CN116657265A - Dasheng viscose fiber containing carrot active ingredient and preparation method thereof - Google Patents
Dasheng viscose fiber containing carrot active ingredient and preparation method thereof Download PDFInfo
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- 239000004480 active ingredient Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
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- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims description 20
- 229960003237 betaine Drugs 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 15
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- 238000001354 calcination Methods 0.000 claims description 13
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 10
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 10
- 230000001112 coagulating effect Effects 0.000 claims description 10
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 10
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 10
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000007710 freezing Methods 0.000 claims description 10
- 230000008014 freezing Effects 0.000 claims description 10
- 229940035034 maltodextrin Drugs 0.000 claims description 10
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 10
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 10
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 10
- 239000000230 xanthan gum Substances 0.000 claims description 10
- 229920001285 xanthan gum Polymers 0.000 claims description 10
- 229940082509 xanthan gum Drugs 0.000 claims description 10
- 235000010493 xanthan gum Nutrition 0.000 claims description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims description 5
- 238000007711 solidification Methods 0.000 claims description 5
- 230000008023 solidification Effects 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 5
- 229960001763 zinc sulfate Drugs 0.000 claims description 5
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 5
- KEAYESYHFKHZAL-OUBTZVSYSA-N sodium-24 Chemical compound [24Na] KEAYESYHFKHZAL-OUBTZVSYSA-N 0.000 claims description 2
- 229920004934 Dacron® Polymers 0.000 claims 2
- 239000005020 polyethylene terephthalate Substances 0.000 claims 2
- 230000003009 desulfurizing effect Effects 0.000 claims 1
- 239000011435 rock Substances 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 37
- 230000035699 permeability Effects 0.000 abstract description 10
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 230000002045 lasting effect Effects 0.000 abstract 1
- 241000588724 Escherichia coli Species 0.000 description 18
- 241000191967 Staphylococcus aureus Species 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 10
- 239000004744 fabric Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- UPYKUZBSLRQECL-UKMVMLAPSA-N Lycopene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1C(=C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=C)CCCC2(C)C UPYKUZBSLRQECL-UKMVMLAPSA-N 0.000 description 4
- 150000001746 carotenes Chemical class 0.000 description 4
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- NCYCYZXNIZJOKI-UHFFFAOYSA-N vitamin A aldehyde Natural products O=CC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C NCYCYZXNIZJOKI-UHFFFAOYSA-N 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000003094 microcapsule Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- OCKGFTQIICXDQW-ZEQRLZLVSA-N 5-[(1r)-1-hydroxy-2-[4-[(2r)-2-hydroxy-2-(4-methyl-1-oxo-3h-2-benzofuran-5-yl)ethyl]piperazin-1-yl]ethyl]-4-methyl-3h-2-benzofuran-1-one Chemical compound C1=C2C(=O)OCC2=C(C)C([C@@H](O)CN2CCN(CC2)C[C@H](O)C2=CC=C3C(=O)OCC3=C2C)=C1 OCKGFTQIICXDQW-ZEQRLZLVSA-N 0.000 description 1
- 241000208173 Apiaceae Species 0.000 description 1
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- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
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Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
Abstract
The invention provides a large raw viscose fiber containing carrot active ingredients and a preparation method thereof, wherein the preparation method comprises the steps of modifying carrot extract, preparing modified particles, loading, preparing functional particles, preparing spinning solution and spinning; the preparation of modified particles comprises the steps of preparing a primary mixed material and carrying out corona treatment; spraying deionized water to the carrot extract, placing the carrot extract in a microwave device for microwave treatment, then reducing the temperature to 68-72 ℃ at the speed of 1.0-1.4 ℃/min, naturally reducing the temperature to room temperature after drying, finally carrying out vacuum freeze-drying treatment, and naturally heating to the room temperature to obtain the modified carrot extract. The large viscose fiber containing the carrot active ingredient prepared by the method has lasting and stable antibacterial performance and excellent service resistance and air permeability.
Description
Technical Field
The invention relates to the field of viscose fibers, in particular to a large-sized viscose fiber containing carrot active ingredients and a preparation method thereof.
Background
Viscose is a full name of viscose, and is prepared by taking natural fibers as raw materials, preparing soluble cellulose xanthate through the procedures of alkalization, aging, sulfonation and the like, preparing viscose by dissolving in dilute alkali solution, and performing wet spinning; the hygroscopicity of the viscose fiber meets the physiological requirement of human skin, has the advantages of smoothness, coolness, ventilation, static resistance, ultraviolet resistance, good color fastness and the like, and is widely applied to the fields of various underwear, textile, clothing and the like.
Carrot, an annual or biennial herb of the genus carrot of the family Umbelliferae; the carrot has the effects of resisting bacteria, strengthening spleen and stomach, nourishing liver and improving eyesight, resolving phlegm and relieving cough, and clearing heat and detoxicating, and the lignin of the carrot also has the functions of improving the anticancer immunity of organisms and indirectly eliminating cancer cells.
