CN102657892B - Preparation method of hydrogel dressing - Google Patents
Preparation method of hydrogel dressing Download PDFInfo
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- CN102657892B CN102657892B CN201210111960.6A CN201210111960A CN102657892B CN 102657892 B CN102657892 B CN 102657892B CN 201210111960 A CN201210111960 A CN 201210111960A CN 102657892 B CN102657892 B CN 102657892B
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Abstract
The invention relates to a preparation method of a hydrogel dressing, comprising the following steps: carrying out cold treatment on a reaction mixed solution to form a viscous colloidal solution, then coating the viscous colloidal solution on a substrate to form a colloid coating, and then carrying out crosslinking reaction on the colloid coating to form a hydrogel layer. According to the invention, by coating the reaction mixed solution on the substrate in the form of colloid to conduct the crosslinking reaction of the colloid coating on the substrate, the hydrogel dressing can be continuously prepared. Therefore, the preparation process of the hydrogel dressing can be simplified to greatly raise the preparation efficiency of the hydrogel dressing, and the hydrogel dressing furthermore can be mass produced.
Description
Technical field
The present invention relates to a kind of preparation method of dressing, and particularly relevant for a kind of preparation method of aerogel dressing.
Background technology
Traditional wound dressing is to consist of natural plant fibre or animal hairs material, and as gauze, cotton pad, Pilus Caprae seu Ovis, all kinds of oil gauzes etc., this class dressing is temporary cladding material, all need within the regular hour, be changed.Yet, these wound dressings easily occur to be mutually stained with glutinous situation with wound when changing, therefore the wound of likely tearing in the lump newborn epithelial cell or heal gradually when removing dressing, causes user pain hard to bear, and is quite unfavorable for naturally restoring of wound.
Compared to traditional wound dressing, that aerogel dressing can provide is preferably ventilative, thoroughly wet, intercept antibacterial and invade and control and absorb the characteristics such as transudate, make wound in good Growth of Cells healing environment.In addition, aerogel dressing can adhere well to wound, and when change dressings more, can not be stained with glutinous wound and cause secondary injury, so aerogel dressing is widely used in medical field.Yet, because hydrogel can present the aqueous solution state that viscosity pole is low before carrying out polyreaction, therefore need splendid attire just can carry out polyreaction in container, and after reacting, need carry out the operations such as multiple tracks cuts to formed hydrogel block, just can produce the aerogel dressing that meets demand thickness and size.In other words, current aerogel dressing manufacturing process have step complicated, need carry out batch producing and cannot be fast and the shortcoming such as productions in a large number, so efficiency is not good.
Summary of the invention
Technical problem solved by the invention is to provide a kind of preparation method of aerogel dressing, is suitable for producing continuously and having preferably preparation efficiency.
The technical solution used in the present invention is:
A preparation method for aerogel dressing, comprises the following steps:
(1) prepare mixed solution, described mixed solution comprises polymerisable monomer, cross-linking agent, polyhydric alcohol and initiator;
(2) mixed solution of step (1) is carried out to cold treatment, cold treatment is carried out under the condition of 0 ℃ to-20 ℃;
(3) colloid solution obtaining after step (2) cold treatment can evenly be coated on base material, form colloid coating; Make colloid coating, under the effect of initiator, cross-linking reaction occur, on base material, form hydrogel layer.
Above-mentioned preparation method, wherein the composition of mixed solution is the chemical raw material material that can cross-linking reaction occur under certain condition and generate hydrogel, comprises polymerisable monomer, cross-linking agent, polyhydric alcohol (playing moisturizing and tackify) and initiator; The concrete material of described composition is selected specifically to select according to the character of the required hydrogel obtaining; The consumption of described composition also can obtain by test.Under room temperature state, the mixed solution of described composition is that stickiness is very low and have an aqueous solution of high fluidity.Need first splendid attire in container, to carry out polyreaction, then after reaction, formed hydrogel block is carried out to the operations such as multiple tracks cuts, just can produce the aerogel dressing that meets demand thickness and size.And preparation method of the present invention is creatively first carried out described mixed solution cold treatment, make its formation there is the colloid solution of the stickiness of 500cps to 5000cps, again it is evenly coated on base material, the production stage such as not only can simplify that the later stage cuts, can also reach and can produce continuously and the technique effect of hydrogel layer coating thickness uniformity.The thickness of the colloid coating that generally the present invention obtains is between 0.05mm to 5mm.
