Physical desinsectization disinfection and killing material and preparation method thereof
By preparing a combination of polyether silane materials, additives, and plant essential oils, a nano-mesh membrane is formed to rapidly kill pests, solving the problems of drug resistance and environmental pollution caused by chemical insecticides, and providing a safe and efficient physical pest control solution.
Patent Information
- Application Number
- CN202511575293.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-31
- Publication Date
- 2026-01-27
AI Technical Summary
Existing chemical insect repellents have problems with drug resistance, environmental pollution risks, and a single mechanism of action, while physical insect repellent products have short-lasting effects and pose a risk of physical irritation to mammals.
Using polyether silane material, with added additives and plant essential oils, a physical insect repellent and pest control material is prepared through an addition reaction. This material forms a nano-mesh membrane that wraps around pests, rapidly killing them and causing them to spontaneously degrade.
It achieves rapid extermination of a variety of pests, is harmless to humans and the environment, does not induce drug resistance, and is suitable for pest control in pets, poultry, livestock, and the environment.
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Figure CN121406111A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of new materials technology, specifically to a physical insect repellent and disinfection material and its preparation method. Background Technology
[0002] The control of pests and pathogens is a crucial aspect of safeguarding public health, agricultural production, and the health of pets and livestock. Currently, most insecticides on the market rely on chemical pesticides. These chemicals, such as pyrethroids and organophosphates, achieve their killing effect by acting on the nervous system of pests or interfering with the metabolic processes of microorganisms. While their effects are rapid, their long-term and widespread use has led to a series of serious problems: 1) Resistance: Under long-term selective pressure, target organisms are highly susceptible to developing resistance, resulting in reduced efficacy and necessitating continuously increasing dosages or the development of new chemical drugs, creating a vicious cycle. 2) Environmental and health risks: Many chemical pesticides are difficult to degrade in the natural environment and may accumulate through the food chain, causing persistent pollution to ecosystems. Furthermore, pesticide residues pose potential health threats to non-target organisms, including humans and pets, such as allergies, toxic reactions, and even carcinogenic risks. 3) Limited mechanism of action: Traditional chemical agents typically target specific physiological targets; once the target changes, the agent becomes ineffective.
[0003] To overcome the shortcomings of chemical methods, physical pest control techniques are gaining increasing attention. For example, mineral oils and diatomaceous earth physically block the spiracles of pests or abrade their waxy epidermal layer, causing them to dehydrate and die. These methods are less likely to induce resistance. However, these physical products suffer from drawbacks such as short-lasting effects, slow action, and the risk of physical irritation to mammals—specifically, the risk of dust inhalation. Therefore, there is an urgent need in this field to develop novel physical pest control materials. Summary of the Invention
[0004] The purpose of this invention is to provide a physical insect repellent and disinfection material and its preparation method. The method is simple, and the prepared material is non-toxic and harmless. It can exhibit excellent bactericidal effects against a variety of bacteria and also has excellent killing rates against mites, fleas, and ants, thus possessing excellent physical disinfection performance.
[0005] To achieve the above-mentioned objectives, the technical solution adopted by this invention is as follows: a physical insect repellent and disinfectant material, formulated from the following components by mass percentage: 82%-88% polyether silane, 10%-12% auxiliaries, 1.5%-7.5% additives, and 0.1%-0.5% plant essential oil; the total mass of the polyether silane, auxiliaries, additives, and plant essential oil is 100%. The polyether silane is obtained by an addition reaction between alkenyl polyether and silane in a certain temperature and solvent under the action of a metal catalyst; the auxiliary agent is one or more of tetraethyl orthosilicate, polydimethylsiloxane, isopropanol, glycerol, ethylene glycol, ethanol, propylene glycol, and butanol; the additive is one or more of keratin, soybean ethyl ethyl sulfate morpholine, zinc castor oil alkyd, fatty alcohol methacrylate, azone, polyvinylpyrrolidone, povidone, and copovidone.
[0006] Preferably, the plant essential oil is one or more of the following: true lavender essential oil, Roman chamomile essential oil, orange blossom essential oil, jasmine essential oil, frankincense essential oil, rose essential oil, grape seed essential oil, geranium essential oil, eucalyptus essential oil, loquat essential oil, sandalwood essential oil, and eucalyptus essential oil.