The viscose fiber containing the carrot active ingredient prepared by combining the carrot component and the viscose fiber has good antibacterial performance, excellent moisture absorption performance, smoothness, coolness and comfort in wearing, but the prior art does not have any record about the viscose fiber containing the carrot active ingredient.
The applicant researches find that in the process of preparing viscose fiber, carrot active ingredients are directly added, and the active ingredients are easy to run off in the subsequent spinning and post-treatment processes, so that the antibacterial performance is unstable, and the antibacterial effect is difficult to last;
the porous materials such as silicon dioxide are used for loading active ingredients such as carrots, so that loss of the active ingredients of carrots in the subsequent spinning and post-treatment processes can be reduced, but macromolecular materials such as silicon dioxide easily influence the strength performance of fibers, and the service performance is seriously influenced.
When the existing microcapsule technology is adopted to improve the viscose fiber, the required addition amount is large, the dispersion performance of a large amount of microcapsules in the viscose fiber is poor in the spinning process, and the prepared viscose fiber has uneven quality, poor service resistance and poor air permeability.
It can be seen that in the process of preparing a large raw viscose fiber containing carrot active ingredient, the following problems exist:
1. the antibacterial performance is unstable, and the antibacterial effect is not durable;
2. the porous materials such as silicon dioxide are adopted to load the active ingredients of carrots, so that the durability of the antibacterial performance can be improved, but the strength performance can be reduced;
3. poor durability and air permeability.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides the large-sized viscose fiber containing the carrot active ingredient and the preparation method thereof, and meanwhile, the antibacterial durability, the use resistance and the air permeability are improved.
In order to solve the technical problems, the invention adopts the following technical scheme:
1. modified carrot extract
(1) Pretreatment of
Spraying deionized water to water content of 28-32%, placing in a microwave device for microwave treatment with microwave power of 780-820W, microwave frequency of 1.3-1.5GHz, microwave time of 6-8min, reducing to 68-72deg.C at a rate of 1.0-1.4deg.C/min, drying at 68-72deg.C for 1.2-1.8 hr, and naturally cooling to room temperature to obtain pretreated radix Dauci Sativae extract;
the carrot extract is sieved by a sieve with 80 meshes, and the carotene content is 3.55-3.59mg/100g;
(2) Secondary treatment
And (3) carrying out vacuum freeze drying treatment on the pretreated carrot extract, wherein the freezing temperature is between-27 ℃ and-23 ℃, the freezing time is between 16 and 20min, the vacuum degree is between 280 and 320Pa, and the secondary treatment step is completed after the carrot extract naturally rises to the room temperature, so as to obtain the modified carrot extract.
2. Preparation of modified particles
(1) Preparation of the Primary mix
Mixing montmorillonite, modified calcite, volcanic powder and betaine, performing primary ball milling, controlling the ball-material ratio in the primary ball milling to be 6-10:1, the ball milling time to be 1.0-1.4h, the ball milling rotating speed to be 590-610rpm, the ball milling temperature to be 48-52 ℃, adding polyethylene glycol and xanthan gum for secondary ball milling, controlling the ball-material ratio in the secondary ball milling to be 4-8:1, the ball milling time to be 1.3-1.8h, the ball milling rotating speed to be 510-530rpm, the ball milling temperature to be 44-46 ℃, and obtaining a primary mixed material after the secondary ball milling is finished;
the preparation method of the modified calcite comprises the steps of crushing calcite into powder with the particle size of 200 meshes, then placing the powder into a calciner for calcination, wherein the calcination temperature is 515-525 ℃, the calcination time is 5.3-5.7h, placing the powder into a microwave treatment device for microwave treatment after natural cooling, placing the powder into a sodium chloride solution for soaking for 9-11h after natural cooling, and washing and drying after the soaking is finished to obtain the modified calcite, wherein the microwave treatment is carried out in a microwave treatment device for microwave time of 14-16min and microwave power of 390-410W;
the mass ratio of montmorillonite, modified calcite, volcanic powder, betaine, polyethylene glycol and xanthan gum is 18-22:28-32:22-24:0.7-0.9:0.8-1.2:1.3-1.5;
(2) Corona treatment
And carrying out corona treatment on the primary mixed material for 32-38min and with a corona voltage of 116-124kV to obtain modified particles.
3. Load(s)
Mixing the modified carrot extract with deionized water, adding modified particles and betaine, controlling stirring speed to 860-880rpm, stirring for 32-36min, adding vinyltriethoxysilane, controlling stirring speed to 250-270rpm, stirring for 45-50min, filtering, and drying to obtain modified particles containing active components of carrot;
the mass ratio of the modified carrot extract to deionized water to modified particles to betaine to vinyltriethoxysilane is 8-12:96-110:1.0-1.4:0.3-0.5:1.6-2.0.
