CN110592954A - Mosquito-repellent fabric finishing liquid, mosquito-repellent finishing fabric and preparation method thereof - Google Patents
Mosquito-repellent fabric finishing liquid, mosquito-repellent finishing fabric and preparation method thereof Download PDFInfo
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
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- D—TEXTILES; PAPER
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
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Abstract
The invention discloses a mosquito-repellent fabric finishing liquid, which is prepared from mosquito-repellent microcapsule emulsion and auxiliary agent by mixing (by weight ratio) 1: 5, the mosquito-repellent microcapsule emulsion is formed by mixing mixed essential oil microcapsule emulsion and delphene microcapsule emulsion; 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 diethyltoluamide. The fabric finished by the finishing liquid is resistant to water washing and rain, can effectively prevent mosquitoes from biting human bodies, is convenient to use and can avoid environmental pollution.
Description
Technical Field
The invention relates to the technical field of daily chemical articles, in particular to a mosquito-repellent fabric finishing liquid, a mosquito-repellent finishing fabric and a preparation method.
Background
The fabric treated by the insecticide can effectively prevent mosquito bites, which is a widely recommended mode of treating mosquito-transmitted diseases by WHO, and the mode can not only protect human health, but also avoid environmental pollution. The traditional mosquito-repellent fabric finishing liquid is mostly composed of a polymer integrated with an insecticide and an organic solvent, and the finishing liquid of the type has the following problems: 1. the release rate of the insecticide in the polymer matrix is not easy to control, and the matrix can be quickly exhausted by too fast releasing the insecticide, so that the insecticidal effect is influenced; 2. the use of the organic solvent causes pollution to the environment and is not environment-friendly; 3. has poor washing resistance and short lasting drug effect. How to design a mosquito repellent finishing liquid which is washable, environment-friendly, controllable in pesticide release speed and long in lasting pesticide effect is a technical problem to be solved at present.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a mosquito-repellent fabric finishing liquid, a mosquito-repellent fabric and a preparation method thereof.
A mosquito-repellent fabric finishing liquid is prepared from a mosquito-repellent microcapsule emulsion and an auxiliary agent according to the weight ratio of 1: 5 in a mass ratio;
the mosquito-repellent microcapsule emulsion 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 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 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, wherein the mass concentration of the gelatin aqueous solution is 3%;
the auxiliary agent is an aqueous solution containing the following components in percentage by mass: 0.5% of SDS, 1% of sodium laureth sulfate, 0.1% of cocamide MEA, 0.1% of guar hydroxypropyl trimethyl ammonium chloride and 5% of glycerol.
The invention compounds the mixed essential oil microcapsule emulsion and the delphene microcapsule emulsion to prepare the compound mosquito repellent agent, and then adds an auxiliary agent into the compound mosquito repellent agent to prepare the mosquito repellent finishing liquid. The compound mosquito repellent agent contains citronellal, citronellol, terpineol, limonene, deet and other substances, the common action of various substances has good repellent effect on mosquitoes, and the gelatin and the Arabic gum are compounded to prepare the capsule with the surface provided with micro-pores, so that various mosquito repellent substances can be slowly released outwards due to good slow release property, the thermal stability is high, and the material is non-toxic, easy to biodegrade and environment-friendly.
Compared with the prior art, the mosquito-repellent fabric finishing liquid provided by the invention has the following beneficial effects:
1. the insect repellent has broad-spectrum repellency, and can play a good repelling role and a long action time on various harmful insects;
2. the product is harmless to human body, has no irritation to skin, no allergy, and is resistant to water washing, rain and sweat, and does not react with sweat or reduce the effect due to sweat;
3. the smell is fragrant and easy to accept, and the clothes are not damaged;
4. the raw material source is rich, and the cost is low.
Preferably, the mosquito-repellent microcapsule emulsion is prepared 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 fabric finishing liquid, 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: preparation of mosquito-repellent microcapsule emulsion
Mixing the mixed essential oil microcapsule emulsion and the delphene microcapsule emulsion in proportion and stirring uniformly;
and 4, step 4: preparation of mosquito-repellent fabric finishing liquid
Adding the auxiliary agent into the mosquito-repellent microcapsule emulsion in proportion and uniformly stirring.
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;
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. After the mosquito repellent amine and the mosquito repellent plant essential oil are microencapsulated by the microcapsule technology, the mosquito repellent effect of various mosquito repellent substances can be fully exerted, the characteristics of controlled release of the microcapsules can be utilized to play the roles of prolonging the repellent time and reducing transdermal absorption, and the method is an effective method for improving the mosquito repellent activity and durability of the mosquito repellent;
and step 3: preparation of mosquito-repellent microcapsule emulsion
Mixing the mixed essential oil microcapsule emulsion and the delphene microcapsule emulsion in proportion, and stirring uniformly at the speed of 400 r/min;
and 4, step 4: preparation of mosquito-repellent fabric finishing liquid
Adding the auxiliary agent into the mosquito-repellent microcapsule emulsion in proportion, adjusting the temperature to 45 ℃, and stirring and mixing at the speed of 60r/min for 30 min.