[0007] Preferably, the alkenyl polyether is one or more of the following: methyl allyl alcohol polyoxyethylene ether, methyl allyl polyoxyethylene ether methyl-terminated, methyl allyl alcohol polyoxypropylene ether, methyl allyl alcohol polyoxyethylene polyoxypropylene ether, isopentenyl alcohol polyoxyethylene ether, isopentenyl polyoxyethylene ether methyl-terminated, isopentenyl alcohol polyoxypropylene ether, isopentenyl alcohol polyoxyethylene polyoxypropylene ether, allyl alcohol polyoxyethylene ether, allyl polyoxyethylene ether methyl-terminated, allyl alcohol polyoxypropylene ether, allyl polyoxyethylene polyoxypropylene ether, and allyl polyoxyethylene polyoxypropylene ether methyl-terminated.
[0008] Preferably, the silane is one or more of trimethoxysilane, triethoxysilane, phenyldimethylsilane, methyldimethoxysilane, methyldiethoxysilane, heptamethyltrisiloxane, tetramethyldisiloxane, diphenylmethylsilane, triphenylsilane, triethylsilane, trimethylsilane, tri(trimethylsilyl)silane, tri(trimethsiloxy)silane, hydrogen-terminated polydimethylsiloxane, and polymethylhydrosiloxane, and the molar ratio between the silane and the alkenyl polyether is (1-5):1.
[0009] Preferably, the catalyst is a supported platinum catalyst or a homogeneous catalyst; the supported platinum catalyst is one of Pt / CeO2, Pt / SiO2, Pt / Al2O3, Pt / TiO2, and Pt / HY, with a metal mass loading of 0.01-30%; the homogeneous catalyst is at least one of H2PtCl6, platinum diethylenetetramethyldisiloxane, and PtCl2(NH3)2; the amount of catalyst used is 1%-100% of the silane mass.
[0010] Preferably, the solvent is selected from at least one of xylene, diethyl ether, tetrahydrofuran, 2-methyltetrahydrofuran, N,N-dimethylformamide, N,N-dimethylacetamide, dichloromethane, dichloroethane, acetonitrile, cyclohexane, toluene, and chlorobenzene.
[0011] Preferably, the concentration of the alkenyl polyether is 0.10~5.0 mol / L; the reaction temperature is 25-200 ℃; and the reaction time is 0.5-36 h.
[0012] To achieve the above-mentioned objectives, the present invention also provides a method for preparing a physical insect repellent and disinfection material, comprising the following steps: S1. Hydrosilylation reaction: Alkenyl polyether, silane, solvent and metal catalyst are added to the reaction flask in sequence. The hydrosilylation reaction is carried out at a certain temperature for a period of time. The solvent and metal catalyst are removed to generate polyether silane. S2. Add polyether silane, auxiliaries, additives and plant essential oils to the container according to the ratio, mix and stir evenly to obtain physical insect repellent and pest control materials.
[0013] Compared with the prior art, the present invention has the following beneficial effects: This invention utilizes a polyether silane with a single silicon atom structure, and adds auxiliaries, additives, and plant essential oils to accelerate the insect-repelling and bactericidal effects. The prepared product has been tested and found to be non-toxic and harmless, and non-irritating to the eyes and skin. When the product is prepared into an aqueous solution with a volume concentration of 2%-8%, it exhibits excellent bactericidal effects against various bacteria and also demonstrates excellent kill rates against mites, fleas, and ants in a short time. The principle of insect repellency and bactericidal action is that after spraying, it rapidly hydrolyzes to form a nano-mesh membrane, encapsulating and binding bacteria and pests, preventing them from breathing and moving, thus causing them to die. This physical mechanism does not produce drug resistance and is harmless to humans and animals. Furthermore, the material spontaneously degrades after spraying and does not accumulate in the environment. Therefore, this material can be used as an environmentally friendly physical insect repellent and pest control product, with promising application prospects in the fields of pet, poultry, livestock, and environmental pest control. Attached Figure Description
[0014] Figure 1 The image shows the 1H NMR spectrum of the synthesized allyl polyether silane. Figure 2 The 1H NMR spectrum of the synthesized methyl allyl polyether silane; Figure 3 Images showing the results of a flea eradication test; Figure 4 This is a test result of ant extermination. Detailed Implementation
[0015] The present application is described in detail below with reference to embodiments, but the present application is not limited to these embodiments. Unless otherwise specified, the raw materials and catalyst precursors in the embodiments of the present application were purchased commercially. The analytical methods in the embodiments of the present application are as follows: nuclear magnetic resonance detection was performed on a Bruker AVANCE III 400 MHz instrument.
