阅读说明：本技术 一种驱蚊微胶囊及其制备方法 (Mosquito-repelling microcapsule and preparation method thereof ) 是由 姚明路 胡冰 高隽 胡军 于 2019-09-05 设计创作，主要内容包括：本发明公开了一种驱蚊微胶囊,由混合精油微胶囊乳浊液和避蚊胺微胶囊乳浊液按照质量比1:(0.5-1)混合而成；混合精油微胶囊乳浊液由壁材A、壁材B与芯材A混合而成；壁材A为明胶乳化剂溶液；壁材B为阿拉伯胶乳化剂溶液；芯材A包括混合植物精油和丁二羟基茴香醚,混合植物精油由Span-80、Tween-20、薰衣草精油、香茅精油混合而成；避蚊胺微胶囊乳浊液由壁材C与芯材B混合而成,壁材C为阿拉伯胶乳化剂溶液；芯材B由明胶水溶液、Tween-20、避蚊胺按照质量比0.5:(0.1-0.5):1混合而成。本发明将避蚊胺与避蚊植物精油微胶囊化后可以增强驱蚊效果,驱避时间长、透皮吸收少。(The invention discloses a mosquito-repellent microcapsule, which is prepared by mixing a mixed essential oil microcapsule emulsion and a delphene microcapsule emulsion according to the mass ratio of 1 (0.5-1); the mixed essential oil microcapsule emulsion is formed by mixing a wall material A, a wall material B and a core material A; the wall material A is gelatin emulsifier solution; the wall material B is Arabic gum emulsifier solution; the core material A comprises mixed plant essential oil and butylated hydroxyanisole, wherein the mixed plant essential oil is formed by mixing Span-80, Tween-20, lavender essential oil and citronella essential oil; the deet microcapsule emulsion is formed by mixing a wall material C and a core material B, wherein the wall material C is a arabic gum emulsifier solution; the core material B is formed by mixing gelatin aqueous solution, Tween-20 and deet according to the mass ratio of 0.5 (0.1-0.5) to 1. The mosquito repellent agent can enhance the mosquito repellent effect after microencapsulating the diethyltoluamide and the mosquito repellent plant essential oil, and has long repellent time and less transdermal absorption.)

1. A mosquito-repellent microcapsule is characterized in that: the mosquito-repellent microcapsule is formed by mixing a mixed essential oil microcapsule emulsion and a delphene microcapsule emulsion according to the mass ratio of 1 (0.5-1);

the mixed essential oil microcapsule emulsion is formed by mixing a wall material A, a wall material B and a core material A according to the mass ratio of (1-2) to (2-4); the wall material A is a gelatin emulsifier solution with the mass concentration of 1%; the wall material B is a Arabic gum emulsifier solution with the mass concentration of 1%; the core material A comprises mixed plant essential oil and butylated hydroxyanisole, wherein the mixed plant essential oil is formed by mixing Span-80, Tween-20, lavender essential oil and citronella essential oil according to the mass ratio of (0.5-1) to (1-2) to (2-2.5), and the butylated hydroxyanisole accounts for 0.5% of the mass of the mixed plant essential oil;

the DEET microcapsule emulsion is formed by mixing a wall material C and a core material B according to the mass ratio of 0.5 (1.5-2), wherein the wall material C is a arabic gum emulsifier solution with the mass concentration of 3%; the core material B is formed by mixing gelatin aqueous solution, Tween-20 and deet according to the mass ratio of 0.5 (0.1-0.5) to 1, and the mass concentration of the gelatin aqueous solution is 3%.

2. A mosquito repellent microcapsule according to claim 1, wherein: the mosquito-repellent microcapsule is formed by mixing a mixed essential oil microcapsule emulsion and a delphene microcapsule emulsion according to the mass ratio of 1: 0.5;

the mixed essential oil microcapsule emulsion is formed by mixing a wall material A, a wall material B and a core material A according to the mass ratio of 1:1: 2; the wall material A is a gelatin emulsifier solution with the mass concentration of 1%; the wall material B is a Arabic gum emulsifier solution with the mass concentration of 1%; the core material A comprises mixed plant essential oil and butylated hydroxyanisole, wherein the mixed plant essential oil is formed by mixing Span-80, Tween-20, lavender essential oil and citronella essential oil according to the mass ratio of 1:2:2.5:2.5, and the butylated hydroxyanisole accounts for 0.5% of the mixed plant essential oil;

the deet microcapsule emulsion is formed by mixing a wall material C and a core material B according to the mass ratio of 0.5:1.5, wherein the wall material C is a gum arabic emulsifier solution with the mass concentration of 3%; the core material B is formed by mixing gelatin aqueous solution, Tween-20 and deet according to the mass ratio of 0.5:0.1:1, and the mass concentration of the gelatin aqueous solution is 3%.

