CN112813680A - Wool and cashmere large biological fiber containing active components of tangerine peel, orange and pomelo and preparation method thereof - Google Patents

Wool and cashmere large biological fiber containing active components of tangerine peel, orange and pomelo and preparation method thereof Download PDF

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Publication number
CN112813680A
CN112813680A CN202110146766.0A CN202110146766A CN112813680A CN 112813680 A CN112813680 A CN 112813680A CN 202110146766 A CN202110146766 A CN 202110146766A CN 112813680 A CN112813680 A CN 112813680A
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wool
treatment
orange
cashmere
active ingredients
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黄效华
甄丽
池姗
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Qingdao Baicao New Material Co ltd
Zhongke Textile Research Institute Qingdao Co ltd
Bestee Material Qingdao Co ltd
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Qingdao Baicao New Material Co ltd
Zhongke Textile Research Institute Qingdao Co ltd
Bestee Material Qingdao Co ltd
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Priority to CN202110146766.0A priority Critical patent/CN112813680A/en
Publication of CN112813680A publication Critical patent/CN112813680A/en
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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
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  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

A preparation method of wool and cashmere biological fiber containing pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis active components comprises soaking for swelling, low temperature treating, biological modifying, anti-pilling treating, and moth preventing treating; the wool and cashmere biological fiber containing the active ingredients of the tangerine peel, the orange and the pomelo has good crease resistance; the resistivity can be reduced to 6 x 104 Ω · m; the durability is good, the yellowing is not easy to occur in the using process, and the yellowing can not occur after the continuous irradiation for 300 hours at the temperature of 30 ℃ and the illumination intensity of 10mW/cm 2; rubbing 150 times under 590cN pressure, still without pilling; the bacteriostatic rate on staphylococcus aureus can reach 98.91%, the bacteriostatic rate on escherichia coli can reach 99.12%, the bacteriostatic rate on pneumobacillus can reach 98.34%, and the bacteriostatic rate on candida albicans can reach 99.33%.

Description

Wool and cashmere large biological fiber containing active components of tangerine peel, orange and pomelo and preparation method thereof
Technical Field
The invention relates to the technical field of cashmere preparation, in particular to a preparation method of wool and cashmere large biological fibers containing active ingredients of tangerine peel, orange and pomelo.
Background
The wool fiber is a deformation object of sheep skin, has excellent heat retention property, is mainly used for clothes in autumn and winter, has better moisture absorption property, has official moisture regain of 15-17 percent, has 40 percent of ultimate moisture absorption rate, and has better moisture absorption property than cotton; the fulling performance is good; the plasticity is strong, the wool swells under the damp and hot condition and loses elasticity, and under the action of external force, the wool is pressed into various shapes and is rapidly cooled, the external force is relieved, and the pressed shapes can be kept unchanged for a long time. Cashmere is a thin and curved fiber, which contains much air and forms an air layer, thus being capable of defending against the invasion of external cold air and keeping the body temperature from being reduced. The cashmere is much finer than wool, and the outer-layer scales are finer and smoother than the wool, so the cashmere is light in weight, soft and good in toughness.
However, wool fibers and cashmere fibers have the defects of easy moth attack, poor wrinkle resistance, easy static electricity generation, yellowing after long-term storage, easy pilling and the like. And the wool fibers and the cashmere fibers which are used as natural protein fibers do not have an antibacterial function, so that bacteria are easy to breed in the using process, and certain threats are caused to the health of a human body and the environment.
Patent CN107974828A discloses a preparation method of antibacterial wool fiber special for wool hat, comprising: soaking the wool fibers in acetone, washing, drying in the air, adding the soaked wool fibers into a mixed aqueous solution of sodium cyanate and hydrogen peroxide, drying in the air, and irradiating by ultraviolet light to obtain pretreated wool fibers; adding thiourea, urea and butyl titanate into absolute ethyl alcohol for mixing, adjusting the pH value, adding deionized water, stirring until a Tyndall effect appears, standing for aging, drying, grinding and calcining to obtain modified nano titanium dioxide; adding chitosan into acetic acid aqueous solution, adjusting the pH value, adding modified nano titanium dioxide, adjusting the pH value of the system, heating, adding glutaraldehyde, standing for reaction, centrifuging, washing and drying to obtain modified chitosan; adding the modified chitosan, the plant extracting solution, the beta-cyclodextrin and the silane coupling agent KH-550 into deionized water, and stirring to obtain an antibacterial solution; adding the pretreated wool fibers into an antibacterial solution for padding treatment, and baking after drying. The patent has the following defects: the prepared wool fiber can be yellowed after being stored for a long time and is easy to fluff and ball.
