide accounts for mixed solution and acrylamide gross mass 16%) it, is uniformly mixed, crosslinking agent N, the N- methylene-bisacrylamide and 0.1% of relative acrylamide's mass 0.08% is added Thermal initiator ammonium persulfate, be uniformly mixed, obtain pre-polymerization liquid;
(3) pre-polymerization liquid is poured into 5 centimetres of length, it is 5 centimetres wide, with a thickness of in 2 millimeters of molds, the mold of pre-polymerization liquid will be poured into Be put into baking oven, at 50 DEG C, react 2.5 hours plastics, demoulding obtain good mechanical properties with photo-thermal anti-microbial property Aerogel dressing.Fig. 5 is that sodium alginate-acrylamide gel (left side) is added and has light in embodiment 3 under illumination condition The optical photograph that hot anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after Escherichia coli co-cultivation afterwards.
Photo-thermal anti-bacterial hydrogel dressing manufactured in the present embodiment is under conditions of illumination, antibiotic rate 100%;And alginic acid Antibiotic rate is 0% to sodium-acrylamide gel (no tungsten disulfide) under light illumination.Two in aerogel dressing manufactured in the present embodiment Tungsten sulfide extent of exfoliation is high, evenly dispersed in aerogel dressing matrix, and performance, which is stablized, has long acting antibiotic effect.
The mechanical experimental results of aerogel dressing manufactured in the present embodiment are as shown in table 3.
The mechanical property parameters of the aerogel dressing of 3 embodiment 3 of table preparation
Embodiment 4
(1) tungsten disulfide is added in the sodium alginate soln that concentration is 0.15wt% and is mixed, then ultrasound 8h (power 800W, frequency 45Hz) is centrifuged 30min with 1500 revs/min of revolving speeds, takes supernatant, then turn with 8500 revs/min Speed centrifugation 30min, collects precipitating;Then it disperses precipitating in the sodium alginate soln that concentration is 2.25wt%, is mixed Solution;Tungsten disulfide concentration in mixed solution is 0.15wt%;
(2) acrylamide is added into mixed solution (acrylamide accounts for mixed solution and acrylamide gross mass 18%) it, is uniformly mixed, crosslinking agent N, the N- methylene-bisacrylamide and 0.1% of relative acrylamide's mass 0.08% is added Thermal initiator ammonium persulfate, be uniformly mixed, obtain pre-polymerization liquid;
(3) pre-polymerization liquid is poured into 5 centimetres of length, it is 5 centimetres wide, with a thickness of in 2 millimeters of molds, the mold of pre-polymerization liquid will be poured into It is put into baking oven, at 50 DEG C, reacts 2.5 hours plastics.Demoulding obtain good mechanical properties with photo-thermal anti-microbial property Aerogel dressing.Fig. 6 is that sodium alginate-acrylamide gel (left side) is added and has light in embodiment 4 under illumination condition The optical photograph that hot anti-bacterial hydrogel dressing (right side) is coated with the plate of the bacterium solution after Escherichia coli co-cultivation afterwards.
Photo-thermal anti-bacterial hydrogel dressing manufactured in the present embodiment is under conditions of illumination, antibiotic rate 100%;And alginic acid Antibiotic rate is 0% to sodium-acrylamide gel (no tungsten disulfide) under light illumination.Two in aerogel dressing manufactured in the present embodiment Tungsten sulfide extent of exfoliation is high, evenly dispersed in aerogel dressing matrix, and performance, which is stablized, has long acting antibiotic effect.
The mechanical experimental results of aerogel dressing manufactured in the present embodiment are as shown in table 4.
The mechanical property parameters of the aerogel dressing of 4 embodiment 4 of table preparation
The mechanical property provided from Examples 1 to 4 is it is found that tungsten disulfide extent of exfoliation is high, in aerogel dressing matrix It is evenly dispersed, and there is no the mechanical properties for reducing hydrogel.

