Polyethylene glycol glycerol liquid dressing and preparation method thereof

By synthesizing nanotitanium dioxide in activated carbon holes and combining polyacrylic acid and glutaraldehyde treatment, a tight antibacterial network is formed, which solves the problem of uneven dispersion of nanotitanium dioxide and achieves more efficient sterilization and wound recovery effects.

CN120267885APending Publication Date: 2025-07-08YUNNAN MINZU UNIV
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Patent Information

Application Number
CN202510457418.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-14
Publication Date
2025-07-08

AI Technical Summary

Technical Problem

The dispersion of nanotitanium dioxide in existing liquid dressings is uneven, resulting in a decrease in local sterilization ability and insufficient contact area, which affects the wound recovery speed.

Method used

Using the modified activated carbon preparation method, nanotitanium dioxide is synthesized in the holes of activated carbon, and treated by polyacrylic acid and glutaraldehyde, combined with polyethylene glycol and polyisocyanate, forming a tight antibacterial network and evenly distributing antibacterial materials.

Benefits of technology

It improves the bactericidal effect, increases the surface area, promotes wound recovery, and significantly accelerates the wound healing speed.

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Abstract

The invention relates to the technical field of liquid dressings, in particular to a polyethylene glycol glycerol liquid dressing and a preparation method thereof. Comprising the following components in parts by weight: 80 to 120 parts of water, 7 to 12 parts of polyethylene glycol, 3 to 5 parts of glycerol, 0.2 to 0.6 part of carbomer, 0.04 to 0.12 part of sodium hyaluronate, 0.005 to 0.02 part of a leech extract, 0.1 to 0.25 part of panthenol, 0.1 to 0.25 part of methylparaben, 0.5 to 1.1 parts of phenoxyethanol, 0.2 to 0.6 part of arginine, 2 to 8 parts of polyisocyanate and 0.8 to 2.2 parts of modified activated carbon. According to the prepared liquid dressing, titanium dioxide is evenly distributed on the liquid dressing through activated carbon, the antibacterial effect is improved, the surface area is increased, and the recovery speed of a wound is increased.
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Description

Technical Field

[0001] The present invention relates to the technical field of liquid dressings, and specifically relates to a polyethylene glycol glycerol liquid dressing and a preparation method thereof. Background Art

[0002] Polyethylene glycol is a high molecular polymer, which is non-irritating, slightly bitter in taste, has good water solubility, and good compatibility with many organic components. It has excellent lubricity, moisturizing property, dispersibility, and adhesiveness. Therefore, polyethylene glycol is often used in liquid dressings to accelerate the recovery of wounds.

[0003] In order to improve the bactericidal ability and accelerate the wound recovery in liquid dressings, other bactericidal materials are often added to the dressings. Nano-titanium dioxide is a relatively common bactericidal material. Nano-titanium dioxide can absorb oxygen and generate free radicals to kill nearby bacteria. In existing liquid dressings, nano-titanium dioxide is not evenly dispersed, which easily causes a decrease in local bactericidal ability and reduces the wound recovery speed. In addition, the contact area of nano-titanium dioxide in the dressing is not large enough, and the bactericidal ability is also difficult to guarantee. For this reason, in view of the problems proposed in the above background art, those skilled in the art propose a polyethylene glycol glycerol liquid dressing and a preparation method thereof. Summary of the Invention

[0004] The purpose of the present invention is to provide a polyethylene glycol glycerol liquid dressing and a preparation method thereof, so as to solve the problems proposed in the above background art.

