CN116497476A - Dacron large biological fiber containing saussurea involucrata active ingredient and preparation method thereof - Google Patents

Dacron large biological fiber containing saussurea involucrata active ingredient and preparation method thereof Download PDF

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Publication number
CN116497476A
CN116497476A CN202310556827.XA CN202310556827A CN116497476A CN 116497476 A CN116497476 A CN 116497476A CN 202310556827 A CN202310556827 A CN 202310556827A CN 116497476 A CN116497476 A CN 116497476A
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saussurea involucrata
active ingredient
temperature
dacron
preparing
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黄效华
甄丽
池姗
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Qingdao Baicao New Material Co ltd
Zhongke Textile Research Institute Qingdao Co ltd
Bestee Material Tsingtao Co Ltd
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Qingdao Baicao New Material Co ltd
Zhongke Textile Research Institute Qingdao Co ltd
Bestee Material Tsingtao Co Ltd
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Publication of CN116497476A publication Critical patent/CN116497476A/en
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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
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • 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
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins

Abstract

The invention discloses a preparation method of a dacron large biological fiber containing a saussurea involucrata active ingredient, which comprises the steps of preparing the saussurea involucrata active ingredient, preparing dacron master batch, coating the master batch and spinning; the preparation method comprises cleaning herba Saussureae Involueratae, oven drying at 30-35deg.C, mixing herba Saussureae Involueratae with sodium pyrophosphate and sodium thiosulfate, freeze vacuum drying, and maintaining at 60-70deg.C for 1-1.5 hr to obtain dried herba Saussureae Involueratae; mixing dried herba Saussureae Involueratae with light calcium carbonate, and vibrating and grinding to break wall to obtain herba Saussureae Involueratae active ingredient; the prepared large biological polyester fiber can overcome the defects of low water absorbability, poor air permeability, poor dyeing property, easy pilling and fuzzing, easy contamination and the like of the polyester, and does not influence the crease resistance and mechanical strength of the polyester.

Description

Dacron large biological fiber containing saussurea involucrata active ingredient and preparation method thereof
Technical Field
The invention relates to a dacron large biological fiber containing a saussurea involucrata active ingredient and a preparation method thereof, belonging to the technical field of dacron.
Background
Polyester, also called polyester fiber, is a synthetic fiber obtained by spinning polyester formed by polycondensation of organic dibasic acid and dihydric alcohol, is abbreviated as PET fiber, belongs to a high molecular compound, and is invented in 1941, and is the first large variety of the current synthetic fiber. The polyester fiber has the greatest advantages of good crease resistance and shape retention, high strength and elastic recovery capability, fastness, durability, crease resistance, no ironing and no sticking.
However, polyester has disadvantages such as low water absorption, poor air permeability, poor dyeing property, easy pilling and easy staining as compared with natural fibers, and in order to improve these disadvantages, there are generally used methods: the hydrophilic group-added monomer or oligomer polyethylene glycol and the like are copolymerized, so that the moisture absorption rate of the fiber can be improved; the antistatic monomer is added for copolymerization, so that the antistatic and anti-staining properties of the fiber can be improved; adding phosphorus, halogen and antimony containing compounds to improve the flame resistance of the fiber; copolymerization with a dye-philic group monomer (e.g., sulfonate, etc.) to improve the dyeing properties of the fiber.
However, the above chemical methods are all to add various monomers or compounds in the copolymerization process, which easily affect the polymerization degree in the production process and the stability of the prepared polyester, and also to modify by material methods, such as composite spinning with other polymers, but the production process is complex, which easily affects the fiber strength. Therefore, the production method of the polyester fiber is sought, the defects of low water absorption, poor air permeability, poor dyeing property, easy pilling and fuzzing, easy contamination and the like of the polyester fiber can be overcome, the crease-resistant capability of the polyester fiber is not influenced, and the mechanical strength is a technical problem which needs to be solved urgently at present.
The patent CN110318147B discloses an antibacterial cationic polyester blended fabric and a preparation process thereof, wherein the preparation process is that the antibacterial cationic polyester blended fabric is prepared by weaving antibacterial cationic polyester blended yarns, and the antibacterial cationic polyester blended yarns are prepared by carding cationic polyester, cotton fiber and chitosan fiber after plasma treatment respectively, and then sequentially carrying out drawing, roving, spinning and spooling procedures after mixing; the deficiency of this patent: the prepared terylene blended fabric is not crease-resistant.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a dacron large biological fiber containing a saussurea involucrata active ingredient and a preparation method thereof, which realizes the following aims: the defects of low water absorption, poor air permeability, poor dyeing property, easy pilling and fuzzing, easy contamination and the like of the terylene can be overcome, and the crease resistance and the mechanical strength of the terylene are not influenced.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a dacron large biological fiber containing a saussurea involucrata active ingredient comprises the steps of preparing the saussurea involucrata active ingredient, preparing dacron master batch, coating the master batch and spinning.
