CN115787295A - Fragrant fabric and preparation method thereof - Google Patents
Fragrant fabric and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a fragrant fabric and a preparation method thereof, and relates to the technical field of fabrics. The invention firstly uses the mixture of essence, urea and 4- (4, 6-dichloro-1, 3, 5-triazine-2-yl) benzaldehyde to react to prepare the composite fragrant microcapsule; then, carrying out mixed reaction on the dihydroxybenzidine, the 3-butenyl isothiocyanate and the compound fragrance type microcapsule to prepare a modified compound fragrance type microcapsule; then mixing and reacting the modified composite fragrant microcapsule and the carboxylated cotton fiber to obtain fragrant cotton fiber; after the fragrant cotton fiber is co-twisted and woven into the cotton fabric, the fragrant cotton fiber is sequentially treated by benzonitrile, p-chlorophenyl dicyandiamide and 4-aminobutyltriethoxysilane to obtain the fragrant fabric. The fragrant fabric prepared by the invention has good aging resistance, antibacterial property and wear resistance.
Description
Technical Field
The invention relates to the technical field of fabrics, in particular to a fragrant fabric and a preparation method thereof.
Background
With the continuous improvement of the physical life and mental life level of people, comfortable and healthy living environment is more and more favored by people. The fragrance has the functions of specially optimizing the environment and optimizing the personal image, and has more and more close relationship with the daily life of people. It can affect the mood of a person and even produce physiological effects on the person. The product can be used for life and work in aromatic environment, and has effects of relieving fatigue, joyful body and mind, and improving work efficiency.
In recent years, aromatic textiles have exhibited vigorous activity. The fabric processed by the special processing is refreshing, such as spring bathing, and has high added value; opens up a new place for realizing the diversification of textiles in China. However, the existing aromatic textile is basically made by processing the fabric by adopting the fragrance auxiliary agent, the fragrance durability of the fabric is poor, and other properties of the fabric are also reduced, such as ageing resistance and wear resistance, and bacteria are easy to breed; therefore, in order to meet the requirements of customers, the fragrant fabric with good ageing resistance, antibacterial property and wear resistance is designed and developed, and can be used for manufacturing various toys, children clothes and bedding.
Disclosure of Invention
The invention aims to provide a fragrant fabric and a preparation method thereof, and aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the fragrant fabric is prepared by sequentially treating benzonitrile-p-chlorophenyl dicyandiamide and 4-aminobutyltriethoxysilane after fragrant cotton fibers are co-twisted and woven into a cotton fabric.
Furthermore, the fragrant cotton fiber is prepared by mixing and reacting carboxylated cotton fiber and modified composite fragrant microcapsules.
Furthermore, the modified complex fragrance type microcapsule is prepared by mixing and reacting dihydroxybenzidine, 3-butenyl isothiocyanate and the complex fragrance type microcapsule.
Furthermore, the composite fragrance type microcapsule is prepared by mixing and reacting essence, urea and 4- (4, 6-dichloro-1, 3, 5-triazine-2-yl) benzaldehyde.
Further, the preparation method of the fragrant fabric comprises the following preparation steps:
(1) Mixing essence, glyceryl monostearate and 10-20% of ethanol solution according to the mass ratio of 1:0.1:20 to 1:0.3:30, stirring at 7000-9000 r/min for 10-20 min to prepare a mixed solution A; urea and 4- (4, 6-dichloro-1, 3, 5-triazin-2-yl) benzaldehyde are mixed in a molar ratio of 1: 1.5-1: 2, stirring for 1-2 h at the speed of 80-100 r/min, adding sodium hydroxide to adjust the pH value to 7.8-8.2, heating to 70-80 ℃, and continuously stirring for 0.5-1.5 h to prepare a mixed solution B; mixing the mixed solution A and the mixed solution B according to a mass ratio of 1:1 to 1:2, continuously and slowly adding ammonium chloride until the pH value is controlled to be 1.5-2.0 after 3-4 h, and stopping adding the ammonium chloride; heating to 60-70 ℃, standing for 1-3 h, adding sodium hydroxide to adjust the pH value to 6.8-7.2, centrifuging for 70-80 min at 800-1000 r/min, and drying at 30-40 ℃ for 4-6 h to obtain the composite fragrance type microcapsule;
(2) Mixing the composite fragrant microcapsule and the dihydroxy benzidine according to the mass ratio of 1:5 to 1:6, mixing, stirring for 10-20 min at 20-30 r/min, adding anhydrous aluminum trichloride with the mass of 0.1-0.2 time of that of the compound odor type microcapsule, heating to 88-92 ℃, continuously stirring for 2-4 h, adding 3-butenyl isothiocyanate with the mass of 3-5 times of that of the compound odor type microcapsule, continuously stirring for 2-4 h, centrifuging for 70-80 min at 800-1000 r/min, and drying for 4-6 h at 30-40 ℃ to obtain the modified compound odor type microcapsule; mixing modified composite fragrant microcapsules, carboxylated cotton fibers and deionized water according to a mass ratio of 1:20:50 to 1:30:60, mixing, carrying out ultrasonic oscillation for 20-30 min at 4-6 kHz, adding stannous oxide with the mass 0.1-0.3 time of that of the modified composite fragrance type microcapsule, heating to 60-70 ℃, stirring for 2-4 h at 360-380 r/min, filtering, and drying for 2-4 h at 30-40 ℃ under 100-200 Pa to obtain fragrance type cotton fiber; the fragrant cotton fiber is twisted and woven together to obtain the fabric with the gram weight of 400-420 g/m 2 The cotton fabric of (2);
(3) Cotton fabric, benzonitrile p-chlorophenyl dicyandiamide, sodium hydride and dimethyl sulfoxide are mixed according to a mass ratio of 1:10:0.6:20 to 1:20:0.8:30, stirring for 20-30 min at 80-100 r/min, heating to 80-100 ℃, adding a mixture A with the mass of 0.1-0.3 time of that of the cotton fabric, stirring for 2-5 h at 80-100 r/min, fishing out, cooling to room temperature, adding 4-aminobutyltriethoxysilane with the mass of 8-10 times of that of the cotton fabric, stirring for 10-20 min at 300-400 r/min, adding a hydrochloric acid solution with the mass fraction of 10-20% and the mass fraction of 0.1-0.3 time of that of the cotton fabric, continuously stirring for 75-85 min in an oil bath at 40-50 ℃, adding ammonia water with the mass fraction of 10-20% to adjust the pH to 7-8, waiting for 24-28 h, fishing out, adding isopropanol with the mass fraction of 8-10 times of the cotton fabric, heating to 98-102 ℃, dripping the hydrochloric acid solution with the mass fraction of 32-40% at 20-30 ml/min, continuously fishing out for 6-8 h, pa, and drying for 6-8 h at 30-40 ℃ and 100-200 h to obtain the fragrant fabric.
