CN112779627A - ES macrobio fiber containing active ingredients of tangerine peel, orange and pomelo and preparation method thereof - Google Patents
ES macrobio fiber containing active ingredients of tangerine peel, orange and pomelo and preparation method thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 76
- 239000004480 active ingredient Substances 0.000 title claims abstract description 34
- 240000000560 Citrus x paradisi Species 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 241000675108 Citrus tangerina Species 0.000 title claims abstract description 22
- 230000000975 bioactive effect Effects 0.000 claims abstract description 43
- 238000000227 grinding Methods 0.000 claims abstract description 33
- 238000002074 melt spinning Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 230000004048 modification Effects 0.000 claims abstract description 13
- 238000012986 modification Methods 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 11
- -1 melt spinning Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 63
- 239000002245 particle Substances 0.000 claims description 63
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 57
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 239000012792 core layer Substances 0.000 claims description 35
- 239000010410 layer Substances 0.000 claims description 32
- 239000000377 silicon dioxide Substances 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 27
- 239000000843 powder Substances 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 24
- 235000012239 silicon dioxide Nutrition 0.000 claims description 23
- 239000011148 porous material Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000009987 spinning Methods 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 238000010008 shearing Methods 0.000 claims description 10
- HDTRYLNUVZCQOY-UHFFFAOYSA-N α-D-glucopyranosyl-α-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OC1C(O)C(O)C(O)C(CO)O1 HDTRYLNUVZCQOY-UHFFFAOYSA-N 0.000 claims description 9
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims description 9
- HDTRYLNUVZCQOY-WSWWMNSNSA-N Trehalose Natural products O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-WSWWMNSNSA-N 0.000 claims description 9
- HDTRYLNUVZCQOY-LIZSDCNHSA-N alpha,alpha-trehalose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 HDTRYLNUVZCQOY-LIZSDCNHSA-N 0.000 claims description 9
- 238000007664 blowing Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000000787 lecithin Substances 0.000 claims description 9
- 229940067606 lecithin Drugs 0.000 claims description 9
- 235000010445 lecithin Nutrition 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000000230 xanthan gum Substances 0.000 claims description 9
- 229920001285 xanthan gum Polymers 0.000 claims description 9
- 229940082509 xanthan gum Drugs 0.000 claims description 9
- 235000010493 xanthan gum Nutrition 0.000 claims description 9
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000002137 ultrasound extraction Methods 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- XEGMDUOAESTQCC-UHFFFAOYSA-N 1-(naphthalen-1-ylmethyl)naphthalene;sodium Chemical compound [Na].C1=CC=C2C(CC=3C4=CC=CC=C4C=CC=3)=CC=CC2=C1 XEGMDUOAESTQCC-UHFFFAOYSA-N 0.000 claims description 5
- 238000013329 compounding Methods 0.000 claims description 5
- 238000004042 decolorization Methods 0.000 claims description 5
- 230000001804 emulsifying effect Effects 0.000 claims description 5
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 5
- DWHOIYXAMUMQTI-UHFFFAOYSA-L disodium;2-[(1-sulfonatonaphthalen-2-yl)methyl]naphthalene-1-sulfonate Chemical compound [Na+].[Na+].C1=CC2=CC=CC=C2C(S(=O)(=O)[O-])=C1CC1=CC=C(C=CC=C2)C2=C1S([O-])(=O)=O DWHOIYXAMUMQTI-UHFFFAOYSA-L 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims 1
- 238000005507 spraying Methods 0.000 claims 1
- 239000004615 ingredient Substances 0.000 abstract description 14
- 230000003385 bacteriostatic effect Effects 0.000 abstract description 9
- 230000035699 permeability Effects 0.000 abstract description 8
- 239000004594 Masterbatch (MB) Substances 0.000 abstract description 5
- 238000002788 crimping Methods 0.000 abstract description 5
- 241000222122 Candida albicans Species 0.000 abstract description 4
- 241000588724 Escherichia coli Species 0.000 abstract description 4
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 4
- 229940095731 candida albicans Drugs 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 3
- 239000003599 detergent Substances 0.000 abstract 1
- 239000000155 melt Substances 0.000 description 12
- 230000000844 anti-bacterial effect Effects 0.000 description 7
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 238000001694 spray drying Methods 0.000 description 7
- 238000001125 extrusion Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 244000276331 Citrus maxima Species 0.000 description 4