Patent CN203977034U discloses a surface fabric with anti-pilling fibre, and the wool fibre is vertical form, and another wool fibre is the level form, and wool fibre and another wool fibre intercrossing, the wool fibre comprises the triangle wool fibre that the cross-section is regular triangle, and triangle wool fibre's inside is equipped with the hole, and another wool fibre comprises the triangle wool fibre that falls that the cross-section is inversion triangle, and triangle wool fibre's inside is equipped with the hole. The patent has the following defects: the prepared fabric has no antibacterial property, and bacteria are easy to breed in the using process.
Disclosure of Invention
The invention provides a preparation method of wool and cashmere large biological fiber containing active ingredients of tangerine peel, orange and pomelo, which aims to solve the technical problems in the prior art.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of wool macrobio fiber containing active ingredients of pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis comprises soaking for swelling, low temperature treatment, biological modification, anti-pilling treatment, and moth-proofing treatment.
Soaking and swelling, namely soaking the wool fibers in an acetic acid solution with the mass fraction of 7%, soaking for 3-4h at 40-50 ℃, then adding white carbon black into the acetic acid solution, then performing ultrasonic oscillation, oscillating for 5-6h, and drying the wool fibers at 40-45 ℃ to obtain the swelled wool fibers.
Wherein, the wool fiber: 7% of acetic acid solution by mass: the mass ratio of the white carbon black is 5-7:50-55: 2-3.
The low-temperature treatment comprises the steps of placing wool fibers at a temperature of between 15 ℃ below zero and 5 ℃ below zero, adding dodecyl trimethyl ammonium chloride, then carrying out ultraviolet treatment, wherein the wavelength of ultraviolet is 250-290nm, the power of an ultraviolet lamp is 50-70W, and the action time of ultraviolet is 30-40min, and then placing the wool fibers at a temperature of between 50 ℃ and 55 ℃ for drying to obtain the wool fibers subjected to the low-temperature treatment.
Wherein the mass ratio of the wool fibers to the dodecyl trimethyl ammonium chloride is 1: 3-4.
And the biological modification comprises the steps of mixing the wool fibers, the bioactive components, the sodium bicarbonate and the ethanol, then starting stirring at the stirring speed of 200-220rpm for 3-4h, then carrying out ultrasonic oscillation treatment, and drying the wool fibers at the temperature of 30-35 ℃ after the oscillation treatment is carried out for 3-4h to obtain the wool fibers after the biological treatment.
Wherein, the wool fiber: the biological active ingredients are as follows: sodium bicarbonate: the mass ratio of ethanol is 5-7: 10-12: 3-5: 45-55.
The preparation of the bioactive components comprises cleaning, wall breaking, fermentation, adsorption and post-treatment.
The cleaning is to clean the white parts of the dried orange peel, the orange peel and the shaddock peel by using a 2% sodium hydroxide solution, dry the white parts at 50-55 ℃ until the water content is lower than 10%, and then cut the white parts into blocks of biological raw materials with the size of 7-9 mm.
And the wall breaking treatment is to carry out wall breaking treatment on the blocky raw material by using normal pressure microwave with the frequency of 600-700MHz to obtain the powdery biological raw material, wherein the microwave treatment power is 900-930W, the treatment temperature is 70-75 ℃, and the treatment time is 20-25 min.
And in the fermentation step, cellulase and pure water are added into the powdery biological raw material, and after uniform mixing, enzymolysis is carried out for 5-7h at 35-40 ℃ to obtain fermentation liquor.
Wherein, the powdery biological raw material: cellulase: the mass ratio of the pure water is 6-7: 1-2: 60-65.
And in the adsorption step, after mixing the heavy calcium carbonate and the aqueous acrylic acid emulsion, stirring for 3-4h at the stirring speed of 300-320rpm, then carrying out spray drying, grinding until the particle size is 0.9-1.4 microns to obtain a composite adsorbent, adding the composite adsorbent into the fermentation broth, uniformly mixing, and standing for 7-9h to obtain the fermentation broth after adsorption.