3. A method for preparing a mosquito repellent microcapsule as claimed in claim 1 or 2, characterized in that: the method comprises the following operation steps:

step 1: preparation of Mixed essential oil microcapsule emulsion

Preparation of wall material A: dissolving gelatin in distilled water to prepare gelatin emulsifier solution with mass concentration of 1%;

preparing a wall material B: dissolving Arabic gum in distilled water to prepare an Arabic gum emulsifier solution with the mass concentration of 1%;

preparation of core material A: mixing Span-80, Tween-20, lavender essential oil, citronella essential oil and butylated hydroxyanisole in proportion, stirring until the mixture is dissolved and uniformly mixed;

preparing mixed essential oil microcapsule emulsion: mixing the wall material A, the wall material B and the core material A in proportion, filtering, homogenizing and curing to obtain a mixed essential oil microcapsule emulsion;

step 2: preparation of deet microcapsule emulsion

Preparation of wall material C: adding distilled water into arabic gum to prepare a arabic gum emulsifier solution with the mass concentration of 3%;

preparation of core material B: adding water into gelatin to prepare gelatin water solution with mass concentration of 3%, adding Tween-20 and diethyltoluamide in proportion, and stirring to form uniform emulsion;

preparing a delphene microcapsule emulsion: mixing the wall material C and the core material B in proportion, filtering, homogenizing and curing to obtain the deet microcapsule emulsion;

and step 3: preparing mosquito-repellent microcapsule

And mixing the mixed essential oil microcapsule emulsion and the diethyltoluamide microcapsule emulsion in proportion and stirring uniformly.

4. A method for preparing mosquito repellent microcapsules according to claim 3, wherein the method comprises the following steps: the method comprises the following operation steps:

step 1: preparation of Mixed essential oil microcapsule emulsion

Preparation of wall material A: putting gelatin in a constant-temperature jacket reaction kettle, adding distilled water with the volume 5 times that of the gelatin, heating to 80 ℃, stirring at the speed of 100r/min until the gelatin is dissolved and uniformly mixed, cooling to 45 ℃, and adding cold distilled water to prepare a gelatin emulsifier solution with the mass concentration of 1%;

preparing a wall material B: putting Arabic gum into a constant-temperature jacket reaction kettle, adding distilled water with the volume 10 times that of the Arabic gum, heating to 90 ℃, stirring at the speed of 100r/min until the Arabic gum is dissolved and uniformly mixed, cooling to 45 ℃, and adding cold distilled water to prepare an Arabic gum emulsifier solution with the mass concentration of 1%;

preparation of core material A: mixing Span-80, Tween-20, lavender essential oil and citronella essential oil in proportion, adding 0.5% of dihydroxyanisole in mass of the mixture, then placing in a constant-temperature jacket reaction kettle, heating to 80 ℃, stirring at a speed of 100r/min until the mixture is dissolved and uniformly mixed, cooling to 45 ℃, and continuously stirring at a speed of 40r/min in the cooling process;

preparing mixed essential oil microcapsule emulsion: mixing the wall material A, the wall material B and the core material A in proportion, filtering by a filter, introducing into a high-pressure homogenizer preheated to 50 ℃, setting the flow rate to be 15L/h, homogenizing at the first stage of homogenizing pressure of 17MPa and the second stage of homogenizing pressure of 4 MPa; homogenizing, introducing into a constant-temperature jacket reaction kettle preheated to 40 ℃, stirring at the speed of 400r/min, adding a glacial acetic acid aqueous solution with the mass concentration of 10% while adjusting the pH of the material to 4, keeping the temperature for 20min, introducing cooling water until the material is cooled to 25 ℃, adding a sodium hydroxide aqueous solution with the mass concentration of 10% to adjust the pH to 10, adding a glutaraldehyde solution with the mass concentration of 25% and the volume of the mixed material of 0.5-2% after 20min for curing and finishing, stirring at the speed of 400r/min at the temperature of 25 ℃ and keeping the temperature for 30min, and quickly heating the constant-temperature jacket reaction kettle to 40 ℃ to obtain a mixed essential oil microcapsule emulsion;