- 235000001759 Citrus maxima Nutrition 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000011162 core material Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000007822 coupling agent Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- LCRMGUFGEDUSOG-UHFFFAOYSA-N naphthalen-1-ylsulfonyloxymethyl naphthalene-1-sulfonate;sodium Chemical compound [Na].C1=CC=C2C(S(=O)(OCOS(=O)(=O)C=3C4=CC=CC=C4C=CC=3)=O)=CC=CC2=C1 LCRMGUFGEDUSOG-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 239000008041 oiling agent Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
Classifications
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- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
- D01D5/092—Cooling filaments, threads or the like, leaving the spinnerettes in shafts or chimneys
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/22—Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
Abstract
A preparation method of ES macrobiological fiber containing active ingredients of pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis comprises preparing bioactive ingredients, preparing master batch containing bioactive ingredients, melt spinning, air cooling, drafting, and crimping; the preparation of the bioactive components comprises extraction, drying, grinding, microencapsulation and grinding modification. The ES macrobio fiber containing the active ingredients of the tangerine peel, the orange and the pomelo has the advantages that: the bacteriostasis rate to escherichia coli is more than 97.89%, the bacteriostasis rate to staphylococcus aureus is more than 99.12%, and the bacteriostasis rate to candida albicans is more than 98.55%; after 100 times of standard washing, the bacteriostatic rate of the detergent on escherichia coli is still greater than 94.12%, the bacteriostatic rate on staphylococcus aureus is still greater than 95.71%, and the bacteriostatic rate on candida albicans is still greater than 95.15%; the air permeability is improved, and the air permeability of the ES large biological fiber is improved to 1800-2100L/m 2-s.
Description
Technical Field
The invention relates to the technical field of preparation of ES fibers, in particular to a preparation method of ES macrobio-fibers containing active ingredients of tangerine peel, orange and pomelo.
Background
The ES fiber is a bi-component skin-core structure composite fiber, the skin tissue has low melting point and good flexibility, and the core tissue has high melting point and high strength. After the fiber is subjected to heat treatment, part of the skin layer is melted to play a role in bonding, the rest of the skin layer still keeps the fiber state, and meanwhile, the fiber has the characteristic of small heat shrinkage rate, is particularly suitable for being used as a hot air penetration process for producing products such as sanitary materials, heat-insulating filling materials, filtering materials and the like, and is most commonly used for manufacturing N95 masks at present.
With the increasing demand of people on sanitary products such as masks and the like, new requirements on the air permeability and the adsorbability of ES fibers are also met, but the air permeability, the adsorbability and the hygroscopicity of the existing ES fibers are poor; moreover, the ES fibers on the market have poor mechanical properties, although the antibacterial agent is added in the production of the ES fibers to ensure that the ES fibers have antibacterial property, the ES fibers on the market have limited antibacterial capability and do not have a lasting antibacterial effect; and the existing ES fiber has poor hydrophilicity and unstable hydrophilicity.
Patent CN201811419082.8 discloses a multifunctional ES fiber for non-woven fabrics and a preparation process thereof, the ES fiber is of a sheath-core structure, and a sheath material consists of refined wollastonite powder, sheath resin, an antioxidant, a dispersant, a stabilizer, a coupling agent, an antistatic agent and an antibacterial agent; the core layer material consists of superfine diatomite, core layer resin, an antioxidant, a dispersant, a lubricant and a coupling agent; the preparation process comprises heating and mixing the leather material in a high-speed mixer; heating and mixing the core layer materials in a high-speed mixer; and putting the mixed sheath layer material and core layer material into a spinning machine, and performing hot melting and high-pressure extrusion, spinning, air cooling, stretching, immersion, secondary stretching, drying and cutting. The patent has the following defects: the multifunctional ES fiber has poor hydrophilicity and unstable hydrophilicity.
Patent CN201910584382.X discloses an ES fiber and a preparation method and application thereof, wherein the ES fiber comprises 30-60 parts by weight of a skin layer resin, 25-45 parts by weight of a core layer resin, 8-15 parts by weight of shell powder, 1-3 parts by weight of titanium dioxide powder, 0.1-1 part by weight of a dispersant and 0.1-2 parts by weight of a coupling agent; the surface of the ES fiber is uniformly coated with an oiling agent. The patent has the following defects: the prepared ES fiber has low air permeability and adsorbability and limited antibacterial ability.
