CN115748000A - Milk chinlon macrobiotic fiber and preparation method thereof - Google Patents
Milk chinlon macrobiotic fiber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a milk chinlon macrobiological fiber, which is prepared from modified mica particles and chinlon-6 in a mass ratio of 15-100. The invention also discloses a preparation method of the milk chinlon macrobiotic fiber, which comprises the steps of rare earth chloride treatment of mica, mica loading of HMO, milk dipping, surface treatment and blending spinning. The fiber has excellent lasting antibacterial performance, the inhibition rate of staphylococcus aureus is 98.3-99.2%, the inhibition rate of escherichia coli is 99.0-99.4%, the inhibition rate of candida albicans is 92.1-92.7%, the inhibition rate of staphylococcus aureus after being washed for 50 times is 91.8-93.2%, the inhibition rate of escherichia coli after being washed for 50 times is 93.2-93.7%, and the inhibition rate of candida albicans after being washed for 50 times is 89.9-90.5%; the fiber of the invention has excellent friction resistance, and the friction times when the split with the length of 6mm or more occurs is 42-45 times.
Description
Technical Field
The invention relates to a milk chinlon macrobiotic fiber and a preparation method thereof, and belongs to the field of chinlon fibers.
Background
The nylon fiber is named as polyamide fiber and mainly comprises nylon 6 and nylon 66, the nylon fiber has unique advantages as a synthetic fiber raw material for clothes and decorative materials, the wear resistance of the nylon fiber is good, the strength of the nylon fiber is high, the wear resistance of common single fiber of the nylon fiber is 10 times that of cotton, 20 times that of wool and 50 times that of viscose, and the prepared fabric has excellent wear resistance.
In hot summer, people prefer environment-friendly, cool and comfortable fibers and textiles, the moisture absorption is important, and chinlon has good moisture absorption performance in synthetic fibers, but the moisture absorption performance is lower than that of natural fibers and artificial fibers, so that the chinlon is not suitable to be used as a textile raw material in summer.
Mica particles can be added into a nylon raw material in the prior art, the mica particles with small particle size and the nylon are melted and blended, and then the fibers are further prepared, so that the moisture absorption performance of the fibers can be improved, and the mica has a natural layered structure and has the functions of heat conduction and water absorption, so that the cooling and heat dissipation capacity of the fibers can be improved after the fibers are prepared and the textiles are prepared, and the fabric is more suitable for being worn in summer.
The milk contains rich proteins, mainly phosphorus-containing proteins, albumin and globulin, all of which contain all essential amino acids including lysine, tryptophan, methionine, leucine, isoleucine, phenylalanine, valine and the like, and in addition, the HMO is a component in milk, belongs to oligosaccharide, has the functions of regulating immunity, regulating intestinal flora and the like, is generally used as an added component in high-grade milk powder, has an inhibiting effect on adhesion of the HMO to escherichia coli, salmonella and other strains in vitro experiments, can load the milk proteins and the HMO serving as antibacterial functional components into nano mica particles through a specific process, and further adds the nano mica particles into fibers to ensure that the fibers have more durable antibacterial property.
CN112626674A train bedding fabric with cool feeling comfortableness, melt spinning mica and nylon, preparing the fabric, utilizing excellent natural heat-conducting property of mica, adding the mica into nylon melt to prepare modified nylon fiber with cool feeling function, the modified fiber can rapidly conduct heat on the skin surface, and the purpose of rapid cooling and heat dissipation is achieved.
However, tests show that when fibers with the same production line density are produced, the tensile property and the friction resistance of the produced fibers are reduced, the applicant reduces the particle size of mica, then adds the mica into the raw materials to produce the fibers, and the problem of the reduction of the tensile property and the friction resistance cannot be solved.