Claims (8)

1. a kind of preparation method of photo-thermal anti-bacterial hydrogel dressing, characterized by the following steps:
(1) by tungsten disulfide ultrasonic disperse in sodium alginate soln, mixed solution is obtained;
(2) mixed solution is mixed with acrylamide, crosslinking agent, initiator, obtains pre-polymerization liquid;
(3) pre-polymerization liquid is subjected to plastic, obtains photo-thermal anti-bacterial hydrogel dressing.
2. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 1, it is characterised in that:
The dosage of tungsten disulfide described in step (1) meets the following conditions: tungsten disulfide accounts for the 0.075% of mixed solution gross mass ~1.5%;
The concentration of sodium alginate is 0.02wt%~5wt% in sodium alginate soln described in step (1).
3. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 1, it is characterised in that: described in step (1) Mixed solution specifically refers to remove tungsten disulfide ultrasound in sodium alginate soln, and low-speed centrifugal removes unstripped material, High speed centrifugation again disperses precipitating in sodium alginate soln again, obtains mixed solution.
4. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 3, it is characterised in that: the stripping of tungsten disulfide ultrasound Concentration from the sodium alginate in sodium alginate soln is 0.02wt%~0.2wt%;It disperses alginic acid again by precipitating The concentration of sodium alginate soln in sodium solution is 1.5wt%~4.8wt%;
The revolving speed of the low-speed centrifugal is 800-2000r/min;The ultracentrifugal revolving speed is 5000-12000r/min, low The time of speed centrifugation is 10-60min, and the ultracentrifugal time is 10~60min.
5. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 1, it is characterised in that: described in step (2) The dosage of acrylamide is the 6%~18.7% of mixed solution and acrylamide gross mass.
6. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 1, it is characterised in that: described in step (2) Crosslinking agent is N, and N- methylene-bisacrylamide, N hydroxymethyl acrylamide, the initiator is ammonium persulfate or potassium peroxydisulfate;
The dosage of crosslinking agent described in step (2) is the 0.04%~1.2% of acrylamide quality;The dosage of initiator is propylene The 0.05%~0.2% of amide quality.
7. the preparation method of photo-thermal anti-bacterial hydrogel dressing according to claim 1, it is characterised in that: described in step (1) The condition of ultrasound is 80~800W, and 20~100Hz, ultrasonic time is 1~100h;
The temperature of plastic described in step (3) is 40~70 DEG C, and gelation time is 1~5h.
8. a kind of photo-thermal anti-bacterial hydrogel dressing obtained by any one of claim 1~7 preparation method.
CN201811166462.5A 2018-09-30 2018-09-30 A kind of photo-thermal anti-bacterial hydrogel dressing and preparation method thereof Withdrawn CN109550073A (en)

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CN111773429A (en) * 2020-01-09 2020-10-16 中国科学院长春应用化学研究所 Hydrogel dressing and preparation method thereof, multifunctional nano composite dressing and preparation method and application thereof
CN113384744A (en) * 2021-06-18 2021-09-14 福州大学 WS (WS)2Nano meterSheet/bioglass microsphere composite material and preparation method thereof
CN113476640A (en) * 2021-06-11 2021-10-08 中南大学 Preparation method of antibacterial hydrogel dressing containing heterogeneous ion doped metal sulfide
CN113633627A (en) * 2020-04-24 2021-11-12 华中科技大学 Transparent photothermal antibacterial hydrogel patch, and preparation and application thereof
CN113651919A (en) * 2021-08-30 2021-11-16 上海应用技术大学 Cold-resistant solar-driven photothermal effect hydrogel electrolyte and preparation and application thereof
CN114522271A (en) * 2022-01-14 2022-05-24 江苏大学 Controllable bactericidal composite hydrogel and preparation method and application thereof
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111773429A (en) * 2020-01-09 2020-10-16 中国科学院长春应用化学研究所 Hydrogel dressing and preparation method thereof, multifunctional nano composite dressing and preparation method and application thereof
CN113633627A (en) * 2020-04-24 2021-11-12 华中科技大学 Transparent photothermal antibacterial hydrogel patch, and preparation and application thereof
CN113633627B (en) * 2020-04-24 2023-06-16 华中科技大学 Transparent photo-thermal antibacterial hydrogel patch, preparation and application thereof
CN113476640A (en) * 2021-06-11 2021-10-08 中南大学 Preparation method of antibacterial hydrogel dressing containing heterogeneous ion doped metal sulfide
CN113384744A (en) * 2021-06-18 2021-09-14 福州大学 WS (WS)2Nano meterSheet/bioglass microsphere composite material and preparation method thereof
CN113384744B (en) * 2021-06-18 2022-05-13 福州大学 WS2 nanosheet/bioglass microsphere composite material and preparation method thereof
CN113651919A (en) * 2021-08-30 2021-11-16 上海应用技术大学 Cold-resistant solar-driven photothermal effect hydrogel electrolyte and preparation and application thereof
CN114522271A (en) * 2022-01-14 2022-05-24 江苏大学 Controllable bactericidal composite hydrogel and preparation method and application thereof
CN115317660A (en) * 2022-07-29 2022-11-11 沈阳药科大学 Near-infrared response antibacterial nano composite hydrogel dressing

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