4. Preparation of functional particles
Adding sodium dodecyl benzene sulfonate and sodium carboxymethyl cellulose into deionized water, stirring for 26-28min, controlling stirring rotation speed at 310-330rpm, stirring at 50-54 ℃, adding maltodextrin, performing ultrasonic dispersion for 47-49min, performing ultrasonic power at 595-604W, performing ultrasonic frequency at 13-15kHz, drying, and standing at 0.8-1.2 ℃ for 5-7h to obtain functional particles;
the mass ratio of deionized water to sodium dodecyl benzene sulfonate to sodium carboxymethyl cellulose to maltodextrin is 96-104:0.5-0.7:0.3-0.5:1.4-1.6.
5. Preparation of spinning solution
Mixing modified particles, functional particles and spinning solution containing carrot components with deionized water, filtering, defoaming and curing to obtain spinning solution;
the content of alpha-fiber of the spinning solution is 8.7-8.9%, and the viscosity is 43-45s;
the mass ratio of the modified particles, the functional particles, the spinning solution and the deionized water containing the carrot active ingredients is 0.7-0.9:1.6-1.8:13-15:87-95.
6. Spinning process
Spraying the spinning solution into a coagulating bath, carrying out spinning treatment, and after spinning solidification, carrying out desulfurization, water washing, oiling and drying to obtain the large-sized viscose fiber containing the carrot active ingredient;
the coagulating bath comprises 95-105g/L sulfuric acid, 197-206g/L sodium sulfate and 24-26g/L zinc sulfate.
Compared with the prior art, the invention has the following beneficial effects:
1. the antibacterial rate of the giant viscose fiber prepared by the method is 96.3-96.7% on staphylococcus aureus, 95.6-95.9% on escherichia coli, the dry breaking strength is 4.3-4.6cN/dtex, the wet breaking strength is 2.4-2.7cN/dtex, and the breaking elongation is 27.3-28%;
2. the large-size viscose fiber prepared by the method of the invention is stood for 7 days at the temperature of 40 ℃ and the humidity of 75%, the antibacterial rate of staphylococcus aureus is 88.5-89.8%, the antibacterial rate of escherichia coli is 87.6-88.6%, the dry breaking strength is 3.8-4.1cN/dtex, the wet breaking strength is 2.15-2.44cN/dtex, and the elongation at break is 24.2-25.4%;
3. the large raw viscose fiber prepared by the method is purely spun into a fabric, the fabric is placed on a friction platform of a friction testing machine, the load of the friction testing machine is controlled to be 8N under the conditions that the temperature is 25 ℃ and the relative humidity is 65%, the friction times are 100 times, the friction speed is 30 times/min, the antibacterial rate of staphylococcus aureus is 86.3-87.7% after friction, the antibacterial rate of escherichia coli is 85.8-86.9%, the dry breaking strength is 3.6-3.9cN/dtex, the wet breaking strength is 2.04-2.32cN/dtex, and the elongation at break is 22.6-23.5%;
4. the air permeability of the large raw viscose fiber prepared by the method is 642-650mm/s, and the dimensional deformation rate of the fiber product is 0.3-0.6% after 50 times of standard washing.
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 Dasheng viscose fiber containing carrot active ingredient and its preparation method
1. Modified carrot extract
(1) Pretreatment of
Spraying deionized water to water content of 30%, then placing in a microwave device for microwave treatment with microwave power of 800W, microwave frequency of 1.4GHz, microwave time of 7min, then reducing to 70deg.C at a rate of 1.2 ℃/min, drying at 70deg.C for 1.5 hr, and naturally cooling to room temperature to obtain pretreated radix Dauci Sativae extract;
the carrot extract is sieved by a sieve with 80 meshes, and the carotene content is 3.57mg/100g;
(2) Secondary treatment
And (3) carrying out vacuum freeze drying treatment on the pretreated carrot extract, wherein the freezing temperature is-25 ℃, the freezing time is 18min, the vacuum degree is 300Pa, and the secondary treatment step is completed after naturally heating to room temperature, so as to obtain the modified carrot extract.
2. Preparation of modified particles
(1) Preparation of the Primary mix
Mixing montmorillonite, modified calcite, volcanic powder and betaine, performing primary ball milling, controlling the ball-material ratio at 8:1 during the primary ball milling, controlling the ball milling time to be 1.2h, the ball milling rotating speed to be 600rpm, the ball milling temperature to be 50 ℃, adding polyethylene glycol and xanthan gum for secondary ball milling, controlling the ball-material ratio of the secondary ball milling to be 6:1, the ball milling time to be 1.5h, the ball milling rotating speed to be 520rpm, and obtaining a primary mixed material after the secondary ball milling is finished;
the preparation method of the modified calcite comprises the steps of crushing calcite into powder with the particle size of 200 meshes, then placing the powder into a calciner for calcination, wherein the calcination temperature is 520 ℃, the calcination time is 5.5 hours, placing the powder into a microwave treatment device for microwave treatment after natural cooling, the microwave time is 15 minutes, the microwave power is 400W, placing the powder into a sodium chloride solution for soaking for 10 hours after natural cooling, and washing and drying after soaking to obtain the modified calcite;
the mass ratio of montmorillonite, modified calcite, volcanic powder, betaine, polyethylene glycol and xanthan gum is 20:30:23:0.8:1:1.4;
(2) Corona treatment
And carrying out corona treatment on the primary mixed material for 35min with a corona voltage of 120kV to obtain modified particles.
