CN111764165A - Preparation method of antibacterial drug-loaded gauze and foot cover for diabetic foot patient - Google Patents
Preparation method of antibacterial drug-loaded gauze and foot cover for diabetic foot patient Download PDFInfo
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- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
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Abstract
The invention discloses a preparation method of antibacterial drug-loaded gauze and a foot cover for a diabetic foot patient by adopting the gauze, relating to the field of gauze preparation and comprising the following steps: (1) carrying out first-stage polymerization reaction on polyethylene; (2) adding double bond modified ursolic acid into the first-stage polymerization product to carry out second-stage polymerization; (3) extruding and granulating to prepare modified polyethylene master batch; (4) preparing polyethylene fibers with a skin-core structure; (5) preparing modified polyethylene gauze; (6) preparing antibacterial drug-loaded gauze; the antibacterial drug-loaded gauze prepared by the invention has long-acting antibacterial performance, can not dissolve out in the using process, has long-acting antibacterial effect, and is safe and free of side effect when being applied to a human body as ursolic acid is used as a natural substance.
Description
Technical Field
The invention relates to the field of gauze preparation, in particular to a preparation method of antibacterial drug-loaded gauze and a foot cover for a diabetic foot patient by adopting the gauze.
Background
Diabetes is a metabolic disease characterized by hyperglycemia due to defective insulin secretion or impaired insulin action; persistent hyperglycemia and long-term metabolic disorders, etc., can lead to damage to tissues and organs throughout the body, particularly the eye, kidney, cardiovascular system and nervous system, as well as dysfunction and failure thereof; serious patients can cause acute complications of ketoacidosis and hyperosmolar coma, such as dehydration, electrolyte disturbance and acid-base balance disturbance. There are many causes for diabetic feet, and there are studies that improper footwear causes more than one third of diabetic feet to be ulcerated, while 85% of diabetic feet are amputated due to the foot ulcers. With the increasing incidence of diabetes and the aging of population, the incidence of diabetic feet is increasing, the wound surface of the foot of a diabetic patient is not healed, the liquid seeps more even if debridement and dressing change are carried out, and the clothes and quilts are easily polluted.
For example, a method for preparing medical antibacterial cotton gauze disclosed in chinese patent literature, whose publication number is CN105671942A, discloses a method for preparing medical antibacterial cotton gauze, comprising the following steps: carrying out puffing pretreatment on cotton gauze; performing carboxymethylation modification treatment on the pretreated cotton gauze; washing with water: washing with water for several times; and (3) antibacterial treatment: putting the washed cotton gauze into water with a bath ratio of 1:25, adding a compound antibacterial agent accounting for 5-8% of the weight of the cotton gauze, raising the temperature to about 40-48 ℃, and treating for 2.5-3 h, wherein the compound antibacterial agent comprises nano titanium dioxide, modified chitosan, artemisia oil and a tea extract; water squeezing: squeezing the cotton gauze subjected to the antibacterial treatment to enable the water content of the cotton gauze to be 10-20% of the weight of the cotton gauze; drying: and putting the cotton gauze after being squeezed into a vacuum drying box for drying. Although the invention endows the cotton gauze with antibacterial performance, the antibacterial agent is easy to separate out in the storage and use process, and the later use function is influenced.
Disclosure of Invention
The invention provides a preparation method of antibacterial drug-loaded gauze and a foot cover for a diabetic foot patient by using the antibacterial drug-loaded gauze, aiming at overcoming the problems that the antibacterial agent is easily separated out in the storage and use process of the antibacterial gauze soaked with the antibacterial agent, the later use function is influenced and the like in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of antibacterial drug-loaded gauze comprises the following preparation steps:
(1) placing raw materials of ethylene gas, comonomer alpha-olefin, hydrogen, catalyst and isobutane in a reaction kettle to carry out a first-stage polymerization reaction;
(2) adding double bond modified ursolic acid into the first-stage polymerization product, carrying out second-stage polymerization, and separating and drying to obtain polymer powder;
(3) extruding and granulating polymer powder to prepare modified polyethylene master batch;
(4) heating and melting the modified polyethylene master batch to obtain a spinning solution A; melting the conventional polyethylene master batch to obtain spinning solution B;
(5) spinning by using the spinning solution A as a skin layer and the spinning solution B as a core layer through a skin-core spinning assembly, and then extracting, drying and carrying out hot drawing to prepare the skin-core structure polyethylene fiber;
(6) dispersing polyethylene fibers with a skin-core structure in water, carding, lapping, drawing, performing two-stage spunlace, drying at high temperature, sterilizing, slitting and rolling to obtain modified polyethylene gauze;
(7) and soaking the modified polyethylene gauze into the medicinal solution, and vibrating and adsorbing under vacuum to prepare the antibacterial medicine-carrying gauze.