[0005] To achieve the above purpose, the present invention provides the following technical solutions: A polyethylene glycol glycerol liquid dressing, comprising the following components: 80 - 120 parts of deionized water, 7 - 12 parts of polyethylene glycol, 3 - 5 parts of glycerol, 0.2 - 0.6 part of carbomer, 0.04 - 0.12 part of sodium hyaluronate, 0.005 - 0.02 part of leech extract, 0.1 - 0.25 part of panthenol, 0.1 - 0.25 part of methylparaben, 0.5 - 1.1 part of phenoxyethanol, 0.2 - 0.6 part of arginine, 2 - 8 parts of polyisocyanate, and 0.8 - 2.2 parts of modified activated carbon; The preparation method of the modified activated carbon comprises the following steps: S101. Add activated carbon to a mixed solution of EDTA and deionized water, stir and mix for 4 - 6 h, then filter and dry at low temperature to obtain pretreated activated carbon; S102. Add the pretreated activated carbon obtained in step S101 into a mixed solution of deionized water and isopropanol, stir evenly, add 3 mol / L hydrochloric acid to adjust the pH to 1 - 2. Slowly add titanium tetrachloride under ice bath conditions, continue stirring for 1 - 2 h, then add 1 mol / L sodium hydroxide solution to adjust the pH to 9 - 10, heat to 70 - 80 °C, and continue to react for 4 - 6 h to obtain a reaction solution. S103. Filter the reaction solution obtained in step S102 to obtain a product, wash the product with deionized water and then continue to calcine to obtain a primary product. S104. Disperse the primary product obtained in step S103 into an aqueous solution of 0.1 mol / L sodium hexadecyl sulfate, then add polyacrylic acid and stir and mix for 20 - 40 min. Then continue to add glutaraldehyde, continue to stir and mix for 1 - 3 h and then filter. After washing with deionized water and drying, a modified activated carbon is obtained.

[0006] Further, the mass ratio of activated carbon, EDTA and deionized water in step S101 is 1:(3 - 5):(40 - 65).

[0007] Further, the mass ratio of titanium tetrachloride, pretreated activated carbon, deionized water and isopropanol in step S102 is 1:(7 - 12):(30 - 35):(25 - 50).

[0008] Further, the calcination in step S103 is completed under a nitrogen atmosphere, the calcination temperature is 500 - 700 °C, and the calcination time is 2 - 5 h.

[0009] Further, the mass ratio of polyacrylic acid, glutaraldehyde, primary product and aqueous sodium hexadecyl sulfate solution in step S104 is 1:(0.6 - 1.4):(6 - 10):(60 - 80).

[0010] A preparation method of a polyethylene glycol glycerol liquid dressing, comprising the following steps: S1. Add polyethylene glycol and polyisocyanate into deionized water and stir evenly to obtain solution A, add modified activated carbon and glycerol into deionized water and stir evenly to obtain solution B, and add carbomer, sodium hyaluronate, leech extract, panthenol, methylparaben, phenoxyethanol and arginine into deionized water to obtain solution C. S2. Slowly add solution B in step S1 into solution A, continuously stir for 15 - 45 min, then continue to add solution C into solution A, and then stir for 15 - 45 min to obtain a liquid dressing.

[0011] Further, the mass ratio of deionized water in solution A, deionized water in solution B and deionized water in solution C in step S1 is 16:3:1.

[0012] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. In the present invention, the modified activated carbon is combined with titanium tetrachloride to directly synthesize nano-titanium dioxide in the pores of the activated carbon. The nano-titanium dioxide adsorbs oxygen near the wound to generate free radicals, killing bacteria. The combination of the activated carbon increases the surface area and promotes the bactericidal effect. The activated carbon is treated with EDTA, which also facilitates the binding of titanium ions and makes the titanium ions evenly distributed; 2. In the present invention, the activated carbon is also treated with polyacrylic acid and glutaraldehyde, which are combined with polyethylene glycol and polyisocyanate. This not only makes the antibacterial material more evenly distributed, but also forms a tight antibacterial network, improving the antibacterial effect and accelerating the wound healing rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 is a process flow chart for preparing the liquid dressing in the present invention; Figure 2 is a process flow chart for preparing the modified activated carbon in the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0014] The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0015] Please refer to Figures 1 to 2 , the present invention provides a technical solution: Embodiment

