Didecyl methyl ammonium bromide iodine composite solution and application thereof
In the disinfectant technology in the field of aquaculture, a stable and efficient decimal bromide iodine composite solution is prepared by using specific mixing and dilution methods of components such as ethanol, decimal bromide, surfactant, iodine element and metal iodide in the field of disinfectant technology, which solves the problem of insufficient stability of complex products in the prior art and achieves excellent disinfection and bactericidal effects.
Patent Information
- Application Number
- CN202510007960.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-03
- Publication Date
- 2025-04-11
AI Technical Summary
In the prior art, the complexing products of iodine and decylmethylammonium bromide are poorly stable, and some of the iodine is converted into invalid iodine, resulting in limited sterilization and disinfection effects, increasing costs and being unfavorable to the aquaculture ecological environment.
Component B was obtained by mixing ethanol, decylammonium bromide and surfactant, and then adding iodine element and metal iodide. Subsequently, a β-cyclodextrin aqueous solution and a polyvinyl alcohol aqueous solution were added to mix, the complexing product was stabilized, and finally diluted with deionized water, and a decylmethyl ammonium bromide iodine composite solution was obtained by physical blending.
It significantly improves the stability of complex products, enhances disinfection and sterilization capabilities, is suitable for aquaculture fields, and reduces the negative impact on the ecological environment of aquaculture.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of disinfectants, and in particular relates to a decanylmethylammonium bromide iodine composite solution and application thereof. Background Art
[0002] Decylmethylammonium bromide is a quaternary ammonium salt cationic surfactant, which is a light yellow transparent liquid with bactericidal and disinfecting effects, while iodine is a dark purple solid, which is in the form of flaky crystals at room temperature and pressure. Due to its strong oxidizing property, iodine is widely used in the field of bactericides and disinfectants. At present, many existing technologies will choose to complex iodine with decanylmethylammonium bromide to prepare a complex product. Through the synergistic compounding of iodine and decanylmethylammonium bromide in the complex product, only a small amount of complex product needs to be added to obtain very excellent bactericidal and disinfecting effects, which is particularly suitable for the field of aquaculture. However, these complex products still have certain disadvantages that limit their actual application results. This is because the stability of these complex products is not good, and part of the iodine is easily converted into invalid iodine, that is, iodine that cannot directly participate in the bactericidal and disinfecting process, which in turn leads to some restrictions on the application effect. Ultimately, it is undoubtedly necessary to increase the amount of input, which not only increases the cost, but also is not conducive to the overall ecological environment of aquaculture. Summary of the invention
[0003] In view of the problems existing in the prior art, the purpose of the present invention is to provide a decanylmethylammonium bromide iodine composite solution and application thereof. The present invention creatively mixes ethanol, decanylmethylammonium bromide and a surfactant to obtain component A, then adds iodine element and metal iodide based on a conventional high-temperature complexing method to obtain component B containing a complex product, then sequentially adds a certain weight and concentration of β-cyclodextrin aqueous solution and a polyvinyl alcohol aqueous solution to mix, so as to stabilize the complex product, and finally uses deionized water as a conventional dilution solvent to obtain a decanylmethylammonium bromide iodine composite solution after physical blending. The decanylmethylammonium bromide iodine composite solution is very suitable for application in the field of aquaculture, not only has excellent disinfection and sterilization capabilities, but also effectively improves the stability of the complex product.
[0004] The purpose of the present invention can be achieved through the following technical solutions:
[0005] A method for preparing a decylmethylammonium bromide iodine composite solution, the preparation method comprising the following steps:
[0006] (1) adding 35-40 parts by weight of decylmethylammonium bromide and 18-20 parts by weight of a surfactant to 40 parts by weight of ethanol, and then stirring and mixing at 60-70° C. for 20-30 minutes under condensation reflux to obtain component A;
[0007] (2) adding 3-5 parts by weight of elemental iodine and 0.1-0.25 parts by weight of metal iodide to the component A, stirring and mixing at 60-70° C. for 2-4 hours under condensation reflux, and naturally cooling to room temperature to obtain component B;
[0008] (3) mixing β-cyclodextrin and deionized water to obtain component C;
[0009] (4) mixing polyvinyl alcohol and deionized water to obtain component D;
[0010] (5) Add 200-220 parts by weight of component C to 100 parts by weight of component B, and then stir and mix at 40-45° C. for 1-2 hours, then add 20-30 parts by weight of component D, continue to stir and mix for 45-60 minutes, and finally add deionized water, stir and mix for 15-30 minutes, and the preparation is completed.