The preparation method of the active ingredient of the saussurea involucrata comprises the steps of cleaning the saussurea involucrata, drying the saussurea involucrata at a low temperature of 30-35 ℃, uniformly mixing the saussurea involucrata with sodium pyrophosphate according to a mass ratio of 55-60:2-3:0.5-1, placing the mixture in a freeze vacuum drier, controlling the vacuum degree to be 0.025-0.03MPa, freezing the mixture for 3-4 hours at a temperature of minus 35-minus 25 ℃, slowly raising the temperature to 60-70 ℃, controlling the temperature raising speed to be 2-3 ℃/min, and then preserving the heat for 1-1.5 hours at the temperature of 60-70 ℃ to obtain the dried saussurea involucrata; uniformly mixing dried herba Saussureae Involueratae and light calcium carbonate with cellulose at a mass ratio of 50-55:1-2:0.5-1, placing into a vibration grinding wall breaking machine, grinding at room temperature for 1-2h, and standing at 50-60deg.C for 20-30min to obtain herba Saussureae Involueratae active ingredient;
the vibration frequency of the vibration grinding wall breaking machine is 800-900cpm, and the vibration amplitude is 4.5-6mm;
the cellulase is a commercial product, and the activity of the cellulase is 120-130U/g.
Adding terephthalic acid, ethylene glycol, a modified titanium-silicon molecular sieve catalyst and active carbon into a reaction kettle, controlling the stirring speed of the reaction kettle to 350-400rpm, controlling the temperature of the reaction kettle to 60-70 ℃, adding ammonium bisulfide and diisobutyl dicarbonate after reacting for 2-3h, continuously reacting for 40-60min to obtain a primary product, placing the primary product into an oven, drying at 50-60 ℃ for 1.5-2h, adding the dried primary product and silicon nitride powder into a co-rotating twin-screw extruder, and extruding from the co-rotating twin-screw extruder to obtain the polyester master batch.
The diameter of the screw of the homodromous double-screw extruder is 20-22mm, the length-diameter ratio is 30-40:1, the rotating speed of a main machine is 80-90Hz, the rotating speed of a feeding machine is 30-35Hz, the granulating is water-cooling granulating, the extruding temperature of the first section is 300-305 ℃, the extruding temperature of the second section is 290-295 ℃, the extruding temperature of the third section is 280-285 ℃, the extruding temperature of the fourth section is 270-275 ℃, the extruding temperature of the fifth section is 260-265 ℃, the extruding temperature of the sixth section is 250-255 ℃, and the extruding temperature of the seventh section is 240-245 ℃.
The raw materials in the preparation of the polyester master batch comprise the following components in parts by weight: 52-56 parts of terephthalic acid, 18-20 parts of ethylene glycol, 0.5-0.8 part of modified titanium silicalite molecular sieve catalyst, 2-3 parts of active carbon, 1-2 parts of ammonium bisulfide, 0.2-0.5 part of diisobutyl carbonate and 3-5 parts of silicon nitride powder.
The preparation method of the modified titanium silicalite molecular sieve catalyst comprises the following steps: uniformly mixing tetrabutyl titanate, tetrapropylammonium bromide, ammonium chloride, dibenzoyl peroxide and sodium acrylate to obtain a mixed solution, uniformly mixing the mixed solution with a titanium silicalite molecular sieve TS-1, performing infrared irradiation modification at 60-70 ℃, controlling the wavelength of the infrared irradiation modification to be 800-900nm, and the time of the infrared irradiation modification to be 1.5-2h, wherein the infrared irradiation modification is finished to obtain the modified titanium silicalite molecular sieve catalyst.
Wherein the mass ratio of tetrabutyl titanate, tetrapropylammonium bromide, ammonium chloride, dibenzoyl peroxide and sodium acrylate is 20-25:30-35:2-5:0.2-0.5:1-2.
The coating master batch is characterized in that active ingredients of saussurea involucrata, polyvinyl alcohol, tetraethoxysilane and absolute ethyl alcohol are uniformly mixed to obtain an active factor, the polyester master batch and the active factor are mixed according to a mass ratio of 1:4-4.2, then microwave oscillation is carried out at 45-50 ℃, the power of the microwave oscillation is controlled to be 320-350W, the time of the microwave oscillation is controlled to be 1-1.5h, vacuum low-temperature drying is carried out after the microwave oscillation is ended, the vacuum degree is controlled to be 0.08-0.09MPa, the temperature is 50-55 ℃, and the coated polyester master batch is obtained after the drying is ended.