3. Load(s)
Mixing the modified carrot extract with deionized water, adding modified particles and betaine, controlling stirring speed to 870rpm, stirring for 34min, adding vinyltriethoxysilane, controlling stirring speed to 260rpm, stirring for 47min, filtering, and drying to obtain modified particles containing active components of carrot;
the mass ratio of the modified carrot extract to deionized water to the modified particles to the betaine to the vinyltriethoxysilane is 10:100:1.2:0.4:1.8.
4. Preparation of functional particles
Adding sodium dodecyl benzene sulfonate and sodium carboxymethyl cellulose into deionized water, stirring for 27min, controlling the stirring rotation speed to 320rpm, controlling the stirring temperature to be 52 ℃, then adding maltodextrin, performing ultrasonic dispersion for 48min, performing ultrasonic power to be 600W, performing ultrasonic frequency to be 14kHz, drying, and standing at the temperature of 1 ℃ for 6h to obtain functional particles;
the mass ratio of the deionized water to the sodium dodecyl benzene sulfonate to the sodium carboxymethyl cellulose to the maltodextrin is 100:0.6:0.4:1.5.
5. Preparation of spinning solution
Mixing modified particles, functional particles and spinning solution containing carrot components with deionized water, filtering, defoaming and curing to obtain spinning solution;
the first fiber content of the spinning solution is 8.8 percent, and the viscosity is 44s;
the mass ratio of the modified particles containing the carrot active ingredients, the functional particles, the spinning solution and the deionized water is 0.8:1.7:14:90.
6. Spinning process
Spraying the spinning solution into a coagulating bath, carrying out spinning treatment, and after spinning solidification, carrying out desulfurization, water washing, oiling and drying to obtain the large-sized viscose fiber containing the carrot active ingredient;
the coagulating bath is 100g/L of sulfuric acid, 200g/L of sodium sulfate and 25g/L of zinc sulfate.
The large-size viscose fiber prepared by the method of the example 1 has a bacteriostasis rate of 96.7% on staphylococcus aureus, 95.9% on escherichia coli, a dry breaking strength of 4.6cN/dtex, a wet breaking strength of 2.7cN/dtex and an elongation at break of 28%;
the giant viscose fiber prepared by the method of example 1 is stood for 7d at the temperature of 40 ℃ and the humidity of 75%, and the antibacterial rate of staphylococcus aureus is 89.8%, the antibacterial rate of escherichia coli is 88.6%, the dry breaking strength is 4.1cN/dtex, the wet breaking strength is 2.44cN/dtex, and the elongation at break is 25.4%;
the large-size viscose fiber prepared by the method of the example 1 is purely spun into a fabric, the fabric is placed on a friction platform of a friction testing machine, the load of the friction testing machine is controlled to be 8N under the conditions that the temperature is 25 ℃ and the relative humidity is 65%, the friction times are 100 times, the friction speed is 30 times/min, the antibacterial rate of staphylococcus aureus is 87.7% after the friction, the antibacterial rate of escherichia coli is 86.9%, the dry breaking strength is 3.9cN/dtex, the wet breaking strength is 2.32cN/dtex, and the breaking elongation is 23.5%;
the large viscose fiber prepared by the method of example 1 has the air permeability of 650mm/s and the dimensional deformation rate of the fiber product after 50 times of standard washing is 0.3 percent.
Example 2A Dasheng viscose fiber containing carrot active ingredient and its preparation method
1. Modified carrot extract
(1) Pretreatment of
Spraying deionized water to water content of 32%, then placing in a microwave device for microwave treatment with microwave power of 820W, microwave frequency of 1.5GHz and microwave time of 6min, then reducing the temperature to 72 ℃ at a speed of 1.4 ℃/min, drying at 72 ℃ for 1.2h, and naturally reducing the temperature to room temperature to obtain pretreated carrot extract;
the carrot extract is sieved by a sieve with 80 meshes, and the carotene content is 3.59mg/100g;
(2) Secondary treatment
And (3) carrying out vacuum freeze drying treatment on the pretreated carrot extract, wherein the freezing temperature is-27 ℃, the freezing time is 16min, the vacuum degree is 320Pa, and the secondary treatment step is completed after the carrot extract naturally rises to room temperature, so as to obtain the modified carrot extract.
