Preparation method of pasty film-forming dressing

Abstract

The invention discloses a preparation method of a paste film-forming dressing, and provides an emulsifying tank in which a stirrer and a homogenizing head are separately arranged and paddles are arranged on the edge of a rotor. The emulsification tank is combined with regulation and control of key process conditions, and ethanol, a high polymer material, a traditional Chinese medicine extract and an additive are used as raw materials, so that the pasty film-forming dressing is prepared. The pasty film-forming dressing disclosed by the invention is uniform and fine, has good pasty formability and stability, and meets the requirements of industrial production.

Description

Technical Field

[0001] This invention belongs to the field of medical device technology, specifically relating to a method for preparing a paste-like film-forming dressing. Background Technology

[0002] Liquid film-forming dressings are a common dosage form in medical dressings, ranging from aqueous fluids to viscous creams. Cream-based film-forming dressings are typically multiphase systems (such as oil-water emulsions or solid particle-emulsion composite systems). During raw material formulation, the dispersed phase may exhibit problems such as coarse particle size and uneven distribution (e.g., partial aggregation), leading to defects in the dressing's texture, stability (e.g., easy delamination), uneven thickness, and variations in mechanical properties.

[0003] Existing homogenizing emulsifiers primarily use a stirring paddle mounted on a stirring shaft and a shear head located at the bottom of the shaft to shear the material, breaking down large-diameter particles or droplets in the raw material to obtain a uniformly dispersed system. For example, patent CN205517303U discloses a vacuum homogenizing emulsifier, patent CN203329650U discloses a frame-type bidirectional stirring homogenizing emulsifier, and patent CN219482281U discloses a homogenizing dispersion device for hydrogen energy fuel cell membrane electrode slurry. In these homogenizing emulsifiers, the stirring paddle and shear head need to rotate synchronously. While high rotation speed can improve homogenization efficiency, it can easily lead to damage or breakage of the stirring paddle; lower rotation speed is beneficial for the maintenance of the stirring paddle, but it also reduces homogenization efficiency.

[0004] Therefore, developing a homogenizing emulsifier that can effectively maintain the stirring paddle and increase the rotational speed of the shear head, thereby improving homogenization efficiency, and applying it to the industrial production of ointment-forming dressings, is of great significance to the development of the dressing industry. Summary of the Invention

[0005] In order to solve the above-mentioned technical problems, improve the quality of ointment-based film-forming dressings, and meet the needs of industrialized dressing production, the present invention provides the following technical solutions.

[0006] In a first aspect, the present invention provides a method for preparing a paste-like film-forming dressing, the method comprising the following steps: (1) Add ethanol to an emulsification tank, and then add polymer materials. The emulsification tank is equipped with a stirrer and a homogenizing and dispersing device.

[0007] (2) Turn on the stirrer and homogenizing device respectively, control the stirring speed to 30~60 rpm and the homogenizing speed to 1000~2000 rpm, mix the materials in the emulsification tank evenly, and obtain a viscous mixture.

[0008] (3) Heat the emulsification tank to 35~45℃, add the Chinese herbal extract, mix and homogenize at a stirring speed of 30~60 rpm and a homogenization speed of 1000~2000 rpm to obtain a paste material, and remove the air bubbles to obtain the paste film-forming dressing.

[0009] The homogenizing and dispersing device is installed at the bottom of the emulsifying tank and includes a stator and a rotor, with blades provided on the edge of the rotor.

[0010] The unique design of the blades can increase the shear force of the homogenizer, and the homogenization effect of the homogenizer is significantly improved compared with a single rotor.

[0011] Preferably, in steps (2) and (3), the stirring speed is 30~60 rpm, for example: 30 rpm, 32 rpm, 35 rpm, 38 rpm, 40 rpm, 43 rpm, 45 rpm, 47 rpm, 50 rpm, 55 rpm, 60 rpm.

[0012] Preferably, in steps (2) and (3), the homogenization speed is 1000~2000 rpm, for example: 1000 rpm, 1200 rpm, 1500 rpm, 1700 rpm, 2000 rpm.