Wherein the mass ratio of the heavy calcium carbonate to the cationic wax emulsion is 2-3: 1.
the aqueous acrylic emulsion was model number Joncryl 142.
And the post-treatment comprises the steps of adding butyronitrile latex into the adsorbed fermentation liquor, carrying out ultrasonic oscillation at 60-75 ℃, drying and grinding at 80-95 ℃ after carrying out ultrasonic oscillation for 2-3h, and grinding until the particle size is 500-700 nm to obtain the bioactive component.
The anti-pilling treatment comprises the steps of diluting an anti-pilling treatment agent to 30-35 times of the original volume by using pure water, soaking the wool fibers subjected to biological treatment into the anti-pilling treatment agent for padding, controlling the rolling residual rate to be 50% -65%, then washing for 2-3 times, and dehydrating and drying to obtain the anti-pilling treated wool macrobio-fibers.
The mass ratio of the wool fiber after biological treatment to the anti-pilling treatment agent is 5-7: 1.
the anti-pilling treatment agent comprises the following components: 3-5 parts of white carbon black, 2-3 parts of an organic silicon defoaming agent, 3-5 parts of sodium dodecyl benzene sulfonate, 4-6 parts of polyoxyethylene ether, 604-7 parts of polysorbate, 4-7 parts of adipic acid, 2-4 parts of sodium hydroxide, 8-11 parts of stearic acid and 30-40 parts of deionized water.
The moth-proof treatment comprises the steps of soaking the wool macrobio-fiber subjected to anti-pilling treatment into moth-proof treatment liquid, and soaking for 2-2.5 hours at 40-50 ℃ to obtain the wool macrobio-fiber containing active ingredients of pericarpium citri reticulatae, orange and pomelo.
The moth-proof treatment liquid comprises the following components: 3-4 parts of alum, 4-7 parts of calcium propionate, 17-21 parts of clove powder, 20-25 parts of sandalwood powder and 230 parts of deionized water 190-.
The preparation method is also suitable for preparing cashmere large biological fiber containing active ingredients of tangerine peel, orange and pomelo.
Compared with the prior art, the invention has the beneficial effects that:
(1) the wool and cashmere large biological fiber containing the active ingredients of the tangerine peel, the orange and the pomelo improves the anti-wrinkle performance by carrying out biological modification on the wool and cashmere fibers, and adopts a wrinkle recovery tester to test the wrinkle recovery angle, wherein the warp direction quick-stretch wrinkle recovery angle is larger than 52 degrees, and the weft direction quick-stretch wrinkle recovery angle is larger than 58 degrees.
(2) The wool and cashmere large biological fiber containing the active components of the tangerine peel, the orange and the pomelo improves the antistatic capability by carrying out biological modification on the wool and cashmere fibers, and the resistivity can be reduced to 6 x 104Ω·m。
(3) The wool and cashmere large biological fiber containing the active ingredients of the tangerine peel, the orange and the pomelo has good durability and is not easy to turn yellow in the using process by adding the active ingredients of the tangerine peel, the orange and the pomelo into the wool and cashmere fiber, and the illumination intensity is 10mW/cm at the temperature of 30 DEG C2After the next continuous irradiation for 300 hours, no yellowing occurred.
(4) According to the wool and cashmere large biological fiber containing the active ingredients of the tangerine peel, the orange and the pomelo, the anti-pilling treatment is carried out on the fabric prepared from the wool and cashmere fibers, so that the anti-pilling performance of the fabric prepared from the wool and cashmere fibers can be improved, and the fabric is not pilling after being rubbed 150 times under the pressure of 590cN according to the GB/T4802.1-2008 test standard.
(5) According to the wool and cashmere large biological fiber containing the active ingredients of the tangerine peel, the orange and the pomelo, disclosed by the invention, by adding the active ingredients containing the tangerine peel, the orange and the pomelo into the wool and cashmere fiber, the bacteriostasis rate on staphylococcus aureus can reach 98.91%, the bacteriostasis rate on escherichia coli can reach 99.12%, the bacteriostasis rate on pneumobacillus can reach 98.34%, and the bacteriostasis rate on candida albicans can reach 99.33%.