step 2: preparation of deet microcapsule emulsion

Preparation of wall material C: putting Arabic gum into a constant-temperature jacket reaction kettle, adding distilled water with the volume 10 times that of the Arabic gum, heating to 90 ℃, stirring at the speed of 100r/min until the Arabic gum is dissolved and uniformly mixed, cooling to 45 ℃, and adding cold distilled water to prepare an Arabic gum emulsifier solution with the mass concentration of 3%;

preparation of core material B: putting gelatin in a constant-temperature jacket reaction kettle, adding distilled water with the volume 10 times that of the gelatin, heating to 80 ℃, stirring at the speed of 100r/min until the gelatin is dissolved and mixed uniformly, adding cold distilled water to prepare gelatin aqueous solution with the mass concentration of 3%, cooling to 50 ℃, adding Tween-20 and diethyltoluamide, stirring at the speed of 200r/min until a uniform emulsion is formed, cooling to 45 ℃, and continuously stirring at the speed of 80 r/min;

preparing a delphene microcapsule emulsion: mixing the wall material C and the core material B in proportion, filtering by a filter, introducing into a high-pressure homogenizer preheated to 50 ℃, and homogenizing at a flow rate of 10L/h and a homogenizing pressure of 17MPa in the first section and 4MPa in the second section; homogenizing, introducing into a constant-temperature jacket reaction kettle preheated to 40 ℃, stirring at the speed of 400r/min, adding a glacial acetic acid aqueous solution with the mass concentration of 10% while adjusting the pH of the material to 4, keeping the temperature for 20min, introducing cooling water until the material is cooled to 25 ℃, adding a sodium hydroxide aqueous solution with the mass concentration of 10% to adjust the pH to 10, adding a glutaraldehyde solution with the mass concentration of 25% and the volume of the mixed material of 0.5-2% after 20min for curing and finishing, stirring at the speed of 400r/min at 25 ℃ and keeping the temperature for 30min, and quickly heating the constant-temperature jacket reaction kettle to 40 ℃ to obtain a mosquito amine microcapsule emulsion;

and step 3: preparing mosquito-repellent microcapsule

And mixing the mixed essential oil microcapsule emulsion and the delphene microcapsule emulsion in proportion, and stirring uniformly at the speed of 400 r/min.

Technical Field

The invention relates to the technical field of daily chemical articles, in particular to a mosquito-repellent microcapsule and a preparation method thereof.

Background

The microcapsule technology is a technology of encapsulating a target material (core material) into a spherical microcapsule having a particle diameter of 1 to 5000 μm by a physical or chemical method using a film-forming material (wall material). The main purpose is to prolong the storage time of the core material, prevent the core material from being oxidized by air, cover the bad smell of the core material, improve the use effect and the like. The existing mosquito-repellent microcapsules only contain one mosquito-repellent component, such as mosquito-repellent amine microcapsules taking hydrophilic polyethylene as a wall material and mosquito-repellent amine as a core material, and mosquito-repellent ester microcapsules taking polyurethane, polyester, polyurea, polyamide or urea resin as a wall material and mosquito-repellent amine as a core material. It has limited mosquito repelling effect because it contains only one kind of mosquito repelling component. Moreover, most wall materials are synthetic polymer materials, so that the cost is high, and the wall materials do not have reproducibility and biodegradability, thereby being not in accordance with the sustainable development principle.

Disclosure of Invention

In order to solve the defects of the prior art, the invention provides a mosquito-repellent microcapsule and a preparation method thereof.

A mosquito-repellent microcapsule is prepared by mixing an essential oil microcapsule emulsion and a delphene microcapsule emulsion according to a mass ratio of 1 (0.5-1);

the mixed essential oil microcapsule emulsion is formed by mixing a wall material A, a wall material B and a core material A according to the mass ratio of (1-2) to (2-4); the wall material A is a gelatin emulsifier solution with the mass concentration of 1%; the wall material B is Arabic gum emulsifier solution with the mass concentration of 1%; the core material A comprises mixed plant essential oil and fat antioxidant butylated hydroxyanisole, wherein the mixed plant essential oil is formed by mixing surfactant Span-80, surfactant Tween-20, lavender essential oil and citronella essential oil according to the mass ratio of (0.5-1) to (1-2) to (2-2.5), and the butylated hydroxyanisole accounts for 0.5% of the mass of the mixed plant essential oil;

the deet microcapsule emulsion is formed by mixing wall material C and core material B according to the mass ratio of 0.5 (1.5-2), wherein the wall material C is a gum arabic emulsifier solution with the mass concentration of 3%; the core material B is formed by mixing gelatin aqueous solution, Tween-20 and deet according to the mass ratio of 0.5 (0.1-0.5) to 1, and the mass concentration of the gelatin aqueous solution is 3%.

