An antibacterial sustained-release gel particle and its preparation method
By preparing antibacterial sustained release gel particles and using polymers and cationic curing agents to form an internal gel crosslinking structure, the problem of frequent addition of existing antibacterial agents is solved, and long-term sustained release and safety is achieved, which is suitable for multiple fields.
Patent Information
- Application Number
- CN202211079265.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-09-05
- Publication Date
- 2025-07-29
- Estimated Expiration
- 2042-09-05
AI Technical Summary
Most of the existing antibacterial agents are used once and need to be added frequently, and there are irritating and corrosive problems.
By preparing an antibacterial sustained release gel granules, using a combination of polymer, binder, chitosan, acid and bactericide, the internal gel crosslinking structure and surface mesh structure are formed using sodium alginate solution and cationic curing agent to achieve long-term sustained release.
It achieves long-term sustained release of antibacterial effects, and lasts for 3 to 6 months without frequent additions, and is not irritating or corrosive.
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Figure CN115304794B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of sterilization technology, and particularly to an antibacterial sustained-release gel particle and a preparation method thereof. Background Art
[0002] In the past 30 years, the polymer discipline has developed rapidly, and polymer materials have been widely used in industries such as industry, agriculture, medical biology, transportation and construction, aerospace, etc. However, with the wide application of polymer materials in life, their products are prone to contact and breed many harmful microorganisms such as bacteria and germs during processing and use, causing corrosion and deterioration of various industrial materials, medical biological materials, sanitary products, and foods. Since the 21st century, public health incidents caused by pathogenic microorganisms such as COVID-19 and SARS have occurred frequently, bringing great harm and panic to mankind. Therefore, the awareness of antibacterial has taken root in people's hearts, and the application significance of antibacterial materials is also very important.
[0003] The antibacterial industry is a new and rising sun industry with great potential for future development.
[0004] The defects of existing antibacterial agents include:
[0005] 1. Existing antibacterial agents are basically used once, sprayed or diluted and sprayed for use. After use, it is necessary to repeatedly add new antibacterial agents or re-dilute for use.
[0006] 2. Existing antibacterial agents are uneven, and many antibacterial disinfectants have irritation and corrosion. Summary of the Invention
[0007] According to the first aspect, a preparation method of an antibacterial sustained-release gel particle is provided, including:
[0008] A first solution preparation step, including dissolving a polymer and an adhesive in a solvent to obtain a first solution;
[0009] A second solution preparation step, including mixing a first raw material, a second raw material, and a third raw material to obtain a second solution, which is a bactericidal solution; the first raw material includes raw materials for preparing a gel, the second raw material includes a solution containing an acid; the third raw material includes a bactericide;
[0010] An antibacterial sol preparation step, including mixing the first solution, the second solution and a first curing agent to obtain an antibacterial sol;
[0011] The forming step includes adding the antibacterial sol into the sodium alginate solution, curing and forming to obtain a cured product, and soaking the cured product in an aqueous solution containing a second curing agent to prepare antibacterial gel sustained-release particles. Under the action of cations (such as calcium ions) in the second curing agent, the epidermis of the cured product will immediately gel and solidify to form a surface network structure. As the cations in the second curing agent gradually diffuse into the interior, a semi-gel structure is formed inside the cured product.
[0012] According to a second aspect, in an embodiment, there is provided an antibacterial sustained-release gel particle, comprising the following components:
[0013] Polymer, binder, chitosan, acid, bactericide, curing agent.
[0014] An antibacterial sustained-release gel particle and a preparation method thereof according to the above embodiment. The antibacterial sustained-release gel particle is prepared by adding an antibacterial sol into an aqueous sodium alginate solution, curing and forming, and then soaking it in an aqueous solution containing a curing agent. Under the action of cations in the curing agent, the epidermis of the cured product immediately gels and solidifies to form a surface network structure. As the curing agent cations gradually diffuse into the interior, a semi-gel structure is formed inside. Finally, a gel cross-linked structure is formed inside, and a capsule structure with a hardened surface is obtained. The particle has an excellent long-acting sustained-release effect and can continuously release for 3 to 6 months. Description of the Drawings
[0015] Figure 1 Photograph of the antibacterial gel sustained-release particles prepared in Example 1. Detailed Description of the Embodiment
[0016] The present invention will be further described in detail below through specific embodiments in conjunction with the drawings. In the following embodiments, many details are described to make the present application better understood. However, those skilled in the art can easily recognize that some of the features can be omitted in different situations, or can be replaced by other materials and methods. In some cases, some operations related to the present application are not shown or described in the specification, which is to avoid the core part of the present application being submerged by excessive description. For those skilled in the art, it is not necessary to describe these related operations in detail, and they can fully understand the related operations according to the description in the specification and the general technical knowledge in the art.