[0013] Preferably, the mixing time in steps (2) and (3) is 3 to 5 hours, for example: 3 hours, 3.5 hours, 4 hours, 4.5 hours, 5 hours.

[0014] Preferably, in step (3), the temperature of the emulsifying tank is 35~45℃, for example: 35℃, 36℃, 37℃, 38℃, 39℃, 40℃, 41℃, 42℃, 43℃, 44℃, 45℃.

[0015] Preferably, in step (1), the ethanol concentration is ≥95%, for example: 95%, 96%, 97%, 98%, 99%, 100%.

[0016] Preferably, the polymeric material includes one or more of polyvinylpyrrolidone, poloxamer, and polyethylene glycol.

[0017] Preferably, the additive includes one or more of antioxidants, pH adjusters, or pigments; more preferably, the additive is an antioxidant.

[0018] Preferably, the herbal extract includes one or more of Bletilla striata extract, Corydalis yanhusuo extract, and Panax notoginseng extract.

[0019] Furthermore, the polymeric material is polyvinylpyrrolidone, poloxamer, and polyethylene glycol; the additive is an antioxidant; the herbal extract is Bletilla striata extract, Corydalis yanhusuo extract, and Panax notoginseng extract; and the mass ratio of ethanol, polyvinylpyrrolidone, poloxamer, antioxidant, polyethylene glycol, Bletilla striata extract, Corydalis yanhusuo extract, and Panax notoginseng extract is 30~40:20~25:3~6:0.1~0.5:1~3:10~15:6~10:1 0~15, for example: 30:20:3:0.1:1:10:6:10, 32:22:5:0.15:2:11:7:13, 35.9:24.7:4.8:0.2:2.4:12:8:12, 38:23:4:0.2:3:13:7:14, 40:25:6:0.5:3:15:10:15, more preferably 35.9:24.7:4.8:0.2:2.4:12:8:12.

[0020] Preferably, in step (3), before removing the air bubbles, the paste material is transferred into a settling tank through a pipe and left to stand for 10 to 15 hours, for example: 10 hours, 11 hours, 12 hours, 13 hours, 14 hours, or 15 hours.

[0021] Preferably, the preparation method further includes the steps of lowering the temperature of the emulsification tank to below 20°C before adding ethanol, and then evacuating and filling it with inert gas to maintain pressure.

[0022] Maintaining a low temperature in the emulsification tank prevents the exothermic dissolution of polyvinylpyrrolidone from causing excessively high local temperatures in the system, which could lead to oxidation and deterioration of the raw materials due to overheating. Maintaining a vacuum in the emulsification tank also prevents dust problems caused by powdery materials.

[0023] Preferably, the vacuum degree of the emulsification tank is 0.03~0.05 Pa.

[0024] Preferably, in the homogenizing device, the blades are evenly distributed around the rotor, and the blades are perpendicular to the plane of rotation of the rotor.

[0025] Furthermore, the number of blades is 4, 6, 8, or 10.

[0026] Preferably, the rotor is located above the stator, the stator and the rotor are coaxial, and the shaft passes through the bottom of the emulsifying tank and is connected to an external homogenizing motor.

[0027] Preferably, the emulsifying tank further includes a condensation reflux device, a temperature control system, a pressure control system, and pipelines.

[0028] The condensation reflux device is installed at the top of the emulsification tank, the temperature control system is installed in the middle and bottom of the emulsification tank, the pressure control system is installed at the top of the emulsification tank, and the agitator is installed in the middle of the emulsification tank.

[0029] Preferably, the temperature control system includes a temperature sensor and a jacket. The temperature sensor is installed at the bottom of the emulsification tank, the jacket is connected to an external cooling water source through a lower opening, and the jacket is connected to an external steam source through an upper opening.

[0030] Preferably, the pressure control system includes a pressure gauge and a safety valve, both of which are installed on the end cap of the emulsifying tank.

[0031] Preferably, the agitator includes a stirring frame, stirring blades, a stirring shaft, a scraper, and a spiral ribbon. The stirring blades are disposed on the inner side of the stirring frame, the scraper is disposed on the outer side and bottom of the stirring frame, and the two ends of the spiral ribbon are respectively connected to the diagonal points of the stirring frame. The stirring shaft passes through the end cap of the emulsification tank and is connected to the stirring motor.