[0016] A polyethylene glycol glycerol liquid dressing, comprising the following components: Water, polyethylene glycol, glycerol, carbomer, sodium hyaluronate, leech extract, panthenol, methylparaben, phenoxyethanol, arginine, polyisocyanate and modified activated carbon; This dressing is mainly composed of polyethylene glycol, glycerol, polyisocyanate and deionized water. The composed dressing has excellent isolation and moisturizing properties, which helps the continuous recovery of the wound; The antibacterial component in the present invention is mainly achieved through modified activated carbon. The modified activated carbon is formed by combining activated carbon with titanium tetrachloride, and nano-titanium dioxide is directly synthesized in the pores of the activated carbon. The nano-titanium dioxide adsorbs oxygen near the wound to generate free radicals, which kill bacteria. The combination of activated carbon increases the surface area and promotes the bactericidal effect. The activated carbon is treated with EDTA, which also facilitates the binding of titanium ions and makes the titanium ions evenly distributed. The activated carbon is also treated with polyacrylic acid and glutaraldehyde, and it binds with polyethylene glycol and polyisocyanate, which not only makes the antibacterial material more evenly distributed, but also forms a tight antibacterial network through the binding, improving the antibacterial effect; Meanwhile, in the present invention, antibacterial materials such as leech extract, panthenol, methylparaben, phenoxyethanol, and arginine are also introduced to further improve the antibacterial effect, accelerate the anti-inflammation of the wound, and have a more significant ability to promote blood circulation and remove blood stasis; Specifically, the liquid dressing in the present invention is prepared through the following four examples Example 1

[0017] A preparation method of a polyethylene glycol glycerol liquid dressing includes the following steps: S1. Add 11 g of polyethylene glycol and 6 g of polyisocyanate to 92 g of deionized water and stir evenly to obtain solution A. Add 1.8 g of modified activated carbon and 4 g of glycerol to 17.25 g of deionized water and stir evenly to obtain solution B. Add 0.4 g of carbomer, 0.08 g of sodium hyaluronate, 0.009 g of leech extract, 0.15 g of panthenol, 0.2 g of methylparaben, 1 g of phenoxyethanol, and 0.3 g of arginine to 5.75 g of deionized water to obtain solution C; S2. Slowly add solution B in step S1 to solution A, continuously stir for 30 min, then continue to add solution C to solution A, and then stir for 35 min to obtain the liquid dressing; The preparation method of the above-mentioned modified activated carbon includes the following steps: S101. Add 2.3 g of activated carbon to a mixed solution of 9.2 g of EDTA and 115 g of deionized water, stir and mix for 5.5 h, then filter and dry at low temperature to obtain pretreated activated carbon; S102. Add 2.1 g of the pretreated activated carbon obtained in step S101 to a mixed solution of 7.4 g of deionized water and 10.3 g of isopropanol, stir evenly, dropwise add 3 mol / L hydrochloric acid to adjust the pH to 1.5, slowly dropwise add 0.23 g of titanium tetrachloride under ice bath conditions, continue to stir for 1.8 h, then dropwise add 1 mol / L sodium hydroxide solution to adjust the pH to 9.5, heat to 78 °C, and continue to react for 5.5 h to obtain a reaction solution; S103. Filter the reaction solution obtained in step S102 to obtain a product, wash the product with deionized water, and calcine it at 650 °C for 4 h under a nitrogen atmosphere to obtain a primary product; S104. Disperse 2.0 g of the crude product obtained in step S103 into 18.8 g of an aqueous solution of sodium dodecyl sulfate with a concentration of 0.1 mol / L, then add 0.25 g of polyacrylic acid and stir and mix for 35 min. Then continue to add 0.3 g of glutaraldehyde, continue to stir and mix for 2.2 h, and then filter. After washing with deionized water and drying, a modified activated carbon is obtained. Example 2

