CN116463748A - Large biological nylon fiber containing coffee active ingredient and preparation method thereof - Google Patents

Large biological nylon fiber containing coffee active ingredient and preparation method thereof Download PDF

Info

Publication number
CN116463748A
CN116463748A CN202310624821.1A CN202310624821A CN116463748A CN 116463748 A CN116463748 A CN 116463748A CN 202310624821 A CN202310624821 A CN 202310624821A CN 116463748 A CN116463748 A CN 116463748A
Authority
CN
China
Prior art keywords
preparing
coffee
preparation
medical stone
large biological
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202310624821.1A
Other languages
Chinese (zh)
Inventor
黄效华
甄丽
刘彦明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Qingdao Baicao New Material Co ltd
Zhongke Textile Research Institute Qingdao Co ltd
Bestee Material Tsingtao Co Ltd
Original Assignee
Qingdao Baicao New Material Co ltd
Zhongke Textile Research Institute Qingdao Co ltd
Bestee Material Tsingtao Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Qingdao Baicao New Material Co ltd, Zhongke Textile Research Institute Qingdao Co ltd, Bestee Material Tsingtao Co Ltd filed Critical Qingdao Baicao New Material Co ltd
Priority to CN202310624821.1A priority Critical patent/CN116463748A/en
Publication of CN116463748A publication Critical patent/CN116463748A/en
Pending legal-status Critical Current

Links

Classifications

    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/90Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/09Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention provides a large biological nylon fiber containing coffee active ingredients and a preparation method thereof, wherein the preparation method comprises the steps of preparing a loading agent, dissolving a coffee extract, preparing a functional agent, preparing a functional master batch, preparing a modified functional master batch and spinning; the preparation of the loading agent comprises the steps of preparing a premix and mixing; the preparation method comprises the steps of firstly carrying out microwave treatment on bentonite and nano silicon dioxide, then carrying out liquid nitrogen ball milling treatment, and controlling the temperature of the liquid nitrogen ball mill to be-160 to-156 ℃ to prepare a premix; the mixing step comprises mixing the premix and modified Maifanitum uniformly, and performing high-frequency electromagnetic oscillation treatment with oscillation frequency of 10-14MHz for 6-8min and maximum current density of 12-16A/cm 2 Completion ofThe step of mixing is carried out to prepare a loading agent; the prepared large biological nylon fiber containing the coffee active ingredient has good immobilization effect, excellent antibacterial performance after multiple times of washing, and good heat resistance, light resistance and antistatic performance.