The invention compounds the mixed essential oil microcapsule emulsion and the delphene amine microcapsule emulsion to prepare the compound mosquito repellent, which contains citronellal, citronellol, terpineol, limonene, delphene and other substances, and the combined action of the various substances has good mosquito repellent effect. Compared with the simple mixed liquid of the mosquito repellent amine and the natural plant essential oil extract, the mosquito repellent microcapsule provided by the invention has micropores on the surface, and the good slow release property of the mosquito repellent microcapsule is convenient for various mosquito repellent substances to be slowly released outwards, so that the heat stability is high; the microcapsule is prepared by compounding the gelatin and the Arabic gum, has the advantages of no toxicity, easy biodegradation and environmental friendliness, and is particularly suitable for wrapping nonpolar volatile oily liquid.

Preferably, the mosquito-repellent microcapsule is formed by mixing an essential oil microcapsule emulsion and a delphene microcapsule emulsion according to the mass ratio of 1: 0.5;

the mixed essential oil microcapsule emulsion is formed by mixing a wall material A, a wall material B and a core material A according to the mass ratio of 1:1: 2; the wall material A is a gelatin emulsifier solution with the mass concentration of 1%; the wall material B is Arabic gum emulsifier solution with the mass concentration of 1%; the core material A comprises mixed plant essential oil and butylated hydroxyanisole, wherein the mixed plant essential oil is formed by mixing Span-80, Tween-20, lavender essential oil and citronella essential oil according to the mass ratio of 1:2:2.5:2.5, and the butylated hydroxyanisole accounts for 0.5% of the mass of the mixed plant essential oil;

the deet microcapsule emulsion is formed by mixing a wall material C and a core material B according to the mass ratio of 0.5:1.5, wherein the wall material C is a arabic gum emulsifier solution with the mass concentration of 3%; the core material B is formed by mixing gelatin aqueous solution, Tween-20 and deet according to the mass ratio of 0.5:0.1:1, and the mass concentration of the gelatin aqueous solution is 3%.

The invention also provides a preparation method of the mosquito-repellent microcapsule, which comprises the following operation steps:

step 1: preparation of Mixed essential oil microcapsule emulsion

Preparation of wall material A: dissolving gelatin in distilled water to prepare gelatin emulsifier solution with mass concentration of 1%;

preparing a wall material B: dissolving Arabic gum in distilled water to prepare an Arabic gum emulsifier solution with the mass concentration of 1%;

preparation of core material A: mixing Span-80, Tween-20, lavender essential oil, citronella essential oil and butylated hydroxyanisole in proportion, stirring until the mixture is dissolved and uniformly mixed;

preparing mixed essential oil microcapsule emulsion: mixing the wall material A, the wall material B and the core material A in proportion, filtering, homogenizing and curing to obtain a mixed essential oil microcapsule emulsion;

step 2: preparation of deet microcapsule emulsion

Preparation of wall material C: adding distilled water into arabic gum to prepare a arabic gum emulsifier solution with the mass concentration of 3%;

preparation of core material B: adding water into gelatin to prepare gelatin water solution with mass concentration of 3%, adding Tween-20 and diethyltoluamide in proportion, and stirring to form uniform emulsion;

preparing a delphene microcapsule emulsion: mixing the wall material C and the core material B in proportion, filtering, homogenizing and curing to obtain the deet microcapsule emulsion;

and step 3: preparing mosquito-repellent microcapsule

And mixing the mixed essential oil microcapsule emulsion and the delphene microcapsule emulsion in a ratio and stirring uniformly.

Preferably, the method comprises the following operation steps:

step 1: preparation of Mixed essential oil microcapsule emulsion

Preparation of wall material A: putting gelatin in a constant temperature jacket reaction kettle, adding distilled water with the volume 5 times that of the gelatin, heating to 80 ℃, stirring at the speed of 100r/min until the gelatin is dissolved and uniformly mixed, cooling to 45 ℃, and adding cold distilled water to prepare gelatin emulsifier solution with the mass concentration of 1%;

preparing a wall material B: placing Arabic gum into a constant temperature jacket reaction kettle, adding distilled water with the volume 10 times that of Arabic gum, heating to 90 ℃, stirring at the speed of 100r/min until the Arabic gum is dissolved and uniformly mixed, cooling to 45 ℃, and adding cold distilled water to prepare Arabic gum emulsifier solution with the mass concentration of 1%;