[0017] In addition, the features, operations or characteristics described in the specification can be combined in any appropriate manner to form various embodiments. At the same time, the steps or actions in the method description can also be reordered or adjusted in an obvious manner by those skilled in the art. Therefore, the various sequences in the specification and drawings are only for clearly describing a certain embodiment and do not mean a necessary sequence, unless it is stated that a certain sequence must be followed.
[0018] The serial numbers assigned to the components in this text itself, such as "first", "second", etc., are only used to distinguish the described objects and do not have any sequential or technical meanings.
[0019] According to a first aspect, there is provided a method for preparing antibacterial sustained-release gel particles, including:
[0020] A first solution preparation step, including dissolving a polymer and an adhesive in a solvent to obtain a first solution;
[0021] A second solution preparation step, including mixing a first raw material, a second raw material, and a third raw material to obtain a second solution, which is a bactericidal solution; the first raw material includes raw materials for preparing the gel, the second raw material includes a solution containing an acid, and the third raw material includes a bactericide; the main function of the acid is to assist dissolution and promote the dissolution of chitosan;
[0022] An antibacterial sol preparation step, including mixing the first solution, the second solution, and a first curing agent to obtain an antibacterial sol;
[0023] A shaping step, including adding the antibacterial sol into a sodium alginate solution, curing and shaping to obtain a cured product, and soaking the cured product in an aqueous solution containing a second curing agent to obtain antibacterial gel sustained-release particles. Under the action of cations (such as calcium ions) in the second curing agent, the skin of the cured product will immediately gel and solidify to form a surface network structure. As the cations in the second curing agent gradually diffuse into the interior, a semi-gel structure is formed inside the cured product.
[0024] In one embodiment, the polymer includes polyvinyl alcohol. The main function of polyvinyl alcohol is to adjust the viscosity, which is equivalent to a thickening agent.
[0025] In one embodiment, the adhesive includes but is not limited to cellulose.
[0026] In one embodiment, the cellulose includes at least one of but is not limited to hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, and hydroxypropyl methyl cellulose.
[0027] In one embodiment, the sodium alginate solution includes an aqueous sodium alginate solution.
[0028] In one embodiment, in the first solution, the mass ratio of the polymer to the adhesive is (1 to 1.5):(0.1 to 0.5).
[0029] In one embodiment, by mass, the first solution contains the following components: 1 to 1.5 parts of polyvinyl alcohol, 0.1 to 0.5 parts of adhesive, and 100 parts of solvent.
[0030] In one embodiment, the solvent in the first solution includes but is not limited to water.
[0031] In one embodiment, the first raw material includes, but is not limited to, chitosan.
[0032] In one embodiment, the acid in the second raw material includes, but is not limited to, at least one of organic acids and inorganic acids.
[0033] In one embodiment, the acid in the second raw material includes, but is not limited to, at least one of acetic acid, citric acid, hydrochloric acid, and sulfuric acid.
[0034] In one embodiment, the bactericide includes, but is not limited to, at least one of quaternary ammonium salt antibacterial agents, organic guanidine antibacterial agents, metal ion antibacterial agents, chlorine antibacterial agents, peroxide antibacterial agents, iodine antibacterial agents, phenolic antibacterial agents, and ethylene oxide antibacterial agents.
[0035] In one embodiment, the bactericide contains single-chain quaternary ammonium salts and double-chain quaternary ammonium salts. This composite quaternary ammonium salt is more efficient and broad-spectrum.
[0036] In one embodiment, the single-chain quaternary ammonium salt includes, but is not limited to, benzalkonium chloride.