Description

Large biological nylon fiber containing coffee active ingredient and preparation method thereof
Technical Field
The invention relates to the field of nylon fibers, in particular to a large biological nylon fiber containing coffee active ingredients and a preparation method thereof.
Background
Nylon fiber is also called polyamide fiber, is the first synthetic fiber in the world, has wide application, is a good material for replacing metals such as steel, iron, copper and the like with plastic, and is an important engineering plastic.
The nylon fiber has better wear resistance and strength performance, but has the defects of poor heat resistance and light resistance, poor retention and poor antistatic performance.
The coffee plant mainly contains saccharide, protein, fat, vitamins, minerals and organic acids; it is found that coffee has antibacterial effect and is used for treating diabetes, cardiovascular diseases, hypertension, cancer and reducing death rate.
In the prior art, in the preparation process of nylon fibers, coffee extracts are loaded into holes of porous materials so as to improve the antibacterial performance of the fibers; however, researchers find that the compatibility of the effective components of the coffee with the nylon fibers is poor, and the coffee is easy to elute after multiple times of washing;
researchers also found that the nylon fiber containing the coffee extract prepared by the prior art still has poor heat resistance and light resistance, and the defect of poor antistatic property is not overcome.
Therefore, the large biological nylon fiber containing the coffee active ingredient prepared by the prior art has the following problems:
1. the immobilization effect is not ideal, and the washing is easy to be eluted after multiple times of washing, so that the use requirement cannot be met;
2. the prepared fiber has poor heat resistance and light resistance and poor antistatic property.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides the large biological nylon fiber containing the coffee active ingredient and the preparation method thereof, which have good immobilization effect, are not easy to elute after multiple times of washing, and have excellent heat resistance, light resistance and antistatic performance.
In order to solve the technical problems, the invention adopts the following technical scheme:
1. preparation of the supporting agent
(1) Preparation of premix
The preparation method of the loading agent comprises the steps of firstly carrying out microwave treatment on bentonite and nano silicon dioxide, wherein the microwave power is 1600-1800MHz, the microwave time is 58-62s, then carrying out liquid nitrogen ball milling treatment, controlling the temperature of a liquid nitrogen ball mill to be-160-156 ℃, controlling the ball-material ratio to be 6-10:1, the rotating speed to be 160-200rpm and the ball milling time to be 13-17min, and preparing a premix;
the mass ratio of the bentonite to the nano silicon dioxide is 1:0.5-2;
the bentonite is a mixture of sodium bentonite and calcium bentonite, and the mass ratio of the sodium bentonite to the calcium bentonite is 1:0.5-2;
(2) Mixing material
Mixing the premix and modified Maifanitum uniformly, and performing high-frequency electromagnetic oscillation treatment with oscillation frequency of 10-14MHz and oscillation time of 6-8min, and maximum current density of 12-16A/cm 2 Completing the mixing step to prepare a loading agent;
the mass ratio of the modified medical stone to the premix is 1.8-2.2:1;
the preparation method of the modified medical stone comprises primary modification, secondary modification and tertiary modification;
a. one-time modification
Calcining Maifanitum powder in muffle furnace for 1.8-2.2 hr at 280-320 deg.C, standing at 1.4-1.8 deg.C for 28-32min, naturally recovering to room temperature, and finishing one-step modification;
sieving the medical stone powder with a 800-mesh sieve;
b. secondary modification
Soaking the medical stone powder subjected to primary modification in 8-12 times of hydrochloric acid solution for 3.3-3.7h, washing and drying, adding aluminum oxide, calcining at 280-320 ℃ for 0.8-1.2h, heating to 355-365 ℃ at a speed of 1.5-2.5 ℃/min, calcining for 1.4-1.6h, and naturally cooling to room temperature to finish the secondary modification step;
the mass concentration of the hydrochloric acid solution is 23-28%;
the mass ratio of the medical stone powder to the alumina after the primary modification is 2.4-2.6:1;
c. three times of modification
Adding pentaerythritol, sodium dodecyl sulfate and polyethylene glycol into the medical stone powder subjected to secondary modification, stirring for 3.8-4.2h at 670-720rpm and 78-83 ℃, and finally drying to finish three modification steps to obtain modified medical stone powder;
the mass ratio of the medical stone powder, pentaerythritol, sodium dodecyl sulfate and polyethylene glycol after secondary modification is 100:1.4-1.6:1.2-1.5:1.8-2.2.
2. Coffee extract dissolution
Mixing the coffee extract with 18-22 times of deionized water, and stirring at 1100-1250rpm for 18-22min to obtain coffee extract solution;
the coffee extract is sieved by a 800-mesh sieve, the chlorogenic acid content is 61.5-62.4%, and the caffeine content is 3.3-3.5%.
3. Preparation of functional agents
Mixing the supporting agent with coffee extract solution, heating to 58-62deg.C, controlling stirring speed to 970-1030rpm, and stirring for 24-28min to obtain functional agent;