(6) The wool and cashmere large biological fiber containing the active ingredients of the tangerine peel, the orange and the pomelo improves the water washing resistance by carrying out wall breaking treatment on the active ingredients of the tangerine peel, the orange and the pomelo, and after 100 times of standard washing, the bacteriostasis rate to staphylococcus aureus can reach 96.57%, the bacteriostasis rate to escherichia coli can reach 94.38%, the bacteriostasis rate to pneumonia bacillus can reach 97.12%, and the bacteriostasis rate to candida albicans can reach 97.85%.
(7) The wool and cashmere large biological fiber containing the active ingredients of the tangerine peel, the orange and the pomelo can play a lasting effect of preventing moths by carrying out moth-proof treatment on the wool and cashmere fiber.
(8) The wool and cashmere large biological fiber containing the active ingredients of the tangerine peel, the orange and the pomelo can avoid the unpleasant odor of the wool and cashmere fiber by adding the active ingredients containing the tangerine peel, the orange and the pomelo after the wall breaking treatment, the adhesion between the active ingredients after the wall breaking and the wool and cashmere fiber is tighter, the fragrance is more durable, and the fragrance can be kept after a plurality of times of water washing.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.
Example 1
A preparation method of wool macrobio fiber containing active ingredients of pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis comprises soaking for swelling, low temperature treatment, biological modification, anti-pilling treatment, and moth-proofing treatment.
Soaking and swelling, namely soaking the wool fibers in an acetic acid solution with the mass fraction of 7%, soaking for 3h at 40 ℃, then adding white carbon black into the acetic acid solution, then performing ultrasonic oscillation, and drying the wool fibers at 40 ℃ after oscillation for 5h to obtain the swelled wool fibers.
Wherein, the wool fiber: 7% of acetic acid solution by mass: the mass ratio of the white carbon black is 5:50: 2.
And the low-temperature treatment comprises the steps of placing the wool fibers under-15 ℃, adding dodecyl trimethyl ammonium chloride, then carrying out ultraviolet treatment, wherein the wavelength of ultraviolet is 250nm, the power of an ultraviolet lamp is 50W, the action time of the ultraviolet is 30min, and then placing the wool fibers at 50 ℃ for drying to obtain the wool fibers after the low-temperature treatment.
Wherein the mass ratio of the wool fibers to the dodecyl trimethyl ammonium chloride is 1: 3.
And the biological modification comprises the steps of mixing the wool fibers, the bioactive components, the sodium bicarbonate and the ethanol, then starting stirring at the stirring speed of 200rpm for 3 hours, then carrying out ultrasonic oscillation treatment, and drying the wool fibers at the temperature of 30 ℃ after the oscillation treatment is carried out for 3-4 hours to obtain the wool fibers after the biological treatment.
Wherein, the wool fiber: the biological active ingredients are as follows: sodium bicarbonate: the mass ratio of ethanol is 5: 10: 3: 45.
the preparation of the bioactive components comprises cleaning, wall breaking, fermentation, adsorption and post-treatment.
And in the cleaning step, the white parts of the dried orange peels, the orange peels and the shaddock peels are cleaned by using a 2% sodium hydroxide solution, and are dried at 50 ℃ until the water content is lower than 10% after being cleaned, and then are cut into blocks of biological raw materials with the size of 7 mm.
And in the step of wall breaking, normal-pressure microwave with the frequency of 600MHZ is used for wall breaking the blocky raw materials to obtain powdery biological raw materials, the microwave treatment power is 900W, the treatment temperature is 70 ℃, and the treatment time is 20 min.
And (3) fermenting, namely adding cellulase and pure water into the powdery biological raw material, uniformly mixing, and performing enzymolysis for 5 hours at 35 ℃ to obtain fermentation liquor.
Wherein, the powdery biological raw material: cellulase: the mass ratio of the pure water is 6: 1: 60.
and in the adsorption step, after mixing the heavy calcium carbonate and the water-based acrylic emulsion, stirring the mixture for 3 hours at a stirring speed of 300rpm, then carrying out spray drying, grinding the mixture until the particle size is 0.9 micron to obtain a composite adsorbent, adding the composite adsorbent into the fermentation liquor, uniformly mixing, and standing for 7 hours to obtain the fermentation liquor after adsorption.