Preparation method of the present invention, in wherein said step (2), the temperature of cold treatment is preferably-20 ℃.
Preparation method of the present invention, the method that wherein said step (1) is prepared mixed solution is included under vacuum polymerisable monomer, cross-linking agent, polyhydric alcohol and initiator described in mix and blend.
Preparation method of the present invention, wherein said polymerisable monomer generates the small molecule monomer compound of gelatinous mass for there is cross-linking reaction.Its alternative is more, as:
2-acrylamide-2-methyl propane sulfonic (2-acrylamido-2-methylpropane sulphonic acid);
2-hydroxyethyl methacry-late (2-hydroxyl ethyl mathacrylate);
Acrylic acid (acrylic acid);
Methacrylic acid (methacrylic acid);
Methacrylate (mathacrylate);
4-acryloyl morpholine (4-acryloymorpholine);
Acrylamide (acrylamide);
Vinylpyrrolidone (vinyl pyrrolide);
Polyethylene acrylate (polyethylene acrylates);
Acrylic acid 3-sulfonic acid propyl ester potassium salt (acrylic acid-(3-sulphopropyl) ester potassium salt);
Polyvinyl alcohol (polyvinyl alcohol);
N,N-DMAA (N, N-dimethylacrylamide);
(3-acrylamide propyl) trimethyl ammonium chloride ((3-acryl-lamidopropyl) trimethyl ammonium chloride);
2-acrylyl oxy-ethyl-trimethyl salmiac ((2-(acryloy-loxy) ethyl) trimethyl ammonium chloride)
Preferably including an ion-type acryl is that monomer (can be dissociated out the monomer solution with electric charge in aqueous solution) is monomer (can be dissociated out uncharged monomer solution in aqueous solution) with a nonionic acryl; The content of described polymerisable monomer in mixed solution is preferably 25 % by weight to 85 % by weight; Wherein ion-type acryl is that the content of monomer in mixed solution is preferably 10 % by weight to 50 % by weight; Nonionic acryl is that the content of monomer in mixed solution is preferably 15 % by weight to 35 % by weight.Ion-type acryl is that monomer comprises 2-acrylamide-2-methyl isophthalic acid-propane sulfonic acid or 2-hydroxyethyl methacrylate etc.Nonionic acryl is that monomer comprises NVP or N,N-DMAA etc.
Preparation method of the present invention, wherein said cross-linking agent is for making the material of above-mentioned polymerisable monomer generation cross-linking reaction polymerization, can be in following substances choice for use:
Tripropylene glycol diacrylate (tripropylene glycerol diacrylate);
Ethylene glycol dimethacrylate (ethylene glycol dimethacrylate);
Triacrylate (triacrylate);
Polyethyleneglycol diacrylate (polyethylene glycol diacrylate);
Methylene diacrylamide (methylene bis acrylamide).
Described cross-linking agent is preferably the difunctionality base esters monomer with unsaturated double-bond, more preferably a polyethyleneglycol diacrylate; The content of described cross-linking agent in mixed solution is preferably 0.01 % by weight to 0.4 % by weight.
Preparation method of the present invention, wherein said polyhydric alcohol mainly plays moisturizing and tackify, as long as the alcohols material that can function as described above can be used, as:
Propylene glycol;
Glycerol (glycerol); Sorbitol (sorbitol);
Polyethylene Glycol (polyethylene glycol);
The content of soluble epoxide ethylene (polyethylene oxide) cross-linking agent in mixed solution is preferably 15 % by weight to 45 % by weight.