In the preparation process of the gauze, polyethylene fibers are used as raw materials to prepare the gauze, modified polyethylene is obtained in a two-stage series polymerization mode, firstly, polyethylene with a certain molecular weight is prepared in a one-stage polymerization mode, then, double-bond modified ursolic acid is added to continue to carry out two-stage polymerization, and the double-bond modified ursolic acid is directly polymerized and grafted into the polyethylene to form a small block in a polyethylene molecular chain. The ursolic acid is used as natural organic acid with antibacterial effect, and after the ursolic acid is subjected to block polymerization with polyethylene, the modified polyethylene is endowed with excellent antibacterial performance, and because the ursolic acid exists in a small block form in a polyethylene molecular chain, the ursolic acid cannot be dissolved out in the using process, the antibacterial effect is long-acting and lasting, and meanwhile, the ursolic acid is used as a natural substance, and is safe and free of side effects when being applied to a human body. In addition, the invention adopts a two-stage polymerization mode during polymerization, firstly polyethylene with a certain molecular weight is prepared, and then double-bond modified ursolic acid is added for polymerization, so that the molecular structure of the modified polyethylene can be effectively controlled, and the performance of the polyethylene is not influenced. And then, when the fiber is prepared, the modified polyethylene is used as a skin layer, the conventional polyethylene is used as a core layer, and the polyethylene fiber with the skin-core structure is prepared, because the spinnability of the modified polyethylene is inevitably poorer than that of the conventional polyethylene, the polyethylene fiber with the skin-core structure is prepared, the problem of the performance of the polyethylene fiber caused by the poor spinnability of the modified polyethylene can be avoided, the modified polyethylene positioned on the skin layer can exert the good antibacterial effect, and the cost is reduced. And finally, soaking the prepared gauze in a medicinal solution to prepare the antibacterial medicine-carrying gauze.
Preferably, the alpha-olefin in step (1) comprises one or more of propylene, 1-butene or 1-hexene, and the alpha-olefin is used in an amount of 0.5 to 1 mol% based on the total production of the polymerization.
Preferably, the molar ratio of the ethylene gas to the hydrogen gas in the step (1) is 1: 2.5-3.
Preferably, the double bond modified ursolic acid is added in the step (2) in an amount of 0.1 to 0.5 wt% of the ethylene gas, and the preparation method comprises the following steps: placing ursolic acid in ethanol solution to prepare mixed solution, then adding stannic chloride, dropwise adding allyl alcohol glycidyl ether at 65-75 ℃, continuously stirring for reaction, and then carrying out reduced pressure distillation to prepare the double-bond modified ursolic acid.
In the invention, the double bond modification of ursolic acid is carried out by adopting allyl alcohol glycidyl ether, because the epoxy group on the allyl alcohol glycidyl ether can carry out ring-opening reaction with the hydroxyl on the ursolic acid under the action of the catalyst, the double bond is successfully grafted on the ursolic acid, and the double bond modification of the ursolic acid is completed.
Preferably, the first-stage polymerization reaction in the step (1) is polymerization for 1-2h at the temperature of 80-90 ℃ and the pressure of 1-2 MPa; the two-stage polymerization reaction in the step (2) is polymerization for 1.5-2h at the temperature of 80-90 ℃ and the pressure of 1-1.5 MPa.
Preferably, the mass ratio of the spinning solution A to the spinning solution B in the step (5) is 1-2: 5.
Preferably, the length of the polyethylene fiber with the sheath-core structure in the step (5) is 10-15 mm; the fineness is 0.8-1.5 dtex.
Preferably, in the two-stage water stabbing in the step (6), the pressure of the first stage is 50-100bar, and the pressure of the first stage is 100-150 bar.
Preferably, the drug in step (7) is diclofenac potassium or mupirocin.
A foot cover for diabetic foot patient with antibacterial drug-loaded gauze is provided.
Therefore, the invention has the following beneficial effects: the antibacterial drug-loaded gauze prepared by the invention has long-acting antibacterial performance, can not dissolve out in the using process, has long-acting antibacterial effect, and is safe and free of side effect when being applied to a human body as ursolic acid is used as a natural substance.