Wherein the saussurea involucrata active ingredient, polyvinyl alcohol, tetraethoxysilane and absolute ethyl alcohol are mixed according to the mass ratio of 15-16:2-3:0.2-0.5:30-40.
And (3) carrying out melt spinning on the coated polyester master batch, wherein the spinning temperature is 280-290 ℃, the spinning speed is 3200-3400m/min, the stretching multiple is 3.5-3.75 times, the air temperature is 35-36 ℃, the air speed is 2.4-2.5m/s, and the polyester large biological fiber is obtained after the spinning is finished.
Compared with the prior art, the invention has the beneficial effects that:
(1) The prepared large terylene biological fiber containing the active ingredient of the saussurea involucrata can improve the water absorption and the evaporation rate by freezing and vacuum drying in the step of preparing the active ingredient of the saussurea involucrata, and the water absorption and the evaporation rate of the large terylene biological fiber prepared by the invention are 120-125 percent and 0.68-0.75g/h;
(2) The strength of the large terylene biological fiber containing the active ingredient of the saussurea involucrata can be improved by freeze vacuum drying in the step of preparing the active ingredient of the saussurea involucrata, the breaking strength of the large terylene biological fiber prepared by the invention can reach 3.8-4.2cN/dex, and the breaking elongation can reach 142-147%;
(3) According to the large terylene biological fiber containing the saussurea involucrata active ingredient, the wrinkle resistance can be improved by using the titanium-silicon molecular sieve TS-1 in the step of preparing the terylene master batch and using mechanical oscillation instead of microwave oscillation in the step of coating the master batch, the acute elastic recovery angle can reach 224.5-228.7 degrees, and the slow elastic recovery angle can reach 248.4-250.5 degrees;
(4) According to the large terylene biological fiber containing the saussurea involucrata active ingredient, mechanical oscillation is used for replacing microwave oscillation in the step of coating the master batch, so that the air permeability can be improved, and the air permeability of the fabric prepared from the large terylene biological fiber can reach 783-814mm/s;
(5) The dacron large biological fiber containing the active component of the saussurea involucrata can improve the dyeing property and the dyeing color fastness by carrying out freeze vacuum drying in the step of preparing the active component of the saussurea involucrata, and the gray card of the fabric prepared by the dacron large biological fiber can reach 5 grades and the color fastness can reach 4.5-5 grades;
(6) According to the large terylene biological fiber containing the active ingredient of the saussurea involucrata, the anti-pilling capacity can be improved by carrying out freeze vacuum drying in the step of preparing the active ingredient of the saussurea involucrata and using mechanical oscillation instead of microwave oscillation in the step of coating master batch, and the large terylene biological fiber is still free from damage after 60000 times of abrasion;
(7) According to the large terylene biological fiber containing the active ingredient of the saussurea involucrata, the anti-contamination capability can be improved, and the oil-repellent grade can reach grade 4 by carrying out freeze vacuum drying in the step of preparing the active ingredient of the saussurea involucrata and using the titanium-silicon molecular sieve TS-1 in the step of preparing the terylene master batch.
Detailed Description
Specific embodiments of the present invention will now be described in order to provide a clearer understanding of the technical features, objects and effects of the present invention.
Example 1
The preparation method of the large terylene biological fiber containing the active ingredient of the saussurea involucrata comprises the following specific steps:
1. preparing active ingredients of saussurea involucrata: cleaning herba Saussureae Involueratae, oven drying at 30deg.C, mixing herba Saussureae Involueratae with sodium pyrophosphate at a mass ratio of 55:2:0.5, placing in a freeze vacuum drier, controlling vacuum degree to 0.025MPa, freezing at-35deg.C for 3 hr, slowly heating to 60deg.C, controlling heating rate to 2deg.C/min, and maintaining at 60deg.C for 1 hr to obtain dried herba Saussureae Involueratae; uniformly mixing dried herba Saussureae Involueratae with light calcium carbonate at a mass ratio of 50:1:0.5, placing in a vibration grinding wall breaking machine, grinding at room temperature to break wall, controlling vibration frequency of the vibration grinding wall breaking machine to 800cpm, vibration amplitude to 4.5mm, grinding wall breaking time to 1h, and standing at 50deg.C for 20min to obtain herba Saussureae Involueratae active ingredient;
the cellulase is a commercial product, and the activity of the cellulase is 120U/g.