[0011] As a preferred technical solution of the present invention, the surfactant in step (1) is at least one of fatty alcohol polyoxyethylene ether and polyethylene glycol.
[0012] As a preferred technical solution of the present invention, the metal iodide in step (2) is potassium iodide.
[0013] As a preferred technical solution of the present invention, the mass ratio of the β-cyclodextrin to the deionized water in step (3) is 4:95-100.
[0014] As a preferred technical solution of the present invention, the mixing in step (3) refers to stirring and mixing at 50-60°C for 1-2h.
[0015] As a preferred technical solution of the present invention, the mass ratio of the polyvinyl alcohol to the deionized water in step (4) is 10:90-100.
[0016] As a preferred technical solution of the present invention, the mixing in step (4) refers to stirring and mixing at 60-70°C for 30-60 minutes.
[0017] As a preferred technical solution of the present invention, the amount of deionized water used in step (5) is 950-1000 parts by weight.
[0018] A decylmethylammonium bromide-iodine composite solution prepared by the preparation method as described above.
[0019] The invention discloses an application of a decanylmethylammonium bromide-iodine composite solution, wherein the decanylmethylammonium bromide-iodine composite solution is applied to disinfection of aquaculture.
[0020] Beneficial effects of the present invention:
[0021] (1) The present invention creatively mixes ethanol, decylmethylammonium bromide and a surfactant to obtain component A, then adds iodine and metal iodide based on a conventional high-temperature complexing method to obtain component B containing a complex product, then adds a certain weight and concentration of β-cyclodextrin aqueous solution and a polyvinyl alcohol aqueous solution in sequence to mix them to stabilize the complex product, and finally uses deionized water as a conventional dilution solvent to obtain a decylmethylammonium bromide iodine composite solution after physical blending. The composite solution is very suitable for application in the field of aquaculture, not only has excellent disinfection and sterilization capabilities, but also effectively improves the stability of the complex product.
[0022] (2) The present invention creatively prepares component B containing the complex product according to a conventional method, then sequentially adds a certain weight and concentration of β-cyclodextrin aqueous solution and a polyvinyl alcohol aqueous solution to mix them, thereby stabilizing the complex product, and finally uses deionized water as a conventional dilution solvent to obtain a decylmethylammonium bromide iodine complex solution after physical blending. On the one hand, β-cyclodextrin has a structure of being hydrophilic on the outside and hydrophobic on the inside. Its introduction can rely on hydrophobic interaction, van der Waals force, etc. to a certain extent to combine with the complex product (from a structural point of view, the complex product is similar to β-cyclodextrin and also has amphiphilic properties), so that the complex product "enters" its cavity, thereby exerting a stabilizing effect. On the other hand, On the one hand, polyvinyl alcohol, as a polyhydroxy compound, has a strong polarity. Its introduction can produce hydrogen bonds with the external hydrophilic structure of β-cyclodextrin to form a hydrogen bond network, achieving the effect of a "barrier layer", effectively reducing collisions and aggregations between molecules, inhibiting the dissociation of iodine, and further improving the stability of the complex product. In addition, the addition method of β-cyclodextrin and polyvinyl alcohol needs to be strictly controlled. If polyvinyl alcohol is added first and then β-cyclodextrin is added, or β-cyclodextrin and polyvinyl alcohol are added together, good technical effects cannot be obtained. The possible reason is that the prior presence of polyvinyl alcohol will change the interaction between the complex product and β-cyclodextrin, and the complex product is difficult to "enter" the cavity of β-cyclodextrin. DETAILED DESCRIPTION
[0023] In order to further illustrate the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the specific implementation methods, structures, features and effects of the present invention are described in detail below in combination with the embodiments.
[0024] The sources of the raw materials are as follows: fatty alcohol polyoxyethylene ether was purchased from Jinan Bio Chemical Co., Ltd. with the item number AEO-3; β-cyclodextrin was purchased from Shandong Jiake Biotechnology Co., Ltd.; polyvinyl alcohol was purchased from Shandong Quantai Chemical Technology Co., Ltd. with the item number 7578.