In summary, in the prior art, the mica component can be added into the nylon fiber to improve the moisture absorption of the fiber and enable the nylon fiber to obtain the cooling and heat dissipation capability, but the tensile property and the friction resistance of the prepared fiber are reduced.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and the nano mica particles are specially treated and finally prepared into fibers, so that the moisture absorption of the fibers is improved, and the tensile property, the friction resistance and the antibacterial property of the fibers are improved.
In order to solve the technical problems, the invention adopts the following technical scheme:
the raw materials of the milk chinlon macrobiotic fiber comprise modified mica particles and chinlon-6, and the mass ratio of the modified mica particles to the chinlon-6 is 15-100.
The following is a further improvement of the above technical scheme:
a preparation method of milk chinlon macro-biological fiber is characterized by comprising the steps of rare earth chloride treatment of mica, mica loading of HMO, milk dipping, surface treatment and blending spinning;
the method for processing mica by rare earth chloride comprises the steps of mixing rare earth chloride with deionized water, stirring to obtain a rare earth chloride solution, mixing nano mica particles with the rare earth chloride solution, controlling the temperature to be 71-75 ℃, stirring for 7.0-8.0h, filtering after stirring, washing filter residues with water, and drying to obtain the rare earth chloride processed nano mica particles.
The mass ratio of the rare earth chloride to the deionized water is 25-170;
the mass ratio of the rare earth chloride solution to the nano mica particles is 15.5-4.5;
the particle size of the nano mica particles is 120-200nm.
The method for loading HMO on mica comprises the steps of mixing HMO with deionized water, stirring to obtain an HMO aqueous solution, mixing rare earth chloride treated nano mica particles with the HMO aqueous solution, controlling the ultrasonic frequency to be 23-28kHz, carrying out ultrasonic treatment for 15-25min, stirring after ultrasonic treatment for 45-55min, filtering, washing with alcohol and drying after stirring to obtain the HMO-loaded nano mica particles.
The mass ratio of the HMO to the deionized water is 20-110;
the mass ratio of the HMO aqueous solution to the rare earth chloride treated nano mica particles is 20.5-3.5.
The milk impregnation method comprises the steps of degreasing milk to obtain degreased milk, mixing HMO-loaded nano mica particles with the degreased milk to obtain a mixed solution, controlling ultrasonic frequency to be 25-30kHz, carrying out ultrasonic treatment for 12-18min, controlling temperature to be 35-42 ℃ after ultrasonic treatment, concentrating the mixed solution to 30-40% of the original volume, freeze-drying, and crushing to 400-600 meshes after freeze-drying to obtain the mica particles subjected to milk impregnation treatment.
The protein content in the milk is 2.4-2.6g/100mL;
the mass ratio of the HMO-loaded nano mica particles to the skimmed milk is 5-110.
The surface treatment method comprises the steps of mixing ethanol, deionized water and sodium hydroxide, uniformly stirring, then adding mica particles subjected to milk impregnation treatment, stirring, slowly dropwise adding 3- (2, 3-epoxypropoxy) propyltrimethoxysilane while stirring for 18-25min, continuously stirring after dropwise adding is finished, stirring for 150-160min, filtering, washing with alcohol and drying after stirring to obtain the modified mica particles.
The mass ratio of the ethanol, the deionized water, the sodium hydroxide, the milk-dipped mica particles and the 3- (2, 3-epoxypropoxy) propyl trimethoxy silane is (135-165).
The blending spinning method comprises the steps of controlling the temperature to be 205-215 ℃, carrying out melt blending on the modified mica particles and the nylon-6 for 40-50min to obtain a spinning master batch after blending, then controlling the spinning temperature to be 225-235 ℃, controlling the spinning speed to be 1400-1600m/min and the cold air temperature to be 12-18 ℃, carrying out spinning, and obtaining the milk nylon macrobio-fiber after spinning.