[0032] In one specific embodiment of the present invention, the preparation process of the ointment-like film-forming dressing is as follows: (1) Reduce the temperature of the emulsification tank to below 20°C, then evacuate to 0.03~0.05 Pa, and then fill with inert gas to maintain pressure.

[0033] (2) Add 30-40 parts by weight of 90% or more of ethanol to the emulsification tank, and then add 20-25 parts by weight of polyvinylpyrrolidone, 3-6 parts by weight of poloxamer, 0.1-0.5 parts by weight of antioxidant and 1-3 parts by weight of polyethylene glycol.

[0034] (3) Turn on the stirrer and homogenizing device respectively, control the stirring speed to 30~60 rpm and the homogenizing speed to 1000~2000 rpm, mix and homogenize the materials in the emulsification tank for 3~5 h to obtain a viscous mixture.

[0035] (4) Heat the emulsification tank to 35~45℃, and add 10~15 parts of Bletilla striata extract, 6~10 parts of Corydalis yanhusuo extract and 10~15 parts of Panax notoginseng extract by weight. Mix and homogenize for 3~5 h at a stirring speed of 30~60 rpm and a homogenization speed of 1000~2000 rpm to obtain a paste.

[0036] (5) Transfer the paste material through a pipe into a settling tank and let it stand for 10-15 hours to remove air bubbles and obtain the paste film-forming dressing.

[0037] In a second aspect, the present invention provides a paste-like film-forming dressing, wherein the film-forming dressing is prepared according to the preparation method described in the first aspect.

[0038] The beneficial effects of this invention are: I. This invention separates the agitator and homogenizing head in existing homogenizing emulsifiers, ensuring both the maintenance requirements of low-speed agitation and the shear force requirements of high-speed homogenizing head. The combined action of the upper agitator and the lower homogenizing head improves the working efficiency of the emulsification tank.

[0039] II. This invention combines a specially structured emulsifying tank with precise control of key process conditions (such as homogenization temperature and homogenization speed) to produce a paste-like film-forming dressing using ethanol, polymeric materials (such as polyvinylpyrrolidone, poloxamer, and polyethylene glycol), antioxidants, and traditional Chinese medicine extracts (such as Bletilla striata extract, Corydalis yanhusuo extract, and Panax notoginseng extract) as raw materials. This dressing is uniform and delicate, exhibiting excellent paste-forming properties and stability, meeting the needs of industrial production. Attached Figure Description

[0040] Figure 1 The diagram shown is an overall structural diagram of the emulsification tank of the present invention; Figure 2 The diagram shown is a structural diagram of a homogenizing dispersion device. Figure 3 The diagram shown is a structural diagram of a stirrer.

[0041] The reference numerals in the figure are as follows: 101-condensation reflux device, 102-stirrer, 103-upper opening of jacket, 104-jacket, 105-discharge port, 106-homogenization and dispersion device, 107-temperature sensor, 108-lower opening of jacket, 109-sampling port, 110-jacket pressure gauge port, 111-feed port, 112-stirring motor, 201-rotor, 202-blade, 203-stator, 204-homogenization motor, 301-stirring shaft, 302-ribbon, 303-stirring frame, 304-stirring blade, 305-scraper. Detailed Implementation

[0042] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments and accompanying drawings. The described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0043] like Figure 1-3 As shown, the emulsifying tank of the present invention includes a condensation reflux device 101, a temperature control system, a pressure control system, a stirrer 102, a discharge port 105, a homogenizing and dispersing device 106, a sampling port 109, a feed port 111, and a pipeline.

[0044] The condensation reflux device 101 is installed on the top of the emulsification tank and includes a condenser and a condenser tube, which is connected to the end cap of the emulsification tank.

[0045] The temperature control system is installed in the middle and bottom of the emulsifying tank. The temperature control system includes a temperature sensor 107 and a jacket 104. The temperature sensor 107 is installed at the bottom of the emulsifying tank. The jacket 104 is connected to an external cooling water source through a lower opening 108, and the jacket 104 is connected to an external steam source through an upper opening 103. A jacket pressure gauge port 110 is provided on the upper part of the jacket 104.