Wherein the mass ratio of the heavy calcium carbonate to the cationic wax emulsion is 2: 1.
the aqueous acrylic emulsion was model number Joncryl 142.
And (3) after the post-treatment, adding butyronitrile latex into the adsorbed fermentation liquor, performing ultrasonic oscillation at 60 ℃, drying and grinding at 80 ℃ after performing ultrasonic oscillation for 2h, and grinding to obtain the bioactive component with the particle size of 500 nm.
The anti-pilling treatment comprises the steps of diluting an anti-pilling treatment agent to 30 times of the original volume by using pure water, soaking the wool fibers subjected to biological treatment in the anti-pilling treatment agent for padding, controlling the rolling retention rate to be 50%, then washing for 2 times, dehydrating and drying to obtain the wool macrobio-fibers subjected to anti-pilling treatment.
The mass ratio of the wool fiber after biological treatment to the anti-pilling treatment agent is 5: 1.
the anti-pilling treatment agent comprises the following components: 3 parts of white carbon black, 2 parts of an organic silicon defoaming agent, 3 parts of sodium dodecyl benzene sulfonate, 4 parts of polyoxyethylene ether, 604 parts of polysorbate, 47 parts of adipic acid, 2 parts of sodium hydroxide, 8 parts of stearic acid and 30 parts of deionized water.
The moth-proof treatment comprises the steps of soaking the wool macrobio-fiber subjected to anti-pilling treatment into moth-proof treatment liquid, and soaking for 2 hours at 40 ℃ to obtain the wool macrobio-fiber containing active ingredients of pericarpium citri reticulatae, orange and pomelo.
The moth-proof treatment liquid comprises the following components: 3 parts of alum, 4 parts of calcium propionate, 17 parts of clove powder, 20 parts of sandalwood powder and 190 parts of deionized water.
The preparation method of the embodiment is also suitable for preparing the cashmere large biological fiber containing the active ingredients of the tangerine peel, the orange and the pomelo.
Example 2
A preparation method of wool macrobio fiber containing active ingredients of pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis comprises soaking for swelling, low temperature treatment, biological modification, anti-pilling treatment, and moth-proofing treatment.
And soaking and swelling, namely soaking the wool fibers in an acetic acid solution with the mass fraction of 7%, soaking for 3.5h at 45 ℃, adding white carbon black into the acetic acid solution, performing ultrasonic oscillation, oscillating for 5.5h, and drying the wool fibers at 42 ℃ to obtain the swelled wool fibers.
Wherein, the wool fiber: 7% of acetic acid solution by mass: the mass ratio of the white carbon black is 6:52: 3.
And the low-temperature treatment comprises the steps of placing the wool fibers at the temperature of minus 10 ℃, adding dodecyl trimethyl ammonium chloride, then carrying out ultraviolet treatment, wherein the wavelength of ultraviolet is 270nm, the power of an ultraviolet lamp is 60W, the action time of ultraviolet is 35min, and then placing the wool fibers at the temperature of 52 ℃ for drying to obtain the wool fibers after the low-temperature treatment.
Wherein the mass ratio of the wool fibers to the dodecyl trimethyl ammonium chloride is 1: 3.
And the biological modification comprises the steps of mixing the wool fibers, the bioactive components, the sodium bicarbonate and the ethanol, then starting stirring at the stirring speed of 210rpm for 3.5 hours, then carrying out ultrasonic oscillation treatment, and drying the wool fibers at the temperature of 32 ℃ after the oscillation treatment is carried out for 3.5 hours to obtain the wool fibers after the biological treatment.
Wherein, the wool fiber: the biological active ingredients are as follows: sodium bicarbonate: the mass ratio of ethanol is 6: 11: 4: 50.
the preparation of the bioactive components comprises cleaning, wall breaking, fermentation, adsorption and post-treatment.
And in the cleaning step, the white parts of the dried orange peels, the orange peels and the shaddock peels are cleaned by using a 2% sodium hydroxide solution, and are dried at 52 ℃ until the water content is lower than 10% after being cleaned, and then are cut into blocks of biological raw materials with the size of 8 mm.
And in the step of wall breaking, normal-pressure microwave with the frequency of 650MHz is used for wall breaking of the massive raw materials to obtain powdery biological raw materials, the microwave treatment power is 910W, the treatment temperature is 72 ℃, and the treatment time is 22 min.