preparation of core material A: mixing Span-80, Tween-20, lavender essential oil and citronella essential oil in proportion, adding 0.5% of dihydroxyanisole in mass of the mixture, then placing in a constant-temperature jacket reaction kettle, heating to 80 ℃, stirring at a speed of 100r/min until the mixture is dissolved and uniformly mixed, cooling to 45 ℃, and continuously stirring at a speed of 40r/min in the cooling process;

preparing mixed essential oil microcapsule emulsion: mixing the wall material A, the wall material B and the core material A in proportion, filtering by a filter, introducing into a high-pressure homogenizer preheated to 50 ℃, setting the flow rate to be 15L/h, homogenizing at the first stage of homogenizing pressure of 17MPa and the second stage of homogenizing pressure of 4 MPa; homogenizing, introducing into a constant-temperature jacket reaction kettle preheated to 40 ℃, stirring at the speed of 400r/min, adding a glacial acetic acid aqueous solution with the mass concentration of 10% while adjusting the pH of the material to 4, keeping the temperature for 20min, introducing cooling water until the material is cooled to 25 ℃, adding a sodium hydroxide aqueous solution with the mass concentration of 10% to adjust the pH to 10, adding a glutaraldehyde solution with the mass concentration of 25% and the volume of the mixed material of 0.5-2% after 20min for curing and finishing, stirring at the speed of 400r/min at the temperature of 25 ℃ and keeping the temperature for 30min, and quickly heating the constant-temperature jacket reaction kettle to 40 ℃ to obtain a mixed essential oil microcapsule emulsion;

step 2: preparation of deet microcapsule emulsion

Preparation of wall material C: putting Arabic gum into a constant-temperature jacket reaction kettle, adding distilled water with the volume 10 times that of the Arabic gum, heating to 90 ℃, stirring at the speed of 100r/min until the Arabic gum is dissolved and uniformly mixed, cooling to 45 ℃, and adding cold distilled water to prepare an Arabic gum emulsifier solution with the mass concentration of 3%;

preparation of core material B: putting gelatin in a constant-temperature jacket reaction kettle, adding distilled water with the volume 10 times that of the gelatin, heating to 80 ℃, stirring at the speed of 100r/min until the gelatin is dissolved and mixed uniformly, adding cold distilled water to prepare gelatin aqueous solution with the mass concentration of 3%, cooling to 50 ℃, adding Tween-20 and diethyltoluamide, stirring at the speed of 200r/min until a uniform emulsion is formed, cooling to 45 ℃, and continuously stirring at the speed of 80 r/min;

preparing a delphene microcapsule emulsion: mixing the wall material C and the core material B in proportion, filtering by a filter, introducing into a high-pressure homogenizer preheated to 50 ℃, and homogenizing at a flow rate of 10L/h and a homogenizing pressure of 17MPa in the first section and 4MPa in the second section; homogenizing, introducing into a constant-temperature jacket reaction kettle preheated to 40 ℃, stirring at the speed of 400r/min, adding a glacial acetic acid aqueous solution with the mass concentration of 10% while adjusting the pH of the material to 4, keeping the temperature for 20min, introducing cooling water until the material is cooled to 25 ℃, adding a sodium hydroxide aqueous solution with the mass concentration of 10% to adjust the pH to 10, adding a glutaraldehyde solution with the mass concentration of 25% and the volume of the mixed material of 0.5-2% after 20min for curing and finishing, stirring at the speed of 400r/min at 25 ℃ and keeping the temperature for 30min, and quickly heating the constant-temperature jacket reaction kettle to 40 ℃ to obtain a mosquito amine microcapsule emulsion;

and step 3: preparing mosquito-repellent microcapsule

And mixing the mixed essential oil microcapsule emulsion and the delphene microcapsule emulsion in proportion, and stirring uniformly at the speed of 400 r/min.

When the mixed essential oil microcapsule emulsion and the deet microcapsule emulsion are prepared, the release rate of the deet essential oil and the deet can be controlled by controlling the dosage of the cross-linking curing agent glutaraldehyde, the larger the dosage of the glutaraldehyde, the fewer the pore structures on the wall film, the slower the slow release rate, and vice versa. The invention utilizes the microcapsule technology to microencapsulate the diethyltoluamide and the anopheline essential oil, can not only fully exert the mosquito repelling effect of various mosquito repelling substances, but also play roles in prolonging the repelling time and reducing transdermal absorption by utilizing the characteristic of microcapsule controlled release, and is an effective method for improving the mosquito repelling activity and durability of the anopheline.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.