[0046] The pressure control system is installed on top of the emulsifying tank. The pressure control system includes a pressure gauge and a safety valve, both of which are mounted on the end cap of the emulsifying tank.

[0047] A stirrer 102 is installed in the middle of the emulsification tank. The stirrer 102 includes a stirring frame 303, stirring blades 304, a stirring shaft 301, scrapers 305, and a spiral ribbon 302. The stirring blades 304 are located inside the stirring frame 303. The scrapers 305 are located on the outer side and bottom of the stirring frame 303. The two ends of the spiral ribbon 302 are connected to opposite corners of the stirring frame 303. The stirring shaft 301 passes through the end cap of the emulsification tank and is connected to a stirring motor 112.

[0048] A homogenizing and dispersing device 106 is installed at the bottom of an emulsifying tank and includes a rotor 201, blades 202, and a stator 203. The rotor 201 is located above the stator 203, and the stator 203 and rotor 201 are coaxial. This shaft passes through the bottom of the emulsifying tank and is connected to an external homogenizing motor 204. Blades 202 are disposed at the edge of the rotor 201 and are evenly distributed around the rotor 201. The blades 202 are perpendicular to the plane of the rotor 201, and their number is even (e.g., 6).

[0049] Example 1: Preparation of ointment-based film-forming dressing sample 1 1.1 Cooling water at 10℃ is used to cool the jacket of the 300 L emulsification tank. When the temperature drops below 20℃, the tank is evacuated to 0.05 Pa and then filled with nitrogen to maintain pressure.

[0050] 1.2 Weigh 35.9 kg of anhydrous ethanol and add it to an emulsification tank. Then add 24.7 kg of polyvinylpyrrolidone, 4.8 kg of poloxamer, 0.2 kg of antioxidant, and 2.4 kg of polyethylene glycol in sequence.

[0051] 1.3 Turn on the agitator and homogenizing device respectively, control the agitation speed to 50 rpm and the homogenization speed to 1000 rpm, mix and homogenize the materials in the emulsification tank for 4 h to obtain a viscous mixture.

[0052] 1.4 Heat the emulsification tank to 35°C, then add 12 kg of Bletilla striata extract, 8 kg of Corydalis yanhusuo extract and 12 kg of Panax notoginseng extract. Maintain a stirring speed of 50 rpm and a homogenization speed of 1000 rpm, and continue mixing and homogenizing for 4 hours to obtain a paste.

[0053] 1.5 The paste material was transferred into a settling tank through a pipeline and allowed to stand for 12 hours. Then, air bubbles were removed to obtain paste film-forming dressing sample 1.

[0054] Example 2 Preparation of paste-like film-forming dressing sample 2 The specific preparation process is the same as in Example 1, except that the homogenization speed is 1500 rpm.

[0055] Example 3 Preparation of ointment-based film-forming dressing sample 3 The specific preparation process is the same as in Example 1, except that the homogenization speed is 2000 rpm.

[0056] Example 4: Preparation of paste-like film-forming dressing sample 4 The specific preparation process is the same as in Example 1, except that the emulsification tank is heated to 40°C.

[0057] Example 5: Preparation of paste-like film-forming dressing sample 5 The specific preparation process is the same as in Example 1, except that the emulsification tank is heated to 45°C and the homogenization speed is 1500 rpm.

[0058] Example 6 Preparation of ointment-based film-forming dressing sample 6 The specific preparation process is the same as in Example 1, except that the emulsification tank is heated to 45°C and the homogenization speed is 2000 rpm.

[0059] Comparative Example 1: Preparation of Ointment-Based Film-Forming Dressing (Comparative Sample 1) The specific preparation process is the same as in Example 1, except that the homogenization speed is 800 rpm.

[0060] Comparative Example 2: Preparation of Ointment-Based Film-Forming Dressing (Comparative Sample 2) The specific preparation process is the same as that of Comparative Example 1, except that the emulsification tank is heated to 45°C and the homogenization speed is 800 rpm.