[0025] Example 1
[0026] A method for preparing a decylmethylammonium bromide iodine composite solution, the preparation method comprising the following steps:
[0027] (1) adding 35 parts by weight of decylmethylammonium bromide and 18 parts by weight of a surfactant to 40 parts by weight of ethanol, and then stirring and mixing at 60° C. under condensation reflux for 20 minutes to obtain component A;
[0028] (2) adding 3 parts by weight of elemental iodine and 0.1 parts by weight of metal iodide to the component A, stirring and mixing at 60° C. for 2 h under condensation reflux, and naturally cooling to room temperature to obtain component B;
[0029] (3) mixing β-cyclodextrin and deionized water to obtain component C;
[0030] (4) mixing polyvinyl alcohol and deionized water to obtain component D;
[0031] (5) Add 200 parts by weight of component C to 100 parts by weight of component B, and then stir and mix at 40° C. for 1 hour. Then add 20 parts by weight of component D, continue to stir and mix for 45 minutes, and finally add deionized water and stir and mix for 15 minutes. The preparation is completed.
[0032] The surfactant in step (1) is fatty alcohol polyoxyethylene ether.
[0033] The metal iodide in step (2) is potassium iodide.
[0034] The mass ratio of the β-cyclodextrin to the deionized water in step (3) is 4:95.
[0035] The mixing in step (3) refers to stirring and mixing at 50° C. for 1 hour.
[0036] The mass ratio of the polyvinyl alcohol to the deionized water in step (4) is 10:90.
[0037] The mixing in step (4) refers to stirring and mixing at 60° C. for 30 minutes.
[0038] The amount of deionized water used in step (5) is 950 parts by weight.
[0039] A decylmethylammonium bromide-iodine composite solution prepared by the preparation method as described above.
[0040] The invention discloses an application of a decanylmethylammonium bromide-iodine composite solution, wherein the decanylmethylammonium bromide-iodine composite solution is applied to disinfection of aquaculture.
[0041] Example 2
[0042] A method for preparing a decylmethylammonium bromide iodine composite solution, the preparation method comprising the following steps:
[0043] (1) adding 40 parts by weight of decylmethylammonium bromide and 20 parts by weight of a surfactant to 40 parts by weight of ethanol, and then stirring and mixing at 70° C. under condensation reflux for 30 minutes to obtain component A;
[0044] (2) adding 5 parts by weight of elemental iodine and 0.25 parts by weight of metal iodide to the component A, stirring and mixing at 70° C. for 4 h under condensation reflux, and naturally cooling to room temperature to obtain component B;
[0045] (3) mixing β-cyclodextrin and deionized water to obtain component C;
[0046] (4) mixing polyvinyl alcohol and deionized water to obtain component D;
[0047] (5) Add 220 parts by weight of component C to 100 parts by weight of component B, and then stir and mix at 45° C. for 2 h. Then add 30 parts by weight of component D, continue to stir and mix for 60 min, and finally add deionized water and stir and mix for 30 min. The preparation is completed.
[0048] The surfactant in step (1) is fatty alcohol polyoxyethylene ether.
[0049] The metal iodide in step (2) is potassium iodide.
[0050] The mass ratio of the β-cyclodextrin to the deionized water in step (3) is 4:100.
[0051] The mixing in step (3) refers to stirring and mixing at 60° C. for 2 h.
[0052] The mass ratio of the polyvinyl alcohol to the deionized water in step (4) is 10:100.
[0053] The mixing in step (4) refers to stirring and mixing at 70° C. for 60 minutes.
[0054] The amount of deionized water used in step (5) is 1000 parts by weight.
[0055] A decylmethylammonium bromide-iodine composite solution prepared by the preparation method as described above.
[0056] The invention discloses an application of a decanylmethylammonium bromide-iodine composite solution, wherein the decanylmethylammonium bromide-iodine composite solution is applied to disinfection of aquaculture.
[0057] Example 3
[0058] A method for preparing a decylmethylammonium bromide iodine composite solution, the preparation method comprising the following steps:
[0059] (1) adding 38 parts by weight of decylmethylammonium bromide and 19 parts by weight of a surfactant to 40 parts by weight of ethanol, and then stirring and mixing at 65° C. under condensation reflux for 25 minutes to obtain component A;
[0060] (2) adding 4 parts by weight of elemental iodine and 0.15 parts by weight of metal iodide to the component A, stirring and mixing at 65° C. for 3 h under condensation reflux, and naturally cooling to room temperature to obtain component B;
[0061] (3) mixing β-cyclodextrin and deionized water to obtain component C;
[0062] (4) mixing polyvinyl alcohol and deionized water to obtain component D;
[0063] (5) Add 210 parts by weight of component C to 100 parts by weight of component B, and then stir and mix at 43° C. for 1.5 hours. Then add 25 parts by weight of component D, continue to stir and mix for 50 minutes, and finally add deionized water and stir and mix for 20 minutes. The preparation is completed.
[0064] The surfactant in step (1) is fatty alcohol polyoxyethylene ether.
[0065] The metal iodide in step (2) is potassium iodide.
[0066] The mass ratio of the β-cyclodextrin to the deionized water in step (3) is 4:98.
[0067] The mixing in step (3) refers to stirring and mixing at 55° C. for 1.5 hours.
[0068] The mass ratio of the polyvinyl alcohol to the deionized water in step (4) is 10:95.
[0069] The mixing in step (4) refers to stirring and mixing at 65° C. for 45 minutes.
[0070] The amount of deionized water used in step (5) is 980 parts by weight.
[0071] A decylmethylammonium bromide-iodine composite solution prepared by the preparation method as described above.
[0072] The invention discloses an application of a decanylmethylammonium bromide-iodine composite solution, wherein the decanylmethylammonium bromide-iodine composite solution is applied to disinfection of aquaculture.
[0073] Example 4
[0074] A method for preparing a decylmethylammonium bromide iodine composite solution, the preparation method comprising the following steps:
[0075] (1) adding 40 parts by weight of decylmethylammonium bromide and 19 parts by weight of a surfactant to 40 parts by weight of ethanol, and then stirring and mixing at 67° C. under condensation reflux for 25 minutes to obtain component A;
[0076] (2) adding 5 parts by weight of elemental iodine and 0.2 parts by weight of metal iodide to the component A, stirring and mixing at 65° C. for 2 h under condensation reflux, and naturally cooling to room temperature to obtain component B;
[0077] (3) mixing β-cyclodextrin and deionized water to obtain component C;
[0078] (4) mixing polyvinyl alcohol and deionized water to obtain component D;
[0079] (5) Add 220 parts by weight of component C to 100 parts by weight of component B, and then stir and mix at 40° C. for 2 h. Then add 25 parts by weight of component D, continue to stir and mix for 60 min, and finally add deionized water and stir and mix for 25 min. The preparation is completed.
[0080] The surfactant in step (1) is fatty alcohol polyoxyethylene ether.
[0081] The metal iodide in step (2) is potassium iodide.
[0082] The mass ratio of the β-cyclodextrin to the deionized water in step (3) is 4:99.
[0083] The mixing in step (3) refers to stirring and mixing at 55° C. for 1.5 hours.
[0084] The mass ratio of the polyvinyl alcohol to the deionized water in step (4) is 10:98.
[0085] The mixing in step (4) refers to stirring and mixing at 70° C. for 30 minutes.
[0086] The amount of deionized water used in step (5) is 1000 parts by weight.
[0087] A decylmethylammonium bromide-iodine composite solution prepared by the preparation method as described above.
[0088] The invention discloses an application of a decanylmethylammonium bromide-iodine composite solution, wherein the decanylmethylammonium bromide-iodine composite solution is applied to disinfection of aquaculture.
[0089] Comparative Example 1
[0090] On the basis of Example 3, β-cyclodextrin was replaced by an equal weight of deionized water, and the rest remained unchanged.
[0091] Comparative Example 2
[0092] On the basis of Example 3, polyvinyl alcohol was replaced with an equal weight of deionized water, and the rest remained unchanged.
[0093] Comparative Example 3
[0094] On the basis of Example 3, β-cyclodextrin and polyvinyl alcohol were replaced by deionized water of equal weight, and the rest remained unchanged.
[0095] Comparative Example 4
[0096] On the basis of Example 3, step (5) is changed to adding 25 parts by weight of component D to 100 parts by weight of component B, followed by stirring at 43°C for 50 minutes, then adding 210 parts by weight of component C, continuing to stir for 1.5 hours, and finally adding deionized water, stirring for 20 minutes, and the preparation is completed; the rest remains unchanged.
[0097] Comparative Example 5
[0098] On the basis of Example 3, step (5) is changed to adding 210 parts by weight of component C and 25 parts by weight of component D to 100 parts by weight of component B, followed by stirring at 43° C. for 140 minutes, and finally adding deionized water and stirring for 20 minutes to complete the preparation; the rest remains unchanged.
[0099] Test Example 1
[0100] Sterilization test:
[0101] The decanylmethylammonium bromide iodine composite solutions prepared in Examples 1-4 and Comparative Examples 1-5 were respectively subjected to bactericidal tests with reference to the Technical Specification for Disinfection (2002 Edition), specifically the minimum inhibitory concentration determination test (nutrient broth dilution method) in Section 2.1.8.4, wherein the test strain selected Staphylococcus aureus ATCC6538, and the prepared decanylmethylammonium bromide iodine composite solution was directly used as the test solution, and the added amount was controlled to be 2.5 mL.
[0102] Table 1. Bactericidal test results
[0103]
[0104]
[0105] Test Example 2
[0106] Stability test:
[0107] The decylmethylammonium bromide iodine composite solutions prepared in Examples 1-4 and Comparative Examples 1-5 were respectively stored according to the storage method of reference standard GB / T38499-2020 (54°C ± 2°C, 14 days), and then the sterilization test of Test Example 1 was performed again.
[0108] Table 2. Stability test results
[0109] Turbid or transparent Example 1 transparent Example 2 transparent Example 3 transparent Example 4 transparent Comparative Example 1 turbid Comparative Example 2 turbid Comparative Example 3 turbid Comparative Example 4 turbid Comparative Example 5 turbid
[0110] From the comparison of Test Examples 1-2, Example 3 and Comparative Examples 1-5, it can be seen that the decylmethylammonium bromide iodine composite solution prepared by the present invention not only has excellent disinfection and bactericidal capabilities, but also effectively improves the stability of the complex product, and is very suitable for application in the field of aquaculture.
[0111] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment as above, it is not used to limit the present invention. Any technical personnel in this field can make some changes or modify the technical contents disclosed above into equivalent embodiments without departing from the scope of the technical solution of the present invention. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.
Claims
1. A method for preparing a decylmethylammonium bromide iodine composite solution, characterized in that: The preparation method comprises the following steps: (1) adding 35-40 parts by weight of decylmethylammonium bromide and 18-20 parts by weight of a surfactant to 40 parts by weight of ethanol, and then stirring and mixing at 60-70° C. for 20-30 minutes under condensation reflux to obtain component A; (2) adding 3-5 parts by weight of elemental iodine and 0.1-0.25 parts by weight of metal iodide to the component A, stirring and mixing at 60-70° C. for 2-4 hours under condensation reflux, and naturally cooling to room temperature to obtain component B; (3) mixing β-cyclodextrin and deionized water to obtain component C; (4) mixing polyvinyl alcohol and deionized water to obtain component D; (5) Add 200-220 parts by weight of component C to 100 parts by weight of component B, and then stir and mix at 40-45° C. for 1-2 hours, then add 20-30 parts by weight of component D, continue to stir and mix for 45-60 minutes, and finally add deionized water, stir and mix for 15-30 minutes, and the preparation is completed.
2. The method for preparing a decylmethylammonium bromide iodine composite solution according to claim 1, wherein: The surfactant in step (1) is at least one of fatty alcohol polyoxyethylene ether and polyethylene glycol.
3. The method for preparing a decylmethylammonium bromide iodine composite solution according to claim 1, wherein: The metal iodide in step (2) is potassium iodide.
4. The method for preparing a decylmethylammonium bromide iodine composite solution according to claim 1, characterized in that: The mass ratio of the β-cyclodextrin to the deionized water in step (3) is 4:95-100.
5. The method for preparing a decanylmethylammonium bromide iodine composite solution according to claim 1, characterized in that: The mixing in step (3) refers to stirring at 50-60° C. for 1-2 hours.
6. The method for preparing a decylmethylammonium bromide iodine composite solution according to claim 1, characterized in that: The mass ratio of the polyvinyl alcohol to the deionized water in step (4) is 10:90-100.
7. The method for preparing a decylmethylammonium bromide iodine composite solution according to claim 1, characterized in that: The mixing in step (4) refers to stirring and mixing at 60-70° C. for 30-60 minutes.
8. The method for preparing a decylmethylammonium bromide iodine composite solution according to claim 1, characterized in that: The amount of deionized water used in step (5) is 950-1000 parts by weight.
9. A decylmethylammonium bromide iodine composite solution prepared by the preparation method according to any one of claims 1 to 8.
10. A decanylmethylammonium bromide iodine composite solution according to claim 9, characterized in that: The decanylmethylammonium bromide iodine composite solution is used for disinfection of aquaculture.