[0037] In one embodiment, the double-chain quaternary ammonium salt includes, but is not limited to, didodecyldimethylammonium chloride.
[0038] In one embodiment, the quaternary ammonium salt includes, but is not limited to, organosilicon quaternary ammonium salts.
[0039] In one embodiment, the organosilicon quaternary ammonium salt includes at least one of double-long-chain alkyl quaternary ammonium salts and single-long-chain alkyl quaternary ammonium salts.
[0040] In one embodiment, the double-long-chain alkyl quaternary ammonium salt includes, but is not limited to, at least one of methyl bis(dodecyl)[3-(dimethoxysilyl)propyl]ammonium chloride, methyl bis(octadecyl)[3-(dimethoxysilyl)propyl]ammonium chloride, methyl bis(hexadecyl)[3-(dimethoxysilyl)propyl]ammonium chloride, methyl bis(tetradecyl)[3-(dimethoxysilyl)propyl]ammonium chloride, and methyl bis(dodecyl)[3-(dimethoxysilyl)propyl]ammonium chloride.
[0041] In one embodiment, the single-long-chain alkyl quaternary ammonium salt includes, but is not limited to, at least one of methyl tetradecyl dodecyl [3-(dimethoxysilyl)propyl]ammonium chloride, methyl tetradecyl hexadecyl [3-(dimethoxysilyl)propyl]ammonium chloride, and methyl tetradecyl dodecyl [3-(diethoxysilyl)propyl]ammonium chloride.
[0042] In one embodiment, in the second solution, by mass, it contains the following raw materials: 0.2 - 10 parts of the first raw material, 1 - 5 parts of acid, 10 - 50 parts of bactericide, and 100 parts of solvent.
[0043] In one embodiment, the solvent in the second solution includes, but is not limited to, water.
[0044] In one embodiment, by mass, the first solution: the second solution = 1:(0.5 - 2).
[0045] In one embodiment, in the step of preparing the antibacterial sol, the added mass of the first curing agent is 1% - 5% of the total mass of the first solution and the second solution.
[0046] In one embodiment, in the aqueous sodium alginate solution, the mass percentage concentration of sodium alginate is 0.1% - 10%, including but not limited to 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%.
[0047] In one embodiment, both the first curing agent and the second curing agent include calcium chloride.
[0048] In one embodiment, by mass, the aqueous solution containing the second curing agent contains the following components: 0.5 - 2.5 parts of the second curing agent and 100 parts of water.
[0049] In one embodiment, in the forming step, the time for the cured product to be immersed in the aqueous solution containing the second curing agent is 1 - 3 min.
[0050] In one embodiment, in the forming step, after the cured product is immersed in the aqueous solution containing the second curing agent, it further includes drying the obtained antibacterial gel sustained-release particles.
[0051] In one embodiment, in the forming step, the drying temperature is 30 - 50 °C.
[0052] In one embodiment, in the forming step, the drying time is 10 - 30 min.
[0053] According to the second aspect, in one embodiment, there is provided an antibacterial sustained-release gel particle, comprising the following components:
[0054] Polymer, binder, chitosan, acid, bactericide, curing agent.
[0055] In one embodiment, by mass, it contains the following components:
[0056] 1 - 1.5 parts of polymer, 0.1 - 0.5 parts of binder, 0.2 - 10 parts of chitosan, 1 - 5 parts of acid, 10 - 50 parts of bactericide, 0.5 - 2.5 parts of curing agent.
[0057] In one embodiment, the polymer includes polyvinyl alcohol.
[0058] In one embodiment, the binder includes but is not limited to cellulose.
[0059] In one embodiment, the cellulose includes but is not limited to at least one of hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, and hydroxypropyl methyl cellulose.
[0060] In one embodiment, the acid includes but is not limited to at least one of acetic acid, citric acid, hydrochloric acid, and sulfuric acid.
[0061] In one embodiment, the bactericide includes but is not limited to at least one of quaternary ammonium antibacterial agents, organic guanidine antibacterial agents, metal ion antibacterial agents, chlorine antibacterial agents, peroxide antibacterial agents, iodine antibacterial agents, phenol antibacterial agents, and ethylene oxide antibacterial agents.