[0061] Comparative Example 3: Preparation of Ointment-Based Film-Forming Dressing (Comparative Sample 3) The specific preparation process is the same as that of Comparative Example 1, except that the emulsification tank is heated to 25°C and the homogenization speed is 2000 rpm.

[0062] Comparative Example 4: Preparation of Ointment-Based Film-Forming Dressing (Comparative Sample 4) The specific preparation process is the same as in Example 1, except that the emulsification tank is heated to 30°C and the homogenization speed is 2000 rpm.

[0063] Comparative Example 5: Preparation of Ointment-Based Film-Forming Dressing (Comparative Sample 5) The specific preparation process is the same as in Example 1, except that the emulsification tank is heated to 50°C and the homogenization speed is 2000 rpm.

[0064] Comparative Example 6: Preparation of Ointment-Based Film-Forming Dressing (Comparative Sample 6) The specific preparation process is the same as in Example 1, except that the emulsification tank is heated to 35°C and the homogenization speed is 2500 rpm.

[0065] Comparative Example 7: Preparation of Ointment-Based Film-Forming Dressing Compared to Sample 6 The specific preparation process is the same as in Example 1, except that the emulsification tank is heated to 45°C and the homogenization speed is 2500 rpm.

[0066] Testing the film-forming effect of ointment-based film-forming dressings Take 2 mL of dressing samples from Examples 1-6 and Comparative Examples 1-7 respectively, spread them evenly on a 10cm×5cm glass plate, and observe the film formation effect in an oven at 37°C.

[0067] Table 1 Film-forming effect of dressing samples

[0068] As shown in Table 1, under the conditions of homogenization temperature of 35-45℃ and homogenization speed of 1000-2000 rpm, Examples 1-6 showed good film formation. Comparative Examples 1-2 showed poor film formation and unevenness, mainly due to the low homogenization speed failing to achieve the desired homogenization effect. Comparative Examples 3-4 showed poor film formation and unevenness, mainly due to the low homogenization temperature, resulting in poor fluidity of the film-forming matrix and affecting the homogenization effect. Comparative Example 5 showed poor film formation and the appearance of black particles, mainly because the homogenization temperature was too high, causing material denaturation and blackening. Comparative Examples 6-7 showed poor film formation and unevenness, mainly because the excessively high homogenization speed led to localized shear force concentration, causing excessive pulverization of the functional particles (traditional Chinese medicine powder), resulting in uneven distribution.

[0069] The above results indicate that homogenization temperature and homogenization speed are the main factors affecting the preparation of ointment film-forming dressings, and the combined effect of the two is necessary to improve the quality of ointment dressings.

[0070] Determination of dynamic viscosity of paste-forming dressings According to the "0633 Viscosity Determination Method III" in the Pharmacopoeia of the People's Republic of China (2020 Edition), the dressing samples of Examples 1-6 and Comparative Examples 1-7 were tested using the rotational viscometer method.

[0071] Table 2 Dynamic viscosity of dressings

[0072] As shown in Table 2, when the homogenization temperature is constant, the higher the homogenization speed, the lower the dynamic viscosity of the film-forming matrix, the better the fluidity, and the better the dispersion effect of the system.

[0073] The above results indicate that both homogenization temperature and homogenization speed affect the preparation of ointment film-forming dressings, and the combined effect of both is necessary to improve the quality of ointment dressings.

[0074] Stability testing of ointment-based film-forming dressings The dressing samples prepared in Examples 1-6 and Comparative Examples 1-7 were placed in a drug stability test chamber (temperature 30℃±2℃; relative humidity 65%±5%) for accelerated testing. Samples were taken after 0, 1, 3 and 6 months to examine the properties of the ointment film-forming dressing.

[0075] Table 3 Stability of Dressings

[0076] Table 3 shows that the dressing products of Examples 1-6 exhibited good stability under homogenization temperatures of 35-45℃ and homogenization speeds of 1000-2000 rpm. The results of Comparative Examples 1-2 indicate that excessively low homogenization speeds negatively impacted the stability of the dressing products. The results of Comparative Examples 3-4 show that excessively low homogenization temperatures affected the homogenization effect, thus affecting the stability of the dressing products. The results of Comparative Example 5 indicate that when the homogenization temperature reached 50℃, some materials underwent denaturation, affecting the stability of the dressing products. The results of Comparative Examples 6-7 show that excessively high homogenization speeds also damaged the materials, affecting the stability of the products.