The invention also provides a mosquito-repellent finishing fabric finished by adopting the mosquito-repellent finishing liquid.
The preparation method of the mosquito-repellent finishing fabric comprises the following operation steps: firstly, pretreating a fabric: immersing clothes in distilled water, adding NaOH accounting for 3-5% of the mass of the distilled water and SDS accounting for 3%, heating to 80 ℃, gently stirring for 1.5h at 50r/min, then spin-drying, washing twice with distilled water, and drying for later use; and then, performing mosquito repellent finishing on the fabric by adopting an impregnation method: placing the fabric into the mosquito repellent finishing liquid, wherein the volume of the mosquito repellent finishing liquid and the fabric is 5:1, then soaking for 1h at 45 ℃, stirring gently at the speed of 60r/min during soaking, dehydrating after soaking, and drying at low temperature of 60 ℃.
Drawings
FIG. 1 is an SEM image of a pretreated fabric of example 1;
fig. 2 is an SEM image of the fabric finished with the mosquito repellent finish in example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious 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.
Example 1
A mosquito-repellent fabric finishing liquid is prepared from a mosquito-repellent microcapsule emulsion and an auxiliary agent according to the weight ratio of 1: 5 in a mass ratio;
the mosquito-repellent microcapsule emulsion is formed by mixing mixed essential oil microcapsule emulsion and delphene microcapsule emulsion according to the mass ratio of 1: 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 1.5:1: 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 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 0.8:1:2.5:2.2, 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 0.5:0.5:1, and the mass concentration of the gelatin aqueous solution is 3%;
the auxiliary agent is an aqueous solution containing the following components in percentage by mass: 0.5% of SDS, 1% of sodium laureth sulfate, 0.1% of cocamide MEA, 0.1% of guar hydroxypropyl trimethyl ammonium chloride and 5% of glycerol.
The preparation method of the mosquito-repellent fabric finishing liquid comprises the following 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: preparation of mosquito-repellent microcapsule emulsion
Mixing the mixed essential oil microcapsule emulsion and the delphene microcapsule emulsion in proportion, and stirring uniformly at the speed of 400 r/min;
and 4, step 4: preparation of mosquito-repellent fabric finishing liquid
Adding the auxiliary agent into the mosquito-repellent microcapsule emulsion in proportion, adjusting the temperature to 45 ℃, and stirring and mixing at the speed of 60r/min for 30 min.
The mosquito-repellent finishing liquid is used for finishing fabrics (pure cotton cloth with the specification of 10cm multiplied by 10cm is taken as a test object), and the specific operation steps are as follows: firstly, pretreating a fabric: immersing clothes in distilled water, adding NaOH accounting for 3% of the mass of the distilled water and SDS accounting for 3% of the mass of the distilled water, heating to 80 ℃, gently stirring for 1.5h at 50r/min, then spin-drying, washing twice by using the distilled water, and drying for later use; and then, performing mosquito repellent finishing on the fabric by adopting an impregnation method: placing the fabric into the mosquito repellent finishing liquid, wherein the volume of the mosquito repellent finishing liquid and the fabric is 5:1, then soaking for 1h at 45 ℃, stirring gently at the speed of 60r/min during soaking, dehydrating after soaking, and drying at low temperature of 60 ℃.
Example 2
The preparation method of the mosquito-repellent fabric finishing liquid is the same as that of the embodiment 1, and the mosquito-repellent fabric finishing liquid is prepared by mixing the mosquito-repellent microcapsule emulsion and an auxiliary agent according to the ratio of 1: 5 in a mass ratio; the mosquito-repellent microcapsule emulsion is formed by mixing mixed essential oil microcapsule emulsion and delphene microcapsule emulsion according to the mass ratio of 1: 0.8;
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: 3; 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 0.5:2:2.2:2, 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 0.5:2, 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 0.5:0.8:1, and the mass concentration of the gelatin aqueous solution is 3%;
the auxiliary agent is an aqueous solution containing the following components in percentage by mass: 0.5% of SDS, 1% of sodium laureth sulfate, 0.1% of cocamide MEA, 0.1% of guar hydroxypropyl trimethyl ammonium chloride and 5% of glycerol.