And in the fermentation step, cellulase and pure water are added into the powdery biological raw material, and after uniform mixing, enzymolysis is carried out for 6 hours at 38 ℃ to obtain fermentation liquor.
Wherein, the powdery biological raw material: cellulase: the mass ratio of the pure water is 6: 1: 63.
and in the adsorption step, after mixing the heavy calcium carbonate and the water-based acrylic emulsion, stirring the mixture for 3.5 hours at a stirring speed of 310rpm, then carrying out spray drying, grinding the mixture until the particle size is 1.2 microns to obtain a composite adsorbent, adding the composite adsorbent into the fermentation liquor, uniformly mixing the mixture, and standing the mixture for 8 hours to obtain the fermentation liquor after adsorption.
Wherein the mass ratio of the heavy calcium carbonate to the cationic wax emulsion is 2: 1.
the aqueous acrylic emulsion was model number Joncryl 142.
And (3) performing post-treatment, namely adding butyronitrile latex into the adsorbed fermentation liquor, performing ultrasonic oscillation at 70 ℃, drying and grinding at 90 ℃ after performing ultrasonic oscillation for 2.5 hours, and grinding to obtain the bioactive component with the particle size of 600 nanometers.
The anti-pilling treatment comprises the steps of diluting an anti-pilling treatment agent to 32 times of the original volume by using pure water, soaking the wool fibers subjected to biological treatment in the anti-pilling treatment agent for padding, controlling the rolling residual rate to be 60%, then washing for 2 times, dehydrating and drying to obtain the wool macrobio-fibers subjected to anti-pilling treatment.
The mass ratio of the wool fibers subjected to biological treatment to the anti-pilling treatment agent is 6: 1.
the anti-pilling treatment agent comprises the following components: 4 parts of white carbon black, 2 parts of an organic silicon defoaming agent, 4 parts of sodium dodecyl benzene sulfonate, 5 parts of polyoxyethylene ether, 605 parts of polysorbate, 5 parts of adipic acid, 3 parts of sodium hydroxide, 9 parts of stearic acid and 35 parts of deionized water.
The moth-proof treatment comprises the steps of soaking the wool macrobio-fiber subjected to anti-pilling treatment into moth-proof treatment liquid, and soaking for 2.2 hours at 45 ℃ to obtain the wool macrobio-fiber containing active ingredients of pericarpium citri reticulatae, orange and pomelo.
The moth-proof treatment liquid comprises the following components: 4 parts of alum, 5 parts of calcium propionate, 20 parts of clove powder, 22 parts of sandalwood powder and 200 parts of deionized water.
The preparation method of the embodiment is also suitable for preparing the cashmere large biological fiber containing the active ingredients of the tangerine peel, the orange and the pomelo.
Example 3
A preparation method of wool macrobio fiber containing active ingredients of pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis comprises soaking for swelling, low temperature treatment, biological modification, anti-pilling treatment, and moth-proofing treatment.
Soaking and swelling, namely soaking the wool fibers in an acetic acid solution with the mass fraction of 7%, soaking for 4h at 50 ℃, then adding white carbon black into the acetic acid solution, then performing ultrasonic oscillation, and drying the wool fibers at 45 ℃ after 6h of oscillation to obtain the swelled wool fibers.
Wherein, the wool fiber: 7% of acetic acid solution by mass: the mass ratio of the white carbon black is 7:55: 3.
And the low-temperature treatment comprises the steps of placing the wool fibers at the temperature of-5 ℃, adding dodecyl trimethyl ammonium chloride, then carrying out ultraviolet treatment, wherein the wavelength of ultraviolet is 290nm, the power of an ultraviolet lamp is 70W, and the action time of ultraviolet is 40min, and then placing the wool fibers at the temperature of 55 ℃ for drying to obtain the wool fibers after the low-temperature treatment.
Wherein the mass ratio of the wool fibers to the dodecyl trimethyl ammonium chloride is 1: 4.
And the biological modification comprises the steps of mixing the wool fibers, the bioactive components, the sodium bicarbonate and the ethanol, then starting stirring at the stirring speed of 220rpm for 4 hours, then carrying out ultrasonic oscillation treatment, and drying the wool fibers at 35 ℃ after 4 hours of oscillation treatment to obtain the wool fibers after biological treatment.
Wherein, the wool fiber: the biological active ingredients are as follows: sodium bicarbonate: the mass ratio of ethanol is 7: 12: 5: 55.
the preparation of the bioactive components comprises cleaning, wall breaking, fermentation, adsorption and post-treatment.
And in the cleaning step, the white parts of the dried orange peels, the orange peels and the shaddock peels are cleaned by using a 2% sodium hydroxide solution, and are dried at 55 ℃ until the water content is lower than 10% after being cleaned, and then are cut into blocks of biological raw materials with the size of 9 mm.
And (3) performing wall breaking treatment, namely performing wall breaking treatment on the blocky raw material by using normal-pressure microwave with the frequency of 700MHz to obtain a powdery biological raw material, wherein the microwave treatment power is 930W, the treatment temperature is 75 ℃, and the treatment time is 25 min.
And (3) fermenting, namely adding cellulase and pure water into the powdery biological raw material, uniformly mixing, and performing enzymolysis for 7 hours at 40 ℃ to obtain fermentation liquor.
Wherein, the powdery biological raw material: cellulase: the mass ratio of the pure water is 7: 2: 65.
and in the adsorption step, after mixing the heavy calcium carbonate and the water-based acrylic emulsion, stirring for 4 hours at a stirring speed of 320rpm, then carrying out spray drying, grinding until the particle size is 1.4 microns to obtain a composite adsorbent, adding the composite adsorbent into the fermentation liquor, uniformly mixing, and standing for 9 hours to obtain the fermentation liquor after adsorption.
Wherein the mass ratio of the heavy calcium carbonate to the cationic wax emulsion is 3: 1.
the aqueous acrylic emulsion was model number Joncryl 142.
And (3) performing post-treatment, namely adding butyronitrile latex into the adsorbed fermentation liquor, performing ultrasonic oscillation at 75 ℃, drying and grinding at 95 ℃ after performing ultrasonic oscillation for 3h, and grinding until the particle size is 700 nm to obtain the bioactive component.
The anti-pilling treatment comprises the steps of diluting an anti-pilling treatment agent to 35 times of the original volume by using pure water, soaking the wool fibers subjected to biological treatment in the anti-pilling treatment agent for padding, controlling the rolling retention rate to be 65%, then washing for 3 times, dehydrating and drying to obtain the wool macrobio-fibers subjected to anti-pilling treatment.
The mass ratio of the wool fibers after biological treatment to the anti-pilling treatment agent is 7: 1.
the anti-pilling treatment agent comprises the following components: 5 parts of white carbon black, 3 parts of an organic silicon defoaming agent, 5 parts of sodium dodecyl benzene sulfonate, 6 parts of polyoxyethylene ether, 607 parts of polysorbate, 7 parts of adipic acid, 4 parts of sodium hydroxide, 11 parts of stearic acid and 40 parts of deionized water.
The moth-proof treatment comprises the steps of soaking the wool macrobio-fiber subjected to anti-pilling treatment into moth-proof treatment liquid, and soaking at 50 ℃ for 2.5 hours to obtain the wool macrobio-fiber containing active ingredients of pericarpium citri reticulatae, orange and pomelo.
The moth-proof treatment liquid comprises the following components: 4 parts of alum, 7 parts of calcium propionate, 21 parts of clove powder, 25 parts of sandalwood powder and 230 parts of deionized water.
The preparation method of the embodiment is also suitable for preparing the cashmere large biological fiber containing the active ingredients of the tangerine peel, the orange and the pomelo.
Example 4
Cashmere macrobio fiber containing active ingredients of pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis is prepared by the method for preparing wool macrobio fiber containing active ingredients of pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis described in example 1.
Example 5
The tests were carried out using wool and cashmere macrofibers containing the active ingredients of orange peel, orange and grapefruit as described in examples 1-4, while setting up comparative tests 1-2 for comparison.
Comparative example 1: the preparation method of the wool macrofiber containing the active ingredients of the tangerine peel, the orange and the pomelo as described in the example 1 is adopted, and the difference is that: the wall breaking treatment is omitted in the preparation of the bioactive components.
Comparative example 2: the preparation method of the wool macrofiber containing the active ingredients of the tangerine peel, the orange and the pomelo as described in the example 1 is adopted, and the difference is that: the anti-pilling treatment was omitted.