[0077] The above results indicate that homogenization temperature and homogenization speed are the main factors affecting the preparation of ointment film-forming dressings, and the combination of the two is necessary to obtain high-performance ointment film-forming dressings.

[0078] The above description is merely an embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural transformations made based on the content of the present invention specification, or direct or indirect applications in other related technical fields, are similarly included within the patent protection scope of the present invention.

Claims

1. A method for preparing a paste-like film-forming dressing, characterized in that, The preparation method includes the following steps: (1) Ethanol is added to an emulsification tank, and then polymer materials and / or additives are added. The emulsification tank is equipped with a stirrer and a homogenizing and dispersing device. (2) Turn on the stirrer and homogenizing device respectively, control the stirring speed to 30~60 rpm and the homogenizing speed to 1000~2000 rpm, mix the materials in the emulsification tank evenly, and obtain a viscous mixture; (3) Heat the emulsification tank to 35~45℃, add the Chinese herbal extract, and mix it at a stirring speed of 30~60 rpm and a homogenization speed of 1000~2000 rpm to obtain a paste-like material. After removing the air bubbles, the paste-like film-forming dressing is obtained. The homogenizing and dispersing device is installed at the bottom of the emulsifying tank and includes a stator and a rotor, with blades provided on the edge of the rotor.

2. The preparation method according to claim 1, characterized in that, The mixing time in steps (2) and (3) is 3 to 5 hours.

3. The preparation method according to claim 1, characterized in that, It also includes the steps of lowering the temperature of the emulsification tank to below 20°C before adding ethanol, and then evacuating and filling it with inert gas to maintain pressure.

4. The preparation method according to claim 1, characterized in that, The blades are evenly distributed around the rotor, and the blades are perpendicular to the plane of rotation of the rotor.

5. The preparation method according to claim 1, characterized in that, The rotor is located above the stator, the stator and the rotor are coaxial, and the shaft passes through the bottom of the emulsifying tank and is connected to the homogenizing motor.

6. The preparation method according to claim 1, characterized in that, The emulsifying tank also includes a condensation reflux device, a temperature control system, a pressure control system, and piping; The condensation reflux device is installed at the top of the emulsification tank, the temperature control system is installed in the middle and bottom of the emulsification tank, the pressure control system is installed at the top of the emulsification tank, and the agitator is installed in the middle of the emulsification tank.

7. The preparation method according to claim 6, characterized in that, The temperature control system includes a temperature sensor and a jacket. The temperature sensor is installed at the bottom of the emulsification tank. The jacket is connected to an external cooling water source through a lower jacket opening and to an external steam source through an upper jacket opening.

8. The preparation method according to claim 6, characterized in that, The pressure control system includes a pressure gauge and a safety valve, both of which are installed on the end cap of the emulsifying tank.

9. The preparation method according to claim 6, characterized in that, The agitator includes a stirring frame, stirring blades, a stirring shaft, a scraper, and a spiral ribbon; the stirring blades are disposed on the inner side of the stirring frame, the scraper is disposed on the outer side and bottom of the stirring frame, the two ends of the spiral ribbon are respectively connected to the diagonal points of the stirring frame, and the stirring shaft passes through the end cap of the emulsification tank and is connected to the stirring motor.

10. The preparation method according to claim 1, characterized in that, The polymeric material is polyvinylpyrrolidone, poloxamer, and polyethylene glycol; the additive is an antioxidant; the herbal extract is Bletilla striata extract, Corydalis yanhusuo extract, and Panax notoginseng extract; and the mass ratio of ethanol, polyvinylpyrrolidone, poloxamer, antioxidant, polyethylene glycol, Bletilla striata extract, Corydalis yanhusuo extract, and Panax notoginseng extract is 30~40:20~25:3~6:0.1~0.5:1~3:10~15:6~10:10~15.

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