[0018] A preparation method of a polyethylene glycol glycerol liquid dressing comprises the following steps: S1. Add 7 g of polyethylene glycol and 2 g of polyisocyanate into 64 g of deionized water and stir evenly to obtain solution A. Add 0.8 g of modified activated carbon and 3 g of glycerol into 12 g of deionized water and stir evenly to obtain solution B. Add 0.2 g of carbomer, 0.04 g of sodium hyaluronate, 0.005 g of leech extract, 0.1 g of panthenol, 0.1 g of methylparaben, 0.5 g of phenoxyethanol and 0.2 g of arginine into 4 g of deionized water to obtain solution C; S2. Slowly add solution B in step S1 into solution A, continuously stir for 15 min, then continue to add solution C into solution A, and then stir for 15 min to obtain a liquid dressing; The preparation method of the above-mentioned modified activated carbon comprises the following steps: S101. Add 1.8 g of activated carbon into a mixed solution of 5.4 g of EDTA and 72 g of deionized water, stir and mix for 4 h, then filter and dry at low temperature to obtain a pretreated activated carbon; S102. Add 1.6 g of the pretreated activated carbon obtained in step S101 into a mixed solution of 6.9 g of deionized water and 5.75 g of isopropanol, stir evenly, dropwise add 3 mol / L hydrochloric acid to adjust the pH to 1, slowly dropwise add 0.23 g of titanium tetrachloride under an ice bath condition, continue to stir for 1 h, then dropwise add 1 mol / L sodium hydroxide solution to adjust the pH to 9, heat to 70 °C, and continue to react for 4 h to obtain a reaction solution; S103. Filter the reaction solution obtained in step S102 to obtain a product, wash the product with deionized water, and calcine it at 500 °C for 2 h under a nitrogen atmosphere to obtain a crude product; S104. Disperse 1.2 g of the crude product obtained in step S103 into 18.8 g of an aqueous solution of sodium dodecyl sulfate with a concentration of 0.1 mol / L, then add 0.2 g of polyacrylic acid and stir and mix for 20 min. Then continue to add 0.12 g of glutaraldehyde, continue to stir and mix for 1 h, and then filter. After washing with deionized water and drying, a modified activated carbon is obtained. Example 3

[0019] A preparation method of a polyethylene glycol glycerol liquid dressing comprises the following steps: S1. Add 12 g of polyethylene glycol and 8 g of polyisocyanate to 96 g of deionized water and stir evenly to obtain solution A. Add 2.2 g of modified activated carbon and 5 g of glycerol to 18 g of deionized water and stir evenly to obtain solution B. Add 0.6 g of carbomer, 0.12 g of sodium hyaluronate, 0.02 g of leech extract, 0.25 g of panthenol, 0.25 g of methylparaben, 1.1 g of phenoxyethanol and 0.6 g of arginine to 6 g of deionized water to obtain solution C; S2. Slowly add solution B in step S1 to solution A, continuously stir for 45 min, then continue to add solution C to solution A and then stir for 45 min to obtain a liquid dressing; The preparation method of the above-mentioned modified activated carbon includes the following steps: S101. Add 3.8 g of activated carbon to a mixed solution of 19 g of EDTA and 247 g of deionized water, stir and mix for 6 h, then filter and dry at low temperature to obtain pretreated activated carbon; S102. Add 3.2 g of the pretreated activated carbon obtained in step S101 to a mixed solution of 9.33 g of deionized water and 13.35 g of isopropanol, stir evenly, add 3 mol / L hydrochloric acid to adjust the pH to 2, slowly add 0.267 g of titanium tetrachloride under ice bath conditions, continue to stir for 2 h, then add 1 mol / L sodium hydroxide solution to adjust the pH to 10, heat to 80 °C, and continue to react for 6 h to obtain a reaction solution; S103. Filter the reaction solution obtained in step S102 to obtain a product, wash the product with deionized water, and calcine it at 700 °C for 5 h under a nitrogen atmosphere to obtain a primary product; S104. Disperse 2.8 g of the primary product obtained in step S103 into 18.8 g of a 0.1 mol / L sodium dodecyl sulfate aqueous solution, then add 0.28 g of polyacrylic acid and stir and mix for 40 min. Then continue to add 0.392 g of glutaraldehyde, continue to stir and mix for 3 h, then filter, wash with deionized water and dry to obtain modified activated carbon. Example 4