Detailed Description
The invention is further described with reference to specific embodiments.
Example 1: a preparation method of antibacterial drug-loaded gauze comprises the following preparation steps:
(1) placing ursolic acid in an ethanol solution to prepare a mixed solution, then adding 1 wt% of stannic chloride, dropwise adding allyl alcohol glycidyl ether at 70 ℃, continuously stirring for reaction, and then carrying out reduced pressure distillation to prepare double-bond modified ursolic acid;
(2) placing raw material ethylene gas, 1-butene with the total polymerization yield of 0.8 mol%, hydrogen, a catalyst BCE and isobutane into a reaction kettle, wherein the molar ratio of the ethylene gas to the hydrogen is 1:2.8, and carrying out primary polymerization for 1.5h at 85 ℃ and 1.5 MPa;
(3) adding ethylene gas 0.3 wt% double bond modified ursolic acid into the first-stage polymerization product, carrying out second-stage polymerization reaction for 1.8h at 85 ℃ and 1.2MPa, and separating and drying to obtain polymer powder;
(4) extruding and granulating polymer powder to prepare modified polyethylene master batch;
(5) heating and melting the modified polyethylene master batch to obtain a spinning solution A; melting the conventional polyethylene master batch to obtain spinning solution B;
(6) spinning by using a spinning solution A as a skin layer and a spinning solution B as a core layer through a skin-core spinning assembly according to the mass ratio of 1.5:5, and then extracting, drying and carrying out hot drawing to prepare a skin-core structure polyethylene fiber with the length of 12mm and the fineness of 1 dtex;
(7) dispersing polyethylene fibers with a skin-core structure in water, carding, lapping, drawing, performing two-stage spunlace, drying at high temperature, sterilizing, slitting and rolling to obtain modified polyethylene gauze, wherein the pressure of one stage is 80bar and the pressure of the other stage is 120 bar;
(8) and soaking the modified polyethylene gauze into a diclofenac potassium solution, and vibrating and adsorbing under vacuum to prepare the antibacterial drug-loaded gauze.
Example 2: a preparation method of antibacterial drug-loaded gauze comprises the following preparation steps:
(1) placing ursolic acid in an ethanol solution to prepare a mixed solution, then adding 1 wt% of stannic chloride, dropwise adding allyl alcohol glycidyl ether at 65 ℃, continuously stirring for reaction, and then carrying out reduced pressure distillation to prepare double-bond modified ursolic acid;
(2) placing raw material ethylene gas, 1-butene with the total polymerization yield of 0.5 mol%, hydrogen, a catalyst BCE and isobutane into a reaction kettle, wherein the molar ratio of the ethylene gas to the hydrogen is 1:2.5, and carrying out primary polymerization for 2 hours at 80 ℃ and 1 MPa;
(3) adding double bond modified ursolic acid with 0.1 wt% of ethylene gas into the first-stage polymerization product, carrying out second-stage polymerization reaction for 1.5h at 80 ℃ and 1MPa, and separating and drying to obtain polymer powder;
(4) extruding and granulating polymer powder to prepare modified polyethylene master batch;
(5) heating and melting the modified polyethylene master batch to obtain a spinning solution A; melting the conventional polyethylene master batch to obtain spinning solution B;
(6) spinning by using a spinning solution A as a skin layer and a spinning solution B as a core layer through a skin-core spinning assembly according to the mass ratio of 1:5, and then extracting, drying and carrying out hot drawing to prepare a skin-core structure polyethylene fiber with the length of 10mm and the fineness of 1.5 dtex;
(7) dispersing polyethylene fibers with a skin-core structure in water, carding, lapping, drawing, performing two-stage spunlace, drying at high temperature, sterilizing, slitting and rolling to obtain modified polyethylene gauze, wherein the pressure of one stage is 50bar and the pressure of the other stage is 100 bar;
(8) and soaking the modified polyethylene gauze into a diclofenac potassium solution, and vibrating and adsorbing under vacuum to prepare the antibacterial drug-loaded gauze.