Compared with the prior art, the invention has the following beneficial effects:
the fiber has excellent lasting antibacterial performance, the inhibition rate of staphylococcus aureus is 98.3-99.2%, the inhibition rate of escherichia coli is 99.0-99.4%, the inhibition rate of candida albicans is 92.1-92.7%, the inhibition rate of staphylococcus aureus after being washed for 50 times is 91.8-93.2%, the inhibition rate of escherichia coli after being washed for 50 times is 93.2-93.7%, and the inhibition rate of candida albicans after being washed for 50 times is 89.9-90.5%;
the fiber has excellent tensile property, the breaking strength is 8.67-9.79cN/dtex, and the elongation at break is 42.7-43.9%;
the fiber has excellent friction resistance, the friction performance is tested by using a cohesion machine, the weight mass of the cohesion machine is set to be 500g, the reciprocating times of a grinding roller are 120 times/min, the reciprocating stroke is 90mm, the number of wound filaments is 20, the friction times when 10 filaments are split at the length of 6mm or more are recorded, each embodiment and each comparative example are tested in parallel for 20 times, the average value is taken, and the friction times of the fiber are 42-45 times;
the fiber has high moisture regain of 8.17-8.55%;
the fiber has small linear density deviation ratio which is-0.72 to-0.75;
the fiber protein content of the invention is high, and the protein content is 1.13-1.30%.
Detailed Description
Example 1
(1) Rare earth chloride treated mica
Mixing rare earth chloride with deionized water, stirring to obtain a rare earth chloride solution, mixing the nano mica particles with the rare earth chloride solution, controlling the temperature to be 73 ℃, stirring for 7.5 hours, filtering after stirring, washing filter residues with water, and drying to obtain rare earth chloride-treated nano mica particles;
the mass ratio of the rare earth chloride to the deionized water is 25;
the mass ratio of the rare earth chloride solution to the nano mica particles is 15;
the particle size of the nano mica particles is 150nm.
(2) Mica loaded HMO
Mixing HMO and deionized water, stirring to obtain an HMO aqueous solution, mixing the rare earth chloride-treated nano mica particles with the HMO aqueous solution, controlling the ultrasonic frequency to be 25kHz, carrying out ultrasonic treatment for 18min, stirring after ultrasonic treatment for 50min, filtering, washing with alcohol and drying after stirring to obtain HMO-loaded nano mica particles;
the mass ratio of the HMO to the deionized water is 20;
the mass ratio of the HMO aqueous solution to the rare earth chloride treated nano mica particles is 20.
(3) Dipped milk
Degreasing milk to obtain degreased milk, mixing HMO-loaded nano mica particles with the degreased milk to obtain a mixed solution, controlling ultrasonic frequency to be 27kHz, carrying out ultrasonic treatment for 15min, controlling the temperature to be 40 ℃ after ultrasonic treatment, concentrating the mixed solution to 35% of the original volume, freeze-drying, and crushing to 500 meshes after freeze-drying to obtain milk-dipped mica particles;
the protein content in the milk is 2.5g/100mL;
the mass ratio of the HMO-loaded nano mica particles to the skimmed milk is 5.
(4) Surface treatment
Mixing ethanol, deionized water and sodium hydroxide, stirring uniformly, adding mica particles soaked in milk, stirring, slowly dropwise adding 3- (2, 3-epoxypropoxy) propyl trimethoxy silane while stirring for 20min, continuously stirring after dropwise adding, stirring for 155min, filtering, washing with alcohol, and drying to obtain modified mica particles;
the mass ratio of ethanol, deionized water, sodium hydroxide, milk-impregnated mica particles, 3- (2, 3-glycidoxy) propyltrimethoxysilane was 150.
(5) Blended spun yarn
Controlling the temperature to be 220 ℃, carrying out melt blending on the modified mica particles and the chinlon-6 for 45min, obtaining a spinning master batch after blending, then controlling the spinning temperature to be 230 ℃, controlling the spinning speed to be 1500m/min and the cold air temperature to be 15 ℃, carrying out spinning, and obtaining the milk chinlon macrobio-fiber after spinning;
the mass ratio of the modified mica particles to the nylon-6 is 15.
