Summary of the invention
The technical problem that the present invention solved provides a kind of method for preparing of aerogel dressing, is suitable for carrying out continuous production and has preferable preparation efficiency.
The technical scheme that the present invention adopts is:
A kind of method for preparing of aerogel dressing may further comprise the steps:
(1) the preparation mixed solution comprises polymerisable monomer, cross-linking agent, polyhydric alcohol and initiator in the said mixed solution;
(2) mixed solution with step (1) carries out cold treatment, and cold treatment is carried out under 0 ℃ to-20 ℃ condition;
(3) colloid solution that obtains after step (2) cold treatment can evenly be coated on the base material, form the colloid coating; Make the colloid coating that cross-linking reaction take place under the effect of initiator, on base material, form hydrogel layer.
Above-mentioned method for preparing, wherein the composition of mixed solution is the chemical raw material material that can cross-linking reaction take place under certain condition and generate hydrogel, comprises polymerisable monomer, cross-linking agent, polyhydric alcohol (plaing a part to preserve moisture and tackify) and initiator; The concrete material of said composition is selected and can be come concrete the selection according to the character of the required hydrogel that obtains; The consumption of said composition also can obtain through test.The mixed solution of said composition is the aqueous solution that stickiness is very low and have high fluidity under the room temperature state.Need first splendid attire in container, to carry out polyreaction, after reaction, formed hydrogel block is carried out operations such as multiple tracks cuts again, just can produce the aerogel dressing that meets demand thickness and size.And method for preparing of the present invention is creatively carried out cold treatment earlier with said mixed solution; Make its formation have the colloid solution of the stickiness of 500cps to 5000cps; Evenly coat it on base material again; Production stage such as not only can simplify that the later stage cuts, but can also reach the technique effect of continuous production and hydrogel layer coating thickness uniformity.The thickness of the colloid coating of the present invention's acquisition is between 0.05mm to 5mm generally speaking.
The temperature of cold treatment is preferably-20 ℃ in the method for preparing of the present invention, wherein said step (2).
The method that method for preparing of the present invention, wherein said step (1) prepare mixed solution is included in the said polymerisable monomer of mixing stirring, cross-linking agent, polyhydric alcohol and initiator under the vacuum.
Method for preparing of the present invention, the small molecule monomer chemical compound that cross-linking reaction generates gelatinous mass for taking place in wherein said polymerisable monomer.Its alternative is more, as:
2-acrylamide-2-methyl propane sulfonic acid (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, and the 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 (in aqueous solution, can be dissociateed the monomer solution that has electric charge) is monomer (in aqueous solution, can be dissociateed uncharged monomer solution) with a nonionic acryl; The content of said polymerisable monomer in mixed solution is preferably 25 weight % to 85 weight %; Wherein the ion-type acryl is that the content of monomer in mixed solution is preferably 10 weight % to 50 weight %; The nonionic acryl is that the content of monomer in mixed solution is preferably 15 weight % to 35 weight %.The ion-type acryl is that monomer comprises 2-acrylamide-2-methyl isophthalic acid-propane sulfonic acid or 2-hydroxyethyl methacrylate etc.The nonionic acryl is that monomer comprises N-vinyl-2-Pyrrolidone or N, N-DMAA etc.
Method for preparing of the present invention, wherein said cross-linking agent can be selected to use in following substances for can make the polymeric material of above-mentioned polymerisable monomer generation cross-linking reaction:
Tripropylene glycol diacrylate (tripropylene glycerol diacrylate);
Ethylene glycol dimethacrylate (ethylene glycol dimethacrylate);
Triacrylate (triacrylate);
Polyethyleneglycol diacrylate (polyethylene glycol diacrylate);
Methylene diacrylamide (methylene bis acrylamide).
Said cross-linking agent be preferably one have a unsaturated double-bond difunctionality base esters monomer, polyethyleneglycol diacrylate more preferably; The content of said cross-linking agent in mixed solution is preferably 0.01 weight % to 0.4 weight %.
Method for preparing of the present invention, wherein said polyhydric alcohol mainly play a part to preserve moisture and tackify, as long as the alcohols material that can function as described above can use, as:
Propylene glycol;
Glycerin (glycerol); Sorbitol (sorbitol);
Polyethylene Glycol (polyethylene glycol);
The content of soluble epoxide ethylene (polyethylene oxide) cross-linking agent in mixed solution is preferably 15 weight % to 45 weight %.
Method for preparing of the present invention, wherein said initiator is for causing the initiator of cross-linking reaction under certain condition; The content of said initiator in mixed solution is preferably 0.01 weight % to 0.2 weight %.A kind of embodiment of simple and preferred initiator for adopting the 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, cause cross-linking reaction under 20~60 seconds the condition of irradiation time and make the polymerisable monomer polymerization.
Method for preparing of the present invention, wherein said base material are preferably adhesive-bonded fabric or resilient adhesive-bonded fabric and screen cloth.
Method for preparing of the present invention, it comprises also that after said step (3) that simultaneously is attached at the step on the carrier with the base material of the aerogel dressing that obtains.Carrier material comprises polyalkenes thin film or polyurethanes thin film, and that one side close adhesion of base material through therapeutic medical viscose and aerogel dressing plays the effect of in use hydrogel layer being protected.
Based on above-mentioned; In the method for preparing of the present invention's aerogel dressing; Make reaction mixture form colloid solution by cold-treating process with stickiness; Then colloid solution is coated on the base material to form the colloid coating, made the colloid coating form hydrogel layer again by cross-linking reaction with coating method.Owing to can reaction mixture be coated on the base material by colloidal form, and make the colloid coating on base material, carry out cross-linking reaction, therefore can the quantity-produced mode make aerogel dressing.Thus, can simplify the manufacturing process of aerogel dressing, significantly promoting the preparation efficiency of aerogel dressing, and then the volume production aerogel dressing.
The specific embodiment
For further specifying the present invention, specify in conjunction with following examples:
A kind of method for preparing of aerogel dressing at first, is carried out step (1), under vacuum, mixes to stir to form 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 with uniform mixing with polymerisable monomer; Add again such as initiators such as light initiators and continue to mix 1 hour; Add polyhydric alcohol then and mixed 1 hour, the cross-linking agent such as difunctionality base esters monomer that add at last such as unsaturated double-bond mixed 1 hour, to obtain reaction mixture.The stickiness of formed reaction mixture is between 50cps to 500cps.In other words, reaction mixture is the aqueous solution that stickiness is very low and have high fluidity.
Then, carry out step (2), reaction mixture is carried out cooling processing, to form colloid solution, wherein refrigerative temperature is between 0 ℃ to-20 ℃.In the present embodiment, refrigerative temperature is-20 ℃.The refrigerative time is the random time between 4 to 12 hours.In detail, be reaction mixture to be placed in-20 ℃ the cooling tank 8 hours, to carry out condensation at low temperature.After cooling, be stickiness with 500cps to 5000cps by the formed colloid solution of reaction mixture.In other words, carry out cooling processing after, the viscosity of reaction mixture can significantly increase, so reaction mixture is to become mobile lower but colloid solution with spreadable property by the aqueous solution with high fluidity.
Then, carry out step (3), colloid solution is coated on the base material, to form the colloid coating.In the present embodiment, base material comprises adhesive-bonded fabric, screen cloth or other suitable substrates.The method of coating colloid solution for example is scraper rubbing method or other appropriate method.Because colloid solution has suitable stickiness and spreadable property, therefore can easily colloid solution be coated on the base material, have the uniform colloid coating of desired thickness with formation.In the present embodiment, the thickness of colloid coating is between any one thickness between the 0.05mm to 5mm.
Then, make the colloid coating carry out cross-linking reaction, on base material, to form hydrogel layer.In the present embodiment, cross-linking reaction is a 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 20~60 seconds condition.After carrying out cross-linking reaction, hydrogel layer is to be transparence, and has suitable thickness, as between 0.05mm to 5mm.But hydrogel layer has water absorption and biological compatibility.In the present embodiment, the method for preparing of aerogel dressing comprises base material and the hydrogel layer on it be pasted to especially carries on the material, to form the aerogel dressing of taking at any time.Carrying material for example is to comprise polyalkenes thin film, polyurethanes thin film or other suitable thin film.In other words, that simultaneously is attached on the carrier with base material with the hydrogel coating that obtains and base material.Carrier can be lived with the substrate backside close adhesion, on hydrogel, covers the tearable striping of one deck simultaneously and maybe can tear paper off, when not using, avoids hydrogel layer to contact with external environment like this; Also avoid destroying the characteristic of hydrogel layer; In use tearable striping or paper are torn off, hydrogel layer is spread on the wound get final product, so the polyalkenes thin film of the superiors or polyurethanes thin film have the waterproof and breathable effect; The internal layer hydrogel is again transparent, situation that can the clear view wound healing.The aerogel dressing of present embodiment in use; Tear tearable striping or paper on the hydrogel layer off; Hydrogel layer is spread on the wound; Whole dressing is respectively waterproof and breathable carrier layer (polyalkenes thin film or polyurethanes thin film, both sides are fixed with medical viscose), substrate layer (adhesive-bonded fabric, ventilative) and hydrogel layer from top to bottom.
In original hydrogel manufacture method; Because the reaction mixture in order to form hydrogel is carrying out can presenting aqueous solution state before the polyreaction; Therefore need first splendid attire in container, to carry out polyreaction, again the hydrogel block is cut into the aerogel dressing with suitable thickness and size to form the hydrogel block.Yet, in the present embodiment, make reaction mixture be condensed into mobile lower high viscosity colloid solution by aqueous solution with high fluidity via cooling processing.Thus, can directly on base material, form colloid coating, and the colloid coating can be carried out cross-linking reaction to form hydrogel layer in base material with desired thickness with coating method.That is to say, can on base material, carry out the coating and the polymerization of reaction mixture by continuation mode, have the hydrogel layer of desired thickness, to accomplish the making of aerogel dressing with formation.Thus, simplify the making step of aerogel dressing, and significantly promote the preparation efficiency of aerogel dressing.Therefore, the method for preparing of the aerogel dressing of present embodiment is fit to factory and makes aerogel dressing with the automatic mode of serialization, to produce the aerogel dressing of the hydrogel layer with various different-thickness apace and in large quantities.
On the other hand, the aerogel dressing of made provide preferable ventilative, pass through wet, intercept that antibacterial is invaded and control and absorb characteristics such as transudate, make wound be in good cell growth healing environment.Moreover, because aerogel dressing is transparence, therefore help direct observation wound healing situation, to control the treatment situation of wound.In addition, aerogel dressing can adhere well to the wound, and when change dressings more, can not be stained with glutinous wound and cause the secondary injury.Therefore, aerogel dressing can be widely used in the living doctor field.
In sum; In the method for preparing of the present invention's aerogel dressing; The colloid solution that reaction mixture is condensed into have stickiness by cooling processing; Therefore can colloid solution be coated on the base material forming the colloid coating with coating method, and can directly carry out cross-linking reaction with the formation hydrogel layer the colloid coating on the base material.Owing to can reaction mixture be coated on the base material by colloidal form, thereby can control the thickness of colloid coating easily, and can continue and carry out cross-linking reaction to form hydrogel layer, so can the quantity-produced mode make aerogel dressing.Therefore, can significantly promote the processing procedure efficient of aerogel dressing and be applicable to the volume production aerogel dressing.
Above-described embodiment describes preferred implementation of the present invention; Be not that scope of the present invention is limited; Design under the prerequisite of spirit not breaking away 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.