Disclosure of Invention
The preparation method of the ES macrobio fiber containing the active ingredients of the tangerine peel, the orange and the pomelo can improve the air permeability, the adsorbability, the hygroscopicity and the antibacterial performance of the ES fiber by adding the active ingredients of the tangerine peel, the orange and the pomelo in the production of the ES fiber, so that the ES fiber has lasting antibacterial capacity, and the hydrophilic performance of the existing ES fiber can be improved.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for preparing ES macrobiological fiber containing active ingredients of pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis comprises preparing bioactive ingredients, preparing master batch containing bioactive ingredients, melt spinning, air cooling, drafting and crimping.
The preparation of the bioactive components comprises extraction, drying, grinding, microencapsulation, grinding modification and porosification.
The extraction comprises the steps of uniformly mixing the dried orange peel, the orange peel and the shaddock peel, drying at 60-75 ℃ until the water content is lower than 7%, then placing the mixture into a crusher to be crushed into coarse powder with the particle size of 1-3mm, adding absolute ethyl alcohol, and carrying out continuous countercurrent ultrasonic extraction at 55-65 ℃ for 110min to obtain an ethanol ultrasonic extracting solution, wherein the ultrasonic frequency is 55-65 KHz; concentrating the ethanol ultrasonic extraction solution at high temperature and high pressure to obtain a concentrated solution, wherein the temperature in the high-temperature and high-pressure process is 90-95 ℃, and the pressure is 0.25-0.4 MPa; and then adding activated carbon into the concentrated solution for decolorization and then filtering to obtain purified concentrated solution.
And drying, namely performing spray drying on the purified concentrated solution to obtain concentrated particles.
And grinding, namely grinding the concentrated particles to obtain concentrated powder with the particle size of 4-7 microns.
Microencapsulation, namely uniformly mixing the concentrated powder, lecithin and deionized water, and then stirring at 60-75 ℃, wherein the stirring speed is 350-420rpm, and the stirring time is 20-30 min; adding zinc stearate, trehalose and xanthan gum after stirring, heating to 45-50 ℃, putting into a high shearing machine, shearing and emulsifying at 6000-.
Wherein the mass ratio of the concentrated powder to the lecithin to the deionized water is 3: 4-5: 60-75.
Wherein the mass ratio of the concentrated powder, the zinc stearate, the trehalose and the xanthan gum is 10: 2-4: 6-7: 6-8.
And grinding modification, namely adding the microencapsulated particles into a ball mill for grinding to obtain the ground microencapsulated particles with the average particle size of 40-50 nm.
And (2) the step of porous treatment, namely mixing the microencapsulated particles and the silicon dioxide, adding the mixture into absolute ethyl alcohol, adding sodium methylenedinaphthalene sulfonate, and stirring for 3-4 hours at the speed of 350rpm, so that the microencapsulated particles are fully dispersed into the pore diameter of the silicon dioxide to form the bioactive material with the average particle size of 500-600nm, wherein the bioactive material is the silicon dioxide porous material with the microencapsulated particles loaded in the pores.
The specific surface area of the silicon dioxide is 90-100m2/g, and the average pore diameter is 80-100 nm.
Wherein the microencapsulated particles: silicon dioxide: the mass ratio of the methylene dinaphthalene sodium sulfonate is 4-5: 1: 2-3.
The melt spinning comprises the steps of uniformly mixing the bioactive material and a PE slice in a mass ratio of 1:9-12 to obtain a skin layer material, uniformly mixing the bioactive material and a PET slice in a mass ratio of 1:30-35 to obtain a core layer material, respectively placing the skin layer material and the core layer material into corresponding hoppers of a screw extruder, extruding a skin layer melt and a core layer melt, compounding the skin layer melt and the core layer melt in a composite spinning assembly, and then ejecting a skin-core layer structure fiber through a spinneret plate.
The mass ratio of the skin layer material to the core layer material in the melt spinning process is 1: 2-2.5.
The melt temperature of the skin layer material in the melt extrusion process is 105-115 ℃; the melt temperature of the melting screw B is 180-195 ℃.
And the air cooling is to perform circular air blowing cooling solidification on the fiber trickle after melt spinning, and send cold air in a deformation area 0-200mm below a spinning assembly plate, wherein the air speed is 0.8-1 m/s, the side blowing air temperature is 18-21 ℃, the air humidity is 50-55%, and the air speed is 1.8-2.2 m/s.