Further, the essence in the step (1) is prepared by mixing lavender essence and one of lemon essence, mint essence, jasmine essence and camellia essence.
Further, the preparation method of benzonitrile and p-chlorophenyl dicyandiamide in the step (3) comprises the following steps: 2- (chloromethyl) benzonitrile and N-p-chlorophenyldicyandiamide were reacted in a molar ratio of 1:1 to 1:1.1, stirring for 3-5 min at 20-26 r/min, adding anhydrous aluminum trichloride with the mass of 0.1-0.2 time of that of 2- (chloromethyl) benzonitrile, heating to 88-92 ℃, continuously stirring for 2-4 h, stirring and cleaning with pure water, extracting with toluene, drying at 30-40 ℃ under 50-100 Pa for 6-8 h, and obtaining the benzonitrile p-chlorophenyl dicyandiamide.
Further, the mixture A in the step (3) is prepared by mixing the raw materials of the imino ketone iodide, the palladium chloride and the tetrabutyl ammonium bromide according to a molar ratio of 1:18:3 to 1:22:5 mixing to obtain the final product.
Compared with the prior art, the invention has the following beneficial effects:
the fragrant fabric prepared by the invention is prepared by sequentially treating benzonitrile-p-chlorophenyl dicyandiamide and 4-aminobutyltriethoxysilane after fragrant cotton fibers are co-twisted and woven into a cotton fabric; has good aging resistance, antibacterial property and wear resistance.
Firstly, mixing essence, urea and 4- (4, 6-dichloro-1, 3, 5-triazine-2-yl) benzaldehyde for reaction to prepare a composite fragrant microcapsule; the chlorine groups on the compound fragrant microcapsules and the benzene rings on the dihydroxybenzidine are subjected to substitution reaction to generate triazine compounds, so that the modified compound fragrant microcapsules have the anti-aging effect; diphenylamine on the dihydroxybiphenylamine reacts with butene on the 3-butenyl isothiocyanate to form hindered amine, so that the anti-aging effect of the modified compound aromatic microcapsule is enhanced; the hydroxyl on the modified composite fragrant microcapsule reacts with the carboxyl on the carboxylated cotton fiber, and the modified composite fragrant microcapsule is stably grafted on the cotton fiber, so that the fragrant cotton fiber has an anti-aging effect and emits fragrance.
Secondly, the benzonitrile on the p-chlorophenyl dicyandiamide reacts with the isothiocyanate on the fragrant cotton fiber to generate benzothiophene, so that the fragrant fabric has an antibacterial effect; 4-aminobutyltriethoxysilane is subjected to ethoxylation removal to form a silicon dioxide gel layer which is firmly wrapped on the surface of the fragrant cotton fiber, so that defects such as cracks and holes on the surface of the fragrant cotton fiber are filled, the surface of the fragrant cotton fiber is smooth, and the wear resistance of the fragrant fabric is enhanced; the amino on the 4-aminobutyltriethoxysilane reacts with dicyandiamide on the benzonitrile-p-chlorophenyldicyandiamide to generate a biguanide compound, and the antibacterial property of the fragrant fabric is further enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for detailed description, and the method for testing each index of the fragrant fabric manufactured in the following examples is as follows:
aging resistance: the fragrant fabrics prepared in the same quality examples and comparative examples are placed in the same sunlight and natural environment for 30 days, and then the tearing strength is tested according to the GB/T3917 standard method.
And (3) antibacterial property: the fragrance type fabric prepared in the same quality example and the comparative example is tested for antibacterial property according to the GB/T20944 standard method.
Wear resistance: taking the fragrant fabric prepared in the same quality example and the comparative example, testing the wear resistance and evaluating the appearance change according to a GB/T21196 standard method.