the mass ratio of the loading agent to the coffee extract solution is 1:6-8.
4. Preparation of functional masterbatch
Mixing nylon slices, a functional agent, zinc stearate, magnesium stearate and butyl hydroxy anisole, adding into a double-screw extruder, controlling the melting temperature to be 256-260 ℃, carrying out melt blending for 40-44min, and carrying out extrusion granulation at the screw speed of 236-240rpm to obtain functional master batches;
the mass ratio of the chinlon slices to the functional agents to the zinc stearate to the magnesium stearate to the butyl hydroxy anisole is 100:4.3-4.6:2.9-3.1:2.8-3.2:4.8-5.1.
5. Preparing modified functional master batch
Placing the functional master batch into 4-6 times volume of impregnating solution, heating to 96-100 ℃ at the speed of 1.4-1.6 ℃/min, impregnating for 6-10min, cooling to 68-72 ℃ at the speed of 0.4-0.6 ℃/min, impregnating for 23-27min, placing into a vacuum homogenizer for homogenizing treatment, filtering, washing and drying after vacuum homogenizing is finished to obtain modified functional master batch;
the homogenizing treatment is carried out for 4-6min, the homogenizing vacuum degree is 17-22Kpa, the rotating speed is 1740-1860rpm, and the homogenizing times are 3 times;
the impregnating solution comprises phytic acid, algal polysaccharide, sodium chloride, microcrystalline cellulose, sodium carboxymethyl cellulose and deionized water;
the mass ratio of the phytic acid, the algal polysaccharide, the sodium chloride, the microcrystalline cellulose, the sodium carboxymethyl cellulose, the octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate and the deionized water is 0.8-1.1:1.2-1.4:2-2.2:8-12:3-5:0.6-0.8:57-62.
6. Spinning process
Spinning the modified functional master batch at 248-252 ℃ and 1770-1830m/min to obtain the large biological nylon fiber containing coffee active ingredients.
Compared with the prior art, the invention has the beneficial effects that:
1. the antibacterial rate of the prepared large biological nylon fiber containing the coffee active ingredient for staphylococcus aureus is 93.9-94.8%, and the antibacterial rate for candida albicans is 93.4-93.7%; after 50 times of standard washing, the antibacterial rate for staphylococcus aureus is 88.2-89.6%, and the antibacterial rate for candida albicans is 86.9-88.4%;
2. the prepared large biological nylon fiber containing the coffee active ingredient has the breaking strength of 12.2-12.8cN/dtex and the breaking elongation of 38.8-40.7%; standing for 7d at 60 ℃ and 75% humidity, wherein the breaking strength is 11.8-12.5cN/dtex, and the breaking elongation is 37.4-39.9%; the ultraviolet irradiation intensity is 600W/m 2 Irradiation ofAfter 6 hours, the breaking strength is 10.9-11.7cN/dtex, and the breaking elongation is 31.8-35.8%;
3. the prepared large biological nylon fiber containing the coffee active ingredient has excellent antistatic performance and surface resistivity of 2.5-2.8x10 7
Detailed Description
For a clearer understanding of the technical features, objects and effects of the present invention, specific embodiments of the present invention will be described.
Example 1A coffee-containing active ingredient macrobioson fiber and method for producing the same
1. Preparation of the supporting agent
(1) Preparation of premix
The preparation method of the loading agent comprises the steps of firstly carrying out microwave treatment on bentonite and nano silicon dioxide, wherein the microwave power is 1700MHz, the microwave time is 60s, then carrying out liquid nitrogen ball milling treatment, controlling the temperature of the liquid nitrogen ball mill to be minus 158 ℃, controlling the ball-material ratio to be 8:1, the rotating speed to be 180rpm, and the ball milling time to be 15min, thus obtaining a premix;
the mass ratio of the bentonite to the nano silicon dioxide is 1:1, a step of;
the bentonite is a mixture of sodium bentonite and calcium bentonite, and the mass ratio of the sodium bentonite to the calcium bentonite is 1:1;
(2) Mixing material
Mixing the premix and modified Maifanitum uniformly, and performing high-frequency electromagnetic oscillation treatment with oscillation frequency of 12MHz and oscillation time of 7min, and maximum current density of 14A/cm 2 Completing the mixing step to prepare a loading agent;
the mass ratio of the modified medical stone to the premix is 2:1;
the preparation method of the modified medical stone comprises primary modification, secondary modification and tertiary modification;
a. one-time modification
Calcining Maifanitum powder in muffle furnace for 2 hr at 320 deg.C, standing at 1.6deg.C for 30min, naturally recovering to room temperature, and finishing primary modification;
sieving the medical stone powder with a 800-mesh sieve;
b. secondary modification
Soaking the medical stone powder subjected to primary modification in hydrochloric acid solution with the volume of 10 times for 3.5 hours, washing and drying, adding aluminum oxide, calcining for 1 hour at 300 ℃, heating to 360 ℃ at the speed of 2 ℃/min, calcining for 1.5 hours, and naturally cooling to room temperature to finish the secondary modification step;
the mass concentration of the hydrochloric acid solution is 25%;
the mass ratio of the medical stone powder to the alumina after the primary modification is 2.5:1;