Example 2
(1) Rare earth chloride treated mica
Mixing rare earth chloride with deionized water, stirring to obtain a rare earth chloride solution, mixing the nano mica particles with the rare earth chloride solution, controlling the temperature to be 71 ℃, stirring for 8.0h, filtering after stirring, washing and drying filter residues to obtain nano mica particles treated by rare earth chloride;
the mass ratio of the rare earth chloride to the deionized water is 25;
the mass ratio of the rare earth chloride solution to the nano mica particles is 15.5;
the particle size of the nano mica particles is 120nm.
(2) Mica loaded HMO
Mixing HMO and deionized water, stirring to obtain an HMO aqueous solution, mixing the rare earth chloride-treated nano mica particles with the HMO aqueous solution, controlling the ultrasonic frequency to be 23kHz, carrying out ultrasonic treatment for 25min, stirring after ultrasonic treatment for 45min, filtering, washing with alcohol and drying after stirring to obtain HMO-loaded nano mica particles;
the mass ratio of the HMO to the deionized water is 20;
the mass ratio of the HMO aqueous solution to the rare earth chloride treated nano mica particles is 20.5.
(3) Dipped milk
Degreasing milk to obtain degreased milk, mixing HMO-loaded nano mica particles with the degreased milk to obtain a mixed solution, controlling ultrasonic frequency to be 25kHz, carrying out ultrasonic treatment for 18min, controlling the temperature to be 35 ℃ after ultrasonic treatment, concentrating the mixed solution to 40% of the original volume, freeze-drying, and crushing to 400 meshes after freeze-drying to obtain milk-dipped mica particles;
the protein content in the milk is 2.6g/100mL;
the mass ratio of the HMO-loaded nano mica particles to the skimmed milk is 5.
(4) Surface treatment
Mixing ethanol, deionized water and sodium hydroxide, stirring uniformly, adding mica particles soaked in milk, stirring, slowly dropwise adding 3- (2, 3-epoxypropoxy) propyl trimethoxy silane while stirring for 18min, continuously stirring after dropwise adding is finished for 160min, filtering, washing with alcohol, and drying to obtain modified mica particles;
the mass ratio of ethanol, deionized water, sodium hydroxide, milk-impregnated mica particles, 3- (2, 3-glycidoxy) propyltrimethoxysilane.
(5) Blended spinning
Controlling the temperature to be 215 ℃, carrying out melt blending on the modified mica particles and the chinlon-6 for 50min, obtaining a spinning master batch after blending, then controlling the spinning temperature to be 225 ℃, the spinning speed to be 1400m/min and the cold air temperature to be 12 ℃, carrying out spinning, and obtaining the milk chinlon macrobio-fiber after spinning;
the mass ratio of the modified mica particles to the nylon-6 is 15.
Example 3
(1) Rare earth chloride treated mica
Mixing rare earth chloride with deionized water, stirring to obtain a rare earth chloride solution, mixing the nano mica particles with the rare earth chloride solution, controlling the temperature to be 75 ℃, stirring for 7.0h, filtering after stirring, washing filter residues with water, and drying to obtain rare earth chloride-treated nano mica particles;
the mass ratio of the rare earth chloride to the deionized water is 25;
the mass ratio of the rare earth chloride solution to the nano mica particles is 15.5;
the particle size of the nano mica particles is 200nm.
(2) Mica loaded HMO
Mixing HMO and deionized water, stirring to obtain an HMO aqueous solution, mixing the rare earth chloride-treated nano mica particles with the HMO aqueous solution, controlling the ultrasonic frequency to be 28kHz, carrying out ultrasonic treatment for 15min, stirring after ultrasonic treatment for 55min, filtering, washing with alcohol and drying after stirring to obtain HMO-loaded nano mica particles;
the mass ratio of the HMO to the deionized water is 20;
the mass ratio of the HMO aqueous solution to the rare earth chloride treated nano mica particles is 20.5.