Example 1
(1) Mixing lavender essence, glyceryl monostearate and an ethanol solution with the mass fraction of 10% according to the mass ratio of 1:0.1:20, stirring at 7000r/min for 10min to prepare a mixed solution A; urea and 4- (4, 6-dichloro-1, 3, 5-triazin-2-yl) benzaldehyde are mixed in a molar ratio of 1:1.5, stirring for 1h at the speed of 80r/min, adding sodium hydroxide to regulate the pH value to 7.8, heating to 70 ℃, and continuously stirring for 0.5h to prepare a mixed solution B; mixing the mixed solution A and the mixed solution B according to a mass ratio of 1:1, continuously and slowly adding ammonium chloride until the pH value is controlled to be 1.5 after 3 hours, and stopping adding the ammonium chloride; heating to 60 ℃, standing for 1h, adding sodium hydroxide to adjust the pH value to 6.8, centrifuging at 800r/min for 70min, and drying at 30 ℃ for 4h to obtain the composite fragrance type microcapsule;
(2) Mixing the composite fragrant microcapsule and the dihydroxy benzidine according to the mass ratio of 1:5, mixing, stirring for 10min at 20r/min, adding anhydrous aluminum trichloride of which the mass is 0.1 time that of the compound fragrance type microcapsule, heating to 88 ℃, continuing to stir for 2h, adding 3-butenyl isothiocyanate of which the mass is 3 times that of the compound fragrance type microcapsule, continuing to stir for 2, centrifuging for 70min at 800r/min, and drying for 4h at 30 ℃ to obtain the modified compound fragrance type microcapsule; mixing modified composite fragrant microcapsules, carboxylated cotton fibers and deionized water according to a mass ratio of 1:20: mixing 50 parts of the raw materials, ultrasonically shaking at 4kHz for 20min, adding stannous oxide with the mass being 0.1 time that of the modified composite fragrant microcapsule, heating to 60 ℃, stirring for 2h at 360r/min, filtering, and drying at 30 ℃ and 100Pa for 2h to obtain fragrant cotton fiber; the fragrant cotton fiber is twisted and woven together to obtain the fabric with the gram weight of 400g/m 2 The cotton fabric of (1);
(3) 2- (chloromethyl) benzonitrile and N-p-chlorophenyldicyandiamide were reacted in a molar ratio of 1:1, stirring for 3min at 20r/min, adding anhydrous aluminum trichloride of which the mass is 0.1 time that of 2- (chloromethyl) benzonitrile, heating to 88 ℃, continuously stirring for 2h, stirring and cleaning with pure water, extracting with toluene, and drying at 30 ℃ and 50Pa for 6h to obtain benzonitrile-p-chlorophenyl dicyandiamide; cotton fabric, benzonitrile p-chlorophenyl dicyandiamide, sodium hydride and dimethyl sulfoxide are mixed according to a mass ratio of 1:10:0.6:20, stirring for 20min at the speed of 80r/min, heating to 80 ℃, adding a mixture A with the weight 0.1 time that of the cotton fabric, wherein the molar ratio of the imino ketone iodide, the palladium chloride and the tetrabutyl ammonium bromide in the mixture A is 1:18:3, stirring for 2 hours at the speed of 80r/min, fishing out, cooling to room temperature, adding 4-aminobutyltriethoxysilane 8 times the mass of the cotton fabric, stirring for 10-20 minutes at the speed of 300r/min, adding a hydrochloric acid solution with the mass fraction of 10% 0.1 times the mass of the cotton fabric, continuously stirring for 75 minutes in an oil bath at the temperature of 40 ℃, adding ammonia water with the mass fraction of 10% to adjust the pH to 7, waiting for 24 hours, fishing out, adding isopropanol with the mass fraction of 8 times the mass of the cotton fabric, heating to 98 ℃, dripping a hydrochloric acid solution with the mass fraction of 32% at the speed of 20ml/min, continuing for 6 hours, fishing out, and drying for 6 hours at the temperature of 30-40 ℃ and under the pressure of 100Pa to obtain the fragrant fabric.
Example 2
(1) Mixing lavender essence, glyceryl monostearate and 15% by mass of ethanol solution according to a mass ratio of 1:0.2:25, stirring for 15min at the speed of 800r/min to prepare a mixed solution A; urea and 4- (4, 6-dichloro-1, 3, 5-triazin-2-yl) benzaldehyde are mixed in a molar ratio of 1:1.75, stirring for 1.5h at 90r/min, adding sodium hydroxide to adjust the pH value to 8, heating to 75 ℃, and continuing stirring for 1h to prepare a mixed solution B; mixing the mixed solution A and the mixed solution B according to the mass ratio of 1:1.5, continuously and slowly adding ammonium chloride until the pH value is controlled to be 1.75 after 3.5 hours, and stopping adding the ammonium chloride; heating to 65 ℃, standing for 2h, adding sodium hydroxide to adjust the pH value to 7, centrifuging for 75min at 900r/min, and drying at 35 ℃ for 5h to obtain the composite fragrant microcapsule;
(2) Mixing the composite fragrant microcapsule and the dihydroxy benzidine according to the mass ratio of 1:5.5, stirring for 15min at 25r/min, adding anhydrous aluminum trichloride of which the mass is 0.15 time that of the composite odor type microcapsule, heating to 90 ℃, continuing to stir for 3h, adding 3-butenyl isothiocyanate of which the mass is 4 times that of the composite odor type microcapsule, continuing to stir for 3h, centrifuging for 75min at 900r/min, and drying for 5h at 35 ℃ to obtain the modified composite odor type microcapsule; mixing modified composite fragrant microcapsules, carboxylated cotton fibers and deionized water according to a mass ratio of 1:25:55, mixing, ultrasonically shaking at 5kHz for 25min, adding stannous oxide with the mass 0.2 time that of the modified composite fragrant microcapsule, heating to 65 ℃, stirring for 3h at 370r/min, filtering, and drying at 35 ℃ and 150Pa for 3h to obtain fragrant cotton fiber; will-fragrance typeAfter cotton fibers are twisted and woven together, the gram weight of the obtained fabric is 410g/m 2 The cotton fabric of (2);
(3) 2- (chloromethyl) benzonitrile and N-p-chlorophenyldicyandiamide were reacted in a molar ratio of 1:05, stirring for 4min at 23r/min, adding anhydrous aluminum trichloride of which the mass is 0.15 time that of 2- (chloromethyl) benzonitrile, heating to 90 ℃, continuously stirring for 3h, stirring and cleaning with pure water, extracting with toluene, and drying at 35 ℃ and 75Pa for 7h to obtain benzonitrile p-chlorophenyl dicyandiamide; cotton fabric, benzonitrile p-chlorophenyl dicyandiamide, sodium hydride and dimethyl sulfoxide are mixed according to a mass ratio of 1:15:0.7:25, stirring for 25min at the speed of 90r/min, heating to 90 ℃, adding a mixture A with the mass of 0.2 time that of the cotton fabric, wherein the molar ratio of the imino ketone iodide, the palladium chloride and the tetrabutyl ammonium bromide in the mixture A is 1:20: and 4, stirring for 3.5h at 90r/min, fishing out, cooling to room temperature, adding 4-aminobutyltriethoxysilane 9 times the mass of the cotton fabric, stirring for 15min at 350r/min, adding a hydrochloric acid solution with the mass fraction of 15% 0.2 times the mass of the cotton fabric, continuously stirring for 80min in an oil bath at 45 ℃, adding ammonia water with the mass fraction of 15% to adjust the pH to 7.5, waiting for 26h, fishing out, adding isopropanol with the mass fraction of 9 times the mass of the cotton fabric, heating to 100 ℃, dripping a hydrochloric acid solution with the mass fraction of 36% at 25ml/min, continuing for 7h, fishing out, and drying for 7h at 35 ℃ and 150Pa to obtain the fragrant fabric.