2. Preparing polyester master batches: adding terephthalic acid, ethylene glycol, a modified titanium silicon molecular sieve catalyst and active carbon into a reaction kettle, controlling the stirring speed of the reaction kettle to 350rpm, controlling the temperature of the reaction kettle to 60 ℃, after reacting for 2 hours, adding ammonium bisulfide and diisobutyl dicarbonate, continuously reacting for 40 minutes to obtain a primary product, placing the primary product into an oven, drying at 50 ℃ for 1.5 hours, adding the dried primary product and silicon nitride powder into a co-rotating twin-screw extruder, controlling the screw diameter of the co-rotating twin-screw extruder to be 20mm, the length-diameter ratio to be 30:1, the rotating speed of a host to be 80Hz, the rotating speed of a feeder to be 30Hz, cutting into water-cooled cut particles, wherein the extrusion temperature of the first section is 300 ℃, the extrusion temperature of the second section is 290 ℃, the extrusion temperature of the third section is 280 ℃, the extrusion temperature of the fourth section is 270 ℃, the extrusion temperature of the fifth section is 260 ℃, the extrusion temperature of the sixth section is 250 ℃, and the extrusion temperature of the seventh section is 240 ℃, and extruding from the co-rotating twin-screw extruder to obtain the polyester master batch.
The raw materials in the preparation of the polyester master batch comprise the following components in parts by weight: 52 parts of terephthalic acid, 18 parts of ethylene glycol, 0.5 part of modified titanium silicalite catalyst, 2 parts of active carbon, 1 part of ammonium bisulfide, 0.2 part of diisobutyl carbonate and 3 parts of silicon nitride powder.
The preparation method of the modified titanium silicalite molecular sieve catalyst comprises the following steps: uniformly mixing tetrabutyl titanate, tetrapropylammonium bromide, ammonium chloride, dibenzoyl peroxide and sodium acrylate according to the mass ratio of 20:30:2:0.2:1 to obtain a mixed solution, uniformly mixing the mixed solution with a titanium silicalite molecular sieve TS-1, performing infrared irradiation modification at 60 ℃, controlling the wavelength of the infrared irradiation modification to be 800nm, and controlling the time of the infrared irradiation modification to be 1.5h, wherein the end of the infrared irradiation modification is to obtain the modified titanium silicalite molecular sieve catalyst.
3. Coating master batches: uniformly mixing active components of saussurea involucrata, polyvinyl alcohol, tetraethoxysilane and absolute ethyl alcohol according to a mass ratio of 15:2:0.2:30 to obtain an active factor, mixing polyester master batch and the active factor according to a mass ratio of 1:4, then carrying out microwave oscillation at 45 ℃, controlling the power of microwave oscillation to be 320W, the time of microwave oscillation to be 1h, carrying out vacuum low-temperature drying after microwave oscillation, controlling the vacuum degree to be 0.08MPa, and obtaining the coated polyester master batch after drying.
4. Spinning: and (3) carrying out melt spinning on the coated polyester master batch, wherein the spinning temperature is 280 ℃, the spinning speed is 3200m/min, the stretching multiple is 3.5 times, the air temperature is 35-36 ℃, the air speed is 2.4m/s, and the polyester large biological fiber is obtained after the spinning is finished.
Example 2
The preparation method of the large terylene biological fiber containing the active ingredient of the saussurea involucrata comprises the following specific steps:
1. preparing active ingredients of saussurea involucrata: cleaning herba Saussureae Involueratae, drying at low temperature of 32deg.C, mixing herba Saussureae Involueratae with sodium pyrophosphate at mass ratio of 57:2.5:0.7, placing in a freeze vacuum drier, controlling vacuum degree to 0.028MPa, freezing at-30deg.C for 3.5 hr, slowly heating to 65deg.C, controlling heating rate to 2.5 ℃/min, and maintaining at 65deg.C for 1.2 hr to obtain dried herba Saussureae Involueratae; uniformly mixing dried herba Saussureae Involueratae with light calcium carbonate at a mass ratio of 52:1.5:0.7, placing in a vibration grinding wall breaking machine, grinding at room temperature to break wall, controlling vibration frequency of 850cpm of the vibration grinding wall breaking machine to be 5mm, grinding wall breaking time to be 1.5h, and standing at 55deg.C for 25min to obtain herba Saussureae Involueratae active ingredient;
the cellulase is a commercial product, and the activity of the cellulase is 125U/g.
