A self-adhesive rapid blood coagulation bandage-type hydrogel and preparation method thereof
By simplifying the preparation process of hydrogel by using raw materials such as quaternary ammonium chitosan, ammonium persulfate and acrylic monomers, the problems of complex hydrogel processes and poor hemostatic effect are solved, and self-adhesion and rapid coagulation are achieved. Simplify production and significantly improve the hemostatic effect.
Patent Information
- Application Number
- CN202310387382.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-04-12
- Publication Date
- 2024-12-24
- Estimated Expiration
- 2043-04-12
AI Technical Summary
The existing hydrogel production process is complex and has many materials, making it difficult to achieve large-scale industrial production, and it has poor clinical hemostatic effect, and lacks rapid hemostatic materials that are simple and easy to produce.
The porous hydrogel is prepared by using raw materials such as quaternary ammonium chitosan, ammonium persulfate and acrylic monomers through simple stirring, degassing and heating reaction steps, simplifying the gel-forming process and improving coagulation performance.
It realizes rapid coagulation of self-adhesion, simplifies the preparation process, reduces the reaction temperature and time, is suitable for industrial production, and significantly improves the hemostatic effect.
Smart Images

Figure CN116510067B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a self-adhesive rapid blood coagulation bandage-type hydrogel and a preparation method thereof, belonging to the technical field of functional polymer material preparation. Background Art
[0002] Smart hydrogel is an important branch of functional polymer materials. Hydrogel is a gel with water as the dispersion medium. A part of hydrophobic groups is introduced into the water-soluble polymer with a cross-linked structure to form a cross-linked polymer that can swell in water. It has a three-dimensional network structure with mild chemical cross-linking and mutual entanglement between molecular chains (physical cross-linking). Hydrophilic small molecules can diffuse in the hydrogel. According to the response of hydrogel to external stimuli, hydrogel can be divided into two categories: one is traditional hydrogel, which is not particularly sensitive to environmental changes; the other is environmentally sensitive hydrogel or smart hydrogel, which responds to different degrees to the stimuli caused by the environment to a considerable extent, has external field response characteristics, and its morphology and performance can change with changes in external environmental conditions such as temperature, pH value, light, electromagnetic field or chemical substances. Its application prospects are very broad.
[0003] At present, many hydrogels can achieve adhesion to the skin, carry drugs, and promote wound healing and repair. Some hydrogels also have a certain coagulation effect, but their production process is slightly complicated, requiring more materials, and it is difficult to achieve large-scale industrial production. There are also few practical applications in clinical practice. Therefore, a simple and easy-to-produce hydrogel is needed to quickly stop bleeding on wounds. Summary of the invention
[0004] Purpose of the invention: The first purpose of the present invention is to provide a self-adhesive rapid blood clotting bandage-like hydrogel; the second purpose of the present invention is to provide a method for preparing the self-adhesive rapid blood clotting bandage-like hydrogel.
[0005] Technical solution: The invention discloses a self-adhesive rapid blood clotting bandage-type hydrogel, which is prepared from raw materials with the following solid-liquid ratio: quaternary ammonium salt chitosan: ammonium persulfate: acrylic acid monomer: water of 8-11: 5-8: 50-70: 180-210 g / g / mL / mL.
[0006] Furthermore, the hydrogel is prepared from raw materials with the following solid-liquid ratio: quaternary ammonium salt chitosan: ammonium persulfate: acrylic acid monomer: water of 9.5-10.5: 5.9-7: 50-60: 185-200 g / g / mL / mL.
[0007] Furthermore, the hydrogel is prepared from raw materials with the following solid-liquid ratio: quaternary ammonium salt chitosan: ammonium persulfate: acrylic acid monomer: water is 10:5.9:50:190 g / g / mL / mL.
[0008] The method for preparing the self-adhesive rapid blood clotting bandage-type hydrogel of the present invention is characterized by comprising the following steps:
[0009] Dissolve acrylic acid monomer and quaternary ammonium salt chitosan in water, stir quickly to evenly mix, add ammonium persulfate, stir quickly to dissolve, degas, seal, and heat to react to obtain the product.
[0010] Furthermore, the temperature of the rapid stirring is greater than 0°C and less than 30°C.
[0011] Furthermore, the temperature greater than 0°C during the continued rapid stirring and dissolution is less than 30°C.
[0012] Furthermore, the degassing is to treat the mixed sample at low temperature and vacuum not higher than 0.1 MPa for about 10 minutes to remove bubbles and form pores.
[0013] Furthermore, the low temperature is greater than 0°C and less than 30°C.
[0014] Furthermore, the sealed environment humidity is higher than 95%.
[0015] Furthermore, the temperature of the heating reaction is 45 to 55° C., and the time of the heating reaction is 0 to 12 hours.