Example 3
(1) Mixing lavender essence, glyceryl monostearate and 20% ethanol solution in a mass ratio of 1:0.3:30, stirring for 20min at 9000r/min to prepare a mixed solution A; urea and 4- (4, 6-dichloro-1, 3, 5-triazin-2-yl) benzaldehyde are mixed in a molar ratio of 1:2, stirring for 2 hours at the speed of 100r/min, adding sodium hydroxide to regulate the pH value to 8.2, heating to 80 ℃, and continuously stirring for 1.5 hours to prepare a mixed solution B; mixing the mixed solution A and the mixed solution B according to a mass ratio of 1:2, continuously and slowly adding ammonium chloride until the pH value is controlled to be 2.0 after 4 hours, and stopping adding the ammonium chloride; heating to 70 deg.C, standing for 3h, adding sodium hydroxide to adjust pH to 7.2, centrifuging at 1000r/min for 80min, and drying at 40 deg.C for 6h to obtain composite fragrant microcapsule;
(2) Mixing the composite fragrant microcapsule and dihydroxybenzidineThe amount ratio is 1:6, mixing, stirring for 20min at 30r/min, adding anhydrous aluminum trichloride of which the mass is 0.2 time that of the compound fragrance type microcapsule, heating to 92 ℃, continuing to stir for 4h, adding 3-butenyl isothiocyanate of which the mass is 5 times that of the compound fragrance type microcapsule, continuing to stir for 4h, centrifuging for 80min at 1000r/min, and drying for 6h at 40 ℃ to obtain the modified compound fragrance type microcapsule; mixing modified composite fragrant microcapsules, carboxylated cotton fibers and deionized water according to a mass ratio of 1:30:60, mixing, ultrasonically shaking at 6kHz for 30min, adding stannous oxide with the mass 0.3 time that of the modified composite fragrant microcapsule, heating to 70 ℃, stirring for 4h at 380r/min, filtering, and drying for 4h at 40 ℃ and 200Pa to obtain fragrant cotton fiber; the fragrant cotton fiber is co-twisted and woven to obtain the fabric with the gram weight of 420g/m 2 The cotton fabric of (2);
(3) 2- (chloromethyl) benzonitrile and N-p-chlorophenyldicyandiamide were reacted in a molar ratio of 1:1.1, stirring for 5min at 26r/min, adding anhydrous aluminum trichloride of which the mass is 0.2 time that of 2- (chloromethyl) benzonitrile, heating to 92 ℃, continuously stirring for 4h, stirring and cleaning with pure water, extracting with toluene, and drying at 40 ℃ under 100Pa for 8h to obtain benzonitrile-p-chlorophenyl dicyandiamide; cotton fabric, benzonitrile p-chlorophenyl dicyandiamide, sodium hydride and dimethyl sulfoxide are mixed according to a mass ratio of 1:20:0.8:30, stirring for 30min at the speed of 100r/min, heating to 100 ℃, adding a mixture A with the mass of 0.3 time that of the cotton fabric, wherein the molar ratio of the imino ketone iodide, the palladium chloride and the tetrabutyl ammonium bromide in the mixture A is 1:22:5, stirring for 5 hours at a speed of 100r/min, fishing out, cooling to room temperature, adding 4-aminobutyltriethoxysilane which is 10 times of the mass of the cotton fabric, stirring for 20 minutes at a speed of 400r/min, adding a hydrochloric acid solution which is 20% of the mass of the cotton fabric and is 0.3 times of the mass of the cotton fabric, continuously stirring for 85 minutes in an oil bath at 50 ℃, adding ammonia water with the mass fraction of 20% to adjust the pH value to 8, fishing out after 28 hours, adding isopropanol with the mass fraction of 10 times of the mass of the cotton fabric, heating to 102 ℃, dripping a hydrochloric acid solution with the mass fraction of 40% at a speed of 30ml/min, continuing for 8 hours, fishing out, and drying for 8 hours at a temperature of 40 ℃ and 200Pa to obtain the fragrant fabric.
Comparative example 1
(1) Mixing lavender essence, glyceryl monostearate and 15% by mass of an ethanol solution according to a mass ratio of 1:0.2:25, stirring for 15min at the speed of 800r/min to prepare a mixed solution A; mixing urea and benzaldehyde according to a molar ratio of 1:1.75, stirring for 1.5h at 90r/min, adding sodium hydroxide to adjust the pH value to 8, heating to 75 ℃, and continuing stirring for 1h to prepare a mixed solution B; mixing the mixed solution A and the mixed solution B according to a mass ratio of 1:1.5, continuously and slowly adding ammonium chloride until the pH value is controlled to be 1.75 after 3.5 hours, and stopping adding the ammonium chloride; heating to 65 ℃, standing for 2h, adding sodium hydroxide to adjust the pH value to 7, centrifuging for 75min at 900r/min, and drying at 35 ℃ for 5h to obtain the composite fragrant microcapsule;
(2) Mixing the composite fragrance type microcapsule and the dihydroxy benzidine according to the mass ratio of 1:5.5, mixing, stirring for 15min at 25r/min, adding anhydrous aluminum trichloride of which the mass is 0.15 time that of the compound fragrance type microcapsule, heating to 90 ℃, continuing to stir for 3h, adding 3-butenyl isothiocyanate of which the mass is 4 times that of the compound fragrance type microcapsule, continuing to stir for 3h, centrifuging for 75min at 900r/min, and drying for 5h at 35 ℃ to obtain the modified compound fragrance type microcapsule; mixing modified composite fragrant microcapsules, carboxylated cotton fibers and deionized water according to a mass ratio of 1:25:55, mixing, vibrating under ultrasonic at 5kHz for 25min, adding stannous oxide with the mass 0.2 time of that of the modified composite aromatic microcapsules, heating to 65 ℃, stirring for 3h at 370r/min, filtering, and drying at 35 ℃ and 150Pa for 3h to obtain aromatic cotton fibers; co-twisting and weaving the fragrant cotton fiber to obtain the fabric with the gram weight of 410g/m 2 The cotton fabric of (2);
(3) 2- (chloromethyl) benzonitrile and N-p-chlorophenyldicyandiamide were reacted in a molar ratio of 1:05, stirring for 4min at 23r/min, adding anhydrous aluminum trichloride of which the mass is 0.15 time that of 2- (chloromethyl) benzonitrile, heating to 90 ℃, continuously stirring for 3h, stirring and cleaning with pure water, extracting with toluene, and drying at 35 ℃ and 75Pa for 7h to obtain benzonitrile p-chlorophenyl dicyandiamide; cotton fabric, benzonitrile p-chlorophenyl dicyandiamide, sodium hydride and dimethyl sulfoxide are mixed according to a mass ratio of 1:15:0.7:25, stirring for 25min at the speed of 90r/min, heating to 90 ℃, adding a mixture A with the mass of 0.2 time that of the cotton fabric, wherein the molar ratio of the imino ketone iodide, the palladium chloride and the tetrabutyl ammonium bromide in the mixture A is 1:20:4, stirring for 3.5h at 90r/min, fishing out, cooling to room temperature, adding 4-aminobutyltriethoxysilane 9 times the mass of the cotton fabric, stirring for 15min at 350r/min, adding a hydrochloric acid solution with the mass fraction of 15% 0.2 times the mass of the cotton fabric, continuously stirring for 80min in an oil bath at 45 ℃, adding ammonia water with the mass fraction of 15% to adjust the pH to 7.5, waiting for 26h, fishing out, adding isopropanol with the mass fraction of 9 times the mass of the cotton fabric, heating to 100 ℃, dripping a hydrochloric acid solution with the mass fraction of 36% at 25ml/min, continuing for 7h, fishing out, and drying for 7h at 35 ℃ and 150Pa to obtain the fragrant fabric.