2. Preparing polyester master batches: adding terephthalic acid, ethylene glycol, a modified titanium silicon molecular sieve catalyst and active carbon into a reaction kettle, controlling the stirring speed of the reaction kettle to 370rpm, controlling the temperature of the reaction kettle to 65 ℃, reacting for 2.5 hours, adding ammonium bisulfide and diisobutyl dicarbonate, continuously reacting for 50 minutes to obtain a primary product, placing the primary product into an oven, drying at 55 ℃ for 1.7 hours, adding the dried primary product and silicon nitride powder into a co-rotating twin-screw extruder, controlling the screw diameter of the co-rotating twin-screw extruder to be 21mm, the length-diameter ratio to be 35:1, the host rotating speed to be 85Hz, the rotating speed of a feeder to be 32Hz, cutting into water-cooled cut particles, wherein the extrusion temperature of the first section is 302 ℃, the extrusion temperature of the second section is 292 ℃, the extrusion temperature of the third section is 282 ℃, the extrusion temperature of the fourth section is 272 ℃, the extrusion temperature of the fifth section is 262 ℃, the extrusion temperature of the sixth section is 252 ℃, the extrusion temperature of the seventh section is 242 ℃, and extruding from the co-rotating twin-screw extruder to obtain the polyester master batch.
The raw materials in the preparation of the polyester master batch comprise the following components in parts by weight: 54 parts of terephthalic acid, 19 parts of ethylene glycol, 0.7 part of modified titanium silicalite catalyst, 2.5 parts of active carbon, 1.5 parts of ammonium bisulfide, 0.3 part of diisobutyl carbonate and 4 parts of silicon nitride powder.
The preparation method of the modified titanium silicalite molecular sieve catalyst comprises the following steps: uniformly mixing tetrabutyl titanate, tetrapropylammonium bromide, ammonium chloride, dibenzoyl peroxide and sodium acrylate according to the mass ratio of 22:32:3:0.4:1.5 to obtain a mixed solution, uniformly mixing the mixed solution with a titanium silicalite molecular sieve TS-1, performing infrared irradiation modification at 65 ℃, controlling the wavelength of the infrared irradiation modification to be 850nm, and controlling the time of the infrared irradiation modification to be 1.8h, wherein the end of the infrared irradiation modification is to obtain the modified titanium silicalite molecular sieve catalyst.
3. Coating master batches: uniformly mixing the active components of saussurea involucrata, polyvinyl alcohol, tetraethoxysilane and absolute ethyl alcohol according to a mass ratio of 15:2.5:0.4:35 to obtain an active factor, mixing the polyester master batch and the active factor according to a mass ratio of 1:4.1, then carrying out microwave oscillation at 47 ℃, controlling the power of microwave oscillation to be 340W, the time of microwave oscillation to be 1.2h, carrying out vacuum low-temperature drying after the microwave oscillation is ended, controlling the vacuum degree to be 0.085MPa, and the temperature to be 52 ℃, and obtaining the coated polyester master batch after the drying is ended.
4. Spinning: and (3) carrying out melt spinning on the coated polyester master batch, wherein the spinning temperature is 285 ℃, the spinning speed is 3300m/min, the stretching multiple is 3.6 times, the air temperature is 35.5 ℃, the air speed is 2.4m/s, and the polyester large biological fiber is obtained after the spinning is finished.
Example 3
The preparation method of the large terylene biological fiber containing the active ingredient of the saussurea involucrata comprises the following specific steps:
1. preparing active ingredients of saussurea involucrata: cleaning herba Saussureae Involueratae, drying at 35 deg.C, mixing herba Saussureae Involueratae with sodium pyrophosphate at a mass ratio of 60:3:1, freezing in a vacuum drier under vacuum of 0.03MPa, freezing at-25deg.C for 4 hr, slowly heating to 70deg.C at a temperature of 3 deg.C/min, and maintaining at 70deg.C for 1.5 hr to obtain dried herba Saussureae Involueratae; uniformly mixing dried herba Saussureae Involueratae and light calcium carbonate at a mass ratio of 55:2:1, placing in a vibration grinding wall breaking machine, grinding at room temperature to break wall, controlling vibration frequency of the vibration grinding wall breaking machine to 900cpm, vibration amplitude to 6mm, grinding wall breaking time to 2h, and standing at 60deg.C for 30min to obtain herba Saussureae Involueratae active ingredient;
the cellulase is a commercial product, and the activity of the cellulase is 130U/g.