[0062] In one embodiment, the bactericide contains a single-chain quaternary ammonium salt and a double-chain quaternary ammonium salt.
[0063] In one embodiment, the quaternary ammonium salt includes but is not limited to organosilicon quaternary ammonium salt.
[0064] In one embodiment, the organosilicon quaternary ammonium salt includes at least one of a di-long-chain alkyl quaternary ammonium salt and a mono-long-chain alkyl quaternary ammonium salt.
[0065] In one embodiment, the di-long-chain alkyl quaternary ammonium salt includes at least one of methyl dibehenyl[3-(dimethoxysilyl)propyl]ammonium chloride, methyl dioctadecyl[3-(dimethoxysilyl)propyl]ammonium chloride, methyl dihexadecyl[3-(dimethoxysilyl)propyl]ammonium chloride, methyl ditetradecyl[3-(dimethoxysilyl)propyl]ammonium chloride, and methyl didodecyl[3-(dimethoxysilyl)propyl]ammonium chloride.
[0066] In one embodiment, the mono-long chain alkyl quaternary ammonium salt includes at least one of methyl dodecyl[3-(dimethoxysilyl)propyl]ammonium chloride, methyl tetradecyl[3-(dimethoxysilyl)propyl]ammonium chloride, and methyl dodecyl[3-(diethoxysilyl)propyl]ammonium chloride.
[0067] In one embodiment, the antibacterial sustained-release gel particles further comprise at least one of sodium alginate and a solvent.
[0068] In one embodiment, the solvent includes but is not limited to water.
[0069] In one embodiment, the curing agent includes calcium chloride.
[0070] In one embodiment, the antibacterial sustained-release gel particles are prepared by any method of the first aspect.
[0071] In one embodiment, the antibacterial gel particles provided by the present invention can achieve long-term sustained release, and only need to be added once, and can be used for several months without reducing the antibacterial effect.
[0072] In one embodiment, the antimicrobial agent provided in the present invention is harmless to humans and pets, non-irritating, and non-corrosive.
[0073] In one embodiment, the method for preparing antibacterial gel particles includes:
[0074] 1) adding a) polyvinyl alcohol and b) hydroxymethyl cellulose or hydroxyethyl cellulose to water, stirring, and heating to 50-80° C. to dissolve them in water, stirring for about 20-40 minutes to completely dissolve the materials, to obtain solution 1;
[0075] 2) Chitosan is added to an aqueous solution containing an acid (such as acetic acid, citric acid, hydrochloric acid, or sulfuric acid), stirred, and heated to 30-50°C to completely dissolve and mix evenly. A certain amount of a quaternary ammonium salt (including single-chain and double-chain) bactericide is then added and mixed evenly to obtain a chitosan quaternary ammonium salt composite bactericidal solution, i.e., Solution 2, which has a broader-spectrum bactericidal effect. Bactericides are also called antimicrobial agents.
[0076] 3) The solution 1 obtained in step 1) and the solution 2 obtained in step 2) are mixed and stirred uniformly, and 1% to 5% by mass of calcium chloride is added to obtain a sol having an antibacterial function, i.e., an antibacterial sol. The calcium chloride has the effect of promoting curing.
[0077] 4) preparing an aqueous solution of calcium chloride (curing agent), wherein the mass percentage concentration of calcium chloride in the aqueous solution is 1% to 5%.
[0078] 5) The antibacterial sol prepared in step 3) is gradually added dropwise to a sodium alginate aqueous solution (sodium alginate plays a role in solidification and shaping, and the sodium alginate aqueous solution is in excess relative to the antibacterial sol), stirred for 5 to 10 minutes, solidified and formed, and the particles are removed and then soaked (the soaking time can be 1 to 3 minutes. If the soaking time is too long, the degree of solidification will increase, which will affect the water absorption and swelling properties, hinder the penetration of water, and thus affect the dissolution of the antibacterial agent) in the calcium chloride aqueous solution prepared in step 4). Under the action of calcium ions, the surface will immediately gel and solidify to form a surface network structure. As the calcium ions gradually diffuse into the interior, a semi-gel structure is formed inside the particles. Subsequently, an appropriate heating and curing treatment (the temperature can be 30 to 50° C. and the time can be 10 to 30 minutes) is performed to evaporate some of the water, gradually forming a capsule structure with an internal gel cross-linked structure and a surface hardened capsule structure, namely the antibacterial sustained-release gel particles. The amount of antibacterial sol added is not limited, and the required amount is added as needed. The formation continues during the dropwise addition process.