Comparative example 2
(1) Mixing lavender essence, glyceryl monostearate and 15% by mass of ethanol solution according to a mass ratio of 1:0.2:25, stirring for 15min at the speed of 800r/min to prepare a mixed solution A; urea and 4- (4, 6-dichloro-1, 3, 5-triazin-2-yl) benzaldehyde are mixed in a molar ratio of 1:1.75, stirring for 1.5h at 90r/min, adding sodium hydroxide to adjust the pH value to 8, heating to 75 ℃, and continuing stirring for 1h to prepare a mixed solution B; mixing the mixed solution A and the mixed solution B according to a mass ratio of 1:1.5, continuously and slowly adding ammonium chloride until the pH value is controlled to be 1.75 after 3.5 hours, and stopping adding the ammonium chloride; heating to 65 ℃, standing for 2h, adding sodium hydroxide to adjust the pH value to 7, centrifuging for 75min at 900r/min, and drying at 35 ℃ for 5h to obtain the composite fragrant microcapsule;
(2) Mixing the composite fragrance type microcapsule and the dihydroxy benzidine according to the mass ratio of 1:5.5, mixing, stirring for 15min at 25r/min, adding anhydrous aluminum trichloride of which the mass is 0.15 time that of the compound odor type microcapsule, heating to 90 ℃, continuing to stir for 3h, then adding dihydroxybenzidine of which the mass is 4 times that of the compound odor type microcapsule, continuing to stir for 3h, centrifuging for 75min at 900r/min, and drying for 5h at 35 ℃ to obtain the modified compound odor type microcapsule; mixing modified composite fragrant microcapsules, carboxylated cotton fibers and deionized water according to a mass ratio of 1:25:55, mixing, ultrasonically shaking at 5kHz for 25min, adding stannous oxide with the mass 0.2 time that of the modified composite fragrant microcapsule, heating to 65 ℃, stirring for 3h at 370r/min, filtering, and drying at 35 ℃ and 150Pa for 3h to obtain fragrant cotton fiber; the fragrant cotton fiber is co-twisted and woven to obtain the fabric with the gram weight of 410g/m 2 The cotton fabric of (2);
(3) 2- (chloromethyl) benzonitrile and N-p-chlorophenyldicyandiamide were mixed in a molar ratio of 1:05, mixing, stirring for 4min at the speed of 23r/min, adding anhydrous aluminum trichloride of which the mass is 0.15 times that of 2- (chloromethyl) benzonitrile, heating to 90 ℃, continuing stirring for 3h, stirring and cleaning with pure water, extracting with toluene, and drying for 7h at the temperature of 35 ℃ and under the pressure of 75Pa to prepare benzonitrile-p-chlorophenyl dicyandiamide; cotton fabric, benzonitrile p-chlorophenyl dicyandiamide, sodium hydride and dimethyl sulfoxide are mixed according to a mass ratio of 1:15:0.7:25, stirring for 25min at the speed of 90r/min, heating to 90 ℃, adding a mixture A with the mass of 0.2 time that of the cotton fabric, wherein the molar ratio of the imino ketone iodide, the palladium chloride and the tetrabutyl ammonium bromide in the mixture A is 1:20: and 4, stirring for 3.5h at 90r/min, fishing out, cooling to room temperature, adding 4-aminobutyltriethoxysilane 9 times the mass of the cotton fabric, stirring for 15min at 350r/min, adding a hydrochloric acid solution with the mass fraction of 15% 0.2 times the mass of the cotton fabric, continuously stirring for 80min in an oil bath at 45 ℃, adding ammonia water with the mass fraction of 15% to adjust the pH to 7.5, waiting for 26h, fishing out, adding isopropanol with the mass fraction of 9 times the mass of the cotton fabric, heating to 100 ℃, dripping a hydrochloric acid solution with the mass fraction of 36% at 25ml/min, continuing for 7h, fishing out, and drying for 7h at 35 ℃ and 150Pa to obtain the fragrant fabric.