2. Preparing polyester master batches: adding terephthalic acid, ethylene glycol, a modified titanium silicon molecular sieve catalyst and active carbon into a reaction kettle, controlling the stirring speed of the reaction kettle to 400rpm, controlling the temperature of the reaction kettle to 70 ℃, after reacting for 3 hours, adding ammonium bisulfide and diisobutyl dicarbonate, continuously reacting for 60 minutes to obtain a primary product, placing the primary product into an oven, drying for 2 hours at 60 ℃, adding the dried primary product and silicon nitride powder into a co-rotating twin-screw extruder, controlling the screw diameter of the co-rotating twin-screw extruder to be 22mm, the length-diameter ratio to be 40:1, the rotating speed of a host to be 90Hz, the rotating speed of a feeder to be 35Hz, cutting into water-cooled cut particles, the extrusion temperature of the first section to be 305 ℃, the extrusion temperature of the second section to be 295 ℃, the extrusion temperature of the third section to be 285 ℃, the extrusion temperature of the fourth section to be 275 ℃, the extrusion temperature of the fifth section to be 265 ℃, the extrusion temperature of the sixth section to be 255 ℃, and the extrusion temperature of the seventh section to be 245 ℃, and extruding from the co-rotating twin-screw extruder to obtain the polyester master batch.
The raw materials in the preparation of the polyester master batch comprise the following components in parts by weight: 56 parts of terephthalic acid, 20 parts of ethylene glycol, 0.8 part of modified titanium silicalite catalyst, 3 parts of active carbon, 2 parts of ammonium bisulfide, 0.5 part of diisobutyl carbonate and 5 parts of silicon nitride powder.
The preparation method of the modified titanium silicalite molecular sieve catalyst comprises the following steps: uniformly mixing tetrabutyl titanate, tetrapropylammonium bromide, ammonium chloride, dibenzoyl peroxide and sodium acrylate according to the mass ratio of 25:35:5:0.5:2 to obtain a mixed solution, uniformly mixing the mixed solution with a titanium silicalite molecular sieve TS-1, performing infrared irradiation modification at 70 ℃, controlling the wavelength of the infrared irradiation modification to be 900nm, and controlling the time of the infrared irradiation modification to be 2 hours, wherein the end of the infrared irradiation modification is to obtain the modified titanium silicalite molecular sieve catalyst.
3. Coating master batches: uniformly mixing the active components of saussurea involucrata, polyvinyl alcohol, tetraethoxysilane and absolute ethyl alcohol according to the mass ratio of 16:3:0.5:40 to obtain an active factor, mixing the polyester master batch and the active factor according to the mass ratio of 1:4.2, then carrying out microwave oscillation at 50 ℃, controlling the power of microwave oscillation to be 350W, the time of microwave oscillation to be 1.5h, carrying out vacuum low-temperature drying after the microwave oscillation is ended, controlling the vacuum degree to be 0.09MPa, and the temperature to be 55 ℃, thereby obtaining the coated polyester master batch after the drying is ended.
4. Spinning: and (3) carrying out melt spinning on the coated polyester master batch, wherein the spinning temperature is 290 ℃, the spinning speed is 3400m/min, the stretching multiple is 3.75 times, the air temperature is 36 ℃, the air speed is 2.5m/s, and the polyester large biological fiber is obtained after the spinning is finished.
Comparative example 1
The preparation method of the large terylene biological fiber containing the active ingredient of the saussurea involucrata is adopted in the embodiment 1, and the difference is that: the preparation method comprises the steps of preparing the active ingredients of the saussurea involucrata, namely uniformly mixing the saussurea involucrata with sodium pyrophosphate and sodium thiosulfate according to the mass ratio of 55:2:0.5, and then obtaining the dried saussurea involucrata after 4.5 hours at 60 ℃.
Comparative example 2
The preparation method of the large terylene biological fiber containing the active ingredient of the saussurea involucrata is adopted in the embodiment 1, and the difference is that: in the step of preparing the terylene master batch, a titanium silicalite molecular sieve TS-1 is used to replace a modified titanium silicalite molecular sieve catalyst.
Comparative example 3
The preparation method of the large terylene biological fiber containing the active ingredient of the saussurea involucrata is adopted in the embodiment 1, and the difference is that: and in the step of coating the master batch, mechanical oscillation is used for replacing microwave oscillation, namely the polyester master batch and the active factor are mixed at a mass ratio of 1:4, then the mechanical oscillation is carried out at 45 ℃, the oscillation frequency of the mechanical oscillation is controlled to be 150 times/min, the time of the mechanical oscillation is controlled to be 1h, the mechanical oscillation is finished, the vacuum low-temperature drying is carried out, the vacuum degree is controlled to be 0.08MPa, the temperature is 50 ℃, and the coated polyester master batch is obtained after the drying is finished.