2. Preparation of modified particles
(1) Preparation of the Primary mix
Mixing montmorillonite, modified calcite, volcanic powder and betaine, performing primary ball milling, controlling the ball-material ratio at 10:1 during the primary ball milling, controlling the ball milling time at 1.0h, the ball milling rotating speed at 610rpm, the ball milling temperature at 52 ℃, adding polyethylene glycol and xanthan gum for secondary ball milling, controlling the ball-material ratio during the secondary ball milling at 8:1, the ball milling time at 1.3h, the ball milling rotating speed at 530rpm, and the ball milling temperature at 46 ℃, and obtaining a primary mixed material after the secondary ball milling is finished;
the preparation method of the modified calcite comprises the steps of crushing calcite into powder with the particle size of 200 meshes, then placing the powder into a calciner for calcination, wherein the calcination temperature is 525 ℃, the calcination time is 5.3 hours, placing the powder into a microwave treatment device for microwave treatment after natural cooling, the microwave time is 16 minutes, the microwave power is 410W, placing the powder into a sodium chloride solution for soaking for 11 hours after natural cooling, and washing and drying after soaking to obtain the modified calcite;
the mass ratio of montmorillonite, modified calcite, volcanic powder, betaine, polyethylene glycol and xanthan gum is 22:28:24:0.9:1.2:1.5;
(2) Corona treatment
And carrying out corona treatment on the primary mixed material for 38min with a corona voltage of 116kV to obtain modified particles.
3. Load(s)
Mixing the modified carrot extract with deionized water, adding modified particles and betaine, controlling stirring speed to 880rpm, stirring for 32min, adding vinyltriethoxysilane, controlling stirring speed to 270rpm, stirring for 45min, filtering, and drying to obtain modified particles containing active components of carrot;
the mass ratio of the modified carrot extract to deionized water to the modified particles to the betaine to the vinyltriethoxysilane is 12:110:1.4:0.5:2.0.
4. Preparation of functional particles
Adding sodium dodecyl benzene sulfonate and sodium carboxymethyl cellulose into deionized water, stirring for 28min, controlling the stirring rotation speed to 310rpm, controlling the stirring temperature to be 50 ℃, then adding maltodextrin, performing ultrasonic dispersion for 49min, performing ultrasonic power to be 604W, performing ultrasonic frequency to be 15kHz, drying, and standing at the temperature of 1.2 ℃ for 5h to obtain functional particles;
the mass ratio of the deionized water to the sodium dodecyl benzene sulfonate to the sodium carboxymethyl cellulose to the maltodextrin is 104:0.7:0.5:1.6.
5. Preparation of spinning solution
Mixing modified particles, functional particles and spinning solution containing carrot components with deionized water, filtering, defoaming and curing to obtain spinning solution;
the first fiber content of the spinning solution is 8.9%, and the viscosity is 45s;
the mass ratio of the modified particles containing the carrot active ingredients, the functional particles, the spinning solution and the deionized water is 0.9:1.8:15:95.
6. Spinning process
Spraying the spinning solution into a coagulating bath, carrying out spinning treatment, and after spinning solidification, carrying out desulfurization, water washing, oiling and drying to obtain the large-sized viscose fiber containing the carrot active ingredient;
the coagulating bath contains 105g/L sulfuric acid, 206g/L sodium sulfate and 26g/L zinc sulfate.
The large-size viscose fiber prepared by the method of the example 2 has a bacteriostasis rate of 96.3 percent on staphylococcus aureus, 95.6 percent on escherichia coli, a dry breaking strength of 4.5cN/dtex, a wet breaking strength of 2.5cN/dtex and an elongation at break of 27.6 percent;
the giant viscose fiber prepared by the method of the example 2 is stood for 7d at the temperature of 40 ℃ and the humidity of 75%, and the antibacterial rate of staphylococcus aureus is 88.9%, the antibacterial rate of escherichia coli is 88.0%, the dry breaking strength is 4.0cN/dtex, the wet breaking strength is 2.24cN/dtex, and the elongation at break is 24.6%;
the large-size viscose fiber prepared by the method of the example 2 is purely spun into a fabric, the fabric is placed on a friction platform of a friction testing machine, the load of the friction testing machine is controlled to be 8N under the conditions that the temperature is 25 ℃ and the relative humidity is 65%, the friction times are 100 times, the friction speed is 30 times/min, the antibacterial rate of staphylococcus aureus is 86.5% after the friction, the antibacterial rate of escherichia coli is 86.0%, the dry breaking strength is 3.8cN/dtex, the wet breaking strength is 2.14cN/dtex, and the breaking elongation is 23.1%;
the resulting large viscose fiber produced by the method of example 2 had an air permeability of 644mm/s and a dimensional deformation of 0.5% after 50 standard washes.