Comparative example 3
(1) Mixing lavender essence, glyceryl monostearate and 15% by mass of ethanol solution according to a mass ratio of 1:0.2:25, stirring for 15min at the speed of 800r/min to prepare a mixed solution A; urea and 4- (4, 6-dichloro-1, 3, 5-triazin-2-yl) benzaldehyde are mixed in a molar ratio of 1:1.75, stirring at 90r/min for 1.5h, adding sodium hydroxide to regulate the pH value to 8, heating to 75 ℃, and continuously stirring for 1h to prepare a mixed solution B; mixing the mixed solution A and the mixed solution B according to a mass ratio of 1:1.5, continuously and slowly adding ammonium chloride until the pH value is controlled to be 1.75 after 3.5 hours, and stopping adding the ammonium chloride; heating to 65 ℃, standing for 2h, adding sodium hydroxide to adjust the pH value to 7, centrifuging for 75min at 900r/min, and drying at 35 ℃ for 5h to obtain the composite fragrant microcapsule;
(2) Mixing the composite fragrant microcapsule and 3-butenyl isothiocyanate according to a mass ratio of 1:5.5, stirring for 15min at 25r/min, adding anhydrous aluminum trichloride with the mass of 0.15 time of that of the compound fragrance type microcapsule, heating to 90 ℃, continuing stirring for 3h, and then adding the compound fragrance type microcapsuleContinuously stirring 3-butenyl isothiocyanate with the mass of 4 times of the capsule for 3h, centrifuging at 900r/min for 75min, and drying at 35 deg.C for 5h to obtain modified composite aromatic microcapsule; mixing modified composite fragrant microcapsules, carboxylated cotton fibers and deionized water according to a mass ratio of 1:25:55, mixing, ultrasonically shaking at 5kHz for 25min, adding stannous oxide with the mass 0.2 time that of the modified composite fragrant microcapsule, heating to 65 ℃, stirring for 3h at 370r/min, filtering, and drying at 35 ℃ and 150Pa for 3h to obtain fragrant cotton fiber; the fragrant cotton fiber is co-twisted and woven to obtain the fabric with the gram weight of 410g/m 2 The cotton fabric of (2);
(3) 2- (chloromethyl) benzonitrile and N-p-chlorophenyldicyandiamide were mixed in a molar ratio of 1:05, mixing, stirring for 4min at the speed of 23r/min, adding anhydrous aluminum trichloride of which the mass is 0.15 times that of 2- (chloromethyl) benzonitrile, heating to 90 ℃, continuing stirring for 3h, stirring and cleaning with pure water, extracting with toluene, and drying for 7h at the temperature of 35 ℃ and under the pressure of 75Pa to prepare benzonitrile-p-chlorophenyl dicyandiamide; cotton fabric, benzonitrile p-chlorophenyl dicyandiamide, sodium hydride and dimethyl sulfoxide are mixed according to a mass ratio of 1:15:0.7:25, stirring for 25min at the speed of 90r/min, heating to 90 ℃, adding a mixture A with the mass of 0.2 time that of the cotton fabric, wherein the molar ratio of the imino ketone iodide, the palladium chloride and the tetrabutyl ammonium bromide in the mixture A is 1:20: and 4, stirring for 3.5h at 90r/min, fishing out, cooling to room temperature, adding 4-aminobutyltriethoxysilane 9 times the mass of the cotton fabric, stirring for 15min at 350r/min, adding a hydrochloric acid solution with the mass fraction of 15% 0.2 times the mass of the cotton fabric, continuously stirring for 80min in an oil bath at 45 ℃, adding ammonia water with the mass fraction of 15% to adjust the pH to 7.5, waiting for 26h, fishing out, adding isopropanol with the mass fraction of 9 times the mass of the cotton fabric, heating to 100 ℃, dripping a hydrochloric acid solution with the mass fraction of 36% at 25ml/min, continuing for 7h, fishing out, and drying for 7h at 35 ℃ and 150Pa to obtain the fragrant fabric.
Comparative example 4
(1) Mixing lavender essence, glyceryl monostearate and 15% by mass of ethanol solution according to a mass ratio of 1:0.2:25, stirring for 15min at the speed of 800r/min to prepare a mixed solution A; urea and 4- (4, 6-dichloro-1, 3, 5-triazin-2-yl) benzaldehyde are mixed in a molar ratio of 1:1.75, stirring for 1.5h at 90r/min, adding sodium hydroxide to adjust the pH value to 8, heating to 75 ℃, and continuing stirring for 1h to prepare a mixed solution B; mixing the mixed solution A and the mixed solution B according to a mass ratio of 1:1.5, continuously and slowly adding ammonium chloride until the pH value is controlled to be 1.75 after 3.5 hours, and stopping adding the ammonium chloride; heating to 65 ℃, standing for 2h, adding sodium hydroxide to adjust the pH value to 7, centrifuging for 75min at 900r/min, and drying at 35 ℃ for 5h to obtain the composite fragrant microcapsule;
(2) Mixing the composite fragrant microcapsule and the dihydroxy benzidine according to the mass ratio of 1:5.5, mixing, stirring for 15min at 25r/min, adding anhydrous aluminum trichloride of which the mass is 0.15 time that of the compound fragrance type microcapsule, heating to 90 ℃, continuing to stir for 3h, adding 3-butenyl isothiocyanate of which the mass is 4 times that of the compound fragrance type microcapsule, continuing to stir for 3h, centrifuging for 75min at 900r/min, and drying for 5h at 35 ℃ to obtain the modified compound fragrance type microcapsule; mixing modified composite fragrant microcapsules, carboxylated cotton fibers and deionized water according to a mass ratio of 1:25:55, mixing, ultrasonically shaking at 5kHz for 25min, adding stannous oxide with the mass 0.2 time that of the modified composite fragrant microcapsule, heating to 65 ℃, stirring for 3h at 370r/min, filtering, and drying at 35 ℃ and 150Pa for 3h to obtain fragrant cotton fiber; the fragrant cotton fiber is co-twisted and woven to obtain the fabric with the gram weight of 410g/m 2 The cotton fabric of (2);
(3) The method comprises the following steps of (1) mixing cotton fabric, 4-aminobutyltriethoxysilane, sodium hydride and dimethyl sulfoxide according to a mass ratio of 1:15:0.7:25, stirring at 90r/min for 25min, heating to 90 ℃, adding a mixture A with the weight 0.2 time that of the cotton fabric, wherein the molar ratio of the imino ketone iodide, the palladium chloride and the tetrabutyl ammonium bromide in the mixture A is 1:20: and 4, stirring for 3.5h at 90r/min, fishing out, cooling to room temperature, adding 4-aminobutyltriethoxysilane 9 times the mass of the cotton fabric, stirring for 15min at 350r/min, adding a hydrochloric acid solution with the mass fraction of 15% 0.2 times the mass of the cotton fabric, continuously stirring for 80min in an oil bath at 45 ℃, adding ammonia water with the mass fraction of 15% to adjust the pH to 7.5, waiting for 26h, fishing out, adding isopropanol with the mass fraction of 9 times the mass of the cotton fabric, heating to 100 ℃, dripping a hydrochloric acid solution with the mass fraction of 36% at 25ml/min, continuing for 7h, fishing out, and drying for 7h at 35 ℃ and 150Pa to obtain the fragrant fabric.