[0020] A preparation method of a polyethylene glycol glycerol liquid dressing includes the following steps: S1. Add 8 g of polyethylene glycol and 6 g of polyisocyanate to 88 g of deionized water and stir evenly to obtain solution A. Add 1.5 g of modified activated carbon and 4.5 g of glycerol to 16.5 g of deionized water and stir evenly to obtain solution B. Add 0.55 g of carbomer, 0.1 g of sodium hyaluronate, 0.008 g of leech extract, 0.18 g of panthenol, 0.15 g of methylparaben, 0.9 g of phenoxyethanol and 0.3 g of arginine to 5.5 g of deionized water to obtain solution C; S2. Slowly add the B solution in step S1 to the A solution. After continuously stirring for 25 min, continue to add the C solution to the A solution, and then stir for 30 min to obtain a liquid dressing; The preparation method of the above modified activated carbon includes the following steps: S101. Add 2.6 g of activated carbon to a mixed solution of 10.1 g of EDTA and 140 g of deionized water. After stirring and mixing for 5 h, filter and dry at low temperature to obtain pretreated activated carbon; S102. Add 2.2 g of the pretreated activated carbon obtained in step S101 to a mixed solution of 8.9 g of deionized water and 11.4 g of isopropanol, stir evenly, add 3 mol / L hydrochloric acid to adjust the pH to 1, slowly add 0.28 g of titanium tetrachloride under an ice bath condition, continue to stir for 2 h, then add 1 mol / L sodium hydroxide solution to adjust the pH to 9, heat to 80 °C, and continue to react for 4 h to obtain a reaction solution; S103. Filter the reaction solution obtained in step S102 to obtain a product. Wash the product with deionized water and calcine it at 600 °C for 3 h under a nitrogen atmosphere to obtain a primary product; S104. Disperse 1.8 g of the primary product obtained in step S103 into 15.6 g of a 0.1 mol / L sodium dodecyl sulfate aqueous solution, then add 0.2 g of polyacrylic acid and stir and mix for 30 min. Then continue to add 0.2 g of glutaraldehyde and continue to stir and mix for 2.5 h, then filter. After washing with deionized water and drying, modified activated carbon is obtained.

[0021] Comparative Example 1 Change the modified activated carbon added in the liquid dressing to ordinary activated carbon, with the same dosage as the modified activated carbon in Example 1, and the remaining steps are exactly the same as those in Example 1.

[0022] Comparative Example 2 Change the modified activated carbon added in the liquid dressing to nano-titanium dioxide, with the particle size of nano-titanium dioxide less than 5 nm and the molar amount the same as that of titanium tetrachloride in step S102 of Example 1, and the remaining steps are exactly the same as those in Example 1.

[0023] Comparative Example 3 Comparative Example 3 cancels step S104 relative to the example, and the remaining steps are exactly the same as those in Example 1.

[0024] Comparative Example 4 Comparative Example 4 completely cancels the addition of modified activated carbon relative to Example 1, and the remaining steps are exactly the same as those in Example 1.

[0025] Wound healing experiment Eight groups of white rats with exactly the same growth conditions were selected, with 5 white rats in each group. The hair on one side of the abdomen of all white rats was removed, and a wound with a diameter of 1 cm was cut at the hairless area. The liquid dressings of Examples 1-4 and Comparative Examples 1-4 were selected and applied to the wounds of all white rats respectively. The same dressing was used for 5 white rats in each group, and the average recovery time of the wounds of each group of white rats was counted. The statistical results are shown in Table 1 below: Table 1: Average wound recovery time table of each group of white rats corresponding to the liquid dressings prepared in Examples 1-4 and Comparative Examples 1-4 Average wound healing time (unit: h) Example 1 69.8 Example 2 73.4 Example 3 71.9 Example 4 67.5 Comparative Example 1 87.6 Comparative Example 2 83.4 Comparative Example 3 77.4 Comparative Example 4 96.1 From the data comparison between Example 1 and Comparative Examples 1-2 in Table 1 above, it can be seen that in the present invention, by loading titanium dioxide on the surface of activated carbon, the wound recovery speed can be effectively improved. Activated carbon can increase the surface area, and together with titanium dioxide, the antibacterial effect is greatly improved. In addition, from the comparison between Comparative Example 3 and Example 1, it can be seen that after activated carbon is treated with polyacrylic acid and glutaraldehyde and combined with polyethylene glycol and polyisocyanate, not only the distribution of the antibacterial material is more uniform, but also the tightly combined antibacterial network generated improves the antibacterial effect and accelerates the wound recovery.