Example 3A Dasheng viscose fiber containing carrot active ingredient and its preparation method
1. Modified carrot extract
(1) Pretreatment of
Spraying deionized water to water content of 28%, placing in a microwave device for microwave treatment with microwave power of 780W, microwave frequency of 1.3GHz, and microwave time of 8min, reducing the temperature to 68 ℃ at a speed of 1.0 ℃/min, drying at 68 ℃ for 1.8h, and naturally reducing the temperature to room temperature to obtain pretreated carrot extract;
the carrot extract is sieved by a sieve with 80 meshes, and the carotene content is 3.55mg/100g;
(2) Secondary treatment
And (3) carrying out vacuum freeze drying treatment on the pretreated carrot extract, wherein the freezing temperature is-23 ℃, the freezing time is 20min, the vacuum degree is 280Pa, and the secondary treatment step is completed after naturally heating to room temperature, so as to obtain the modified carrot extract.
2. Preparation of modified particles
(1) Preparation of the Primary mix
Mixing montmorillonite, modified calcite, volcanic powder and betaine, performing primary ball milling, controlling the ball-material ratio at 6:1 during the primary ball milling, controlling the ball milling time at 1.4h, the ball milling rotating speed at 590rpm, the ball milling temperature at 48 ℃, adding polyethylene glycol and xanthan gum for secondary ball milling, controlling the ball-material ratio of the secondary ball milling at 4:1, the ball milling time at 1.8h, the ball milling rotating speed at 510rpm, the ball milling temperature at 44 ℃, and obtaining a primary mixed material after the secondary ball milling is finished;
the preparation method of the modified calcite comprises the steps of crushing calcite into powder with the particle size of 200 meshes, then placing the powder into a calciner for calcination, wherein the calcination temperature is 515 ℃, the calcination time is 5.7 hours, placing the powder into a microwave treatment device for microwave treatment after natural cooling, the microwave time is 14 minutes, the microwave power is 390W, placing the powder into a sodium chloride solution for soaking for 9 hours after natural cooling, and washing and drying after soaking to obtain the modified calcite;
the mass ratio of montmorillonite, modified calcite, volcanic powder, betaine, polyethylene glycol and xanthan gum is 18:32:22:0.7:0.8:1.3;
(2) Corona treatment
And carrying out corona treatment on the primary mixed material for 32min with a corona voltage of 124kV to obtain modified particles.
3. Load(s)
Mixing the modified carrot extract with deionized water, adding modified particles and betaine, controlling stirring speed to 860rpm, stirring for 36min, adding vinyltriethoxysilane, controlling stirring speed to 250rpm, stirring for 50min, filtering, and drying to obtain modified particles containing active components of carrot;
the mass ratio of the modified carrot extract to deionized water to the modified particles to the betaine to the vinyltriethoxysilane is 8:96:1.0:0.3:1.6.
4. Preparation of functional particles
Adding sodium dodecyl benzene sulfonate and sodium carboxymethyl cellulose into deionized water, stirring for 26min, controlling the stirring rotation speed to 330rpm, controlling the stirring temperature to be 54 ℃, then adding maltodextrin, performing ultrasonic dispersion for 47min, performing ultrasonic power to be 595W, performing ultrasonic frequency to be 13kHz, drying, and standing at the temperature of 0.8 ℃ for 7h to obtain functional particles;
the mass ratio of deionized water to sodium dodecyl benzene sulfonate to sodium carboxymethyl cellulose to maltodextrin is 96:0.5:0.3:1.4.
5. Preparation of spinning solution
Mixing modified particles, functional particles and spinning solution containing carrot components with deionized water, filtering, defoaming and curing to obtain spinning solution;
the first fiber content of the spinning solution is 8.7 percent, and the viscosity is 43 seconds;
the mass ratio of the modified particles containing the carrot active ingredients, the functional particles, the spinning solution and the deionized water is 0.7:1.6:13:87.
6. Spinning process
Spraying the spinning solution into a coagulating bath, carrying out spinning treatment, and after spinning solidification, carrying out desulfurization, water washing, oiling and drying to obtain the large-sized viscose fiber containing the carrot active ingredient;
the coagulating bath comprises 95g/L sulfuric acid, 197g/L sodium sulfate and 24g/L zinc sulfate.