The properties of the wool or cashmere macrofibers containing active ingredients of tangerine peel, orange and pomelo prepared in examples 1 to 4 and comparative examples 1 to 2 are as follows:
Figure 624050DEST_PATH_IMAGE001
all percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A preparation method of wool and cashmere biological fiber containing active components of tangerine peel, orange and pomelo is characterized by comprising soaking swelling, low-temperature treatment, biological modification, anti-pilling treatment and moth-proof treatment.
2. The preparation method of wool and cashmere biological fiber containing active ingredients of tangerine peel, orange and pomelo according to claim 1, characterized in that the soaking and swelling step comprises soaking the wool fiber in 7% acetic acid solution at 40-50 ℃ for 3-4h, adding white carbon black into the acetic acid solution, performing ultrasonic oscillation, after 5-6h, drying the wool fiber at 40-45 ℃ to obtain the swollen wool fiber.
3. The method for preparing wool and cashmere bio-fibers containing active ingredients of tangerine peel, orange and pomelo according to claim 2, wherein the wool fibers: 7% of acetic acid solution by mass: the mass ratio of the white carbon black is 5-7:50-55: 2-3.
4. The preparation method of wool and cashmere biological fiber containing active ingredients of tangerine peel, orange and pomelo as claimed in claim 1, wherein the low temperature treatment is carried out by placing the wool fiber at-15 to-5 ℃, adding dodecyl trimethyl ammonium chloride, then carrying out ultraviolet treatment with ultraviolet wavelength of 250-290nm, ultraviolet lamp power of 50-70W and ultraviolet action time of 30-40min, and then placing the wool fiber at 50-55 ℃ and drying to obtain the wool fiber after the low temperature treatment.
5. The preparation method of the wool and cashmere bio-fiber containing the active ingredients of tangerine peel, orange and pomelo according to claim 4, wherein the mass ratio of the wool fiber to the dodecyl trimethyl ammonium chloride is 1: 3-4.
6. The preparation method of wool and cashmere bio-fiber containing active ingredients of tangerine peel, orange and pomelo according to claim 1, characterized in that the bio-modification comprises mixing the wool fiber, the bio-active ingredients, sodium bicarbonate and ethanol, stirring at a stirring speed of 200-220rpm for 3-4h, then performing ultrasonic oscillation treatment, and drying the wool fiber at 30-35 ℃ after the oscillation treatment for 3-4h to obtain the biologically treated wool fiber;
wherein, the wool fiber: the biological active ingredients are as follows: sodium bicarbonate: the mass ratio of ethanol is 5-7: 10-12: 3-5: 45-55.
7. The method for preparing wool and cashmere bio-fibers containing active ingredients of tangerine peel, orange and pomelo according to claim 6, wherein the preparation of the bio-active ingredients comprises cleaning, wall breaking treatment, fermentation, adsorption and post-treatment.
8. The preparation method of wool and cashmere biological fiber containing active ingredients of tangerine peel, orange and pomelo according to claim 1, wherein the anti-pilling treatment comprises diluting the anti-pilling treatment agent to 30-35 times of the original volume with pure water, soaking the biologically treated wool fiber into the anti-pilling treatment agent for padding, controlling the rolling residual rate to be 50% -65%, then washing with water for 2-3 times, dewatering and drying to obtain the anti-pilling treated wool biological fiber.
9. The method for preparing wool and cashmere bio-fibers containing active ingredients of tangerine peel, orange and pomelo according to claim 8, wherein the anti-pilling treatment agent comprises the following components: 3-5 parts of white carbon black, 2-3 parts of an organic silicon defoaming agent, 3-5 parts of sodium dodecyl benzene sulfonate, 4-6 parts of polyoxyethylene ether, 604-7 parts of polysorbate, 4-7 parts of adipic acid, 2-4 parts of sodium hydroxide, 8-11 parts of stearic acid and 30-40 parts of deionized water.
10. The method for preparing wool and cashmere biological fibers containing active ingredients of tangerine peel, orange and pomelo according to claim 1, wherein the moth-proof treatment comprises the steps of immersing the wool biological fibers subjected to anti-pilling treatment in moth-proof treatment solution, and performing immersion treatment at 40-50 ℃ for 2-2.5 hours to obtain the wool biological fibers containing active ingredients of tangerine peel, orange and pomelo.
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