c. three times of modification
Adding pentaerythritol, sodium dodecyl sulfate and polyethylene glycol into the medical stone powder subjected to secondary modification, stirring for 4 hours at the stirring speed of 700rpm and the stirring temperature of 80 ℃, and finally drying to finish the three modification steps to obtain modified medical stone powder;
the mass ratio of the medical stone powder after the secondary modification to the pentaerythritol to the sodium dodecyl sulfate to the polyethylene glycol is 100:1.5:1.3:2.
2. Coffee extract dissolution
Mixing the coffee extract with deionized water of 20 times volume, controlling stirring speed to 1200rpm, and stirring for 20min to obtain coffee extract solution;
the coffee extract is sieved by a 800-mesh sieve, the chlorogenic acid content is 62%, and the caffeine content is 3.4%.
3. Preparation of functional agents
Mixing the loading agent with the coffee extract solution, heating to 60deg.C, controlling stirring speed to 1000rpm, and stirring for 26min to obtain functional agent;
the mass ratio of the loading agent to the coffee extract solution is 1:7.
4. Preparation of functional masterbatch
Mixing nylon slices, a functional agent, zinc stearate, magnesium stearate and butyl hydroxy anisole, adding into a double-screw extruder, controlling the melting temperature to 258 ℃, carrying out melt blending for 42min, and carrying out extrusion granulation at the screw speed of 238rpm to obtain functional master batch;
the mass ratio of the chinlon slices to the functional agents to the zinc stearate to the magnesium stearate to the butyl hydroxy anisole is 100:4.5:3:3: 5.
5. preparing modified functional master batch
Placing the functional master batch in impregnating solution with the volume of 5 times, heating to 98 ℃ at the speed of 1.5 ℃/min, impregnating for 8min, then cooling to 70 ℃ at the speed of 0.5 ℃/min, impregnating for 25min, placing in a vacuum homogenizer for homogenizing treatment, filtering, washing and drying after the vacuum homogenizing is finished to obtain the modified functional master batch;
the homogenizing treatment is carried out for 5min, the homogenizing vacuum degree is 20Kpa, the rotating speed is 1800rpm, and the homogenizing times are 3 times;
the impregnating solution comprises phytic acid, algal polysaccharide, sodium chloride, microcrystalline cellulose, sodium carboxymethyl cellulose and deionized water;
the mass ratio of the phytic acid, the algal polysaccharide, the sodium chloride, the microcrystalline cellulose, the sodium carboxymethyl cellulose, the octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate and the deionized water is 1:1.3:2.1:10:4:0.7:60.
6. Spinning process
Spinning the modified functional master batch at the spinning temperature of 250 ℃ and the spinning speed of 1800m/min to obtain the large biological nylon fiber containing the coffee active ingredient.
Example 2A macrobiosurful chinlon fiber containing coffee active ingredient and method for preparing the same
1. Preparation of the supporting agent
(1) Preparation of premix
The preparation method of the loading agent comprises the steps of firstly carrying out microwave treatment on bentonite and nano silicon dioxide, wherein the microwave power is 1800MHz, the microwave time is 58s, then carrying out liquid nitrogen ball milling treatment, controlling the temperature of the liquid nitrogen ball milling machine to be-160 ℃, controlling the ball-material ratio to be 10:1, the rotating speed to be 200rpm and the ball milling time to be 13min, and preparing a premix;
the mass ratio of the bentonite to the nano silicon dioxide is 1:0.5;
the bentonite is a mixture of sodium bentonite and calcium bentonite, and the mass ratio of the sodium bentonite to the calcium bentonite is 1:0.5;
(2) Mixing material
Mixing the premix and modified Maifanitum uniformly, and performing high-frequency electromagnetic oscillation treatment with oscillation frequency of 14MHz and oscillation time of 6min, and maximum current density of 16A/cm 2 Completing the mixing step to prepare a loading agent;
the mass ratio of the modified medical stone to the premix is 2.2:1;
the preparation method of the modified medical stone comprises primary modification, secondary modification and tertiary modification;
a. one-time modification
Calcining Maifanitum powder in muffle furnace for 2.2 hr at 300 deg.C, immediately standing at 1.8deg.C for 28min, naturally recovering to room temperature, and finishing primary modification;
sieving the medical stone powder with a 800-mesh sieve;
b. secondary modification
Soaking the medical stone powder subjected to primary modification in hydrochloric acid solution with the volume of 12 times for 3.3 hours, washing and drying, adding aluminum oxide, calcining at 320 ℃ for 0.8 hour, heating to 365 ℃ at the speed of 2.5 ℃/min, calcining for 1.4 hours, and naturally cooling to room temperature to finish the secondary modification step;
the mass concentration of the hydrochloric acid solution is 28%;
the mass ratio of the medical stone powder to the alumina after the primary modification is 2.6:1;
c. three times of modification
Adding pentaerythritol, sodium dodecyl sulfate and polyethylene glycol into the medical stone powder subjected to secondary modification, stirring for 4.2 hours at 670rpm and 83 ℃, and finally drying to finish the three modification steps to obtain modified medical stone powder;