Referring to GB/T21655.1-2008 standard, the terylene large biological fibers prepared in examples 1-3 and comparative examples 1-3 are tested for water absorption and evaporation rate, and the test results are as follows:
the dacron macrofibers prepared in examples 1 to 3 and comparative examples 1 to 3 were tested for breaking strength and breaking elongation with reference to FZ/T54003-2012 standard, and the test results are as follows:
the large biological fibers of terylene prepared in examples 1-3 and comparative examples 1-3 were respectively woven into terylene fabrics, and then the acute elastic recovery angle and the gentle elastic recovery angle were tested by referring to GB/T3819-1997 standard, and the test results are as follows:
the large biological fibers of terylene prepared in examples 1-3 and comparative examples 1-3 were respectively woven into terylene fabrics, and then the air permeability was tested by referring to GB/T5453-1997 standard, and the test results were as follows:
the large biological fibers of terylene prepared in examples 1-3 and comparative examples 1-3 were respectively woven into terylene fabrics, and then the dyeing uniformity and the color fastness were tested by referring to GB/T6508-2015 standards, and the test results are as follows:
the large biological fibers of terylene prepared in examples 1-3 and comparative examples 1-3 were respectively woven into terylene fabrics, and then, the abrasion of the fabrics after 60000 times was recorded by referring to a Martindale test of GB/T21196.3-2007 standard, and the recording results are as follows:
the large biological fibers of terylene prepared in examples 1 to 3 and comparative examples 1 to 3 were respectively woven into terylene face fabric, and then the oil repellency grade was tested with reference to AATCC118-2013 standard, and the test results were as follows:
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 terylene biological fiber containing the active ingredient of the saussurea involucrata is characterized by comprising the steps of preparing the active ingredient of the saussurea involucrata, preparing terylene master batches, coating the master batches and spinning;
the preparation method of the active ingredient of the saussurea involucrata comprises the steps of cleaning the saussurea involucrata, drying the saussurea involucrata at a low temperature of 30-35 ℃, uniformly mixing the saussurea involucrata with sodium pyrophosphate according to a mass ratio of 55-60:2-3:0.5-1, placing the mixture in a freeze vacuum drier, controlling the vacuum degree to be 0.025-0.03MPa, freezing the mixture for 3-4 hours at a temperature of minus 35-minus 25 ℃, slowly raising the temperature to 60-70 ℃, controlling the temperature raising speed to be 2-3 ℃/min, and then preserving the heat for 1-1.5 hours at the temperature of 60-70 ℃ to obtain the dried saussurea involucrata; uniformly mixing dried herba Saussureae Involueratae and light calcium carbonate at a mass ratio of 50-55:1-2:0.5-1, placing into a vibration grinding wall breaking machine, grinding at room temperature for 1-2 hr, and standing at 50-60deg.C for 20-30min to obtain herba Saussureae Involueratae active ingredient.
2. The method for preparing the large terylene biological fiber containing the active ingredient of the saussurea involucrata according to claim 1, wherein the vibration frequency of the vibration grinding wall breaking machine is 800-900cpm, and the vibration amplitude is 4.5-6mm.
3. The preparation method of the large terylene biological fiber containing the saussurea involucrata active ingredient according to claim 1, which is characterized in that terephthalic acid, glycol, a modified titanium-silicon molecular sieve catalyst and active carbon are added into a reaction kettle, the stirring speed of the reaction kettle is controlled to 350-400rpm, the temperature of the reaction kettle is controlled to 60-70 ℃, ammonium bisulfide and diisobutyl dicarbonate are added after 2-3 hours of reaction, a primary product is obtained after the reaction is continued for 40-60 minutes, the primary product is placed into an oven, the primary product is baked for 1.5-2 hours at 50-60 ℃, and then the dried primary product and silicon nitride powder are added into a homodromous double screw extruder together, and the polyester master batch is obtained after extrusion from the homodromous double screw extruder.
4. The method for preparing the large polyester biofiber containing the active ingredient of the saussurea involucrata according to claim 3, wherein the diameter of a screw of the homodromous double screw extruder is 20-22mm, the length-diameter ratio is 30-40:1, the rotating speed of a host machine is 80-90Hz, the rotating speed of a feeder is 30-35Hz, the granulating is water-cooled granulating, the extruding temperature of the first section is 300-305 ℃, the extruding temperature of the second section is 290-295 ℃, the extruding temperature of the third section is 280-285 ℃, the extruding temperature of the fourth section is 270-275 ℃, the extruding temperature of the fifth section is 260-265 ℃, the extruding temperature of the sixth section is 250-255 ℃, and the extruding temperature of the seventh section is 240-245 ℃.