[0016] Furthermore, the heating reaction temperature is 50° C. and the heating reaction time is 12 hours.
[0017] The present invention uses quaternary ammonium salt chitosan as a raw material to polymerize into a porous hydrogel carrier, simplifies the gelling step, makes it easier to carry out industrial production, and improves the coagulation performance of the material.
[0018] Beneficial effects: Compared with the prior art, the present invention has the following significant advantages:
[0019] (1) The preparation process of the present invention is simple, the reaction temperature is low, the product can be obtained by one-step reaction, the reaction time is short, and it is convenient for industrial production.
[0020] (2) The hydrogel prepared by the present invention can achieve self-adhesion and rapid coagulation, and has a better hemostatic effect than the commonly used materials available on the market. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 The results of blood coagulation tests on the hydrogels and other materials prepared in Examples 1 and 4 are shown. DETAILED DESCRIPTION
[0022] The technical solution of the present invention is further described below in conjunction with the accompanying drawings.
[0023] Example 1
[0024] A self-adhesive rapid blood coagulation bandage-type hydrogel, the raw material composition is as follows:
[0025] 0.1g quaternary ammonium salt chitosan, 0.059g ammonium persulfate, 0.5mL acrylic acid, 1.9mL water. The preparation method is as follows:
[0026] Dissolve acrylic acid monomer and quaternary ammonium salt chitosan in water, stir quickly and uniformly at a temperature above 0°C and below 30°C, add ammonium persulfate, stir quickly and dissolve at a temperature above 0°C and below 30°C, then remove bubbles and make holes at low temperature (above 0°C and below 30°C) and vacuum 0.1MPa, seal under a humidity of more than 95%, and react at 55°C for 10 hours to obtain the product. It has excellent coagulation effect.
[0027] Example 2
[0028] A self-adhesive rapid blood coagulation bandage-type hydrogel, the raw material composition is as follows:
[0029] 0.11g quaternary ammonium salt chitosan, 0.062g ammonium persulfate, 0.6mL acrylic acid, 2.0mL water. The preparation method is as follows:
[0030] Dissolve acrylic acid monomer and quaternary ammonium salt chitosan in water, stir quickly and uniformly at a temperature above 0°C and below 30°C, add ammonium persulfate, stir quickly and dissolve at a temperature above 0°C and below 30°C, then remove bubbles and make holes at low temperature (above 0°C and below 30°C) and vacuum 0.1MPa, seal under a humidity of more than 95%, and react at 50°C for 11 hours to obtain the product. It has excellent coagulation effect.
[0031] Example 3
[0032] A self-adhesive rapid blood coagulation bandage-type hydrogel, the raw material composition is as follows:
[0033] 0.09g quaternary ammonium salt chitosan, 0.059g ammonium persulfate, 0.55mL acrylic acid, 1.9mL water. The preparation method is as follows:
[0034] Dissolve acrylic acid monomer and quaternary ammonium salt chitosan in water, stir quickly and uniformly at a temperature above 0°C and below 30°C, add ammonium persulfate, stir quickly and dissolve at a temperature above 0°C and below 30°C, then remove bubbles and make holes at low temperature (above 0°C and below 30°C) and vacuum 0.1MPa, seal under a humidity of more than 95%, and react at 48°C for 12 hours to obtain the product. It has excellent coagulation effect.
[0035] Example 4
[0036] A self-adhesive rapid blood coagulation bandage-type hydrogel, the raw material composition is as follows:
[0037] 0.08g quaternary ammonium salt chitosan, 0.059g ammonium persulfate, 0.5mL acrylic acid, 2.0mL water. The preparation method is as follows:
[0038] Dissolve acrylic acid monomer and quaternary ammonium salt chitosan in water, stir quickly and evenly at a temperature above 0°C but below 30°C, add ammonium persulfate, stir quickly and dissolve at a temperature above 0°C but below 30°C, then remove bubbles and make holes at low temperature (above 0°C but below 30°C) and vacuum 0.1MPa, seal at a humidity above 95%, and react at 50°C for 11 hours to obtain the product with excellent coagulation effect.
[0039] Example 5
[0040] A self-adhesive rapid blood coagulation bandage-type hydrogel, the raw material composition is as follows:
[0041] 0.1g quaternary ammonium salt chitosan, 0.059g ammonium persulfate, 0.5mL acrylic acid, 1.9mL water. The preparation method is as follows:
[0042] Dissolve acrylic acid monomer and quaternary ammonium salt chitosan in water, stir quickly and uniformly at a temperature above 0°C and below 30°C, add ammonium persulfate, stir quickly and dissolve at a temperature above 0°C and below 30°C, then remove bubbles and make holes at low temperature (above 0°C and below 30°C) and vacuum 0.1MPa, seal at a humidity of more than 95%, and react at 40°C for 12 hours. The resulting hydrogel is not fully polymerized and cannot be completely gelled. Because it cannot be completely gelled, the coagulation effect is not measured.