The mosquito-repellent finishing liquid is used for finishing fabrics (pure cotton cloth with the specification of 10cm multiplied by 10cm is taken as a test object), and the specific operation steps are as follows: firstly, pretreating a fabric: immersing clothes in distilled water, adding NaOH accounting for 4% of the mass of the distilled water and SDS accounting for 3% of the mass of the distilled water, heating to 80 ℃, gently stirring for 1.5h at 50r/min, then spin-drying, washing twice by using the distilled water, and drying for later use; and then, performing mosquito repellent finishing on the fabric by adopting an impregnation method: placing the fabric into the mosquito repellent finishing liquid, wherein the volume of the mosquito repellent finishing liquid and the fabric is 5:1, then soaking for 1h at 45 ℃, stirring gently at the speed of 60r/min during soaking, dehydrating after soaking, and drying at low temperature of 60 ℃.
Example 3
The preparation method of the mosquito-repellent fabric finishing liquid is the same as that of the embodiment 1, and the mosquito-repellent fabric finishing liquid is prepared by mixing the mosquito-repellent microcapsule emulsion and an auxiliary agent according to the ratio of 1: 5 in a mass ratio; the mosquito-repellent microcapsule emulsion is formed by mixing mixed essential oil microcapsule emulsion and 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 2:1.5: 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 1:1.5:2:2.5, 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 0.5:1.8, 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 auxiliary agent is an aqueous solution containing the following components in percentage by mass: 0.5% of SDS, 1% of sodium laureth sulfate, 0.1% of cocamide MEA, 0.1% of guar hydroxypropyl trimethyl ammonium chloride and 5% of glycerol.
The mosquito-repellent finishing liquid is used for finishing fabrics (pure cotton cloth with the specification of 10cm multiplied by 10cm is taken as a test object), and the specific operation steps are as follows: firstly, pretreating a fabric: immersing clothes in distilled water, adding NaOH accounting for 5% of the mass of the distilled water and SDS accounting for 3% of the mass of the distilled water, heating to 80 ℃, gently stirring for 1.5h at 50r/min, then spin-drying, washing twice by using the distilled water, and drying for later use; and then, performing mosquito repellent finishing on the fabric by adopting an impregnation method: placing the fabric into the mosquito repellent finishing liquid, wherein the volume of the mosquito repellent finishing liquid and the fabric is 5:1, then soaking for 1h at 45 ℃, stirring gently at the speed of 60r/min during soaking, dehydrating after soaking, and drying at low temperature of 60 ℃.
Example 4
The preparation method of the mosquito-repellent fabric finishing liquid is the same as that of the embodiment 1, and the mosquito-repellent fabric finishing liquid is prepared by mixing the mosquito-repellent microcapsule emulsion and an auxiliary agent according to the ratio of 1: 5 in a mass ratio; the mosquito-repellent microcapsule emulsion is formed by mixing mixed essential oil microcapsule emulsion and 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 auxiliary agent is an aqueous solution containing the following components in percentage by mass: 0.5% of SDS, 1% of sodium laureth sulfate, 0.1% of cocamide MEA, 0.1% of guar hydroxypropyl trimethyl ammonium chloride and 5% of glycerol.
The mosquito-repellent finishing liquid is used for finishing fabrics (pure cotton cloth with the specification of 10cm multiplied by 10cm is taken as a test object), and the specific operation steps are as follows: firstly, pretreating a fabric: immersing clothes in distilled water, adding NaOH accounting for 4% of the mass of the distilled water and SDS accounting for 3% of the mass of the distilled water, heating to 80 ℃, gently stirring for 1.5h at 50r/min, then spin-drying, washing twice by using the distilled water, and drying for later use; and then, performing mosquito repellent finishing on the fabric by adopting an impregnation method: placing the fabric into the mosquito repellent finishing liquid, wherein the volume of the mosquito repellent finishing liquid and the fabric is 5:1, then soaking for 1h at 45 ℃, stirring gently at the speed of 60r/min during soaking, dehydrating after soaking, and drying at low temperature of 60 ℃.
Measurement of appearance form:
the fabric pretreated in example 1 and the fabric finished with the mosquito repellent fabric finishing liquid were each cut into 6mm × 6mm pieces, adhered to a silicon wafer with a conductive adhesive, subjected to vacuum gold spraying treatment, and observed on a Scanning Electron Microscope (SEM). Fig. 1 shows the pretreated fabric, and fig. 2 shows the fabric finished with the mosquito repellent finishing liquid. As can be seen by careful observation, the dried mixed essential oil microcapsules have two structures, one is a small spherical unit with the diameter of 10-90 mu m, and the other is a coagulated complex formed by aggregating the small spherical units with the diameter of 90-800 mu m.