Preparation method of the present invention, wherein said initiator is for can cause the initiator of cross-linking reaction under certain condition; The content of described initiator in mixed solution is preferably 0.01 % by weight to 0.2 % by weight.An embodiment for simple and preferred initiator, for adopting light initiator, comprising:
2,2-dimethoxy-1, the two phenyl thiophene (2,2-dimethoxy-1,2-di (phenyl) ethanone) of 2-;
1-hydroxycyclohexylphenylketone (1-Hydroxy-Cyclohexyl Phenyl Ketone);
2-hydroxyl-2-butyrophenone (2-Hydroxy-2-propyl phenyl ketone) etc.
It can be at ultraviolet light wave scope: 240～480nm, and ultraviolet ray intensity is 25～200mW/cm
2, under the irradiation time condition of 20～60 seconds, cause cross-linking reaction and make polymerisable monomer polymerization.
Preparation method of the present invention, wherein said base material is preferably adhesive-bonded fabric or resilient adhesive-bonded fabric and screen cloth.
Preparation method of the present invention, it also comprises the base material side of the aerogel dressing obtaining is attached to the step on a carrier after described step (3).Carrier material comprises polyalkenes thin film or polyurethanes thin film, and the base material side close adhesion by therapeutic medical viscose and aerogel dressing, plays the effect of in use hydrogel layer being protected.
Based on above-mentioned, in the preparation method of the present invention's aerogel dressing, by cold-treating process, make reaction mixture form the colloid solution with stickiness, then with coating method, colloid solution is coated on base material to form colloid coating, then made colloid coating form hydrogel layer by cross-linking reaction.Owing to can reaction mixture being coated on base material by colloidal form, and make colloid coating on base material, carry out cross-linking reaction, therefore can quantity-produced mode make aerogel dressing.Thus, can simplify the manufacturing process of aerogel dressing, significantly to promote the preparation efficiency of aerogel dressing, and then volume production aerogel dressing.
The specific embodiment
For further illustrating the present invention, illustrate with the following Examples:
A preparation method for aerogel dressing, first, carries out step (1), and under vacuum, mix and blend forms reaction mixture, and reaction mixture comprises polymerisable monomer, cross-linking agent, polyhydric alcohol and initiator.Wherein some preferred implementations of the selection of polymerisable monomer, cross-linking agent, polyhydric alcohol and initiator and consumption are as shown in the table:
In the present embodiment, high speed with 500rpm to 1500rpm under vacuum stirs 1 hour evenly to mix by polymerisable monomer, add again such as initiators such as light initiators and continue to mix 1 hour, then adding polyhydric alcohol mixes 1 hour, finally add the cross-linking agent such as difunctionality base esters monomer such as unsaturated double-bond to mix 1 hour, to obtain reaction mixture.The stickiness of formed reaction mixture is between 50cps to 500cps.In other words, reaction mixture is that stickiness is very low and have an aqueous solution of high fluidity.
Then, carry out step (2), reaction mixture is carried out to cooling processing, to form colloid solution, wherein cooling temperature is between 0 ℃ to-20 ℃.In the present embodiment, cooling temperature is-20 ℃.The cooling time is the random time between 4 to 12 hours.In detail, be reaction mixture to be placed in the cooling tank of-20 ℃ to 8 hours, to carry out condensation at low temperature.After cooling, by the formed colloid solution of reaction mixture, be the stickiness with 500cps to 5000cps.In other words, carry out after cooling processing, the viscosity of reaction mixture can significantly increase, so reaction mixture is that by the aqueous solution with high fluidity, to become mobility lower but have the colloid solution of spreadable property.
Then, carry out step (3), colloid solution is coated on base material, to form colloid coating.In the present embodiment, base material comprises adhesive-bonded fabric, screen cloth or other suitable substrates.The method of glue coating liquid solution is for example scraper for coating method or other appropriate method.Because colloid solution has suitable stickiness and spreadable property, therefore can easily colloid solution be coated on base material, to form the uniform colloid coating with desired thickness.In the present embodiment, the thickness of colloid coating is between any one thickness between 0.05mm to 5mm.