the mass ratio of the medical stone powder, the pentaerythritol, the sodium dodecyl sulfate and the polyethylene glycol after the secondary modification is 100:1.6:1.5:2.2.
2. Coffee extract dissolution
Mixing the coffee extract with 22 times of deionized water, controlling stirring speed to 1250rpm, and stirring for 18min to obtain coffee extract solution;
the coffee extract is sieved by a 800-mesh sieve, the chlorogenic acid content is 62.4%, and the caffeine content is 3.3%.
3. Preparation of functional agents
Mixing the loading agent with the coffee extract solution, heating to 62 ℃, controlling the stirring speed to 1030rpm, and stirring for 24min to obtain the functional agent;
the mass ratio of the loading agent to the coffee extract solution is 1:8.
4. Preparation of functional masterbatch
Mixing nylon slices, a functional agent, zinc stearate, magnesium stearate and butyl hydroxy anisole, adding into a double-screw extruder, controlling the melting temperature to 260 ℃, carrying out melt blending for 40min, and carrying out extrusion granulation at the screw speed of 240rpm to obtain functional master batch;
the mass ratio of the chinlon slices to the functional agents to the zinc stearate to the magnesium stearate to the butyl hydroxy anisole is 100:4.6:3.1:3.2:4.8.
5. preparing modified functional master batch
Placing the functional master batch in an impregnating solution with the volume of 6 times, heating to 100 ℃ at the speed of 1.6 ℃/min, impregnating for 6min, then cooling to 72 ℃ at the speed of 0.6 ℃/min, impregnating for 23min, placing in a vacuum homogenizer for homogenizing treatment, filtering, washing and drying after the vacuum homogenizing is finished to obtain the modified functional master batch;
the homogenizing treatment is carried out for 6min, the homogenizing vacuum degree is 17Kpa, the rotating speed is 1740rpm, and the homogenizing times are 3 times;
the impregnating solution comprises phytic acid, algal polysaccharide, sodium chloride, microcrystalline cellulose, sodium carboxymethyl cellulose and deionized water;
the mass ratio of the phytic acid, the algal polysaccharide, the sodium chloride, the microcrystalline cellulose, the sodium carboxymethyl cellulose, the octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate and the deionized water is 1.1:1.4:2:12:3:0.8:62.
6. Spinning process
Spinning the modified functional master batch at 248 ℃ and 1830m/min to obtain the large biological nylon fiber containing the coffee active ingredient.
Example 3A coffee-containing active ingredient macrobioson fiber and method for producing the same
1. Preparation of the supporting agent
(1) Preparation of premix
The preparation method of the loading agent comprises the steps of firstly carrying out microwave treatment on bentonite and nano silicon dioxide, wherein the microwave power is 1600MHz, the microwave time is 62s, then carrying out liquid nitrogen ball milling treatment, controlling the temperature of the liquid nitrogen ball milling machine to be-156 ℃, controlling the ball-material ratio to be 6:1, the rotating speed to be 160rpm, and the ball milling time to be 17min, thus obtaining a premix;
the mass ratio of the bentonite to the nano silicon dioxide is 1:2;
the bentonite is a mixture of sodium bentonite and calcium bentonite, and the mass ratio of the sodium bentonite to the calcium bentonite is 1:2;
(2) Mixing material
Mixing the premix and modified Maifanitum uniformly, and performing high-frequency electromagnetic oscillation treatment with oscillation frequency of 10MHz and oscillation time of 8min, and maximum current density of 12A/cm 2 Completing the mixing step to prepare a loading agent;
the mass ratio of the modified medical stone to the premix is 1.8:1;
the preparation method of the modified medical stone comprises primary modification, secondary modification and tertiary modification;
a. one-time modification
Calcining Maifanitum powder in muffle furnace for 1.8 hr at 280 deg.C, standing at 1.4deg.C for 32min, naturally recovering to room temperature, and finishing primary modification;
sieving the medical stone powder with a 800-mesh sieve;
b. secondary modification
Soaking the medical stone powder subjected to primary modification in 8 times of hydrochloric acid solution for 3.7 hours, washing and drying, adding aluminum oxide, calcining at 280 ℃ for 1.2 hours, heating to 355 ℃ at a speed of 1.5 ℃/min, calcining for 1.6 hours, and naturally cooling to room temperature to finish the secondary modification step;
the mass concentration of the hydrochloric acid solution is 23%;
the mass ratio of the medical stone powder to the alumina after the primary modification is 2.4:1;
c. three times of modification
Adding pentaerythritol, sodium dodecyl sulfate and polyethylene glycol into the medical stone powder subjected to secondary modification, stirring for 3.8 hours at the stirring speed of 720rpm and the stirring temperature of 78 ℃, and finally drying to finish the three modification steps to obtain modified medical stone powder;
the mass ratio of the medical stone powder, the pentaerythritol, the sodium dodecyl sulfate and the polyethylene glycol after the secondary modification is 100:1.4:1.2:1.8.
2. Coffee extract dissolution
Mixing the coffee extract with 18 times of deionized water, controlling stirring speed to 1100rpm, and stirring for 22min to obtain coffee extract solution;