[0079] The capsule structure formed in step 5) is immersed in water, the capsule skin gradually swells, water enters the interior, penetrates into the gel network structure, and gradually dissolves the quaternary ammonium salt and chitosan, achieving a long-term sustained release effect (can be used continuously for 3 to 6 months).
[0080] In one embodiment, the raw materials used to prepare the antibacterial gel particles include, by mass:
[0081] 1) 1-1.5 parts of polyvinyl alcohol, 0.1-0.5 parts of hydroxymethyl cellulose and / or hydroxyethyl cellulose, and 100 parts of water;
[0082] 2) 0.2-10 parts chitosan, 1-5 parts acid, 10-50 parts quaternary ammonium salt, 100 parts water;
[0083] 3) 0.5-2.5 parts calcium chloride to 100 parts water;
[0084] 4) An aqueous solution of sodium alginate with a mass concentration of 0.1% to 10%.
[0085] Example 1
[0086] In this embodiment, the preparation method of antibacterial gel sustained-release granules is as follows:
[0087] 1) Add polyvinyl alcohol, hydroxymethyl cellulose, and hydroxyethyl cellulose according to the formula amount into water, stir, and heat to 60° C. to dissolve them in water. Stir for about 30 minutes to completely dissolve the materials to obtain solution 1;
[0088] 2) adding chitosan to an aqueous solution containing citric acid (the acid may be acetic acid, citric acid, hydrochloric acid, sulfuric acid, etc.), stirring, and heating to 40° C. to completely dissolve it and mix it evenly, then adding a quaternary ammonium salt (including a single-chain quaternary ammonium salt and a double-chain quaternary ammonium salt, the single-chain quaternary ammonium salt is benzalkonium chloride, and the double-chain quaternary ammonium salt is didecyldimethylammonium chloride) bactericide according to the formula amount, and mixing evenly to obtain a chitosan quaternary ammonium salt composite bactericidal solution, namely solution 2, which is a bactericidal solution with a broader spectrum of bactericidal effects.
[0089] 3) Solution 1 obtained in step 1) and solution 2 obtained in step 2) are mixed in a mass ratio of 1:1, stirred evenly, and a 3% by mass calcium chloride aqueous solution is added to obtain a sol having antibacterial function, i.e., an antibacterial sol.
[0090] 4) Prepare an aqueous solution of calcium chloride (curing agent).
[0091] 5) gradually dripping the antibacterial sol prepared in step 3) into the sodium alginate aqueous solution, stirring for 5 to 10 minutes to solidify and form, and then soaking (the soaking time can be 1 to 3 minutes. If the soaking time is too long, the degree of solidification will be higher, which will affect the water absorption and swelling properties, which is not conducive to water penetration and thus affect the dissolution of the antibacterial agent) in the calcium chloride aqueous solution prepared in step 4). Under the action of calcium ions, the surface will immediately gel and solidify to form a surface network structure. As the calcium ions gradually diffuse into the interior, a semi-gel structure is formed inside. Subsequently, an appropriate heating and curing treatment (temperature of 40° C., time for 20 minutes) is performed to evaporate part of the water, gradually forming a capsule structure with an internal gel cross-linked structure and a hardened surface, i.e., the antibacterial sustained-release gel particles.
[0092] The capsule structure formed in step 5) is immersed in water, the capsule skin gradually swells, water enters the interior, penetrates into the gel network structure, and gradually dissolves the quaternary ammonium salt and chitosan, achieving a long-term sustained release effect (can be used continuously for 3 to 6 months).
[0093] In this embodiment, the raw materials used to prepare the antibacterial gel particles include, by mass:
[0094] 1) 1 part of polyvinyl alcohol, 0.3 parts of hydroxymethyl cellulose and hydroxyethyl cellulose, and 100 parts of water; hydroxymethyl cellulose and hydroxyethyl cellulose were purchased separately and mixed in a mass ratio of 1:1 to prepare solution 1.