The large-size viscose fiber prepared by the method of the example 3 has a bacteriostasis rate of 96.4% on staphylococcus aureus, 95.7% on escherichia coli, a dry breaking strength of 4.3cN/dtex, a wet breaking strength of 2.4cN/dtex and an elongation at break of 27.3%;
the giant viscose fiber prepared by the method of example 3 is stood for 7d at the temperature of 40 ℃ and the humidity of 75%, and the antibacterial rate of staphylococcus aureus is 88.5%, the antibacterial rate of escherichia coli is 87.6%, the dry breaking strength is 3.8cN/dtex, the wet breaking strength is 2.15cN/dtex, and the elongation at break is 24.2%;
the large-size viscose fiber prepared by the method of the example 3 is purely spun into a fabric, the fabric is placed on a friction platform of a friction testing machine, the load of the friction testing machine is controlled to be 8N under the conditions that the temperature is 25 ℃ and the relative humidity is 65%, the friction times are 100 times, the friction speed is 30 times/min, the antibacterial rate of staphylococcus aureus is 86.3% after the friction, the antibacterial rate of escherichia coli is 85.8%, the dry breaking strength is 3.6cN/dtex, the wet breaking strength is 2.04cN/dtex, and the breaking elongation is 22.6%;
the large viscose fiber prepared by the method of example 3 has air permeability of 642mm/s and the dimensional deformation rate of the fiber product is 0.6% after 50 times of standard washing.
Comparative example 1
The modification of the carrot extract was omitted on the basis of example 1, the untreated carrot extract was directly used, and the rest of the operations were the same.
The antibacterial rate of the large-size viscose fiber prepared by adopting the method of the comparative example 1 to staphylococcus aureus is 82.3 percent, the antibacterial rate to escherichia coli is 81.4 percent, the dry breaking strength is 4.0cN/dtex, the wet breaking strength is 2.35cN/dtex, and the breaking elongation is 24.7 percent;
the large viscose fiber prepared by the method of comparative example 1 is stood for 7 days at the temperature of 40 ℃ and the humidity of 75%, and the antibacterial rate of staphylococcus aureus is 61.7%, the antibacterial rate of escherichia coli is 61.0%, the dry breaking strength is 3.1cN/dtex, the wet breaking strength is 1.85cN/dtex, and the elongation at break is 19.8%;
the large-size viscose fiber prepared by the method of the comparative example 1 is purely spun into a fabric, and is placed on a friction platform of a friction testing machine, under the conditions that the temperature is 25 ℃, the relative humidity is 65%, the load of the friction testing machine is controlled to be 8N, the friction times are 100 times, the friction speed is 30 times/min, the antibacterial rate of staphylococcus aureus is 60.3% after friction, the antibacterial rate of escherichia coli is 60.2%, the dry breaking strength is 2.9cN/dtex, the wet breaking strength is 1.73cN/dtex, and the elongation at break is 18.1%;
the large viscose fiber prepared by the method of comparative example 1 has the air permeability of 540mm/s and the dimensional deformation rate of the fiber product after 50 times of standard washing is 2.6 percent.
Comparative example 2
On the basis of example 1, the modification of calcite was performed in the step of preparing modified particles, and the corona treatment step was omitted, except that the modified calcite was replaced with calcite, and the rest of the operations were the same.
The antibacterial rate of the large-size viscose fiber prepared by adopting the method of the comparative example 2 to staphylococcus aureus is 81.4 percent, the antibacterial rate to escherichia coli is 80.6 percent, the dry breaking strength is 3.8cN/dtex, the wet breaking strength is 2.17cN/dtex, and the breaking elongation is 22.6 percent;
the large viscose fiber prepared by adopting the method of comparative example 2 is stood for 7 days at the temperature of 40 ℃ and the humidity of 75%, and the antibacterial rate of staphylococcus aureus is 58.5%, the antibacterial rate of escherichia coli is 60.4%, the dry breaking strength is 2.8cN/dtex, the wet breaking strength is 1.62cN/dtex, and the elongation at break is 16.9%;
the large-size viscose fiber prepared by the method of the comparative example 2 is purely spun into a fabric, and is placed on a friction platform of a friction testing machine, under the conditions that the temperature is 25 ℃, the relative humidity is 65%, the load of the friction testing machine is controlled to be 8N, the friction times are 100 times, the friction speed is 30 times/min, the antibacterial rate of staphylococcus aureus is 57.8%, the antibacterial rate of escherichia coli is 57.2%, the dry breaking strength is 2.7cN/dtex, the wet breaking strength is 1.54cN/dtex, and the elongation at break is 16.1%;
the large viscose fiber prepared by the method of comparative example 2 has air permeability of 532mm/s, and the dimensional deformation rate of the fiber product is 3.0% after 50 times of standard washing.