the coffee extract is sieved by a 800-mesh sieve, the chlorogenic acid content is 61.5%, and the caffeine content is 3.5%.
3. Preparation of functional agents
Mixing the loading agent with the coffee extract solution, heating to 58 ℃, controlling the stirring speed to 970rpm, and stirring for 28min to obtain the functional agent;
the mass ratio of the loading agent to the coffee extract solution is 1:6.
4. Preparation of functional masterbatch
Mixing nylon slices, a functional agent, zinc stearate, magnesium stearate and butyl hydroxy anisole, adding into a double-screw extruder, controlling the melting temperature to be 256 ℃, carrying out melt blending for 44min, and carrying out extrusion granulation at the screw speed of 236rpm to obtain functional master batch;
the mass ratio of the chinlon slices to the functional agents to the zinc stearate to the magnesium stearate to the butyl hydroxy anisole is 100:4.3:2.9:2.8:5.1.
5. preparing modified functional master batch
Placing the functional master batch in an impregnating solution with the volume being 4 times that of the functional master batch, heating to 96 ℃ at the speed of 1.4 ℃/min, impregnating for 10min, then cooling to 68 ℃ at the speed of 0.4 ℃/min, impregnating for 27min, placing in a vacuum homogenizer for homogenizing treatment, filtering, washing and drying after the vacuum homogenizing treatment is finished to obtain the modified functional master batch;
the homogenizing treatment is carried out for 4min, the homogenizing vacuum degree is 22Kpa, the rotating speed is 1860rpm, and the homogenizing times are 3 times;
the impregnating solution comprises phytic acid, algal polysaccharide, sodium chloride, microcrystalline cellulose, sodium carboxymethyl cellulose and deionized water;
the mass ratio of the phytic acid, the algal polysaccharide, the sodium chloride, the microcrystalline cellulose, the sodium carboxymethyl cellulose, the octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate and the deionized water is 0.8:1.2:2.2:8:5:0.6:57.
6. Spinning process
Spinning the modified functional master batch at 252 ℃ and at 1770m/min to obtain the large biological nylon fiber containing the coffee active ingredient.
Comparative example 1
On the basis of the embodiment 1, the method is changed in that the step of preparing the loading agent is to uniformly mix bentonite, nano silicon dioxide and modified medical stone, wherein the mass ratio of the modified medical stone to the bentonite to the nano silicon dioxide is 2:0.5:0.5, and the rest operations are the same.
Comparative example 2
On the basis of the embodiment 1, the modification step of the medical stone is omitted, the untreated medical stone is directly adopted, and the rest operations are the same.
Comparative example 3
The modification step of the functional master batch is omitted and the rest operations are the same on the basis of the embodiment 1 except that the functional master batch is directly adopted for spinning.
Performance detection
(1) Antibacterial property
(2) High temperature resistance and light resistance
(3) Antistatic property
The percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. The preparation method of the large biological chinlon containing the coffee active ingredients is characterized by comprising the steps of preparing a loading agent, dissolving a coffee extract, preparing a functional agent, preparing a functional master batch, preparing a modified functional master batch and spinning;
the preparation of the loading agent comprises the steps of preparing a premix and mixing;
firstly, carrying out microwave treatment on bentonite and nano silicon dioxide, wherein the microwave power is 1600-1800MHz, the microwave time is 58-62s, then carrying out liquid nitrogen ball milling treatment, controlling the temperature of a liquid nitrogen ball mill to be-160-156 ℃, controlling the ball-material ratio to be 6-10:1, the rotating speed to be 160-200rpm, and the ball milling time to be 13-17min, thus obtaining the premix;
the mixing step comprises mixing the premix and modified Maifanitum uniformly, and performing high-frequency electromagnetic oscillation treatment with oscillation frequency of 10-14MHz for 6-8min and maximum current density of 12-16A/cm 2 Completing the mixing step to prepare a loading agent;
the preparation method of the modified functional master batch comprises the steps of placing the functional master batch in impregnating solution with the volume of 4-6 times, heating to 96-100 ℃ at the speed of 1.4-1.6 ℃/min, impregnating for 6-10min, cooling to 68-72 ℃ at the speed of 0.4-0.6 ℃/min, impregnating for 23-27min, homogenizing in a vacuum homogenizer, filtering, washing and drying to obtain the modified functional master batch after vacuum homogenization is finished;
the impregnating solution comprises phytic acid, algal polysaccharide, sodium chloride, microcrystalline cellulose, sodium carboxymethyl cellulose and deionized water.
2. The method for preparing the large biological nylon fiber containing the coffee active ingredient according to claim 1, wherein,
the preparation method of the modified medical stone comprises primary modification, secondary modification and tertiary modification;