[0095] 2) 7 parts chitosan, 3 parts citric acid, 25 parts quaternary ammonium salt, 100 parts water;
[0096] 3) 1.5 parts calcium chloride, 100 parts water;
[0097] 4) The mass concentration of the sodium alginate aqueous solution is 2%.
[0098] Figure 1 This is a photo of the antibacterial gel sustained-release particles prepared in this example.
[0099] ① Sterilization effect test
[0100] The experimental method is as follows:
[0101] Take one antibacterial gel particle with a diameter of about 5 mm and place it in 100 mL of deionized water. After placing it for different times, take samples and test their concentration using quaternary ammonium salt test paper.
[0102] The sterilization experiment is carried out in accordance with the national standard "GB / T 38502-2020 Laboratory Sterilization Effect Test Method of Disinfectants".
[0103] Neutralizer identification test:
[0104] Bactericidal rate detection method: Refer to the suspension quantitative identification test in the "Disinfection Technical Specification" (2002 edition) of the Chinese Ministry of Health, 2.1.1.5.5.
[0105] Test strain: Escherichia coli 8099.
[0106] Detection method: Refer to the suspension quantitative bactericidal test in the "Disinfection Technical Specification" (2002 edition) of the Chinese Ministry of Health, 2.1.1.7.4.
[0107] The test results are shown in Table 1 and Table 2.
[0108] Table 1
[0109] Sustained release time 1d 2d 3d 4d 5d 6d Sterilization rate 90% 95% 97% 98% 99.9% 99.999%
[0110] Table 2
[0111]
[0112] In Table 1 and Table 2, "d" represents the number of days.
[0113] It can be seen that after 1 day, the bactericidal rate of the antibacterial gel sustained-release particles is as high as 90%, and after 56 days, the bactericidal rate still remains at 99.999%, showing excellent long-term bactericidal effect.
[0114] ② Bactericidal rate test after water change
[0115] The experimental method is as follows: Take 1 antibacterial gel particle with a diameter of about 5 mm and place it in 100 mL of deionized water. After 7 days, empty the solution, add 100 mL of deionized water again, and after placing for different times, take samples to test their bactericidal performance. The test results are shown in Table 3.
[0116] Table 3
[0117] Sustained release time 1d 2d 3d 4d 5d 6d 7d 14d 21d 28d Sterilization rate 91% 95% 96% 98% 99.999% 99.999% 99.999% 99.999% 99.999% 99.999%
[0118] In Table 3, "d" represents the number of days.
[0119] It can be seen that on the first day after liquid change, the bactericidal rate of the antibacterial gel sustained-release particles is as high as 91%, and on the 28th day, it is still as high as 99.999%, confirming its excellent long-term bactericidal effect.
[0120] Comparative Example 1
[0121] In this comparative example, 1.5 parts of calcium chloride in raw material 3) in Example 1 was changed to 0.1 part of calcium chloride, and the rest was the same as in Example 1. The experimental results showed that it could not be finally solidified into gel particles.
[0122] In one embodiment, the preparation process of the antibacterial sustained-release gel particles of the present invention is simple and the cost is low.
[0123] In one embodiment, the sustained-release effect of the capsule structure prepared by the present invention is excellent and the sustained-release period is long.
[0124] In one embodiment, the present invention provides a novel antibacterial sustained-release gel particle, which has broad-spectrum bactericidal activity, long-lasting effect, safe and non-toxic components, low preparation cost and simple process, and can be widely applied in various fields such as medicine, industry and agriculture. Especially for the scenarios where the solution needs to be replaced regularly or irregularly, the sustained release can continue after the solution is replaced, maintaining the antibacterial effect of the solution.
[0125] The above uses specific examples to elaborate on the present invention, which is only used to help understand the present invention and is not intended to limit the present invention. For those skilled in the technical field to which the present invention pertains, based on the idea of the present invention, several simple deductions, deformations or substitutions can also be made.