[0026] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A polyethylene glycol glycerol liquid dressing, characterized in that, By mass parts, it includes the following components: 80 - 120 parts of deionized water, 7 - 12 parts of polyethylene glycol, 3 - 5 parts of glycerol, 0.2 - 0.6 parts of carbomer, 0.04 - 0.12 parts of sodium hyaluronate, 0.005 - 0.02 parts of leech extract, 0.1 - 0.25 parts of panthenol, 0.1 - 0.25 parts of methylparaben, 0.5 - 1.1 parts of phenoxyethanol, 0.2 - 0.6 parts of arginine, 2 - 8 parts of polyisocyanate and 0.8 - 2.2 parts of modified activated carbon; The preparation method of the said modified activated carbon includes the following steps: S101: Add activated carbon into the mixed solution of EDTA and deionized water, stir and mix for 4 - 6 h, then filter and dry at low temperature to obtain pretreated activated carbon; S102: Add the pretreated activated carbon obtained in step S101 into the mixed solution of deionized water and isopropanol, stir evenly, add 3 mol / L hydrochloric acid to adjust the pH to 1 - 2, slowly add titanium tetrachloride under ice bath condition, continue to stir for 1 - 2 h, then add 1 mol / L sodium hydroxide solution to adjust the pH to 9 - 10, heat to 70 - 80 °C, and continue to react for 4 - 6 h to obtain the reaction solution; S103: Filter the reaction solution obtained in step S102 to obtain the product, wash the product with deionized water and then continue to calcine to obtain the primary product; S104: Disperse the primary product obtained in step S103 into 0.1 mol / L sodium dodecyl sulfate aqueous solution, then add polyacrylic acid and stir and mix for 20 - 40 min, then continue to add glutaraldehyde, continue to stir and mix for 1 - 3 h and then filter, wash with deionized water and dry to obtain modified activated carbon.

2. The polyethylene glycol glycerol liquid dressing according to claim 1, characterized in that, In step S101, the mass ratio among activated carbon, EDTA and deionized water is 1:(3 - 5):(40 - 65).

3. The polyethylene glycol glycerol liquid dressing according to claim 1, wherein In step S102, the mass ratio among titanium tetrachloride, pretreated activated carbon, deionized water and isopropanol is 1:(7 - 12):(30 - 35):(25 - 50).

4. The polyethylene glycol glycerol liquid dressing according to claim 1, characterized in that, The calcination in step S103 is completed under nitrogen atmosphere, the calcination temperature is 500 - 700 °C, and the calcination time is 2 - 5 h.

5. The polyethylene glycol glycerol liquid dressing according to claim 1, wherein In step S104, the mass ratio among polyacrylic acid, glutaraldehyde, primary product and sodium dodecyl sulfate aqueous solution is 1:(0.6 - 1.4):(6 - 10):(60 - 80).

6. A preparation method of the polyethylene glycol glycerol liquid dressing according to any one of claims 1-5, characterized in that, It includes the following steps: S1: Add polyethylene glycol and polyisocyanate into deionized water and stir evenly to obtain solution A, add modified activated carbon and glycerol into deionized water and stir evenly to obtain solution B, and add carbomer, sodium hyaluronate, leech extract, panthenol, methylparaben, phenoxyethanol and arginine into deionized water to obtain solution C; S2: Slowly add solution B in step S1 into solution A, continuously stir for 15 - 45 min, then continue to add solution C into solution A, and then stir for 15 - 45 min to obtain the liquid dressing.

7. The preparation method of the polyethylene glycol glycerol liquid dressing according to claim 6, characterized in that, In step S1, the mass ratio of deionized water in solution A, deionized water in solution B and deionized water in solution C is 16:3:1.