Then, make colloid coating carry out cross-linking reaction, to form hydrogel layer on base material.In the present embodiment, cross-linking reaction is photopolymerization reaction, and under the ultraviolet radiation of 260nm, light intensity is 25～200mW/cm
2between any one intensity, irradiation time can cause photopolymerization reaction under the condition of 20～60 seconds.After carrying out cross-linking reaction, hydrogel layer is to be transparence, and has suitable thickness, as between 0.05mm to 5mm.Hydrogel layer has can water absorption and biological compatibility.In the present embodiment, the preparation method of aerogel dressing comprises especially base material and the hydrogel layer on it is pasted to and is carried on material, to form the aerogel dressing of taking at any time.Carrying material is for example to comprise polyalkenes thin film, polyurethanes thin film or other suitable thin film.In other words, the hydrogel coating obtaining and base material are attached on a carrier with the base material side.Carrier can be lived with substrate backside close adhesion, on hydrogel, cover the tearable striping of one deck and maybe can tear paper off simultaneously, when not using, avoid like this hydrogel layer to contact with external environment, also avoid destroying the characteristic of hydrogel layer, in use tearable striping or paper are torn off, hydrogel layer is spread on wound, so the polyalkenes thin film of the superiors or polyurethanes thin film have waterproof and breathable effect, internal layer hydrogel is again transparent, situation that can clear view wound healing.The aerogel dressing of the present embodiment in use, tear tearable striping or paper on hydrogel layer off, hydrogel layer is spread on to wound, whole dressing is respectively waterproof and breathable carrier layer (polyalkenes thin film or polyurethanes thin film from top to bottom, both sides are fixed with medical viscose), substrate layer (adhesive-bonded fabric, ventilative) and hydrogel layer.
In original hydrogel manufacture method, owing to can presenting aqueous solution state in order to form the reaction mixture of hydrogel before carrying out polyreaction, therefore need first splendid attire in container, to carry out polyreaction to form hydrogel block, then hydrogel block is cut into the aerogel dressing with suitable thickness and size.Yet, in the present embodiment, via cooling processing, make reaction mixture be condensed into by the aqueous solution with high fluidity the high viscosity colloid solution that mobility is lower.Thus, can directly with coating method, on base material, form the colloid coating with desired thickness, and colloid coating can be carried out cross-linking reaction to form hydrogel layer in base material.That is to say, can on base material, carry out in a continuous manner coating and the polymerization of reaction mixture, to form the hydrogel layer with desired thickness, to complete the making of aerogel dressing.Thus, simplify the making step of aerogel dressing, and significantly promote the preparation efficiency of aerogel dressing.Therefore, the preparation method of the aerogel dressing of the present embodiment is applicable to factory and manufactures aerogel dressing in the automatic mode of serialization, with rapidly and produce in large quantities the aerogel dressing of the hydrogel layer with various different-thickness.
On the other hand, that the aerogel dressing of made provides is preferably ventilative, thoroughly wet, intercept antibacterial and invade and control and absorb the characteristics such as transudate, make wound in good Growth of Cells healing environment.Moreover, because aerogel dressing is transparence, be therefore conducive to directly observe wound healing situation, to control the treatment situation of wound.In addition, aerogel dressing can adhere well to wound, and when change dressings more, can not be stained with glutinous wound and cause secondary injury.Therefore, aerogel dressing can be widely used in raw doctor field.
In sum, in the preparation method of the present invention's aerogel dressing, by cooling processing, reaction mixture is condensed into have the colloid solution of stickiness, therefore can colloid solution be coated on base material to form colloid coating with coating method, and can directly to the colloid coating on base material, carry out cross-linking reaction with formation hydrogel layer.Owing to can reaction mixture being coated on base material by colloidal form, thereby can control easily the thickness of colloid coating, and can continue and carry out cross-linking reaction to form hydrogel layer, therefore can quantity-produced mode make aerogel dressing.Therefore, can significantly promote the processing procedure efficiency of aerogel dressing and be applicable to volume production aerogel dressing.