Claims
1. A preparation method of an antibacterial sustained-release gel particle, characterized in that, Comprising: A first solution preparation step, including dissolving a polymer and an adhesive in a solvent to obtain a first solution; A second solution preparation step, including mixing a first raw material, a second raw material, and a third raw material to obtain a second solution; the first raw material includes a raw material for preparing a gel, the second raw material includes an acid, and the third raw material includes a bactericide; An antibacterial sol preparation step, including mixing the first solution, the second solution, and a first curing agent to obtain an antibacterial sol; A molding step, including gradually dropping the antibacterial sol into a sodium alginate solution, curing and molding to obtain a cured product, and soaking the cured product in an aqueous solution containing a second curing agent to obtain antibacterial gel sustained-release particles; Wherein, the polymer includes polyvinyl alcohol; the adhesive includes cellulose; the cellulose includes at least one of hydroxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl cellulose, and hydroxypropyl methyl cellulose; the first raw material includes chitosan; the bactericide includes a quaternary ammonium salt antibacterial agent; both the first curing agent and the second curing agent include calcium chloride; in the aqueous solution containing the second curing agent, the mass percentage concentration of calcium chloride is 1% - 5%; in the molding step, the time for the cured product to be soaked in the aqueous solution containing the second curing agent is 1 - 3 min.
2. The preparation method according to claim 1, characterized in that, The sodium alginate solution includes an aqueous sodium alginate solution.
3. The preparation method according to claim 1, characterized in that, In the first solution, the mass ratio of the polymer to the adhesive is (1 - 1.5):(0.1 - 0.5).
4. The preparation method according to claim 1, characterized in that, By mass, the first solution contains the following components: 1 - 1.5 parts of polyvinyl alcohol, 0.1 - 0.5 parts of adhesive, and 100 parts of solvent; The solvent in the first solution includes water.
5. The preparation method according to claim 1, characterized in that, The acid in the second raw material includes at least one of organic acid and inorganic acid; The quaternary ammonium salt antibacterial agent includes an organosilicon quaternary ammonium salt; The organosilicon quaternary ammonium salt includes at least one of a double long-chain alkyl quaternary ammonium salt and a single long-chain alkyl quaternary ammonium salt; The double long-chain alkyl quaternary ammonium salt includes at least one of methyl bis(dodecyl)[3-(dimethoxysilyl)propyl]ammonium chloride, methyl bis(octadecyl)[3-(dimethoxysilyl)propyl]ammonium chloride, methyl bis(hexadecyl)[3-(dimethoxysilyl)propyl]ammonium chloride, methyl bis(tetradecyl)[3-(dimethoxysilyl)propyl]ammonium chloride, and methyl bis(dodecyl)[3-(dimethoxysilyl)propyl]ammonium chloride; The single long-chain alkyl quaternary ammonium salt includes at least one of methyl tetradecyl dodecyl [3-(dimethoxysilyl)propyl]ammonium chloride, methyl hexadecyl tetradecyl [3-(dimethoxysilyl)propyl]ammonium chloride, and methyl tetradecyl dodecyl [3-(diethoxysilyl)propyl]ammonium chloride.
6. The preparation method according to claim 1, characterized in that, The bactericide contains a single-chain quaternary ammonium salt and a double-chain quaternary ammonium salt; The acid in the second raw material includes at least one of acetic acid, citric acid, hydrochloric acid, and sulfuric acid.
7. The preparation method according to claim 1, characterized in that, In the second solution, by mass, it contains the following raw materials: 0.2 - 10 parts of the first raw material, 1 - 5 parts of acid, 10 - 50 parts of bactericide, and 100 parts of solvent; The solvent in the second solution includes water; In the preparation steps of the antibacterial sol, the added mass of the first curing agent is 1% - 5% of the total mass of the first solution and the second solution; In the sodium alginate solution, the mass percentage concentration of sodium alginate is 0.1% - 10%.
8. The preparation method according to claim 1, wherein In the shaping step, after soaking the solidified product in an aqueous solution containing a second curing agent, it further includes drying the obtained antibacterial gel sustained-release particles; the drying temperature is 30 - 50 °C; the drying time is 10 - 30 min.
9. An antibacterial sustained-release gel particle, characterized in that, The antibacterial sustained-release gel particles are prepared by the preparation method according to any one of claims 1 - 8.
Citation Information
Patent Citations
Polymer gel particles, preparation method thereof, composite gel particles containing polymer gel particles and application of composite gel particles
CN107855080A