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 comprises the steps of modifying carrot extract, preparing modified particles, loading, preparing functional particles, preparing spinning solution and spinning;
the preparation of the modified carrot extract comprises pretreatment and secondary treatment; the preparation of modified particles comprises the steps of preparing a primary mixed material and carrying out corona treatment;
spraying deionized water to the carrot extract until the water content is 28-32%, then placing the carrot extract in a microwave device for microwave treatment, wherein the microwave power is 780-820W, the microwave frequency is 1.3-1.5GHz, the microwave time is 6-8min, then reducing the temperature to 68 ℃ at a speed of 1.0-1.4 ℃/min, controlling the temperature to 68-72 ℃ and drying for 1.2-1.8h, and naturally reducing the temperature to room temperature to obtain the pretreated carrot extract;
the secondary treatment step is that the pretreated carrot extract is subjected to vacuum freeze drying treatment, the freezing temperature is between-27 ℃ and-23 ℃, the freezing time is between 16 and 20 minutes, the vacuum degree is between 280Pa and 320Pa, and the secondary treatment step is completed after the carrot extract is naturally warmed to room temperature, so that the modified carrot extract is prepared;
the primary mixed material comprises modified calcite, and the preparation method of the modified calcite comprises the steps of crushing calcite into powder with the particle size of 200 meshes, then placing the powder in a calciner for calcination at the temperature of 515-525 ℃ for 5.3-5.7h, naturally cooling, placing the powder in a microwave treatment device for microwave treatment for 14-16min, placing the powder in a sodium chloride solution for soaking for 9-11h after naturally cooling, and washing and drying the powder after soaking to obtain the modified calcite.
2. The method for preparing the large-sized viscose fiber containing carrot as active ingredient of claim 1,
the carrot extract has a particle size of 3.55-3.59mg/100g and is sieved by a 80-mesh sieve.
3. The method for preparing the large-sized viscose fiber containing carrot as active ingredient of claim 1,
mixing montmorillonite and modified calcite with volcanic powder and betaine, performing first ball milling, controlling the ball-material ratio at 6-10:1, the ball milling time at 1.0-1.4h, the ball milling rotating speed at 590-610rpm, the ball milling temperature at 48-52 ℃, adding polyethylene glycol and xanthan gum for second ball milling, controlling the ball-material ratio at 4-8:1, the ball milling time at 1.3-1.8h, the ball milling rotating speed at 510-530rpm, the ball milling temperature at 44-46 ℃, and obtaining the initial mixture after the second ball milling is finished;
the corona treatment step is that the primary mixed material is subjected to corona treatment for 32-38min with corona voltage of 116-124kV to obtain modified particles.
4. A method for preparing a large-sized viscose fiber containing active ingredient of carrot as claimed in claim 3,
the mass ratio of montmorillonite, modified calcite, volcanic rock powder, betaine, polyethylene glycol and xanthan gum is 18-22:28-32:22-24:0.7-0.9:0.8-1.2:1.3-1.5.
5. The method for preparing the large-sized viscose fiber containing carrot as active ingredient of claim 1,
the loading step comprises the steps of mixing the modified carrot extract with deionized water, adding modified particles and betaine, controlling the stirring speed to 860-880rpm, stirring for 32-36min, adding vinyl triethoxysilane, controlling the stirring speed to 250-270rpm, stirring for 45-50min, filtering, and drying to obtain the modified particles containing active ingredients of the carrot.
6. The method for preparing the active ingredient of the Dacron viscose fiber according to claim 5,
the mass ratio of the modified carrot extract to deionized water to modified particles to betaine to vinyltriethoxysilane is 8-12:96-110:1.0-1.4:0.3-0.5:1.6-2.0.
7. The method for preparing the large-sized viscose fiber containing carrot as active ingredient of claim 1,
the preparation method of the functional particles comprises the steps of adding sodium dodecyl benzene sulfonate and sodium carboxymethyl cellulose into deionized water, stirring for 26-28min, controlling the stirring rotation speed to 310-330rpm, stirring at 50-54 ℃, adding maltodextrin, performing ultrasonic dispersion for 47-49min, performing ultrasonic power to 595-604W, performing ultrasonic frequency to 13-15kHz, drying, and standing at 0.8-1.2 ℃ for 5-7h to obtain the functional particles.
8. The method for preparing the active ingredient of the Dacron viscose fiber according to claim 7,
the mass ratio of deionized water to sodium dodecyl benzene sulfonate to sodium carboxymethyl cellulose to maltodextrin is 96-104:0.5-0.7:0.3-0.5:1.4-1.6.
9. The method for preparing the large-sized viscose fiber containing carrot as active ingredient of claim 1,
the step of preparing the spinning solution comprises the steps of mixing modified particles containing carrot components, functional particles, spinning solution and deionized water, and filtering, defoaming and curing to obtain the spinning solution;
the content of alpha-fiber of the spinning solution is 8.7-8.9%, and the viscosity is 43-45s;
the mass ratio of the modified particles, the functional particles, the spinning solution and the deionized water containing the carrot active ingredients is 0.7-0.9:1.6-1.8:13-15:87-95.
10. The method for preparing the large-sized viscose fiber containing carrot as active ingredient of claim 1,
spraying spinning solution into a coagulating bath for spinning treatment, desulfurizing, washing, oiling and drying after spinning solidification to obtain the large-sized viscose fiber containing carrot active ingredients;
the coagulating bath comprises 95-105g/L sulfuric acid, 197-206g/L sodium sulfate and 24-26g/L zinc sulfate.
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