[0043] Example 6
[0044] A self-adhesive rapid blood coagulation bandage-type hydrogel, the raw material composition is as follows:
[0045] 0.05g quaternary ammonium salt chitosan, 0.059g ammonium persulfate, 0.5mL acrylic acid, 1.9mL water. The preparation method is as follows:
[0046] Dissolve acrylic acid monomer and quaternary ammonium salt chitosan in water, stir quickly and uniformly at a temperature above 0°C and below 30°C, add ammonium persulfate, stir quickly and dissolve at a temperature above 0°C and below 30°C, then remove bubbles and make holes at low temperature (above 0°C and below 30°C) and vacuum 0.1MPa, seal at a humidity above 95%, react at 50°C for 11 hours, and the resulting hydrogel is not fully polymerized and cannot be completely gelled. Because it cannot be completely gelled, the coagulation effect is not measured.
[0047] The hydrogels prepared in Examples 1-4 were subjected to a coagulation performance test, and the coagulation performance was preliminarily determined by the amount of blood cells precipitated on the surface of the hydrogels.
[0048] Divide six areas on a clean glass plate. Figure 1 , recorded as a, b, c, d, e, f, where a is a blank control without blood coagulation, b uses a PE film, which is the same material as the middle part of the Band-Aid, c is the hydrogel material prepared in Example 1, d is an acrylic film, e is a commercial hemostatic sponge (Kuaikang hemostatic sponge), and f is the hydrogel material prepared in Example 4. After thawing human blood (collected from Zhongda Hospital affiliated to Southeast University) in a 37-degree Celsius water bath, the divided areas on the glass plate were dripped separately. Use a dropper to drop 1 drop of blood on each of the six areas to ensure that the area covered by each drop of blood is basically the same. After 20 seconds, the six areas are rinsed with standard PBS buffer to wash away excess blood, leaving only the deposited red blood cells. The results are as follows: Figure 1 shown. Figure 1 The results of the blood coagulation test of the hydrogels and other materials prepared in Examples 1 and 4 are shown in FIG. Figure 1 It is observed that, compared with PE film and commercial hemostatic sponge, the hydrogel materials prepared in Examples 1 and 4 of the present invention have obvious rapid coagulation effect, and the effect of Example 1 is better than that of Example 4. That is, within the scope of the claims, the prepared hydrogel materials have rapid coagulation effect, and the optimal ratio is the best.
Claims
1. A self-adhesive rapid coagulation bandage-type hydrogel, characterized in that: The hydrogel is prepared from raw materials with the following solid-liquid ratio: quaternary ammonium salt chitosan: ammonium persulfate: acrylic acid monomer: water in a ratio of 8-11: 5-8: 50-70: 180-210 g / g / mL / mL.
2. The self-adhesive rapid blood clotting bandage-type hydrogel according to claim 1, characterized in that: The hydrogel is prepared from raw materials with the following solid-liquid ratio: quaternary ammonium salt chitosan: ammonium persulfate: acrylic acid monomer: water (9.5-10.5: 5.9-7: 50-60: 185-200 g / g / mL / mL).
3. The self-adhesive rapid blood clotting bandage-type hydrogel according to claim 1, characterized in that: The hydrogel is prepared from raw materials with the following solid-liquid ratio: quaternary ammonium salt chitosan: ammonium persulfate: acrylic acid monomer: water in a ratio of 10:5.9:50:190 g / g / mL / mL.
4. The method for preparing the self-adhesive rapid blood clotting bandage-type hydrogel according to any one of claims 1 to 3, characterized in that: The following steps are involved: Dissolve acrylic acid monomer and quaternary ammonium salt chitosan in water, stir quickly to evenly mix, add ammonium persulfate, stir quickly to dissolve, degas, seal, and heat to react to obtain the product.
5. The preparation method according to claim 4, characterized in that: The temperature of the rapid stirring is greater than 0°C and less than 30°C.
6. The preparation method according to claim 4, characterized in that: The temperature of the rapid stirring and dissolving is greater than 0°C and less than 30°C.
7. The preparation method according to claim 4, characterized in that: The degassing is to treat the mixed sample at low temperature and vacuum not higher than 0.1 MPa for 10 minutes to remove bubbles and form pores.
8. The preparation method according to claim 7, characterized in that: The low temperature is greater than 0°C and less than 30°C.
9. The preparation method according to claim 4, characterized in that: The sealed ambient humidity is higher than 95%.
10. The preparation method according to claim 4, characterized in that: The temperature of the heating reaction is 45-55° C., and the time of the heating reaction is 10-12 hours.
Citation Information
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