Testing the mosquito repelling effect:
in view of the fact that no test standard of mosquito repellent liquid exists in China at present, the test is carried out by referring to GB 13917.3-1992, pesticide indoor efficacy test method for pesticide registration hygiene, small aerosol and aerosol tablet test method, GB 13917.1-1992, pesticide indoor efficacy test method for rural registration hygiene, propellant indoor efficacy test method and GB/T17322.10-1998, pesticide indoor efficacy evaluation for pesticide registration hygiene, repellent. The mosquitoes used in the tests were all female Anopheles sinensis (Anopheles sinensis) caught in the field, and were raised temporarily in dark room cages at 25 ℃ and a relative humidity RH of 70 since the catching. 100 female anopheles sinensis are placed into an organic glass box with the specification of 60cm multiplied by 60cm, the upper surface of the organic glass box is provided with an opening and is covered by a nylon gauze, and the nylon gauze is provided with an opening for taking and placing the mosquitoes and 6 hand stretching openings. The testers (all women of 20-40 ages and all B blood types) wear disposable latex gloves with openings of 6cm x 6cm on the backs of the gloves. 1 tester (the test group in which the tester is located is recorded as a blank test) directly extends hands into the organic glass box from the extending mouths without any treatment, and the other 5 testers wear gloves and then cover the openings of the gloves with fabrics which are only subjected to pretreatment and mosquito repellent finishing fabrics prepared in examples 1-4 respectively. Each tester places the hands in the perspex box for 10min, counts the number of mosquitoes falling at the opening of the back of the hand and repeats 5 times to take an average value, with the test interval of each time being at least 1 h. And (4) comparing with a blank test, and calculating the mosquito repelling rate (the mosquito repelling rate is (blank test mosquito number-specific mosquito number)/blank test mosquito number).
TABLE 1 comparison of mosquito repellent effects in different ways
Obviously, the fabric finished by the mosquito-repellent fabric finishing liquid provided by the invention has a good mosquito-repellent effect, and the mosquito-repellent rate is at least 93%. And the mosquito repellent rate of over 85 percent can still be kept after 24 hours of retesting.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. A mosquito repellent fabric finishing liquid is characterized in that: the mosquito-repellent fabric finishing liquid is prepared from a mosquito-repellent microcapsule emulsion and an auxiliary agent according to the weight ratio of 1: 5 in a mass ratio;
the mosquito-repellent microcapsule emulsion 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%;
the auxiliary agent is an aqueous solution containing the following components in percentage by mass: 0.5% of SDS, 1% of sodium laureth sulfate, 0.1% of cocamide MEA, 0.1% of guar hydroxypropyl trimethyl ammonium chloride and 5% of glycerol.
2. A mosquito repellent fabric finishing liquid according to claim 1, characterized in that: the mosquito-repellent microcapsule emulsion is formed by mixing mixed essential oil microcapsule emulsion and 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 fabric finishing liquid as claimed in claim 1 or 2, which is 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: preparation of mosquito-repellent microcapsule emulsion
Mixing the mixed essential oil microcapsule emulsion and the delphene microcapsule emulsion in proportion and then uniformly stirring;
and 4, step 4: preparation of mosquito-repellent fabric finishing liquid
And adding the auxiliary agent into the mosquito-repellent microcapsule emulsion in proportion and uniformly stirring.
4. A method for preparing mosquito repellent fabric finishing liquid according to claim 3, which is characterized in that: 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: preparation of mosquito-repellent microcapsule emulsion
Mixing the mixed essential oil microcapsule emulsion and the delphene microcapsule emulsion in proportion and then uniformly stirring at the speed of 400 r/min;
and 4, step 4: preparation of mosquito-repellent fabric finishing liquid
And adding the auxiliary agent into the mosquito-repellent microcapsule emulsion in proportion, adjusting the temperature to 45 ℃, and stirring and mixing at the speed of 60r/min for 30 min.
5. A mosquito repellent finish fabric is characterized in that: finishing by using the mosquito-repellent finishing liquid as claimed in claim 1 or 2.
6. A method for preparing the mosquito-repellent finishing fabric according to claim 5, which is characterized by comprising the following steps: the method comprises the following operation steps:
firstly, pretreating a fabric: immersing clothes in distilled water, adding NaOH accounting for 3-5% of the mass of the distilled water and SDS accounting for 3%, heating to 80 ℃, gently stirring for 1.5h at 50r/min, then spin-drying, washing twice with distilled water, and drying for later use;
and then, performing mosquito repellent finishing on the fabric by adopting an impregnation method: placing a fabric into the mosquito repellent finishing liquid, wherein the volume of the mosquito repellent finishing liquid and the fabric is 5:1, then soaking for 1h at 45 ℃, stirring gently at the speed of 60r/min during soaking, dehydrating after soaking, and drying at low temperature of 60 ℃.
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