Comparative example 5
(1) Mixing lavender essence, glyceryl monostearate and 15% by mass of ethanol solution according to a mass ratio of 1:0.2:25, stirring for 15min at the speed of 800r/min to prepare a mixed solution A; urea and 4- (4, 6-dichloro-1, 3, 5-triazin-2-yl) benzaldehyde are mixed in a molar ratio of 1:1.75, stirring for 1.5h at 90r/min, adding sodium hydroxide to adjust the pH value to 8, heating to 75 ℃, and continuing stirring for 1h to prepare a mixed solution B; mixing the mixed solution A and the mixed solution B according to a mass ratio of 1:1.5, continuously and slowly adding ammonium chloride until the pH value is controlled to be 1.75 after 3.5 hours, and stopping adding the ammonium chloride; heating to 65 ℃, standing for 2h, adding sodium hydroxide to adjust the pH value to 7, centrifuging for 75min at 900r/min, and drying at 35 ℃ for 5h to obtain the composite fragrant microcapsule;
(2) Mixing the composite fragrant microcapsule and the dihydroxy benzidine according to the mass ratio of 1:5.5, mixing, stirring for 15min at 25r/min, adding anhydrous aluminum trichloride of which the mass is 0.15 time that of the compound fragrance type microcapsule, heating to 90 ℃, continuing to stir for 3h, adding 3-butenyl isothiocyanate of which the mass is 4 times that of the compound fragrance type microcapsule, continuing to stir for 3h, centrifuging for 75min at 900r/min, and drying for 5h at 35 ℃ to obtain the modified compound fragrance type microcapsule; mixing modified composite fragrant microcapsules, carboxylated cotton fibers and deionized water according to a mass ratio of 1:25:55, mixing, ultrasonically shaking at 5kHz for 25min, adding stannous oxide with the mass 0.2 time that of the modified composite fragrant microcapsule, heating to 65 ℃, stirring for 3h at 370r/min, filtering, and drying at 35 ℃ and 150Pa for 3h to obtain fragrant cotton fiber; the fragrant cotton fiber is co-twisted and woven to obtain the fabric with the gram weight of 410g/m 2 The cotton fabric of (2);
(3) 2- (chloromethyl) benzonitrile and N-p-chlorophenyldicyandiamide were reacted in a molar ratio of 1:05, mixing, stirring for 4min at the speed of 23r/min, adding anhydrous aluminum trichloride of which the mass is 0.15 times that of 2- (chloromethyl) benzonitrile, heating to 90 ℃, continuing stirring for 3h, stirring and cleaning with pure water, extracting with toluene, and drying for 7h at the temperature of 35 ℃ and under the pressure of 75Pa to prepare benzonitrile-p-chlorophenyl dicyandiamide; cotton fabric, benzonitrile p-chlorophenyl dicyandiamide, sodium hydride and dimethyl sulfoxide are mixed according to a mass ratio of 1:15:0.7:25, stirring for 25min at the speed of 90r/min, heating to 90 ℃, adding a mixture A with the mass of 0.2 time that of the cotton fabric, wherein the molar ratio of the imino ketone iodide, the palladium chloride and the tetrabutyl ammonium bromide in the mixture A is 1:20:4, stirring for 3.5h at 90r/min, fishing out, cooling to room temperature, adding 4-aminobutyltriethoxysilane 9 times the mass of the cotton fabric, stirring for 15min at 350r/min, adding a hydrochloric acid solution with the mass fraction of 15% 0.2 times the mass of the cotton fabric, continuously stirring for 80min in an oil bath at 45 ℃, adding ammonia water with the mass fraction of 15% to adjust the pH to 7.5, waiting for 26h, fishing out, adding isopropanol with the mass fraction of 9 times the mass of the cotton fabric, heating to 100 ℃, dripping a hydrochloric acid solution with the mass fraction of 36% at 25ml/min, continuing for 7h, fishing out, and drying for 7h at 35 ℃ and 150Pa to obtain the fragrant fabric.
Examples of effects
The following table 1 shows the results of the performance analysis of the aging resistance, the antibacterial property and the wear resistance of the fragrant fabrics prepared by the examples 1 to 3 and the comparative examples 1 to 5 of the present invention.
TABLE 1
From table 1, it can be found that the fragrant fabrics prepared in examples 1, 2 and 3 have strong aging resistance, antibacterial property and wear resistance; from the comparison of the experimental data of examples 1, 2 and 3 and comparative example 1, it can be found that the triazine compound can be formed by using 4- (4, 6-dichloro-1, 3, 5-triazine-2-yl) benzaldehyde to prepare the composite fragrance type microcapsule, and then preparing the modified composite fragrance type microcapsule, so that the prepared fragrance type fabric has strong aging resistance; compared with the experimental data of the examples 1, 2 and 3 and the comparative example 2, the 3-butenyl isothiocyanate is used for modifying the compound fragrance type microcapsule to form hindered amine, so that benzothiophene can be formed in the subsequent preparation of fragrance type fabric, and the prepared fragrance type fabric has strong aging resistance and antibacterial property; the experimental data comparison of examples 1, 2 and 3 and comparative example 3 shows that the aromatic fabric prepared by modifying the composite aromatic microcapsule with the dihydroxybenzidine can form a triazine compound and hindered amine and has strong aging resistance; from the comparison of the experimental data of the examples 1, 2 and 3 and the comparative example 4, it can be found that when the cotton fabric is treated by the benzonitrile and the chlorophenyl dicyandiamide, benzothiophene and biguanide compounds can be formed, and the prepared fragrant fabric has stronger antibacterial property; from the comparison of the experimental data of examples 1, 2 and 3 and comparative example 5, it can be found that the use of 4-aminobutyltriethoxysilane for treating cotton fabric can form silica gel layer and biguanide compound, and the prepared fragrant fabric has strong wear resistance and antibacterial property.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (8)
1. The fragrant fabric is characterized in that the fragrant fabric is prepared by sequentially treating benzonitrile-p-chlorophenyl dicyandiamide and 4-aminobutyltriethoxysilane after fragrant cotton fibers are co-twisted and woven into a cotton fabric.