[0016] The synthesis method of the polyether silane used in the following examples is as follows: Method 1: In a 100 mL reaction flask, methyl allyl alcohol polyoxyethylene ether (CAS: 31497-33-3, molecular weight 1500, 20.0 mmol) was dissolved in 20 mL of toluene. An isopropanol solution of H₂PtCl₆ (10 mg / mL, 0.2 mmol) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was refluxed and stirred at 120°C for 24 h. After the reaction was complete, activated carbon (20 g) was added, and the mixture was stirred at 60°C for 30 min. The activated carbon was removed by filtration, and the filtrate was evaporated to remove toluene, yielding methyl allyl polyether silane P1 with a separation yield of 85%.
[0017] Method 2: In a 100 mL reaction flask, methyl allyl alcohol polyoxyethylene ether (CAS: 31497-33-3, molecular weight 1500, 20.0 mmol) was dissolved in 20 mL of toluene. Commercially available diethylenetetramethyldisiloxane (0.2 mmol) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was refluxed and stirred at 120°C for 24 h. After the reaction was complete, activated carbon (20 g) was added, and the mixture was stirred at 60°C for 30 min. The activated carbon was removed by filtration, and the filtrate was evaporated to remove toluene, yielding methyl allyl polyether silane P1 with a separation yield of 88%.
[0018] Method 3: In a 100 mL reaction flask, methyl allyl alcohol polyoxyethylene ether (CAS: 31497-33-3, molecular weight 1500, 20.0 mmol) was dissolved in 20 mL of toluene. Platinum-supported alumina catalyst (5% Pt / Al₂O₃, 1.5 g) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was stirred at 180°C for 24 h. After the reaction was complete, the catalyst was removed by filtration, and the filtrate was evaporated to remove toluene, yielding methyl allyl polyether silane P1 with a yield of 35%.
[0019] Method 4: In a 100 mL reaction flask, methyl allyl alcohol polyoxyethylene ether (CAS: 31497-33-3, molecular weight 1500, 20.0 mmol) was dissolved in 20 mL of toluene. Platinum-supported cerium oxide catalyst (5% Pt / CeO2, 1.5 g) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was stirred at 180°C for 24 h. After the reaction was complete, the catalyst was removed by filtration, and the filtrate was evaporated to remove toluene, yielding methyl allyl polyether silane P1 with a yield of 75%.
[0020] Method 5: In a 100 mL reaction flask, methyl allyl alcohol polyoxyethylene ether (CAS: 31497-33-3, molecular weight 1500, 20.0 mmol) was dissolved in 20 mL of toluene. Platinum-supported silica catalyst (5% Pt / SiO2, 1.5 g) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was stirred at 180°C for 24 h. After the reaction was complete, the catalyst was removed by filtration, and the filtrate was evaporated to remove toluene, yielding methyl allyl polyether silane P1 with a yield of 68%.
[0021] Method 6: In a 100 mL reaction flask, allyl alcohol polyoxyethylene ether (CAS: 27274-31-3, molecular weight 1000, 20.0 mmol) was dissolved in 20 mL of toluene. An isopropanol solution of H₂PtCl₆ (10 mg / mL, 0.2 mmol) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was refluxed and stirred at 120°C for 24 h. After the reaction was complete, activated carbon (20 g) was added, and the mixture was stirred at 60°C for 30 min. The activated carbon was removed by filtration, and the filtrate was evaporated to remove toluene, yielding allyl polyether silane P₂ with a yield of 80%.
[0022] Method 7: In a 100 mL reaction flask, allyl alcohol polyoxyethylene ether (CAS: 27274-31-3, molecular weight 1000, 20.0 mmol) was dissolved in 20 mL of toluene. Commercially available platinum diethylenetetramethyldisiloxane (0.2 mmol) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was refluxed and stirred at 120°C for 24 h. After the reaction was complete, activated carbon (20 g) was added, and the mixture was stirred at 60°C for 30 min. The activated carbon was removed by filtration, and the filtrate was evaporated to remove toluene, yielding allyl polyether silane P2 with a separation yield of 87%.
[0023] Method 8: In a 100 mL reaction flask, allyl alcohol polyoxyethylene ether (CAS: 27274-31-3, molecular weight 1000, 20.0 mmol) was dissolved in 20 mL of toluene. Platinum-supported cerium oxide catalyst (5% Pt / CeO2, 1.0 g) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was stirred at 180°C for 24 h. After the reaction was complete, the catalyst was removed by filtration, and the filtrate was evaporated to remove toluene, yielding allyl polyether silane P2 with a yield of 70%.
[0024] Method 9: In a 100 mL reaction flask, isopentenyl polyoxyethylene ether (molecular weight 1200, 20.0 mmol) was dissolved in 20 mL of toluene. Commercially available platinum-diethylenetetramethyldisiloxane (0.2 mmol) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was refluxed and stirred at 120°C for 24 h. After the reaction was complete, activated carbon (20 g) was added, and the mixture was stirred at 60°C for 30 min. The activated carbon was removed by filtration, and the filtrate was evaporated to remove toluene, yielding isopentenyl polyether silane P3 with a separation yield of 82%.
[0025] Method 10: In a 100 mL reaction flask, isopentenyl polyoxyethylene ether (molecular weight 1200, 20.0 mmol) was dissolved in 20 mL of toluene. Platinum-supported cerium oxide catalyst (5% Pt / CeO2, 1.2 g) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was stirred at 180°C for 24 h. After the reaction was complete, the catalyst was removed by filtration, and the filtrate was evaporated to remove toluene, yielding isopentenyl polyether silane P3 with a yield of 73%.
[0026] Method 11: In a 100 mL reaction flask, methyl-terminated allyl polyoxyethylene ether (27252-80-8, molecular weight 1000, 20.0 mmol) was dissolved in 20 mL of toluene. Commercially available diethylenetetramethyldisiloxane (0.2 mmol) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was refluxed and stirred at 120°C for 24 h. After the reaction was complete, activated carbon (20 g) was added, and the mixture was stirred at 60°C for 30 min. The activated carbon was removed by filtration, and the filtrate was evaporated to remove toluene, yielding allyl methyl polyether silane P4 with a separation yield of 87%.
[0027] Method 12: In a 100 mL reaction flask, methyl-terminated allyl polyoxyethylene ether (27252-80-8, molecular weight 1000, 20.0 mmol) was dissolved in 20 mL of toluene. Platinum-supported cerium oxide catalyst (5% Pt / CeO2, 1.0 g) and heptamethyltrisiloxane (22.0 mmol) were added sequentially, and the mixture was stirred at 180°C for 24 h. After the reaction was complete, the catalyst was removed by filtration, and the filtrate was evaporated to remove toluene, yielding allyl methyl polyether silane P4 with a yield of 68%.
[0028] The 1H NMR spectrum of methylallyl polyether silane P1 is shown below. Figure 2 As shown, the proton NMR data are: 1H NMR (400MHz, CDCl3) δ 3.66–3.48 (m, 40H), 3.45–3.38 (m, 2H), 1.63–1.51 (m, 1H), 0.86–0.42 (m, 5H), 0.08 (s, 18H), 0.07 (s, 3H).
[0029] The 1H NMR spectrum of allyl polyether silane P2 is shown below. Figure 1 As shown, the proton NMR data are: 1 H NMR (400 MHz, CDCl3) δ 3.67–3.46 (m, 40H), 3.32 (t, J = 7.2 Hz, 2H), 2.84 (s, 1H), 1.57–1.42 (m, 2H), 0.41–0.27 (m, 2H), 0.08 (s, 18H), 0.06 (s, 3H).
[0030] P3 NMR data of isopentenyl polyether silane: 1 H NMR (400 MHz, CDCl3) δ 3.64–3.50 (m,40H), 3.48–3.41 (m, 2H), 1.57–1.40 (m, 3H), 0.76–0.49 (m, 5H), 0.08 (s, 18H), 0.07 (s, 3H).
[0031] P4 NMR data for allyl methyl polyether silane: 1 H NMR (400 MHz, CDCl3) δ 3.60–3.53(m, 38H), 3.53–3.43 (m, 4H), 3.36–3.31 (m, 2H), 3.30 (s, 3H), 1.57–1.42 (m,2H), 0.41–0.27 (m, 2H), 0.08 (s, 18H), 0.06 (s, 3H).
[0032] Example 1 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 88% methyl allyl polyether silane P1, 10% tetraethyl orthosilicate as an auxiliary agent, 1.5% zinc castor oil alkyd as an additive, and 0.5% real lavender essential oil.
[0033] The preparation method is as follows: Add 88 g of methyl allyl polyether silane P1, 10 g of tetraethyl orthosilicate, 1.5 g of zinc castor oil alkyd, and 0.5 g of real lavender essential oil to a 100 mL beaker in sequence, stir well, and obtain product P1-M1.
[0034] Example 2 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 85% methyl allyl polyether silane P1, 10% glycerin (an auxiliary agent), 4.5% polyvinylpyrrolidone (an additive), and 0.5% real lavender essential oil.
[0035] The preparation method is as follows: Add 85 g of methyl allyl polyether silane P1, 10 g of glycerin, 4.5 g of polyvinylpyrrolidone, and 0.5 g of real lavender essential oil to a 100 mL beaker in sequence, stir well, and obtain product P1-M2.
[0036] Example 3 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 88% methyl allyl polyether silane P1, 10% auxiliary agent polydimethylsiloxane, 1.5% additive methacrylate fatty alcohol, and 0.5% Roman chamomile essential oil.
[0037] The preparation method is as follows: Add 88 g of methyl allyl polyether silane P1, 10 g of polydimethylsiloxane, 1.5 g of fatty alcohol methacrylate, and 0.5 g of Roman chamomile essential oil to a 100 mL beaker in sequence, stir evenly, and obtain product P1-M3.
[0038] Example 4 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 82% methyl allyl polyether silane P1, 10% ethylene glycol as an auxiliary agent, 7.5% keratin peptide as an additive, and 0.5% Roman chamomile essential oil.
[0039] The preparation method is as follows: Add 82 g of methyl allyl polyether silane P1, 10 g of ethylene glycol, 7.5 g of keratin peptide, and 0.5 g of Roman chamomile essential oil to a 100 mL beaker in sequence, stir well, and obtain product P1-M4.
[0040] Example 5 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 88% allyl polyether silane P2, 10% tetraethyl orthosilicate as an auxiliary agent, 1.5% zinc castor oil alkyd as an additive, and 0.5% real lavender essential oil.
[0041] The preparation method is as follows: Add 88 g of allyl polyether silane P2, 10 g of tetraethyl orthosilicate, 1.5 g of zinc castor oil alkyd, and 0.5 g of real lavender essential oil to a 100 mL beaker in sequence, stir well, and obtain product P2-M1.
[0042] Example 6 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 85% allyl polyether silane P2, 10% glycerin (an auxiliary agent), 1.5% azone (an additive), and 0.5% real lavender essential oil.
[0043] The preparation method is as follows: Add 85 g of allyl polyether silane P2, 10 g of glycerol, 4.5 g of azone, and 0.5 g of real lavender essential oil to a 100 mL beaker in sequence, stir well, and obtain product P2-M2.
[0044] Example 7 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 88% allyl polyether silane P2, 10% auxiliary agent polydimethylsiloxane, 1.5% additive methacrylate fatty alcohol, and 0.5% Roman chamomile essential oil.
[0045] The preparation method is as follows: Add 88 g of allyl polyether silane P2, 10 g of polydimethylsiloxane, 1.5 g of fatty alcohol methacrylate, and 0.5 g of Roman chamomile essential oil to a 100 mL beaker in sequence, stir evenly, and obtain product P2-M3.
[0046] Example 8 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 82% allyl polyether silane P2, 10% ethylene glycol as an auxiliary agent, 7.5% keratin peptide as an additive, and 0.5% Roman chamomile essential oil.
[0047] The preparation method is as follows: Add 82 g of allyl polyether silane P2, 10 g of ethylene glycol, 7.5 g of keratin peptide, and 0.5 g of Roman chamomile essential oil to a 100 mL beaker in sequence, stir well, and obtain product P2-M4.
[0048] Example 9 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 88% isopentenyl polyether silane P3, 10% tetraethyl orthosilicate as an auxiliary agent, 1.5% zinc castor oil alkyd as an additive, and 0.5% real lavender essential oil.
[0049] The preparation method is as follows: Add 88 g of isopentenyl polyether silane P3, 10 g of tetraethyl orthosilicate, 1.5 g of zinc castor oil alkyd, and 0.5 g of real lavender essential oil to a 100 mL beaker in sequence, stir well, and obtain product P3-M1.
[0050] Example 10 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 85% isopentenyl polyether silane P3, 10% glycerin (an auxiliary agent), 4.5% azone (an additive), and 0.5% real lavender essential oil.
[0051] The preparation method is as follows: Add 85 g of isopentenyl polyether silane P3, 10 g of glycerin, 4.5 g of azone, and 0.5 g of real lavender essential oil to a 100 mL beaker in sequence, stir well, and obtain product P3-M2.
[0052] Example 11 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 88% allyl methyl polyether silane P4, 10% tetraethyl orthosilicate as an auxiliary agent, 1.5% zinc castor oil alkyd as an additive, and 0.5% real lavender essential oil.
[0053] The preparation method is as follows: Add 88 g of allyl methyl polyether silane P4, 10 g of tetraethyl orthosilicate, 1.5 g of zinc castor oil alkyd, and 0.5 g of real lavender essential oil to a 100 mL beaker in sequence, stir well, and obtain product P4-M1.
[0054] Example 12 A physical insect repellent and pest control material is formulated from the following components in weight percentage: 85% allyl methyl polyether silane P4, 10% glycerin (an auxiliary agent), 4.5% azone (an additive), and 0.5% real lavender essential oil.
[0055] The preparation method is as follows: Add 85 g of allyl methyl polyether silane P4, 10 g of glycerol, 4.5 g of azone, and 0.5 g of real lavender essential oil to a 100 mL beaker in sequence, stir well, and obtain product P4-M2.
[0056] The obtained products were diluted with deionized water to a 5% (v / v) milky white solution, and their toxicological and disinfection properties were tested. In addition, pure polyether silane materials P1-P4 were also diluted with deionized water to a 5% (v / v) milky white solution as comparative examples, namely products P1-M0, P2-M0, P3-M0, and P4-M0, respectively.
[0057] Acute oral toxicity tests were conducted on the obtained products P1-M1, P1-M2, P1-M3, P1-M4, P2-M1, P2-M2, P2-M3, P2-M4, P3-M1, P3-M2, P4-M1, P4-M2, and the comparative products P1-M0, P2-M0, P3-M0, and P4-M0. The tests were performed according to Section 2.3.1 of the "Disinfection Technical Specifications" (2002 edition). A single maximum limit experiment was conducted, with KM mice (10 males and 10 females) administered the product via gavage at a dose of 5000 mg / kg, and observed for 14 consecutive days. After euthanasia, no abnormalities were observed in the major organs of the P1, P2, and P3 series upon visual inspection. The acute oral LD50 in KM mice was determined. 50 >5000 mg / kg body weight is practically non-toxic. However, for products P4-M1, P4-M2, and P4-M0, visual observation showed abnormalities in the livers of 2-3 female mice, indicating that the P4 series products are not suitable for medical / veterinary use.
[0058] The acaricidal performance of the obtained products P1-M1, P1-M2, P1-M3, P1-M4, P2-M1, P2-M2, P2-M3, P2-M4, P3-M1, P3-M2, and the comparative products P1-M0, P2-M0, and P3-M0 was tested. The testing and evaluation were conducted according to NY / T 1151.2-2006 "Indoor Efficacy Testing and Evaluation of Pesticides for Sanitary Use - Part 2: Acaricides and Mite Repellents". The specific procedure was as follows: Three clean textile fabrics with a diameter of 58 mm were placed in three petri dishes. The samples were soaked in the entire fabric, and then 200 test insects were placed on the wet fabric. After 30 minutes, 0.05 g of mite feed was placed in the center of the petri dish. In the fourth culture dish, a clean piece of textile was placed as a control. 200 test mites were placed on the textile, and 0.05 g of mite feed was added to the center of the dish after 30 minutes. A mixture of white oil and petrolatum was evenly coated on the upper edge of the inner wall of each culture dish, and then the dishes were placed in a constant temperature and humidity incubator. The number of dead mites was observed and recorded after 1 h, 2 h, 6 h, 12 h, 24 h, and 48 h of incubation. In comparison, products P1-M0, P2-M0, and P3-M0 without other added ingredients had a longer action time, requiring 24-48 h to achieve a high mite eradication rate (92-98%). In contrast, products P1, P2, and P3 series with added ingredients achieved a high mite eradication rate (≥98%) within 1 hour, with a shorter action time. This is because additives, auxiliaries, and plant essential oils can promote the rapid spreading and penetration of polyether silane, accelerate hydrogen bond formation, form a mesh-like film, encapsulate the parasites, and achieve a rapid killing effect.
[0059] The flea-killing performance of the obtained products P1-M1, P1-M2, P1-M3, P1-M4, P2-M1, P2-M2, P2-M3, P2-M4, P3-M1, P3-M2, and the comparative products P1-M0, P2-M0, and P3-M0 was tested. The testing and evaluation were conducted in accordance with GB / T13917.1-2009 "Indoor Efficacy Testing and Evaluation of Pesticides for Sanitary Use - Part 1: Sprays". A square transparent test box was used, placed on a test platform with a 300×300mm non-woven fabric pad at the bottom. One hundred fleas were released through the release hole into the central area of the non-woven fabric. After the test insects resumed normal activity, the sample was sprayed 10 times into the square transparent test box using a spray bottle. The spray bottle was immediately removed, and the release hole was sealed. Timing was started immediately after spraying. After 20 minutes, all test insects were collected into clean petri dishes. The number of dead fleas was checked at 1 h, 2 h, 6 h, 12 h, and 24 h. In comparison, products P1-M0, P2-M0, and P3-M0 without added ingredients had a longer action time, requiring 6-12 hours to achieve a high flea kill rate. The kill rate for P1-M0 was 98%, for P2-M0 it was 96%, and for P3-M0 it was 92%. In contrast, products with added ingredients achieved a high flea kill rate within 1 hour. The kill rates for the P1 and P2 series products were both 100%, and the kill rate for the P3 series product was 92-95%. The flea kill test results are as follows: Figure 3 As shown.
[0060] The ant-killing performance of the obtained products P1-M1, P1-M2, P1-M3, P1-M4, P2-M1, P2-M2, P2-M3, P2-M4, P3-M1, P3-M2, and the comparative products P1-M0, P2-M0, and P3-M0 was tested. The testing and evaluation were conducted in accordance with GB / T13917.1-2009 "Indoor Efficacy Testing and Evaluation of Pesticides for Sanitary Use - Part 1: Sprays". Ten ants were placed in a foam box. After the test insects resumed normal activity, the sample was sprayed 10 times directly onto the ants using a spray bottle. The spray bottle was immediately removed, and the insect-placement hole was sealed. The number of dead insects was checked at 3 min, 10 min, 30 min, and 1 h. In comparison, products P1-M0, P2-M0, and P3-M0 without added ingredients had a longer action time, requiring 30 minutes to achieve a high ant killing rate. P1-M0 achieved a 100% killing rate, P2-M0 a 100% killing rate, and P3-M0 a 90% killing rate. In contrast, products with added ingredients achieved a high ant killing rate within 3-10 minutes. The P1 and P2 series products both achieved a 100% killing rate, while the P3 series product achieved a 90% killing rate. The ant killing test results are as follows: Figure 4 As shown.
[0061] The results above show that the P1 and P2 series products have better insect-repelling effects, and the added additives, auxiliaries, and plant essential oils result in a faster onset of action. This is because the additives, auxiliaries, and plant essential oils promote the rapid spreading and penetration of polyether silane, accelerate hydrogen bond formation, and form a mesh-like film, achieving a rapid killing effect. Therefore, the P1 and P2 series products will be further tested for antibacterial properties and irritation.
[0062] Antibacterial performance tests were conducted on products P1 and P2 series. Following the evaluation method for antibacterial and bacteriostatic effects in WS / T 650-2019, the quantitative suspension bactericidal test (section 5.2.1) was used. Products P1 and P2 series showed excellent bactericidal effects against Escherichia coli, Staphylococcus aureus, and Pasteurella multocida, with bactericidal rates all exceeding 95%.
[0063] Skin irritation tests were conducted on products P1 and P2 series. A complete skin irritation test was performed according to Section 2.3.3.3.1 of the "Disinfection Technical Specifications" (2002 edition). The test solution was prepared at five times the maximum permitted concentration, i.e., a 25% (v / v) milky white solution diluted with deionized water. The treatment method was as follows: 24 hours prior to the test, the hair on both sides of the spine on the back of New Zealand rabbits was removed, without damaging the skin. The hair removal area was approximately 3cm × 3cm on each side. The next day, 0.5 mL of the test sample was directly applied to one side of the intact hairless skin, then covered with a layer of non-irritating plastic film, and then secured with non-irritating adhesive tape. The other side served as a blank control. The application time was 4 hours. After the test, the skin was washed with warm water to remove any remaining test sample. Local skin reactions were observed and scored at 1 hour, 24 hours, and 48 hours after removal of the test sample. The scoring criteria and irritation intensity grading were based on the "Disinfection Technical Specifications" (2002 edition). According to testing, the P1 and P2 series products showed no irritation in a single complete skin irritation test on New Zealand rabbits.
[0064] Eye irritation tests were conducted on products P1 and P2 series. The testing was based on section 2.3.4 of the "Disinfection Technical Specifications" (2002 edition) for acute eye irritation testing. The test solution was prepared using five times the maximum permitted concentration, i.e., a 25% (v / v) milky white solution diluted with deionized water. The exposure method involved instilling 0.1 mL of the test sample into the conjunctival sac of the left eye of a New Zealand rabbit, with physiological saline used as a normal control in the right eye. After instillation, the eye was passively closed for 4 seconds, followed by rinsing with physiological saline after 30 seconds. Observations and records were kept for 24 hours before and after exposure. All animals' eyes were examined with sodium fluorescein. Damage and recovery of the conjunctiva, iris, and cornea of the New Zealand rabbits were observed visually at 1 hour, 24 hours, 48 hours, 72 hours, 7 days, 14 days, and 21 days after instillation. If no irritation reaction occurs within 72 hours, or if the eye irritation reaction completely subsides by day 7 or 14, the test should be terminated early. The scoring criteria and irritation intensity grading refer to the "Disinfection Technical Specifications" (2002 edition). Testing showed that products P1 and P2 series exhibited a non-irritating reaction in the acute eye irritation test on New Zealand rabbits.
[0065] Based on this, the products prepared by the present invention have good application prospects in the fields of pet, poultry, animal husbandry and environmental pest control.
Claims
1. A physical insect repellent and pest control material, characterized in that, It is formulated from the following components by weight percentage: 82%-88% polyether silane, 10%-12% auxiliaries, 1.5%-7.5% additives, and 0.1%-0.5% plant essential oil; the total weight of the polyether silane, auxiliaries, additives, and plant essential oil is 100%. The polyether silane is obtained by an addition reaction between alkenyl polyether and silane in a certain temperature and solvent under the action of a metal catalyst; the auxiliary agent is one or more of tetraethyl orthosilicate, polydimethylsiloxane, isopropanol, glycerol, ethylene glycol, ethanol, propylene glycol, and butanol; the additive is one or more of keratin, soybean ethyl ethyl sulfate morpholine, zinc castor oil alkyd, fatty alcohol methacrylate, azone, polyvinylpyrrolidone, povidone, and copovidone.
2. The physical insect repellent and pest control material according to claim 1, characterized in that, The plant essential oils mentioned are one or more of the following: true lavender essential oil, Roman chamomile essential oil, orange blossom essential oil, jasmine essential oil, frankincense essential oil, rose essential oil, grape seed essential oil, geranium essential oil, eucalyptus essential oil, loquat essential oil, sandalwood essential oil, and eucalyptus essential oil.
3. The physical insect repellent and pest control material according to claim 1 or 2, characterized in that, The alkenyl polyether is one or more of the following: methyl allyl alcohol polyoxyethylene ether, methyl allyl polyoxyethylene ether methyl-terminated, methyl allyl alcohol polyoxypropylene ether, methyl allyl alcohol polyoxyethylene polyoxypropylene ether, isopentenyl alcohol polyoxyethylene ether, isopentenyl polyoxyethylene ether methyl-terminated, isopentenyl alcohol polyoxypropylene ether, isopentenyl alcohol polyoxyethylene polyoxypropylene ether, allyl alcohol polyoxyethylene ether, allyl polyoxyethylene ether methyl-terminated, allyl alcohol polyoxypropylene ether, allyl polyoxyethylene polyoxypropylene ether, allyl polyoxyethylene polyoxypropylene ether methyl-terminated.
4. A physical insect repellent and pest control material according to claim 1 or 2, characterized in that, The silane is one or more of trimethoxysilane, triethoxysilane, phenyldimethylsilane, methyldimethoxysilane, methyldiethoxysilane, heptamethyltrisiloxane, tetramethyldisiloxane, diphenylmethylsilane, triphenylsilane, triethylsilane, trimethylsilane, tri(trimethylsilyl)silane, tri(trimethsiloxy)silane, hydrogen-terminated polydimethylsiloxane, and polymethylhydrosiloxane, and the molar ratio between the silane and the alkenyl polyether is (1-5):
1.
5. A physical insect repellent and pest control material according to claim 1 or 2, characterized in that, The catalyst is a supported platinum catalyst or a homogeneous catalyst; The supported platinum catalyst is one of Pt / CeO2, Pt / SiO2, Pt / Al2O3, Pt / TiO2, and Pt / HY, with a metal mass loading of 0.01-30%; the homogeneous catalyst is at least one of H2PtCl6, platinum diethylenetetramethyldisiloxane, and PtCl2(NH3)2; the amount of catalyst used is 1%-100% of the silane mass.
6. A physical insect repellent and pest control material according to claim 1 or 2, characterized in that, The solvent is selected from at least one of xylene, diethyl ether, tetrahydrofuran, 2-methyltetrahydrofuran, N,N-dimethylformamide, N,N-dimethylacetamide, dichloromethane, dichloroethane, acetonitrile, cyclohexane, toluene, and chlorobenzene.
7. A physical insect repellent and pest control material according to claim 1 or 2, characterized in that, The concentration of the alkenyl polyether is 0.10~5.0 mol / L; the reaction temperature is 25-200 ℃, and the reaction time is 0.5-36 h.
8. The method for preparing a physical insect repellent and disinfectant material according to claims 1-7, characterized in that, Includes the following steps: S1. Hydrosilylation reaction: Alkenyl polyether, silane, solvent and metal catalyst are added to the reaction flask in sequence. The hydrosilylation reaction is carried out at a certain temperature for a period of time. The solvent and metal catalyst are removed to generate polyether silane. S2. Add polyether silane, auxiliaries, additives and plant essential oils to the container according to the ratio, mix and stir evenly to obtain physical insect repellent and pest control materials.
Citation Information
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