(3) Dipped milk
Degreasing milk to obtain degreased milk, mixing HMO-loaded nano mica particles with the degreased milk to obtain a mixed solution, controlling ultrasonic frequency to be 30kHz, carrying out ultrasonic treatment for 12min, controlling the temperature to be 42 ℃ after ultrasonic treatment, concentrating the mixed solution to 32% of the original volume, freeze-drying, and crushing the mixed solution to 600 meshes to obtain milk-impregnated mica particles;
the protein content in the milk is 2.4g/100mL;
the mass ratio of the HMO-loaded nano mica particles to the skimmed milk is 5.
(4) Surface treatment
Mixing ethanol, deionized water and sodium hydroxide, stirring uniformly, adding mica granules treated by milk impregnation, stirring, slowly dropwise adding 3- (2, 3-epoxypropoxy) propyl trimethoxy silane while stirring for 25min, continuously stirring after dropwise adding is finished, stirring for 150min, filtering, washing with alcohol, drying, and modifying the mica granules;
the mass ratio of ethanol, deionized water, sodium hydroxide, milk-impregnated mica particles, 3- (2, 3-glycidoxy) propyltrimethoxysilane was 165.
(5) Blended spun yarn
Controlling the temperature to be 225 ℃, carrying out melt blending on the modified mica particles and the chinlon-6 for 40min, obtaining a spinning master batch after blending, then controlling the spinning temperature to be 235 ℃, controlling the spinning speed to be 1600m/min, and controlling the cold air temperature to be 18 ℃, carrying out spinning, and obtaining the milk chinlon macrobio-fiber after spinning;
the mass ratio of the modified mica particles to the chinlon-6 is 15.
Comparative example 1
On the basis of example 1, a rare earth chloride treated mica step was omitted, and in the mica-supported HMO step, untreated nano mica particles were used instead of rare earth chloride treated nano mica particles for supporting, and the other steps were the same to prepare a fiber.
Comparative example 2
On the basis of the embodiment 1, the surface treatment step is omitted, the mica particles subjected to milk impregnation treatment are directly subjected to melt blending with the chinlon-6, the spinning is further carried out, and the fibers are prepared by the same steps as the rest steps.
Example 4 fiber antimicrobial Performance testing
The fibers of examples 1-3 and comparative examples 1-2 were tested for inhibition against staphylococcus aureus, escherichia coli, and candida albicans according to the method of GB/T20944.3-2008, and were tested for inhibition against staphylococcus aureus, escherichia coli, and candida albicans after 50 washes, and the results are shown in table 1.
Example 5 fiber tensile Property testing
The fibers of examples 1-3 and comparative examples 1-2 were tested for breaking strength and elongation at break according to the method in FZ/T52002-2012, and the results are shown in Table 2.
Example 6 fiber rub resistance test
The fibers of examples 1-3 and comparative examples 1-2 were tested for cohesive friction performance by the following test methods:
the weight mass of a heavy hammer of a cohesion machine is set to be 500g, the reciprocating times of a grinding roller are 120 times/min, the reciprocating stroke is 90mm, the number of wound filaments is 20, the friction times of 10 filaments with 6mm or more length splitting are recorded, each of the examples and the comparative examples is tested in parallel for 20 times, and the results are shown in table 3.
Example 7 testing of other Properties of fibers
The fibers of examples 1 to 3 and comparative examples 1 to 2 were subjected to the moisture regain and the linear density deviation of the fibers in accordance with the method of FZ/T52002-2012, and the results are shown in Table 4.
EXAMPLE 8 detection of fibrin content
The fibers prepared in examples 1 to 3 and comparative examples 1 to 2 were subjected to the FZ/T50018-2013 test for the protein content, and the results are shown in Table 5.
Claims (10)
1. The milk chinlon macro-biological fiber is characterized in that the raw materials of the fiber consist of modified mica particles and chinlon-6, and the mass ratio of the modified mica particles to the chinlon-6 is 15-100.