the primary modification step is that medical stone powder is placed in a muffle furnace for calcination for 1.8-2.2h, the calcination temperature is 280-320 ℃, the calcined medical stone powder is immediately placed in an environment of 1.4-1.8 ℃ for 28-32min after the calcination is completed, and the medical stone powder is naturally restored to room temperature, so that the primary modification step is completed;
the secondary modification step is that medical stone powder after primary modification is placed in hydrochloric acid solution with the volume of 8-12 times to be soaked for 3.3-3.7 hours, alumina is added after washing and drying, then the mixture is calcined for 0.8-1.2 hours at the temperature of 280-320 ℃, the mixture is heated to 355-365 ℃ at the speed of 1.5-2.5 ℃/min to be calcined for 1.4-1.6 hours, and the mixture is naturally cooled to room temperature, so that the secondary modification step is completed;
the three-time modification step is to add pentaerythritol, sodium dodecyl sulfate and polyethylene glycol into the medical stone powder after the two-time modification, stir for 3.8-4.2h, the stirring speed is 670-720rpm, the stirring temperature is 78-83 ℃, and finally dry to complete the three-time modification step, thus obtaining the modified medical stone powder.
3. The method for preparing the large biological nylon fiber containing the coffee active ingredient according to claim 2, wherein,
in the primary modification step, the medical stone powder is sieved by a 800-mesh sieve;
in the secondary modification step, the mass concentration of the hydrochloric acid solution is 23-28%;
the mass ratio of the medical stone powder to the alumina after the primary modification is 2.4-2.6:1;
in the three-time modification step, the mass ratio of the medical stone powder, pentaerythritol, sodium dodecyl sulfate and polyethylene glycol after the secondary modification is 100:1.4-1.6:1.2-1.5:1.8-2.2.
4. The method for preparing the large biological nylon fiber containing the coffee active ingredient according to claim 1, wherein,
the mass ratio of the bentonite to the nano silicon dioxide is 1:0.5-2;
the bentonite is a mixture of sodium bentonite and calcium bentonite, and the mass ratio of the sodium bentonite to the calcium bentonite is 1:0.5-2;
the mass ratio of the modified medical stone to the premix is 1.8-2.2:1.
5. The method for preparing the large biological nylon fiber containing the coffee active ingredient according to claim 1, wherein,
in the step of preparing the modified functional master batch, the homogenization treatment is carried out for 4-6min, the homogenization vacuum degree is 17-22Kpa, the rotating speed is 1740-1860rpm, and the homogenization times are 3 times;
the mass ratio of the phytic acid, the algal polysaccharide, the sodium chloride, the microcrystalline cellulose, the sodium carboxymethyl cellulose, the octadecyl dimethyl hydroxyethyl quaternary ammonium nitrate and the deionized water is 0.8-1.1:1.2-1.4:2-2.2:8-12:3-5:0.6-0.8:57-62.
6. The method for preparing the large biological nylon fiber containing the coffee active ingredient according to claim 1, wherein,
the preparation method of the functional master batch comprises the steps of mixing nylon slices, a functional agent, zinc stearate, magnesium stearate and butyl hydroxy anisole, adding the mixture into a double-screw extruder, controlling the melting temperature to be 256-260 ℃, carrying out melt blending for 40-44min, controlling the screw rotating speed to be 236-240rpm, and carrying out extrusion granulation to obtain the functional master batch.
7. The method for preparing the large biological nylon fiber containing the coffee active ingredient according to claim 6, wherein,
the mass ratio of the chinlon slices to the functional agents to the zinc stearate to the magnesium stearate to the butyl hydroxy anisole is 100:4.3-4.6:2.9-3.1:2.8-3.2:4.8-5.1.
8. The method for preparing the large biological nylon fiber containing the coffee active ingredient according to claim 1, wherein,
the preparation method comprises mixing the loading agent with coffee extract solution, heating to 58-62deg.C, controlling stirring speed to 970-1030rpm, and stirring for 24-28min to obtain functional agent;
the mass ratio of the loading agent to the coffee extract solution is 1:6-8.
9. The method for preparing the large biological nylon fiber containing the coffee active ingredient according to claim 1, wherein,
the coffee extract dissolving step comprises mixing coffee extract with 18-22 times of deionized water, and stirring at 1100-1250rpm for 18-22min to obtain coffee extract solution;
the coffee extract is sieved by a 800-mesh sieve, the chlorogenic acid content is 61.5-62.4%, and the caffeine content is 3.3-3.5%.
10. The method for preparing the large biological nylon fiber containing the coffee active ingredient according to claim 1, wherein,
the spinning step is that the modified functional master batch is spun at 248-252 ℃ and at 1770-1830m/min to obtain the large biological nylon fiber containing coffee active ingredients.
CN202310624821.1A 2023-05-30 2023-05-30 Large biological nylon fiber containing coffee active ingredient and preparation method thereof Pending CN116463748A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310624821.1A CN116463748A (en) 2023-05-30 2023-05-30 Large biological nylon fiber containing coffee active ingredient and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310624821.1A CN116463748A (en) 2023-05-30 2023-05-30 Large biological nylon fiber containing coffee active ingredient and preparation method thereof