5. The method for preparing the dacron large biological fiber containing the active ingredient of the saussurea involucrata according to claim 3, wherein the raw materials in preparing the dacron master batch comprise the following raw materials in parts by weight: 52-56 parts of terephthalic acid, 18-20 parts of ethylene glycol, 0.5-0.8 part of modified titanium silicalite molecular sieve catalyst, 2-3 parts of active carbon, 1-2 parts of ammonium bisulfide, 0.2-0.5 part of diisobutyl carbonate and 3-5 parts of silicon nitride powder.
6. The preparation method of the dacron large biological fiber containing the saussurea involucrata active ingredient as claimed in claim 1, wherein the preparation method of the modified titanium silicalite molecular sieve catalyst is as follows: uniformly mixing tetrabutyl titanate, tetrapropylammonium bromide, ammonium chloride, dibenzoyl peroxide and sodium acrylate to obtain a mixed solution, uniformly mixing the mixed solution with a titanium silicalite molecular sieve TS-1, performing infrared irradiation modification at 60-70 ℃, controlling the wavelength of the infrared irradiation modification to be 800-900nm, and the time of the infrared irradiation modification to be 1.5-2h, wherein the infrared irradiation modification is finished to obtain the modified titanium silicalite molecular sieve catalyst.
7. The method for preparing the dacron large biological fiber containing the active ingredient of the saussurea involucrata according to claim 6, wherein the mass ratio of tetrabutyl titanate, tetrapropylammonium bromide, ammonium chloride, dibenzoyl peroxide and sodium acrylate is 20-25:30-35:2-5:0.2-0.5:1-2.
8. The preparation method of the large polyester biological fiber containing the active ingredients of the saussurea involucrata according to claim 1, wherein the coating master batch is characterized in that the active ingredients of the saussurea involucrata, the polyvinyl alcohol, the tetraethoxysilane and the absolute ethyl alcohol are uniformly mixed to obtain the active factors, the polyester master batch and the active factors are mixed according to a mass ratio of 1:4-4.2, then microwave oscillation is carried out at 45-50 ℃, the power of the microwave oscillation is controlled to be 320-350W, the time of the microwave oscillation is controlled to be 1-1.5h, the vacuum low-temperature drying is carried out after the microwave oscillation is ended, the vacuum degree is controlled to be 0.08-0.09MPa, and the temperature is 50-55 ℃, so that the coated polyester master batch is obtained after the drying is ended.
9. The method for preparing the dacron large biological fiber containing the active ingredient of the saussurea involucrata according to claim 8, wherein the mass ratio of the active ingredient of the saussurea involucrata to the polyvinyl alcohol to the ethyl orthosilicate to the absolute ethyl alcohol is 15-16:2-3:0.2-0.5:30-40.
10. The method for preparing the dacron large biological fiber containing the active ingredients of the saussurea involucrata according to claim 1, wherein the spinning is characterized in that the coated dacron master batch is subjected to melt spinning, the spinning temperature is 280-290 ℃, the spinning speed is 3200-3400m/min, the stretching multiple is 3.5-3.75 times, the air temperature is 35-36 ℃, the air speed is 2.4-2.5m/s, and the dacron large biological fiber is obtained after the spinning is finished.
CN202310556827.XA 2023-05-17 2023-05-17 Dacron large biological fiber containing saussurea involucrata active ingredient and preparation method thereof Pending CN116497476A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104291352A (en) * 2014-09-30 2015-01-21 浙江大学 Method for preparing and modifying titanium silicalite molecular sieve catalyst and application of titanium silicalite molecular sieve catalyst in ketone oximation
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
CN109487360A (en) * 2018-08-22 2019-03-19 中科纺织研究院(青岛)有限公司 A kind of polyester fiber containing plant extracts
CN114768864A (en) * 2022-04-22 2022-07-22 山东亮剑环保新材料有限公司 Preparation method of metal modified TS-1 titanium silicalite molecular sieve CO catalyst
CN116114851A (en) * 2023-01-09 2023-05-16 江西沐恩堂生物科技有限公司 Rosa roxburghii paste and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104291352A (en) * 2014-09-30 2015-01-21 浙江大学 Method for preparing and modifying titanium silicalite molecular sieve catalyst and application of titanium silicalite molecular sieve catalyst in ketone oximation
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
CN109487360A (en) * 2018-08-22 2019-03-19 中科纺织研究院(青岛)有限公司 A kind of polyester fiber containing plant extracts
CN114768864A (en) * 2022-04-22 2022-07-22 山东亮剑环保新材料有限公司 Preparation method of metal modified TS-1 titanium silicalite molecular sieve CO catalyst
CN116114851A (en) * 2023-01-09 2023-05-16 江西沐恩堂生物科技有限公司 Rosa roxburghii paste and preparation method thereof

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