CN112030262A - Bodhi-containing polyester fiber and preparation method thereof - Google Patents

Bodhi-containing polyester fiber and preparation method thereof Download PDF

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Publication number
CN112030262A
CN112030262A CN202011050035.8A CN202011050035A CN112030262A CN 112030262 A CN112030262 A CN 112030262A CN 202011050035 A CN202011050035 A CN 202011050035A CN 112030262 A CN112030262 A CN 112030262A
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bodhi
porous
polyester fiber
preparing
preparation
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黄效华
甄丽
王丙伟
黄效龙
刘彦明
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Zhongke Textile Research Institute Qingdao Co ltd
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Zhongke Textile Research Institute Qingdao Co ltd
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    • 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
    • D01F6/92Monocomponent 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 polyesters
    • 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

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention provides a preparation method of bodhi-containing polyester fiber, which comprises the steps of preparing porous silicon dioxide microspheres; fully mixing the secondary distilled water and the ethanol to prepare ethanol solution; adding hexadecyl trimethyl ammonium bromide and ammonia water as catalysts into the ethanol solution, dropwise adding ethyl orthosilicate, drying the reacted solid, and calcining the dried solid to obtain the porous silicon dioxide. Also comprises a preparation step of the porous molecular nest containing the linden extract; adding porous silicon dioxide powder and ethanol water solution into a ball mill for grinding, shearing and dispersing to obtain porous nano material dispersion liquid; shearing and dispersing the saturated aqueous solution of the linden extract, the porous nano material dispersion liquid, the coupling agent and the surfactant to obtain the nano material dispersion liquid containing the linden extract, and volatilizing the solvent to obtain the dried porous molecular nest containing the linden extract. The prepared fiber finished product has high mechanical strength and good hygroscopicity.

Description

Bodhi-containing polyester fiber and preparation method thereof
Technical Field
The invention belongs to the technical field of fiber manufacturing, and particularly relates to a bodhi-containing polyester fiber and a preparation method thereof.
Background
The basic composition of the terylene is polyethylene terephthalate, the molecular formula is HO-H2C-H2C-O [ -OC-Ph-COOCH2CH2O- ] n, the terylene is called polyester fiber (PET) because a large amount of ester groups exist on the molecular chain, the chemical structural formula of the long chain molecule is H (OCH2CCOCO) NOCH2CH2OH, the relative molecular weight of the polyester used for the fiber is generally about 18000-25000, the molecular weight of the wool-like terylene is lower, and the molecular weight of the industrial terylene is higher. In practice, small amounts of monomers and oligomers are also present. These oligomers have a relatively low degree of polymerization and are present in cyclic form. The polyethylene terephthalate can be prepared by polycondensation after preparing 9BHET (ethylene terephthalate) from terephthalic acid (PTA) and Ethylene Glycol (EG) by a direct esterification method.
Bodhi (with the academic name: Ficus religiosa L.) is a large tree plant of Ficus genus, which is attached to other trees when young, with the height of 15-25 m, leaf leatheroid, triangle-shaped oval, three primary veins and 5-7 pairs of lateral veins; the petiole is fine, the ficus microcarpa fruit is spherical to oblate, the style is fine, and the stigma is narrow. The main body of the artificial tooth is made of phyllanthus, is in a triangular oval shape, is 9-17 cm long, 8-12 cm wide, is dark green in surface, bright, green in back, sharp at the front end, tail-shaped in a manner that the top extends, 2-5 cm long at the tail tip, wide and truncated at the base to be shallow heart-shaped, is complete in edge or wavy, and has three primary veins and 5-7 pairs of lateral veins; the petiole is slender, and the related joint is as long as or longer than the leaf; the leaves are small, oval, pointed at the tip. The Ficus microcarpa fruits are spherical to oblate, have the diameter of 1-1.5 cm, are red and smooth when ripe; basal bract 3, oval; the total stem length is about 4-9 mm; the flower has less male flowers, grows near the mouth, has no handle, 2-3 flower quilts are split, and has an inner roll, 1 stamen and short filaments; goiter with handle, 3-4 cracks of floral quilt, smooth ovary, spherical shape, short style, and 2 cracks of stigma; the female flower has no handle, the flower quilt sheet is 4, the shape of the flower quilt sheet is wide and needle-shaped, and the ovary is smooth and spherical. The stigmas are fine and narrow. The flowering period is 3-4 months, and the fruit period is 5-6 months.
The technology of fiber modification using linden extract as a plant modifier is not yet established. Particularly, in the preparation technology of the modified polyester fiber, the bodhi extract has poor dispersion uniformity in the preparation process, and the bodhi extract accumulation can cause great reduction of the mechanical properties of the fiber, thereby causing weak functionality and difficult playing due roles. The applicant finds the following technical defects difficult to overcome in the development process: (1) the bodhi extract has poor dispersion uniformity and high loss rate in the process of preparing the polyester fiber; (2) the moisture absorption of the finished fiber product is poor; (3) the polyester fiber prepared by modifying the linden extract has low mechanical strength; (4) the stability is poor.
Disclosure of Invention
In order to solve the problems in the prior art and further optimize the prior art, the invention provides the bodhi-containing polyester fiber and the preparation method thereof, which aim to realize the following purposes:
the dispersion uniformity of the bodhi extract in the polyester fiber is improved, the loss rate of the bodhi extract in the process of preparing the polyester fiber is reduced, the moisture absorption performance and the mechanical strength of the modified polyester fiber are improved, and the antibacterial stability of the modified polyester fiber is improved.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of bodhi-containing polyester fibers comprises the following steps:
step 1, preparation of porous silica microspheres
Fully mixing the secondary distilled water and the ethanol to prepare ethanol solution; the volume ratio of the secondary distilled water to the ethanol is 9-10: 7-8.
Adding Cetyl Trimethyl Ammonium Bromide (CTAB) into an ethanol solution, adding ammonia water as a catalyst, stirring by magnetic force at the stirring speed of 2000rpm, dropwise adding Tetraethoxysilane (TEOS) during stirring, continuously stirring for reacting for 4-4.5h, drying at 80-85 ℃, feeding the dried solid into a muffle furnace, heating to 550-580 ℃ at the speed of 1-2 ℃/min, and calcining at the temperature for 6-6.5h to prepare porous silicon dioxide; the porous silica obtained: specific surface area of 800-2A particle size of 160-180nm and a pore diameter of 8-13 nm.
The addition amount of the cetyl trimethyl ammonium bromide is 13.5 to 14.8 percent of the mass of the ethanol solution;
the addition amount of the ammonia water is 8.5-9.5% of the mass of the ethanol solution, and the concentration of the ammonia water is 37.58 g/L;
the adding amount of the ethyl orthosilicate is 50-55% of the mass of the ethanol solution.
Step 2, preparation of porous molecular nest containing linden extract
(1) Preparation of bodhi extract solution: preparing the linden extract into a saturated aqueous solution of the linden extract by using deionized water, wherein the temperature of the deionized water is 20-24 ℃. The linden extract: contains triterpenoid saponins 45% and sesquiterpene glycosides 32%.
(2) Preparation of a dispersion of porous silica: adding porous silicon dioxide powder and ethanol water solution into a ball mill for grinding, shearing and dispersing to obtain porous nano material dispersion liquid; the mass ratio of the porous silicon dioxide powder to the ethanol water solution is 2: 6-8; the concentration of the ethanol water solution is 96-97% (mass percentage concentration).
(3) Preparation of porous molecular nest: shearing and dispersing the saturated aqueous solution of the linden extract, the porous nano material dispersion, the coupling agent and the surfactant to obtain a nano material dispersion containing the linden extract, and volatilizing the solvent to obtain a dry porous molecular nest containing the linden extract; the mass ratio of the saturated aqueous solution of the linden extract, the dispersed porous nano material, the coupling agent and the surfactant is 10-12:6-8:0.4-0.7: 0.6-1.1; the coupling agent is a silane coupling agent KH-570, and the surfactant is oleic acid.
Step 3, preparing modified polyester master batch
(1) Uniformly mixing polyester chips and porous molecular nests containing linden extracts according to the mass ratio of 7-9:1 to obtain a mixture A; the terylene slice comprises the following components: purity is 97%, and particle diameter is 0.1-0.15 cm.
(2) Mixing tea polyphenol, dodecyl dimethyl betaine and montmorillonite according to the weight ratio of 3-3.5: 1-2: 5-6, and carrying out ultrasonic treatment at the ultrasonic frequency of 100-120KHZ and the ultrasonic temperature of 72-74 ℃ for 20-25min to obtain a mixture B.
The montmorillonite is as follows: the fineness is 800 and 1000 meshes.
(3) Mixing the mixture A, the mixture B, the antioxidant and the dispersant according to the weight ratio of 10-12: 1-2.5: 0.8-1.2: mixing at a mass ratio of 0.5-0.8, stirring uniformly, and heating by turning on microwave under anaerobic condition with a microwave frequency of 3005-3400MHz for 10-20min to obtain a mixture C.
The antioxidant is as follows: the anti-aging agent is prepared by mixing pentaerythritol, didodecanol ester and tridecyl ester according to the mass ratio of 4:1: 1.5.
The dispersing agent is as follows: is stearic acid monoglyceride.
(4) And (3) introducing the mixture C into a double-screw extrusion machine, controlling the melting temperature of 259-262 ℃, carrying out melt blending for 40-45min, and carrying out extrusion granulation at the screw rotation speed of 180-210 rpm to obtain the modified polyester master batch.
Step 4, spinning
Heating and drying the modified polyester master batch, then loading the dried modified polyester master batch into a double-screw extrusion machine, heating and melting, and spinning through a spinneret plate-drafting two-step method, wherein the spinning temperature is 278-284 ℃, the spinning speed is 880-900m/min, the hot plate temperature is 80-85 ℃ during drafting, the hot plate temperature is 140-145 ℃, and the drafting multiple is 4 times.
By adopting the technical scheme, the invention has the beneficial effects that:
1. the preparation method of the bodhi-containing polyester fiber adopts the molecular nest technology, greatly improves the dispersion uniformity of bodhi extract, and has low loss rate of the bodhi extract.
2. The polyester fiber containing bodhi prepared by the invention has good moisture absorption performance; compared with unmodified polyester fiber, the moisture regain is 0.6-0.8% under standard conditions, and the moisture regain is 0.9-1.5% under the condition that the relative humidity is 100%.
3. The polyester fiber containing bodhi prepared by the invention has the fiber strength of 8.5-8.9cN/tex, the elongation at break of 22-24 percent and the elastic modulus of 144-146 cN/dtex.
4. The polyester fiber containing the bodhi prepared by the invention has good bacteriostatic property and good bacteriostatic effect on staphylococcus aureus, escherichia coli, candida albicans and mycobacterium tuberculosis. The antibacterial stability is good, and the prepared polyester fiber containing bodhi still keeps high antibacterial performance after being washed by 100 times of water at normal temperature.
Detailed Description
The invention is further illustrated below with reference to specific examples.
EXAMPLE 1 preparation of bodhi-containing polyester fiber
Step 1, preparation of porous silica microspheres
Fully mixing the secondary distilled water and the ethanol to prepare ethanol solution; the volume ratio of the secondary distilled water to the ethanol is 9: 7.
Adding hexadecyl trimethyl ammonium bromide into an ethanol solution, adding ammonia water as a catalyst, magnetically stirring at the stirring speed of 2000rpm, dropwise adding tetraethoxysilane during stirring, continuously stirring for reacting for 4 hours, drying at 80 ℃, feeding dried solids into a muffle furnace, heating to 550 ℃ at the speed of 1 ℃/min, and calcining at the temperature for 6 hours to obtain porous silicon dioxide; the porous silica obtained: specific surface area of 800-2A particle size of 160-180nm and a pore diameter of 8-13 nm.
The addition amount of the hexadecyl trimethyl ammonium bromide is 13.5 percent of the mass of the ethanol solution;
the addition amount of the ammonia water is 9.5 percent of the mass of the ethanol solution, and the concentration of the ammonia water is 37.58 g/L;
the adding amount of the ethyl orthosilicate is 50% of the mass of the ethanol solution.
Step 2, preparation of porous molecular nest containing linden extract
(1) Preparation of bodhi extract solution: the bodhi extract is prepared into a saturated aqueous solution of the bodhi extract by using deionized water, and the temperature of the deionized water is 20 ℃. The linden extract: contains triterpenoid saponins 45% and sesquiterpene glycosides 32%.
(2) Preparation of a dispersion of porous silica: adding porous silicon dioxide powder and ethanol water solution into a ball mill for grinding, shearing and dispersing to obtain porous nano material dispersion liquid; the mass ratio of the porous silicon dioxide powder to the ethanol aqueous solution is 2: 6; the concentration of the ethanol water solution is 96 percent (mass percentage concentration).
(3) Preparation of porous molecular nest: shearing and dispersing the saturated aqueous solution of the linden extract, the porous nano material dispersion, the coupling agent and the surfactant to obtain a nano material dispersion containing the linden extract, and volatilizing the solvent to obtain a dry porous molecular nest containing the linden extract; the mass ratio of the saturated aqueous solution of the linden extract, the dispersed porous nano material, the coupling agent and the surfactant is 10:6:0.4: 1.1; the coupling agent is a silane coupling agent KH-570, and the surfactant is oleic acid.
Step 3, preparing modified polyester master batch
(1) Uniformly mixing polyester chips and porous molecular nests containing linden extracts according to the mass ratio of 7:1 to obtain a mixture A; the terylene slice comprises the following components: purity is 97%, and particle diameter is 0.1-0.15 cm.
(2) Mixing tea polyphenol, dodecyl dimethyl betaine and montmorillonite according to the weight ratio of 3: 1: 5, and performing ultrasonic treatment at an ultrasonic frequency of 100KHZ and an ultrasonic temperature of 72 ℃ for 25min to obtain a mixture B.
The montmorillonite is as follows: the fineness is 800-900 meshes.
(3) Mixing the mixture A, the mixture B, the antioxidant and the dispersant according to the proportion of 10: 1: 1.2: mixing at a mass ratio of 0.5, stirring, heating with microwave at 3005MHz for 10min under anaerobic condition, and collecting the mixture C.
The antioxidant is as follows: the anti-aging agent is prepared by mixing pentaerythritol, didodecanol ester and tridecyl ester according to the mass ratio of 4:1: 1.5.
The dispersing agent is as follows: is stearic acid monoglyceride.
(4) And (3) introducing the mixture C into a double-screw extrusion machine, controlling the melting temperature to be 262 ℃, carrying out melt blending for 45min at the screw rotation speed of 180 revolutions per minute, and carrying out extrusion granulation to obtain the modified polyester master batch.
Step 4, spinning
Heating and drying the modified polyester master batch, then loading the dried modified polyester master batch into a double-screw extruder, heating and melting, and spinning by a spinneret plate-drafting two-step method, wherein the spinning temperature is 278 ℃, the spinning speed is 880m/min, the hot plate temperature is 80 ℃ during drafting, the hot plate temperature is 140 ℃, and the drafting multiple is 4 times.
The polyester fiber containing bodhi prepared by the embodiment has good moisture absorption performance; compared with unmodified polyester fiber, the moisture regain is 0.6 percent under standard conditions, and the moisture regain is 0.9 percent under the condition that the relative humidity is 100 percent; the prepared polyester fiber containing bodhi has high mechanical strength, fiber strength of 8.5cN/tex, elongation at break of 22% and elastic modulus of 144 cN/dtex; the bacteriostatic property is good, and the bacteriostatic rate on staphylococcus aureus, escherichia coli, candida albicans and mycobacterium tuberculosis is more than 92 percent; the antibacterial stability is good, and the prepared polyester fiber containing bodhi is washed by 100 times of water at normal temperature, and the antibacterial rate is still kept above 85%.
Example 2 preparation method of Ficus religiosa-containing polyester fiber
Step 1, preparation of porous silica microspheres
Fully mixing the secondary distilled water and the ethanol to prepare ethanol solution; the volume ratio of the secondary distilled water to the ethanol is 9: 7.
Adding hexadecyl trimethyl ammonium bromide into an ethanol solution, adding ammonia water as a catalyst, magnetically stirring at the stirring speed of 2000rpm, dropwise adding tetraethoxysilane during stirring, continuously stirring for reacting for 4.5 hours, drying at 80 ℃, feeding dried solids into a muffle furnace, heating to 570 ℃ at the speed of 2 ℃/min, and calcining at the temperature for 6 hours to obtain porous silicon dioxide; the porous silica obtained: specific surface area of 800-2A particle size of 160-180nm and a pore diameter of 8-13 nm.
The addition amount of the hexadecyl trimethyl ammonium bromide is 14.5 percent of the mass of the ethanol solution;
the addition amount of the ammonia water is 8.8 percent of the mass of the ethanol solution, and the concentration of the ammonia water is 37.58 g/L;
the adding amount of the ethyl orthosilicate is 55 percent of the mass of the ethanol solution.
Step 2, preparation of porous molecular nest containing linden extract
(1) Preparation of bodhi extract solution: the bodhi extract is prepared into a saturated aqueous solution of the bodhi extract by using deionized water, and the temperature of the deionized water is 22 ℃. The linden extract: contains triterpenoid saponins 45% and sesquiterpene glycosides 32%.
(2) Preparation of a dispersion of porous silica: adding porous silicon dioxide powder and ethanol water solution into a ball mill for grinding, shearing and dispersing to obtain porous nano material dispersion liquid; the mass ratio of the porous silicon dioxide powder to the ethanol aqueous solution is 2: 7; the concentration of the ethanol water solution is 96 percent (mass percentage concentration).
(3) Preparation of porous molecular nest: shearing and dispersing the saturated aqueous solution of the linden extract, the porous nano material dispersion, the coupling agent and the surfactant to obtain a nano material dispersion containing the linden extract, and volatilizing the solvent to obtain a dry porous molecular nest containing the linden extract; the mass ratio of the saturated aqueous solution of the linden extract, the dispersed porous nano material, the coupling agent and the surfactant is 11:7:0.6: 0.9; the coupling agent is a silane coupling agent KH-570, and the surfactant is oleic acid.
Step 3, preparing modified polyester master batch
(1) Uniformly mixing polyester chips and porous molecular nests containing linden extracts according to the mass ratio of 8:1 to obtain a mixture A; the terylene slice comprises the following components: purity is 97%, and particle diameter is 0.1-0.15 cm.
(2) Mixing tea polyphenol, dodecyl dimethyl betaine and montmorillonite according to the weight ratio of 3: 1.5: 5, and performing ultrasonic treatment at an ultrasonic frequency of 110KHZ and an ultrasonic temperature of 73 ℃ for 22min to obtain a mixture B.
The montmorillonite is as follows: the fineness is 900 and 1000 meshes.
(3) Mixing the mixture A, the mixture B, the antioxidant and the dispersant according to the proportion of 11: 1.5: 0.9: mixing at a mass ratio of 0.8, stirring uniformly, and heating by starting microwave under anaerobic condition, wherein the microwave frequency is 3200MHz, and the time is 15min to obtain a mixture C.
The antioxidant is as follows: the anti-aging agent is prepared by mixing pentaerythritol, didodecanol ester and tridecyl ester according to the mass ratio of 4:1: 1.5.
The dispersing agent is as follows: is stearic acid monoglyceride.
(4) And (3) introducing the mixture C into a double-screw extrusion machine, controlling the melting temperature to be 262 ℃, carrying out melt blending for 40min at the screw rotation speed of 180 revolutions per minute, and carrying out extrusion granulation to obtain the modified polyester master batch.
Step 4, spinning
Heating and drying the modified polyester master batch, then loading the dried modified polyester master batch into a double-screw extruder, heating and melting, and spinning by a spinneret plate-drafting two-step method, wherein the spinning temperature is 280 ℃, the spinning speed is 900m/min, the hot plate temperature during drafting is 83 ℃, the hot plate temperature is 145 ℃, and the drafting multiple is 4 times.
The polyester fiber containing bodhi prepared by the embodiment has good moisture absorption performance; compared with unmodified polyester fiber, the moisture regain is 0.8% under standard conditions, and the moisture regain is 1.5% under the condition that the relative humidity is 100%; the prepared polyester fiber containing bodhi has high mechanical strength, fiber strength of 8.9cN/tex, elongation at break of 24% and elastic modulus of 146 cN/dtex; the bacteriostatic property is good, and the bacteriostatic rate on staphylococcus aureus, escherichia coli, candida albicans and mycobacterium tuberculosis is more than 94%; the antibacterial stability is good, and the prepared polyester fiber containing bodhi is washed by 100 times of water at normal temperature, and the antibacterial rate is still kept above 86%.
EXAMPLE 3 preparation of Ficus religiosa-containing polyester fiber
Step 1, preparation of porous silica microspheres
Fully mixing the secondary distilled water and the ethanol to prepare ethanol solution; the volume ratio of the secondary distilled water to the ethanol is 10: 7.
Adding hexadecyl trimethyl ammonium bromide into an ethanol solution, adding ammonia water as a catalyst, magnetically stirring at the stirring speed of 2000rpm, dropwise adding tetraethoxysilane during stirring, continuously stirring for reacting for 4 hours, drying at 85 ℃, feeding dried solids into a muffle furnace, heating to 580 ℃ at the speed of 2 ℃/min, and calcining at the temperature for 6 hours to obtain porous silicon dioxide; the porous silica obtained: specific surface area of 800-2A particle size of 160-180nm and a pore diameter of 8-13 nm.
The addition amount of the hexadecyl trimethyl ammonium bromide is 14.8 percent of the mass of the ethanol solution;
the addition amount of the ammonia water is 9.5 percent of the mass of the ethanol solution, and the concentration of the ammonia water is 37.58 g/L;
the adding amount of the ethyl orthosilicate is 55 percent of the mass of the ethanol solution.
Step 2, preparation of porous molecular nest containing linden extract
(1) Preparation of bodhi extract solution: the bodhi extract is prepared into a saturated aqueous solution of the bodhi extract by using deionized water, and the temperature of the deionized water is 24 ℃. The linden extract: contains triterpenoid saponins 45% and sesquiterpene glycosides 32%.
(2) Preparation of a dispersion of porous silica: adding porous silicon dioxide powder and ethanol water solution into a ball mill for grinding, shearing and dispersing to obtain porous nano material dispersion liquid; the mass ratio of the porous silicon dioxide powder to the ethanol aqueous solution is 2: 7; the concentration of the ethanol water solution is 97 percent (mass percentage concentration).
(3) Preparation of porous molecular nest: shearing and dispersing the saturated aqueous solution of the linden extract, the porous nano material dispersion, the coupling agent and the surfactant to obtain a nano material dispersion containing the linden extract, and volatilizing the solvent to obtain a dry porous molecular nest containing the linden extract; the mass ratio of the saturated aqueous solution of the linden extract, the dispersed porous nano material, the coupling agent and the surfactant is 12: 8: 0.7: 1.1; the coupling agent is a silane coupling agent KH-570, and the surfactant is oleic acid.
Step 3, preparing modified polyester master batch
(1) Uniformly mixing polyester chips and porous molecular nests containing linden extracts according to a mass ratio of 9:1 to obtain a mixture A; the terylene slice comprises the following components: purity is 97%, and particle diameter is 0.1-0.15 cm.
(2) Mixing tea polyphenol, dodecyl dimethyl betaine and montmorillonite according to the weight ratio of 3.5: 1: 6, and performing ultrasonic treatment at an ultrasonic frequency of 120KHZ and an ultrasonic temperature of 72 ℃ for 25min to obtain a mixture B.
The montmorillonite is as follows: the fineness is 950 meshes and 1000 meshes.
(3) Mixing the mixture A, the mixture B, the antioxidant and the dispersant according to the proportion of 10: 2.5: 0.8: mixing at a mass ratio of 0.5, stirring uniformly, and heating by turning on microwave under anaerobic condition, wherein the microwave frequency is 3400MHz, and the time is 10min to obtain a mixture C.
The antioxidant is as follows: the anti-aging agent is prepared by mixing pentaerythritol, didodecanol ester and tridecyl ester according to the mass ratio of 4:1: 1.5.
The dispersing agent is as follows: is stearic acid monoglyceride.
(4) And (3) introducing the mixture C into a double-screw extrusion machine, controlling the melting temperature to be 262 ℃, carrying out melt blending for 40min at the screw rotation speed of 210 rpm, and carrying out extrusion granulation to obtain the modified polyester master batch.
Step 4, spinning
Heating and drying the modified polyester master batch, then loading the dried modified polyester master batch into a double-screw extruder, heating and melting, and spinning by a spinneret plate-drafting two-step method, wherein the spinning temperature is 284 ℃, the spinning speed is 900m/min, the hot plate temperature is 85 ℃ during drafting, the hot plate temperature is 145 ℃, and the drafting multiple is 4 times.
The polyester fiber containing bodhi prepared by the embodiment has good moisture absorption performance; compared with unmodified polyester fiber, the moisture regain is 0.7% under standard conditions, and the moisture regain is 1.0% under the condition that the relative humidity is 100%; the prepared polyester fiber containing bodhi has high mechanical strength, fiber strength of 8.8cN/tex, elongation at break of 23 percent and elastic modulus of 146 cN/dtex; the bacteriostatic property is good, and the bacteriostatic rate on staphylococcus aureus, escherichia coli, candida albicans and mycobacterium tuberculosis is more than 91%; the antibacterial stability is good, and the prepared polyester fiber containing bodhi is washed by 100 times of water at normal temperature, and the antibacterial rate is still kept above 82%.
Unless otherwise specified, the proportions in the present invention are mass proportions, and the percentages are mass percentages.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the present 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 bodhi-containing polyester fiber is characterized by comprising the following steps: the preparation method comprises the steps of preparing porous silica microspheres; the preparation of the porous silica microspheres comprises the following steps: fully mixing the secondary distilled water and the ethanol to prepare ethanol solution; adding hexadecyl trimethyl ammonium bromide and ammonia water as catalysts into the ethanol solution, dropwise adding ethyl orthosilicate, drying the reacted solid, and calcining the dried solid to obtain the porous silicon dioxide.
2. The method for preparing bodhi-containing polyester fiber according to claim 1, wherein:
the preparation of the porous silica microspheres comprises the following steps: the reaction time is 4-4.5h, the drying temperature is 80-85 ℃, and the calcining: the solid was heated to 550 ℃ and 580 ℃ at a rate of 1-2 ℃/min in a muffle furnace and calcined at this temperature for 6-6.5 h.
3. The method for preparing bodhi-containing polyester fiber according to claim 1, wherein: the addition amount of the cetyl trimethyl ammonium bromide is 13.5 to 14.8 percent of the mass of the ethanol solution; the addition amount of the ammonia water is 8.5-9.5% of the mass of the ethanol solution; the adding amount of the ethyl orthosilicate is 50-55% of the mass of the ethanol solution.
4. The method for preparing bodhi-containing polyester fiber according to claim 1, wherein: the porous silica obtained: specific surface area of 800-2A particle size of 160-180nm and a pore diameter of 8-13 nm.
5. The method for preparing bodhi-containing polyester fiber according to claim 1, wherein: also comprises a preparation step of the porous molecular nest containing the linden extract; the preparation of the bodhi extract-containing porous molecular nest: preparing the linden extract into a saturated aqueous solution of the linden extract by using deionized water; adding porous silicon dioxide powder and ethanol water solution into a ball mill for grinding, shearing and dispersing to obtain porous nano material dispersion liquid; shearing and dispersing the saturated aqueous solution of the linden extract, the porous nano material dispersion liquid, the coupling agent and the surfactant to obtain the nano material dispersion liquid containing the linden extract, and volatilizing the solvent to obtain the dried porous molecular nest containing the linden extract.
6. The method for preparing bodhi-containing polyester fiber according to claim 5, wherein: the mass ratio of the porous silicon dioxide powder to the ethanol water solution is 2: 6-8.
7. The method for preparing bodhi-containing polyester fiber according to claim 5, wherein: the mass ratio of the saturated aqueous solution of the linden extract, the dispersed porous nano material, the coupling agent and the surfactant is 10-12:6-8:0.4-0.7: 0.6-1.1; the coupling agent is a silane coupling agent KH-570, and the surfactant is oleic acid.
8. The method for preparing bodhi-containing polyester fiber according to claim 1, wherein: also comprises the step of preparing modified terylene master batch; the preparation of the modified polyester master batch comprises the following steps: mixing dacron slices and the porous molecular nest containing the linden extract uniformly to obtain a mixture A; mixing tea polyphenol, dodecyl dimethyl betaine and montmorillonite, and performing ultrasonic treatment to obtain a mixture B; mixing the mixture A, the mixture B, the antioxidant and the dispersant, uniformly stirring, and starting microwaves to heat under an anaerobic condition to obtain a mixture C; and (3) introducing the mixture C into a double-screw extrusion machine, and carrying out extrusion granulation to obtain the modified polyester master batch.
9. The method for preparing bodhi-containing polyester fiber according to claim 8, wherein: the mass ratio of the terylene slices to the bodhi extract is 7-9: 1; the mass ratio of the tea polyphenol to the dodecyl dimethyl betaine to the montmorillonite is 3-3.5: 1-2: 5-6; the mass ratio of the mixture A to the mixture B to the antioxidant to the dispersant is 10-12: 1-2.5: 0.8-1.2: 0.5-0.8.
10. The method for preparing bodhi-containing polyester fiber according to claim 8, wherein: the antioxidant is as follows: the anti-aging agent is prepared by mixing pentaerythritol, didodecanol ester and tridecyl ester according to the mass ratio of 4:1: 1.5; the dispersing agent is as follows: is stearic acid monoglyceride.
CN202011050035.8A 2020-09-29 2020-09-29 Bodhi-containing polyester fiber and preparation method thereof Pending CN112030262A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113818237A (en) * 2021-07-30 2021-12-21 百事基材料(青岛)股份有限公司 Silk large biological fiber containing peach blossom active ingredients and preparation method thereof
CN115506042A (en) * 2022-09-30 2022-12-23 青岛邦特生态纺织科技有限公司 Preparation method of multifunctional plant source composite material for fiber spinning
CN116199460A (en) * 2023-02-27 2023-06-02 浙江新都水泥有限公司 High-crack-resistance wear-resistant cement and preparation method thereof
CN117430121A (en) * 2023-10-23 2024-01-23 博路天成新能源科技有限公司 Silica microsphere manufacturing process based on Stober method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111171531A (en) * 2020-03-18 2020-05-19 百事基材料(青岛)股份有限公司 Seaweed polyester master batch and preparation process thereof
CN111304776A (en) * 2020-04-01 2020-06-19 百事基材料(青岛)股份有限公司 Naringin modified polyester filament
CN111393802A (en) * 2020-05-09 2020-07-10 黄礼辉 SiO (silicon dioxide)2Modified epoxy resin toughened by grafted polyamide curing agent and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111171531A (en) * 2020-03-18 2020-05-19 百事基材料(青岛)股份有限公司 Seaweed polyester master batch and preparation process thereof
CN111304776A (en) * 2020-04-01 2020-06-19 百事基材料(青岛)股份有限公司 Naringin modified polyester filament
CN111393802A (en) * 2020-05-09 2020-07-10 黄礼辉 SiO (silicon dioxide)2Modified epoxy resin toughened by grafted polyamide curing agent and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113818237A (en) * 2021-07-30 2021-12-21 百事基材料(青岛)股份有限公司 Silk large biological fiber containing peach blossom active ingredients and preparation method thereof
CN115506042A (en) * 2022-09-30 2022-12-23 青岛邦特生态纺织科技有限公司 Preparation method of multifunctional plant source composite material for fiber spinning
CN115506042B (en) * 2022-09-30 2024-02-13 青岛邦特生态纺织科技有限公司 Preparation method of multifunctional plant source composite material for fiber spinning
CN116199460A (en) * 2023-02-27 2023-06-02 浙江新都水泥有限公司 High-crack-resistance wear-resistant cement and preparation method thereof
CN117430121A (en) * 2023-10-23 2024-01-23 博路天成新能源科技有限公司 Silica microsphere manufacturing process based on Stober method
CN117430121B (en) * 2023-10-23 2024-03-22 博路天成新能源科技有限公司 Silica microsphere manufacturing process based on Stober method

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