Publications (1)

Publication Number Publication Date
CN116463748A true CN116463748A (en) 2023-07-21

Family

ID=87182731

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310624821.1A Pending CN116463748A (en) 2023-05-30 2023-05-30 Large biological nylon fiber containing coffee active ingredient and preparation method thereof

Country Status (1)

Country Link
CN (1) CN116463748A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116903921A (en) * 2023-09-13 2023-10-20 山东科迈生物制浆有限公司 Pulp foam material and preparation method thereof
CN117343531A (en) * 2023-12-05 2024-01-05 潍坊瑞银纺织科技有限公司 Large biological PA master batch containing plant active ingredients and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108517578A (en) * 2018-04-20 2018-09-11 刘凡领 A kind of preparation method of modified medical stone base nylon fibre
CN108998852A (en) * 2018-06-29 2018-12-14 百事基材料(青岛)股份有限公司 Draft mixing nylon fibre and preparation method
CN110106705A (en) * 2019-04-30 2019-08-09 石雅琴 A kind of preparation method of bristles
CN112323171A (en) * 2020-11-06 2021-02-05 百事基材料(青岛)股份有限公司 Lavender-containing nylon fiber and preparation method thereof
CN112981590A (en) * 2021-03-23 2021-06-18 百事基材料(青岛)股份有限公司 Chinlon macrobio-fiber containing coffee active ingredient and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108517578A (en) * 2018-04-20 2018-09-11 刘凡领 A kind of preparation method of modified medical stone base nylon fibre
CN108998852A (en) * 2018-06-29 2018-12-14 百事基材料(青岛)股份有限公司 Draft mixing nylon fibre and preparation method
CN110106705A (en) * 2019-04-30 2019-08-09 石雅琴 A kind of preparation method of bristles
CN112323171A (en) * 2020-11-06 2021-02-05 百事基材料(青岛)股份有限公司 Lavender-containing nylon fiber and preparation method thereof
CN112981590A (en) * 2021-03-23 2021-06-18 百事基材料(青岛)股份有限公司 Chinlon macrobio-fiber containing coffee active ingredient and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116903921A (en) * 2023-09-13 2023-10-20 山东科迈生物制浆有限公司 Pulp foam material and preparation method thereof
CN116903921B (en) * 2023-09-13 2023-12-26 山东科迈生物制浆有限公司 Pulp foam material and preparation method thereof
CN117343531A (en) * 2023-12-05 2024-01-05 潍坊瑞银纺织科技有限公司 Large biological PA master batch containing plant active ingredients and preparation method thereof
CN117343531B (en) * 2023-12-05 2024-02-27 潍坊瑞银纺织科技有限公司 Large biological PA master batch containing plant active ingredients and preparation method thereof

Similar Documents

Publication Publication Date Title
CN116463748A (en) Large biological nylon fiber containing coffee active ingredient and preparation method thereof
CN111171531B (en) Seaweed polyester master batch and preparation process thereof
CN105084930B (en) A kind of preparation method of the modified fluorine gypsum powder for brushing gypsum
CN102524410B (en) Preparation method of soybean milk
CN111440339B (en) Tea polyphenol, naringin or emodin modified PET master batch and preparation process thereof
CN103668523B (en) The manufacture method of dry acrylic fiber fiber
CN107096574A (en) Photocatalyst formaldehyde removing composition and preparation method thereof
CN104775587A (en) Environment-friendly pollution-free PVC wallpaper capable of removing formaldehyde
CN108084871A (en) Environment protection oil paint
CN107216588A (en) A kind of new sound-absorbing material for building and preparation method thereof
CN111634917A (en) Preparation method of porous active silica gel
CN206328512U (en) A kind of negative ion antibiotic polyester fiber, negative ion antibiotic fabric and clothes
CN108585578B (en) High-strength pervious concrete additive and preparation method thereof
CN102718825A (en) Preparation method of hydrocortisone hemisuccinat
CN106283670A (en) A kind of preparation method of antibiotic finish of the fabric liquid
CN106669650A (en) Pretreatment method of ceramic microspheres serving as catalyst carrier
CN108249802A (en) It is a kind of for solubilized stabilizer of high concentration polyaluminum sulfate aluminum solutions and preparation method thereof
CN105648776A (en) Antibacterial and anti-ultraviolet finishing agent and method for preparing same
CN105755831A (en) Antibacterial deodorization type finishing agent and preparation method thereof
CN115521536A (en) Preparation process of antibacterial plastic color master batch formula
CN106893242A (en) A kind of aqueous abscess regulator suitable for synthetic leather
CN115323804B (en) Breathable ultraviolet-proof PU composite fabric and manufacturing process thereof
CN116516514A (en) Large biological polyester fiber containing coffee active ingredients and preparation method thereof
CN117924855B (en) Breathable black mask for automobile and preparation method thereof
CN106668957A (en) Far infrared anti-microbial low-temperature thermoplastic material for orthopedic therapy and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination