CN107233607B - Preparation method of wound surface protection film material - Google Patents
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- CN107233607B CN107233607B CN201710499922.5A CN201710499922A CN107233607B CN 107233607 B CN107233607 B CN 107233607B CN 201710499922 A CN201710499922 A CN 201710499922A CN 107233607 B CN107233607 B CN 107233607B
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
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- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
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- A61L15/42—Use of materials characterised by their function or physical properties
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Abstract
The invention discloses a preparation method of a wound surface protective film material, which comprises the steps of firstly preparing polyvinyl alcohol with high purity, mixing and stirring the prepared polyvinyl alcohol and purified water until the solid is dissolved to obtain a mixture 1; mixing rosin and ethanol, stirring until the solid is dissolved, then adding potassium sorbate, and stirring until the solid is dissolved to obtain a mixture 2; mixing the prepared mixture 1 and the prepared mixture 2 to obtain a mixed solution; pouring the obtained mixed solution into a filling machine for filling, then filling into a plastic sealing bag, sealing at 200 ℃, putting the sealed product and the specification into a paper box, and performing irradiation sterilization to obtain the wound surface protection film material. The wound surface protection film material prepared by the invention is non-toxic and non-irritating, has good chemical stability, and can be used for protecting small body surface wound surfaces such as burns, scalds and skin damages.
Description
The technical field is as follows:
the invention relates to the field of biomedicine, in particular to a preparation method of a wound surface protection film material.
Background art:
in daily life of people, burn, scald and skin injury can frequently occur, wound surfaces with different depths are caused, infection is easily caused, various complications are caused, the wound surfaces are well protected and are not infected by bacteria, a closed environment isolated from the outside is caused, and the wound surface healing promotion treatment link is provided.
For the research of wound protection films, it has been reported at home and abroad that the wound protection films synthesized from pig skin, cow skin, chicken skin, chitosan, pig skin and the like, or the wound protection film materials synthesized from high polymers such as acrylic acid and the like are used. However, the existing common wound protective film material has the problems of randomness, poor adhesion, low strength and poor film forming performance, and the preparation method is relatively complex and has higher cost.
The invention content is as follows:
the invention aims to provide a wound surface protective film material which is non-toxic, non-irritating, good in chemical stability, low in preparation cost and good in film forming property, and can be used for protecting small wound surfaces on body surfaces such as burns, scalds and skin damages.
The invention also aims to provide a preparation method of the wound surface protection film material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a wound surface protection film material comprises the following steps:
(1) dispersing porous alumina in a mixed solution of toluene and xylene, stirring and dispersing uniformly, adding 4-n-butylphenol isocyanate, mixing uniformly, dropwise adding triethylamine, heating to 75-85 ℃ under the condition of introducing nitrogen, reacting for 50-100min under the protection of nitrogen, cooling to room temperature after the reaction is finished, filtering, washing the solid with ethanol for 3-5 times, and drying to obtain modified porous alumina;
(2) uniformly mixing polyethylene glycol, toluene and xylene, adding the prepared modified porous alumina, heating to 80-90 ℃ under the condition of introducing nitrogen, reacting for 1-2 hours under stirring, cooling to room temperature after the reaction is finished, filtering, washing the obtained solid for 2-3 times by using toluene and ethanol in sequence, and drying in vacuum to obtain polyethylene glycol grafted porous alumina;
(3) placing the prepared polyethylene glycol grafted porous alumina in a reaction vessel with the pressure intensity of less than 0.1MPa, and then slowly injecting triethylamine into the reaction vessel to obtain a supported catalyst;
(4) adding a polyvinyl acetate solution into a reactor, adding the prepared supported catalyst under stirring at the stirring speed of 3000-5000r/min, uniformly mixing, slowly heating to 40-65 ℃, reacting for 10-30min, after the reaction is finished, adding excessive water into the reactor, filtering, and drying the filtrate to obtain polyvinyl alcohol;
(5) mixing the prepared polyvinyl alcohol and purified water, and stirring until the solid is dissolved to obtain a mixture 1; mixing rosin and ethanol, stirring until the solid is dissolved, then adding potassium sorbate, and stirring until the solid is dissolved to obtain a mixture 2;
(6) mixing the prepared mixture 1 and the prepared mixture 2 to obtain a mixed solution; pouring the obtained mixed solution into a filling machine for filling, then filling into a plastic sealing bag, sealing at 200 ℃, putting the sealed product and the specification into a paper box, and performing irradiation sterilization to obtain the wound surface protection film material.
As the optimization of the technical scheme, the use amounts of the components are respectively as follows in parts by weight: 10-15 parts of polyvinyl alcohol, 0.1-0.5 part of rosin, 2-5 parts of ethanol, 0.03-0.06 part of potassium sorbate and 70-90 parts of purified water.
As the optimization of the technical scheme, the use amounts of the components are respectively as follows in parts by weight: 14 parts of polyvinyl alcohol, 0.1 part of rosin, 2 parts of ethanol, 0.05 part of potassium sorbate and 83.85 parts of purified water.
Preferably, in the step (2), the mass ratio of the polyethylene glycol to the modified porous alumina is 8: 1.
Preferably, in the step (3), the mass ratio of the polyethylene glycol grafted porous alumina to the triethylamine is (3-5): 1.
preferably, in the step (4), the mass concentration of the polyvinyl acetate solution is 28.5 to 37.9%.
Preferably, in the step (4), the mass ratio of the polyvinyl acetate solution to the supported catalyst is 1: (0.1-0.8).
The invention has the following beneficial effects:
firstly, polyvinyl alcohol is prepared by alcoholysis of a polyvinyl acetate solution, and porous alumina loaded triethylamine is used as a catalyst, in order to improve the dispersibility of the porous alumina, polyethylene glycol is grafted on the surface of the porous alumina, so that the dispersibility of the porous alumina in the polyvinyl acetate solution can be improved, and the prepared polyvinyl alcohol has high purity and high yield;
the wound surface protection film material prepared by the invention has good film forming property; the raw materials adopted by the invention are nontoxic, environment-friendly and non-irritating, do not damage human bodies, and the prepared wound surface protection film material has good chemical stability and can be used for protecting small wound surfaces on body surfaces such as burns, scalds and skin damages.
The specific implementation mode is as follows:
in order to better understand the present invention, the following examples are given for illustration only and not for limiting the present invention.
Example 1
A wound surface protection film material comprises the following components in parts by weight:
14 parts of polyvinyl alcohol, 0.1 part of rosin, 2 parts of ethanol,
0.05 part of potassium sorbate and 83.85 parts of purified water;
the preparation method of the material comprises the following steps:
(1) dispersing porous alumina in a mixed solution of toluene and xylene, stirring and dispersing uniformly, adding 4-n-butylphenol isocyanate, mixing uniformly, dropwise adding triethylamine, heating to 75-85 ℃ under the condition of introducing nitrogen, reacting for 50min under the protection of nitrogen, cooling to room temperature after the reaction is finished, filtering, washing the solid with ethanol for 3-5 times, and drying to obtain modified porous alumina; wherein the mass ratio of the porous alumina to the 4-n-butylphenol isocyanate to the triethylamine is 1:1:5: 0.1;
(2) uniformly mixing polyethylene glycol, toluene and xylene, adding the prepared modified porous alumina, heating to 80-90 ℃ under the condition of introducing nitrogen, reacting for 1h under stirring, cooling to room temperature after the reaction is finished, filtering, washing the obtained solid for 2-3 times by using toluene and ethanol in sequence, and drying in vacuum to obtain polyethylene glycol grafted porous alumina; wherein the mass ratio of the polyethylene glycol to the modified porous alumina is 8: 1;
(3) placing the prepared polyethylene glycol grafted porous alumina in a reaction vessel with the pressure intensity of less than 0.1MPa, and then slowly injecting triethylamine into the reaction vessel to obtain a supported catalyst; wherein the mass ratio of the polyethylene glycol grafted porous alumina to the triethylamine is 3: 1;
(4) adding a polyvinyl acetate solution into a reactor, adding the prepared supported catalyst under stirring at a stirring speed of 3000r/min, uniformly mixing, slowly heating to 40 ℃, reacting for 30min, adding excessive water into the reactor after the reaction is finished, filtering, and drying the filtrate to obtain polyvinyl alcohol; wherein the mass ratio of the polyvinyl acetate solution to the supported catalyst is 1: 0.1;
(5) mixing the prepared polyvinyl alcohol and purified water, and stirring until the solid is dissolved to obtain a mixture 1; mixing rosin and ethanol, stirring until the solid is dissolved, then adding potassium sorbate, and stirring until the solid is dissolved to obtain a mixture 2;
(6) mixing the prepared mixture 1 and the prepared mixture 2 to obtain a mixed solution; pouring the obtained mixed solution into a filling machine for filling, then filling into a plastic sealing bag, sealing at 200 ℃, putting the sealed product and the specification into a paper box, and performing irradiation sterilization to obtain the wound surface protection film material.
Example 2
A wound surface protection film material comprises the following components in parts by weight:
10 portions of polyvinyl alcohol, 0.1 portion of rosin, 2 portions of ethanol,
0.03 part of potassium sorbate and 70 parts of purified water;
the preparation method of the material comprises the following steps:
(1) dispersing porous alumina in a mixed solution of toluene and xylene, stirring and dispersing uniformly, adding 4-n-butylphenol isocyanate, mixing uniformly, dropwise adding triethylamine, heating to 75-85 ℃ under the condition of introducing nitrogen, reacting for 100min under the protection of nitrogen, cooling to room temperature after the reaction is finished, filtering, washing the solid with ethanol for 3-5 times, and drying to obtain modified porous alumina; wherein the mass ratio of the porous alumina to the 4-n-butylphenol isocyanate to the triethylamine is 1:1:5: 0.1;
(2) uniformly mixing polyethylene glycol, toluene and xylene, adding the prepared modified porous alumina, heating to 80-90 ℃ under the condition of introducing nitrogen, reacting for 2 hours under stirring, cooling to room temperature after the reaction is finished, filtering, washing the obtained solid for 2-3 times by using toluene and ethanol in sequence, and drying in vacuum to obtain polyethylene glycol grafted porous alumina; wherein the mass ratio of the polyethylene glycol to the modified porous alumina is 8: 1;
(3) placing the prepared polyethylene glycol grafted porous alumina in a reaction vessel with the pressure intensity of less than 0.1MPa, and then slowly injecting triethylamine into the reaction vessel to obtain a supported catalyst; wherein the mass ratio of the polyethylene glycol grafted porous alumina to the triethylamine is 5: 1;
(4) adding a polyvinyl acetate solution into a reactor, adding the prepared supported catalyst under stirring at a stirring speed of 5000r/min, uniformly mixing, slowly heating to 65 ℃, reacting for 10min, adding excessive water into the reactor after the reaction is finished, filtering, and drying the filtrate to obtain polyvinyl alcohol; wherein the mass ratio of the polyvinyl acetate solution to the supported catalyst is 1: 0.8;
(5) mixing the prepared polyvinyl alcohol and purified water, and stirring until the solid is dissolved to obtain a mixture 1; mixing rosin and ethanol, stirring until the solid is dissolved, then adding potassium sorbate, and stirring until the solid is dissolved to obtain a mixture 2;
(6) mixing the prepared mixture 1 and the prepared mixture 2 to obtain a mixed solution; pouring the obtained mixed solution into a filling machine for filling, then filling into a plastic sealing bag, sealing at 200 ℃, putting the sealed product and the specification into a paper box, and performing irradiation sterilization to obtain the wound surface protection film material.
Example 3
A wound surface protection film material comprises the following components in parts by weight:
11 parts of polyvinyl alcohol, 0.2 part of rosin, 3 parts of ethanol,
0.04 part of potassium sorbate and 75 parts of purified water;
the preparation method of the material comprises the following steps:
(1) dispersing porous alumina in a mixed solution of toluene and xylene, stirring and dispersing uniformly, adding 4-n-butylphenol isocyanate, mixing uniformly, dropwise adding triethylamine, heating to 75-85 ℃ under the condition of introducing nitrogen, reacting for 60min under the protection of nitrogen, cooling to room temperature after the reaction is finished, filtering, washing the solid with ethanol for 3-5 times, and drying to obtain modified porous alumina; wherein the mass ratio of the porous alumina to the 4-n-butylphenol isocyanate to the triethylamine is 1:1:5: 0.1;
(2) uniformly mixing polyethylene glycol, toluene and xylene, adding the prepared modified porous alumina, heating to 80-90 ℃ under the condition of introducing nitrogen, reacting for 1.3h under stirring, cooling to room temperature after the reaction is finished, filtering, washing the obtained solid for 2-3 times by using toluene and ethanol in sequence, and drying in vacuum to obtain polyethylene glycol grafted porous alumina; wherein the mass ratio of the polyethylene glycol to the modified porous alumina is 8: 1;
(3) placing the prepared polyethylene glycol grafted porous alumina in a reaction vessel with the pressure intensity of less than 0.1MPa, and then slowly injecting triethylamine into the reaction vessel to obtain a supported catalyst; wherein the mass ratio of the polyethylene glycol grafted porous alumina to the triethylamine is 3.5: 1;
(4) adding a polyvinyl acetate solution into a reactor, adding the prepared supported catalyst under stirring at a stirring speed of 3500r/min, uniformly mixing, slowly heating to 45 ℃, reacting for 15min, adding excessive water into the reactor after the reaction is finished, filtering, and drying the filtrate to obtain polyvinyl alcohol; wherein the mass ratio of the polyvinyl acetate solution to the supported catalyst is 1: 0.2;
(5) mixing the prepared polyvinyl alcohol and purified water, and stirring until the solid is dissolved to obtain a mixture 1; mixing rosin and ethanol, stirring until the solid is dissolved, then adding potassium sorbate, and stirring until the solid is dissolved to obtain a mixture 2;
(6) mixing the prepared mixture 1 and the prepared mixture 2 to obtain a mixed solution; pouring the obtained mixed solution into a filling machine for filling, then filling into a plastic sealing bag, sealing at 200 ℃, putting the sealed product and the specification into a paper box, and performing irradiation sterilization to obtain the wound surface protection film material.
Example 4
A wound surface protection film material comprises the following components in parts by weight:
12 parts of polyvinyl alcohol, 0.3 part of rosin, 4 parts of ethanol,
0.04 part of potassium sorbate and 80 parts of purified water;
the preparation method of the material comprises the following steps:
(1) dispersing porous alumina in a mixed solution of toluene and xylene, stirring and dispersing uniformly, adding 4-n-butylphenol isocyanate, mixing uniformly, dropwise adding triethylamine, heating to 75-85 ℃ under the condition of introducing nitrogen, reacting for 70min under the protection of nitrogen, cooling to room temperature after the reaction is finished, filtering, washing the solid with ethanol for 3-5 times, and drying to obtain modified porous alumina; wherein the mass ratio of the porous alumina to the 4-n-butylphenol isocyanate to the triethylamine is 1:1:5: 0.1;
(2) uniformly mixing polyethylene glycol, toluene and xylene, adding the prepared modified porous alumina, heating to 80-90 ℃ under the condition of introducing nitrogen, reacting for 1.6h under stirring, cooling to room temperature after the reaction is finished, filtering, washing the obtained solid for 2-3 times by using toluene and ethanol in sequence, and drying in vacuum to obtain polyethylene glycol grafted porous alumina; wherein the mass ratio of the polyethylene glycol to the modified porous alumina is 8: 1;
(3) placing the prepared polyethylene glycol grafted porous alumina in a reaction vessel with the pressure intensity of less than 0.1MPa, and then slowly injecting triethylamine into the reaction vessel to obtain a supported catalyst; wherein the mass ratio of the polyethylene glycol grafted porous alumina to the triethylamine is 4: 1;
(4) adding a polyvinyl acetate solution into a reactor, adding the prepared supported catalyst under stirring at a stirring speed of 4000r/min, uniformly mixing, slowly heating to 50 ℃, reacting for 20min, adding excessive water into the reactor after the reaction is finished, filtering, and drying the filtrate to obtain polyvinyl alcohol; wherein the mass ratio of the polyvinyl acetate solution to the supported catalyst is 1: 0.4;
(5) mixing the prepared polyvinyl alcohol and purified water, and stirring until the solid is dissolved to obtain a mixture 1; mixing rosin and ethanol, stirring until the solid is dissolved, then adding potassium sorbate, and stirring until the solid is dissolved to obtain a mixture 2;
(6) mixing the prepared mixture 1 and the prepared mixture 2 to obtain a mixed solution; pouring the obtained mixed solution into a filling machine for filling, then filling into a plastic sealing bag, sealing at 200 ℃, putting the sealed product and the specification into a paper box, and performing irradiation sterilization to obtain the wound surface protection film material.
Example 5
A wound surface protection film material comprises the following components in parts by weight:
13 portions of polyvinyl alcohol, 0.4 portion of rosin, 4.5 portions of ethanol,
0.05 part of potassium sorbate and 85 parts of purified water;
the preparation method of the material comprises the following steps:
(1) dispersing porous alumina in a mixed solution of toluene and xylene, stirring and dispersing uniformly, adding 4-n-butylphenol isocyanate, mixing uniformly, dropwise adding triethylamine, heating to 75-85 ℃ under the condition of introducing nitrogen, reacting for 80min under the protection of nitrogen, cooling to room temperature after the reaction is finished, filtering, washing the solid with ethanol for 3-5 times, and drying to obtain modified porous alumina; wherein the mass ratio of the porous alumina to the 4-n-butylphenol isocyanate to the triethylamine is 1:1:5: 0.1;
(2) uniformly mixing polyethylene glycol, toluene and xylene, adding the prepared modified porous alumina, heating to 80-90 ℃ under the condition of introducing nitrogen, reacting for 1.8h under stirring, cooling to room temperature after the reaction is finished, filtering, washing the obtained solid for 2-3 times by using toluene and ethanol in sequence, and drying in vacuum to obtain polyethylene glycol grafted porous alumina; wherein the mass ratio of the polyethylene glycol to the modified porous alumina is 8: 1;
(3) placing the prepared polyethylene glycol grafted porous alumina in a reaction vessel with the pressure intensity of less than 0.1MPa, and then slowly injecting triethylamine into the reaction vessel to obtain a supported catalyst; wherein the mass ratio of the polyethylene glycol grafted porous alumina to the triethylamine is 4.5: 1;
(4) adding a polyvinyl acetate solution into a reactor, adding the prepared supported catalyst under stirring at the stirring speed of 4500r/min, uniformly mixing, slowly heating to 60 ℃, reacting for 25min, adding excessive water into the reactor after the reaction is finished, filtering, and drying the filtrate to obtain polyvinyl alcohol; wherein the mass ratio of the polyvinyl acetate solution to the supported catalyst is 1: 0.6;
(5) mixing the prepared polyvinyl alcohol and purified water, and stirring until the solid is dissolved to obtain a mixture 1; mixing rosin and ethanol, stirring until the solid is dissolved, then adding potassium sorbate, and stirring until the solid is dissolved to obtain a mixture 2;
(6) mixing the prepared mixture 1 and the prepared mixture 2 to obtain a mixed solution; pouring the obtained mixed solution into a filling machine for filling, then filling into a plastic sealing bag, sealing at 200 ℃, putting the sealed product and the specification into a paper box, and performing irradiation sterilization to obtain the wound surface protection film material.
The wound surface protection film material prepared by the invention is dried into a film within 5 minutes under the conditions that the pH is 5.5-8.5, the temperature is 35-37 ℃ and the relative humidity is less than 65%.
Claims (7)
1. A preparation method of a wound surface protection film material is characterized by comprising the following steps:
(1) dispersing porous alumina in a mixed solution of toluene and xylene, stirring and dispersing uniformly, adding 4-n-butylphenol isocyanate, mixing uniformly, dropwise adding triethylamine, heating to 75-85 ℃ under the condition of introducing nitrogen, reacting for 50-100min under the protection of nitrogen, cooling to room temperature after the reaction is finished, filtering, washing the solid with ethanol for 3-5 times, and drying to obtain modified porous alumina;
(2) uniformly mixing polyethylene glycol, toluene and xylene, adding the prepared modified porous alumina, heating to 80-90 ℃ under the condition of introducing nitrogen, reacting for 1-2 hours under stirring, cooling to room temperature after the reaction is finished, filtering, washing the obtained solid for 2-3 times by using toluene and ethanol in sequence, and drying in vacuum to obtain polyethylene glycol grafted porous alumina;
(3) placing the prepared polyethylene glycol grafted porous alumina in a reaction vessel with the pressure intensity of less than 0.1MPa, and then slowly injecting triethylamine into the reaction vessel to obtain a supported catalyst;
(4) adding a polyvinyl acetate solution into a reactor, adding the prepared supported catalyst under stirring at the stirring speed of 3000-5000r/min, uniformly mixing, slowly heating to 40-65 ℃, reacting for 10-30min, after the reaction is finished, adding excessive water into the reactor, filtering, and drying the filtrate to obtain polyvinyl alcohol;
(5) mixing the prepared polyvinyl alcohol and purified water, and stirring until the solid is dissolved to obtain a mixture 1; mixing rosin and ethanol, stirring until the solid is dissolved, then adding potassium sorbate, and stirring until the solid is dissolved to obtain a mixture 2;
(6) mixing the prepared mixture 1 and the prepared mixture 2 to obtain a mixed solution; pouring the obtained mixed solution into a filling machine for filling, then filling into a plastic sealing bag, sealing at 200 ℃, putting the sealed product and the specification into a paper box, and performing irradiation sterilization to obtain the wound surface protection film material.
2. A method for preparing a wound-protecting film material as claimed in claim 1, wherein the amounts of each component are, in parts by weight: 10-15 parts of polyvinyl alcohol, 0.1-0.5 part of rosin, 2-5 parts of ethanol, 0.03-0.06 part of potassium sorbate and 70-90 parts of purified water.
3. A method for preparing a wound-protecting film material as claimed in claim 2, wherein the amounts of each component are, in parts by weight: 14 parts of polyvinyl alcohol, 0.1 part of rosin, 2 parts of ethanol, 0.05 part of potassium sorbate and 83.85 parts of purified water.
4. A preparation method of a wound protecting film material as claimed in claim 1, wherein in step (2), the mass ratio of the polyethylene glycol to the modified porous alumina is 8: 1.
5. A method for preparing a wound protecting film material as claimed in claim 1, wherein in step (3), the mass ratio of the polyethylene glycol grafted porous alumina to the triethylamine is (3-5): 1.
6. a method for preparing a wound-protecting film material as claimed in claim 1, wherein in step (4), the mass concentration of the polyvinyl acetate solution is 28.5-37.9%.
7. A method for preparing a wound-protecting film material as claimed in claim 1, wherein in step (4), the mass ratio of polyvinyl acetate solution to supported catalyst is 1: (0.1-0.8).
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