2. The fragrant fabric of claim 1, wherein said fragrant cotton fiber is prepared by mixing and reacting carboxylated cotton fiber with modified composite fragrant microcapsule.
3. The fabric with compound scent of claim 2, wherein the modified microcapsule with compound scent is prepared by mixing and reacting dihydroxybenzidine, 3-butenyl isothiocyanate and the microcapsule with compound scent.
4. The fragrant fabric of claim 3, wherein said composite fragrant microcapsule is prepared by mixing and reacting essence, urea and 4- (4, 6-dichloro-1, 3, 5-triazin-2-yl) benzaldehyde.
5. The fragrant fabric and the preparation method thereof are characterized by comprising the following preparation steps:
(1) Mixing essence, glyceryl monostearate and 10-20% ethanol solution in a mass ratio of 1:0.1:20 to 1:0.3:30, stirring at 7000-9000 r/min for 10-20 min to prepare a mixed solution A; urea and 4- (4, 6-dichloro-1, 3, 5-triazin-2-yl) benzaldehyde are mixed in a molar ratio of 1: 1.5-1: 2, stirring for 1-2 h at the speed of 80-100 r/min, adding sodium hydroxide to adjust the pH value to 7.8-8.2, heating to 70-80 ℃, and continuously stirring for 0.5-1.5 h to prepare a mixed solution B; mixing the mixed solution A and the mixed solution B according to a mass ratio of 1:1 to 1:2, continuously and slowly adding ammonium chloride until the pH value is controlled to be 1.5-2.0 after 3-4 h, and stopping adding the ammonium chloride; heating to 60-70 ℃, standing for 1-3 h, adding sodium hydroxide to adjust the pH value to 6.8-7.2, centrifuging for 70-80 min at 800-1000 r/min, and drying at 30-40 ℃ for 4-6 h to obtain the composite fragrance type microcapsule;
(2) Mixing the composite fragrance type microcapsule and the dihydroxy benzidine according to the mass ratio of 1:5 to 1:6, mixing, stirring for 10-20 min at 20-30 r/min, adding anhydrous aluminum trichloride with the mass of 0.1-0.2 time of that of the compound odor type microcapsule, heating to 88-92 ℃, continuously stirring for 2-4 h, adding 3-butenyl isothiocyanate with the mass of 3-5 times of that of the compound odor type microcapsule, continuously stirring for 2-4 h, centrifuging for 70-80 min at 800-1000 r/min, and drying for 4-6 h at 30-40 ℃ to obtain the modified compound odor type microcapsule; mixing modified composite fragrant microcapsules, carboxylated cotton fibers and deionized water according to a mass ratio of 1:20: 50-1: 30:60, mixing, carrying out ultrasonic oscillation for 20-30 min at 4-6 kHz, adding stannous oxide with the mass of 0.1-0.3 time of that of the modified compound fragrance type microcapsule, heating to 60-70 ℃, stirring for 2-4 h at 360-380 r/min, filtering, and drying for 2-4 h at 30-40 ℃ under 100-200 Pa to obtain fragrance type cotton fiber; the fragrant cotton fiber is co-twisted and woven to obtain the fabric with the gram weight of 400-420 g/m 2 The cotton fabric of (2);
(3) Cotton fabric, benzonitrile p-chlorophenyl dicyandiamide, sodium hydride and dimethyl sulfoxide are mixed according to a mass ratio of 1:10:0.6:20 to 1:20:0.8:30, stirring for 20-30 min at 80-100 r/min, heating to 80-100 ℃, adding a mixture A with the mass of 0.1-0.3 time of that of the cotton fabric, stirring for 2-5 h at 80-100 r/min, fishing out, cooling to room temperature, adding 4-aminobutyltriethoxysilane with the mass of 8-10 times of that of the cotton fabric, stirring for 10-20 min at 300-400 r/min, adding a hydrochloric acid solution with the mass fraction of 10-20% and the mass fraction of 0.1-0.3 time of that of the cotton fabric, continuously stirring for 75-85 min in an oil bath at 40-50 ℃, adding ammonia water with the mass fraction of 10-20% to adjust the pH to 7-8, waiting for 24-28 h, fishing out, adding isopropanol with the mass fraction of 8-10 times of the cotton fabric, heating to 98-102 ℃, dripping the hydrochloric acid solution with the mass fraction of 32-40% at 20-30 ml/min, continuously fishing out for 6-8 h, pa, and drying for 6-8 h at 30-40 ℃ and 100-200 h to obtain the fragrant fabric.
6. The fragrant fabric and the preparation method thereof according to claim 5, wherein the essence in the step (1) is prepared by mixing lavender essence and one of lemon essence, mint essence, jasmine essence and camellia essence.
7. The fragrant fabric and the preparation method thereof according to claim 5, wherein the preparation method of benzonitrile in step (3) comprises: 2- (chloromethyl) benzonitrile and N-p-chlorophenyldicyandiamide were reacted in a molar ratio of 1:1 to 1:1.1, stirring for 3-5 min at 20-26 r/min, adding anhydrous aluminum trichloride with the mass of 0.1-0.2 time of that of 2- (chloromethyl) benzonitrile, heating to 88-92 ℃, continuously stirring for 2-4 h, stirring and cleaning with pure water, extracting with toluene, drying at 30-40 ℃ under 50-100 Pa for 6-8 h, and obtaining the benzonitrile p-chlorophenyl dicyandiamide.
8. The fragrant fabric and the preparation method thereof as claimed in claim 5, wherein the mixture A in step (3) is prepared from the raw materials of the iodonium ketone, the palladium chloride and the tetrabutyl ammonium bromide according to the molar ratio of 1:18:3 to 1:22:5 mixing to obtain the final product.
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