Example 3: a preparation method of antibacterial drug-loaded gauze comprises the following preparation steps:
(1) placing ursolic acid in an ethanol solution to prepare a mixed solution, then adding 1 wt% of stannic chloride, dropwise adding allyl alcohol glycidyl ether at 75 ℃, continuously stirring for reaction, and then carrying out reduced pressure distillation to prepare double-bond modified ursolic acid;
(2) placing raw material ethylene gas, 1-butene with the total polymerization yield of 1 mol%, hydrogen, a catalyst BCE and isobutane into a reaction kettle, wherein the molar ratio of the ethylene gas to the hydrogen is 1:3, and carrying out primary polymerization for 1h at 90 ℃ and 2 MPa;
(3) adding double bond modified ursolic acid with 0.5 wt% of ethylene gas into the first-stage polymerization product, carrying out second-stage polymerization reaction for 1.5h at 90 ℃ and 1.5MPa, and separating and drying to obtain polymer powder;
(4) extruding and granulating polymer powder to prepare modified polyethylene master batch;
(5) heating and melting the modified polyethylene master batch to obtain a spinning solution A; melting the conventional polyethylene master batch to obtain spinning solution B;
(6) spinning by using a spinning solution A as a skin layer and a spinning solution B as a core layer through a skin-core spinning assembly according to the mass ratio of 2:5, and then extracting, drying and carrying out hot drawing to prepare a skin-core structure polyethylene fiber with the length of 15mm and the fineness of 0.8 dtex;
(7) dispersing polyethylene fibers with a skin-core structure in water, carding, lapping, drawing, performing two-stage spunlace, drying at high temperature, sterilizing, slitting and rolling to obtain modified polyethylene gauze, wherein the pressure of one stage is 100bar and the pressure of the other stage is 150 bar;
(8) and soaking the modified polyethylene gauze into mupirocin solution, and vibrating and adsorbing under vacuum to prepare the antibacterial drug-loaded gauze.
The modified polyethylene gauze prepared in example 1 and the conventional polyethylene gauze were cut into 6mm round pieces, which were placed on a culture agar plate for Staphylococcus aureus, and heat-preserved at 37 ℃ for 24 hours, and the bacteriostatic areas were observed, and the average widths of the bacteriostatic areas are shown in the following table.
From the data, the modified polyethylene gauze prepared in example 1 has a staphylococcus aureus inhibition zone, which shows that the modified polyethylene gauze has excellent antibacterial performance.
Comparative example 1: a preparation method of antibacterial drug-loaded gauze comprises the following preparation steps:
(1) heating and melting conventional polyethylene to prepare a spinning solution, adding 5 wt% of ursolic acid into the spinning solution, then spinning, extracting, drying and carrying out hot drawing to prepare a physical blending polyethylene fiber with the length of 12mm and the fineness of 1 dtex;
(2) dispersing polyethylene fibers in water, carding, lapping and drawing, then carrying out two-stage spunlace, wherein the pressure of one stage is 80bar, the pressure of the other stage is 120bar, and then drying at high temperature, sterilizing, slitting and rolling to obtain modified polyethylene gauze;
(3) and soaking the modified polyethylene gauze into a diclofenac potassium solution, and vibrating and adsorbing under vacuum to prepare the antibacterial drug-loaded gauze.
Comparative example 2: a preparation method of antibacterial drug-loaded gauze comprises the following preparation steps:
(1) placing ursolic acid in an ethanol solution to prepare a mixed solution, then adding 1 wt% of stannic chloride, dropwise adding allyl alcohol glycidyl ether at 70 ℃, continuously stirring for reaction, and then carrying out reduced pressure distillation to prepare double-bond modified ursolic acid;
(2) placing raw materials of ethylene gas, 1-butene with the total polymerization yield of 0.8 mol%, hydrogen, a catalyst BCE, double-bond modified ursolic acid and isobutane into a reaction kettle, wherein the molar ratio of the ethylene gas to the hydrogen is 1:2.8, the addition amount of the double-bond modified ursolic acid is 0.3 wt% of the ethylene gas, carrying out primary polymerization for 3.3h at 85 ℃ and 1.5MPa, and separating and drying to prepare polymer powder;
(3) extruding and granulating polymer powder to prepare modified polyethylene master batch;
(4) heating and melting the modified polyethylene master batch to obtain a spinning solution A; melting the conventional polyethylene master batch to obtain spinning solution B;
(5) spinning by using a spinning solution A as a skin layer and a spinning solution B as a core layer through a skin-core spinning assembly according to the mass ratio of 1.5:5, and then extracting, drying and carrying out hot drawing to prepare a skin-core structure polyethylene fiber with the length of 12mm and the fineness of 1 dtex;
(6) dispersing polyethylene fibers with a skin-core structure in water, carding, lapping, drawing, performing two-stage spunlace, drying at high temperature, sterilizing, slitting and rolling to obtain modified polyethylene gauze, wherein the pressure of one stage is 80bar and the pressure of the other stage is 120 bar;
(7) and soaking the modified polyethylene gauze into a diclofenac potassium solution, and vibrating and adsorbing under vacuum to prepare the antibacterial drug-loaded gauze.
The polyethylene fiber having a sheath-core structure prepared in example 1 and the polyethylene fibers prepared in comparative examples 1 and 2 were subjected to a strength test according to GB/T14337-2008, and were again subjected to a strength test after artificial heat aging at 90 ℃ for 1 month, and the data are shown in the following table.
From the above data, it can be seen that the polyethylene fiber prepared in example 1 has high strength and less strength loss after aging; the polyethylene fiber prepared in the comparative example 1 adopts a physical blending mode, so that the ursolic acid is gradually dissolved out in the aging process, and the strength is greatly reduced; in comparative example 3, since the polyethylene fiber was prepared by the one-step polymerization preparation method, the initial strength was low.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The preparation method of the antibacterial drug-loaded gauze is characterized by comprising the following preparation steps:
(1) placing raw materials of ethylene gas, comonomer alpha-olefin, hydrogen, catalyst and isobutane in a reaction kettle to carry out a first-stage polymerization reaction;
(2) adding double bond modified ursolic acid into the first-stage polymerization product, carrying out second-stage polymerization, and separating and drying to obtain polymer powder;
(3) extruding and granulating polymer powder to prepare modified polyethylene master batch;
(4) heating and melting the modified polyethylene master batch to obtain a spinning solution A; melting the conventional polyethylene master batch to obtain spinning solution B;
(5) spinning by using the spinning solution A as a skin layer and the spinning solution B as a core layer through a skin-core spinning assembly, and then extracting, drying and carrying out hot drawing to prepare the skin-core structure polyethylene fiber;
(6) dispersing polyethylene fibers with a skin-core structure in water, carding, lapping, drawing, performing two-stage spunlace, drying at high temperature, sterilizing, slitting and rolling to obtain modified polyethylene gauze;
(7) and soaking the modified polyethylene gauze into the medicinal solution, and vibrating and adsorbing under vacuum to prepare the antibacterial medicine-carrying gauze.
2. The method for preparing antibacterial drug-loaded gauze according to claim 1, wherein the α -olefin in step (1) comprises one or more of propylene, 1-butene or 1-hexene, and the α -olefin is used in an amount of 0.5 to 1 mol% of the total polymerization yield.
3. The method for preparing antibacterial drug-loaded gauze according to claim 1, wherein the molar ratio of the ethylene gas to the hydrogen gas in the step (1) is 1: 2.5-3.
4. The preparation method of antibacterial drug-loaded gauze according to claim 1, wherein the amount of the double-bond modified ursolic acid added in step (2) is 0.1-0.5 wt% of ethylene gas, and the preparation method comprises: placing ursolic acid in ethanol solution to prepare mixed solution, then adding stannic chloride, dropwise adding allyl alcohol glycidyl ether at 65-75 ℃, continuously stirring for reaction, and then carrying out reduced pressure distillation to prepare the double-bond modified ursolic acid.
5. The method for preparing antibacterial drug-loaded gauze according to claim 1, wherein the first-stage polymerization reaction in the step (1) is polymerization at 80-90 ℃ and 1-2MPa for 1-2 h; the two-stage polymerization reaction in the step (2) is polymerization for 1.5-2h at the temperature of 80-90 ℃ and the pressure of 1-1.5 MPa.
6. The preparation method of the antibacterial and drug-loaded gauze according to claim 1, wherein the mass ratio of the spinning solution A to the spinning solution B in the step (5) is 1-2: 5.
7. The method for preparing antibacterial drug-loaded gauze according to claim 1, wherein the length of the skin-core structure polyethylene fiber in the step (5) is 10-15 mm; the fineness is 0.8-1.5 dtex.
8. The method for preparing antibacterial drug-loaded gauze according to claim 1, wherein in the two-stage water stabbing in the step (6), the pressure at one stage is 50-100bar, and the pressure at one stage is 100-150 bar.
9. The method for preparing antibacterial drug-loaded gauze according to claim 1, wherein the drugs in step (7) are diclofenac potassium and mupirocin.
10. A diabetic foot cover obtained from gauze by the method of any one of claims 1 to 9.
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