Above-described embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not departing from the present invention; various distortion and improvement that the common engineers and technicians in this area make technical scheme of the present invention, all should fall in the definite protection domain of claims of the present invention.
Claims (10)
1. a preparation method for aerogel dressing, is characterized in that: comprise the following steps:
(1) prepare mixed solution, described mixed solution comprises polymerisable monomer, cross-linking agent, polyhydric alcohol and initiator;
(2) mixed solution of step (1) is carried out to cold treatment, cold treatment is carried out under the condition of 0 ℃ to-20 ℃;
(3) colloid solution obtaining after step (2) cold treatment is evenly coated on base material, forms colloid coating; Make colloid coating, under the effect of initiator, cross-linking reaction occur, on base material, form hydrogel layer.
2. preparation method according to claim 1, is characterized in that: in described step (2), the temperature of cold treatment is-20 ℃.
3. preparation method according to claim 1, is characterized in that: the method that described step (1) is prepared mixed solution is included under vacuum polymerisable monomer, cross-linking agent, polyhydric alcohol and initiator described in mix and blend.
4. preparation method according to claim 1, is characterized in that: the content of described polymerisable monomer in mixed solution is 25 % by weight to 85 % by weight.
5. preparation method according to claim 1, is characterized in that: described cross-linking agent is one to have the difunctionality base esters monomer of unsaturated double-bond; The content of described cross-linking agent in mixed solution is preferably 0.01 % by weight to 0.4 % by weight.
6. preparation method according to claim 1, is characterized in that: the content of described polyhydric alcohol in mixed solution is 15 % by weight to 45 % by weight.
7. preparation method according to claim 1, is characterized in that: the content of described initiator in mixed solution is 0.01 % by weight to 0.2 % by weight.
8. preparation method according to claim 7, is characterized in that: described initiator is light initiator.
9. preparation method according to claim 1, is characterized in that: described base material is adhesive-bonded fabric or screen cloth.
10. preparation method according to claim 1, is characterized in that: after described step (3), also comprise the base material side of the aerogel dressing obtaining is attached to the step on a carrier.
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| CN201210111960.6A CN102657892B (en) | 2012-04-16 | 2012-04-16 | Preparation method of hydrogel dressing |
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| CN201210111960.6A CN102657892B (en) | 2012-04-16 | 2012-04-16 | Preparation method of hydrogel dressing |
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| CN103044703A (en) * | 2013-01-17 | 2013-04-17 | 古元安 | Preparation processes of porous hydrogel and nonporous hydrogel |
| CN105926056A (en) * | 2016-06-30 | 2016-09-07 | 北京健康广济生物技术有限公司 | Hydrogel fiber production technology and equipment |
| CN109316621A (en) * | 2018-10-15 | 2019-02-12 | 苏州汇涵医用科技发展有限公司 | A kind of preparation method of aerogel dressing |
| CN109432490A (en) * | 2018-10-17 | 2019-03-08 | 苏州汇涵医用科技发展有限公司 | A kind of transparent aquagel and its preparation method and application |
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| US4750482A (en) * | 1982-02-25 | 1988-06-14 | Pfizer Inc. | Hydrophilic, elastomeric, pressure-sensitive adhesive |
| DK0610056T3 (en) * | 1993-02-02 | 2002-09-16 | Johnson & Johnson Consumer | hydrogel dressings |
| AU728281B2 (en) * | 1996-09-23 | 2001-01-04 | Genzyme Corporation | Polymerizable biodegradable polymers including carbonate or dioxanone linkages |
| CN101959539B (en) * | 2008-02-25 | 2014-06-04 | 帝国制药株式会社 | Wound-covering hydrogel material |
| CA2716733A1 (en) * | 2008-02-27 | 2009-09-03 | Athlone Institute Of Technology | Composite gel-based materials |
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