2. A preparation method of milk chinlon macro-biological fiber is characterized by comprising the steps of rare earth chloride treatment of mica, mica loading of HMO, milk dipping, surface treatment and blending spinning;
the method for processing mica by rare earth chloride comprises the steps of mixing rare earth chloride with deionized water, stirring to obtain a rare earth chloride solution, mixing nano mica particles with the rare earth chloride solution, controlling the temperature to be 71-75 ℃, stirring for 7.0-8.0h, filtering after stirring, washing filter residues with water, and drying to obtain the nano mica particles processed by rare earth chloride.
3. The preparation method of the milk chinlon macrobiological fiber according to claim 2, characterized by comprising the following steps:
the mass ratio of the rare earth chloride to the deionized water is 25-170;
the mass ratio of the rare earth chloride solution to the nano mica particles is 15.5-4.5;
the particle size of the nano mica particles is 120-200nm.
4. The preparation method of the milk chinlon macrobiological fiber according to claim 2, characterized by comprising the following steps:
the method for loading HMO on mica comprises the steps of mixing HMO with deionized water, stirring to obtain an HMO aqueous solution, mixing rare earth chloride-treated nano mica particles with the HMO aqueous solution, controlling the ultrasonic frequency to be 23-28kHz, carrying out ultrasonic treatment for 15-25min, stirring after ultrasonic treatment for 45-55min, filtering, washing with alcohol and drying after stirring to obtain the HMO-loaded nano mica particles.
5. The method for preparing the milk chinlon macrobiotic fiber according to claim 4, characterized in that:
the mass ratio of the HMO to the deionized water is 20-110;
the mass ratio of the HMO aqueous solution to the rare earth chloride treated nano mica particles is 20.5-3.5.
6. The preparation method of the milk chinlon macrobiological fiber according to claim 2, characterized by comprising the following steps:
the method for impregnating the milk comprises the steps of degreasing the milk to obtain degreased milk, mixing the HMO-loaded nano mica particles with the degreased milk to obtain a mixed solution, controlling the ultrasonic frequency to be 25-30kHz, carrying out ultrasonic treatment for 12-18min, controlling the temperature to be 35-42 ℃ after the ultrasonic treatment, concentrating the mixed solution to 30-40% of the original volume, freeze-drying, and crushing to 400-600 meshes to obtain the mica particles subjected to milk impregnation treatment.
7. The preparation method of the milk chinlon macrobiological fiber according to claim 6, characterized in that:
the protein content in the milk is 2.4-2.6g/100mL;
the mass ratio of the HMO-loaded nano mica particles to the skimmed milk is 5-110.
8. The preparation method of the milk chinlon macrobiological fiber according to claim 2, characterized by comprising the following steps:
the surface treatment method comprises the steps of mixing ethanol, deionized water and sodium hydroxide, uniformly stirring, adding mica particles subjected to milk impregnation treatment, stirring, slowly dropwise adding 3- (2, 3-epoxypropoxy) propyl trimethoxy silane while stirring for 18-25min, continuously stirring after dropwise adding is finished, stirring for 150-160min, filtering after stirring, washing with alcohol, and drying to obtain the modified mica particles.
9. The preparation method of the milk chinlon macrobiological fiber according to claim 8, characterized in that:
the mass ratio of the ethanol, the deionized water, the sodium hydroxide, the milk-dipped mica particles and the 3- (2, 3-epoxypropoxy) propyl trimethoxy silane is (135-165).
10. The method for preparing the milk chinlon macrobiotic fiber according to claim 2, characterized in that:
the blending spinning method comprises the steps of controlling the temperature to be 205-215 ℃, carrying out melt blending on the modified mica particles and the nylon-6 for 40-50min to obtain a spinning master batch after blending, then controlling the spinning temperature to be 225-235 ℃, controlling the spinning speed to be 1400-1600m/min and the cold air temperature to be 12-18 ℃, carrying out spinning, and obtaining the milk nylon macrobiotic fiber after spinning.
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