The drafting is carried out by adopting a drafting machine, the drafting multiple is 7-9 times, and the drafting speed is 20-24 m/min;
and the curling is carried out in a curling machine, the curling pressure is 0.1-0.15MPa, the curling degree is 4.5% -5.2%, and the fiber after the curling is cut into broken filaments.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the ES macrobio-fiber containing the active ingredients of the tangerine peel, the orange and the pomelo, the biological active ingredients are added in the production of the ES fiber, so that the ES fiber has an antibacterial effect, and according to a test, the bacteriostatic rate of the ES macrobio-fiber on escherichia coli is more than 97.89%, the bacteriostatic rate on staphylococcus aureus is more than 99.12%, and the bacteriostatic rate on candida albicans is more than 98.55%;
(2) according to the ES macrobio-fiber containing the active ingredients of the tangerine peel, the orange and the pomelo, the loss of the bioactive ingredients in washing can be reduced by microencapsulating the bioactive ingredients, and after 100 times of standard washing, the bacteriostatic rate of the ES macrobio-fiber on escherichia coli is still greater than 94.12%, the bacteriostatic rate on staphylococcus aureus is still greater than 95.71%, and the bacteriostatic rate on candida albicans is still greater than 95.15%;
(3) according to the ES macrobio-fiber containing the active ingredients of the dried orange peel, the orange and the pomelo, the silica porous material with microencapsulated particles loaded in the pores is prepared by mixing the microencapsulated bioactive particles and the silica, so that the air permeability is improved, and the air permeability of the ES macrobio-fiber is improved to 1800-2100L/m2 & s;
(4) according to the ES macrobio-fiber containing the active ingredients of the dried orange peel, the orange and the pomelo, the moisture absorption and moisture regain are improved by microencapsulating the active ingredients, and the moisture absorption and moisture regain of the prepared ES macrobio-fiber is 0.3% -0.5%;
(5) the fabric prepared from the ES macrobio-fiber containing the active ingredients of the tangerine peel, the orange and the pomelo improves the hydrophilic property by adding the bioactive ingredients into the core layer material, and can improve the water retention rate to 78.5-87.1%;
(6) according to the ES macrobio-fiber containing the active ingredients of the dried orange peel, the orange and the pomelo, the mechanical strength is improved by adding the bioactive ingredients in the production of the ES fiber, and the dry fracture strength of the prepared ES macrobio-fiber is 3-4cN/dtex, and the wet fracture strength is 2-3 cN/dtex.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.
Example 1
A method for preparing ES macrobiological fiber containing active ingredients of pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis comprises preparing bioactive ingredients, preparing master batch containing bioactive ingredients, melt spinning, air cooling, drafting and crimping.
The preparation of the bioactive components comprises extraction, drying, grinding, microencapsulation, grinding modification and porosification.
The extraction comprises the steps of uniformly mixing the dried orange peel, the orange peel and the shaddock peel, drying at 60 ℃ until the water content is lower than 7%, then placing the mixture into a crusher to be crushed into coarse powder with the particle size of 1mm, adding absolute ethyl alcohol, and carrying out continuous countercurrent ultrasonic extraction at 55 ℃ for 100min to obtain an ethanol ultrasonic extracting solution, wherein the ultrasonic frequency is 55 KHz; carrying out high-temperature high-pressure concentration on the ethanol ultrasonic extracting solution to obtain a concentrated solution, wherein the temperature in the high-temperature high-pressure process is 90 ℃, and the pressure is 0.25 MPa; and then adding activated carbon into the concentrated solution for decolorization and then filtering to obtain purified concentrated solution.
And drying, namely performing spray drying on the purified concentrated solution to obtain concentrated particles.
And grinding, namely grinding the concentrated particles to obtain concentrated powder with the particle size of 4 microns.
Microencapsulation, namely uniformly mixing concentrated powder, lecithin and deionized water, and then stirring at 60 ℃, wherein the stirring speed is 350rpm, and the stirring time is 20 min; adding zinc stearate, trehalose and xanthan gum after stirring, heating to 45 ℃, putting into a high shearing machine, shearing and emulsifying at 6000rpm for 15min, and then performing spray drying to obtain microencapsulated particles.
Wherein the mass ratio of the concentrated powder to the lecithin to the deionized water is 3: 4: 60.
wherein the mass ratio of the concentrated powder, the zinc stearate, the trehalose and the xanthan gum is 10: 2: 6: 6.
and grinding modification, namely adding the microencapsulated particles into a ball mill for grinding to obtain the ground microencapsulated particles with the average particle size of 40 nm.
And (2) carrying out porosification, namely mixing the microencapsulated particles with silicon dioxide, adding the mixture into absolute ethyl alcohol, then adding sodium methylene dinaphthalene sulfonate, and stirring for 3 hours at 300rpm, so that the microencapsulated particles are fully dispersed into the pore diameter of the silicon dioxide to form a bioactive material with the average particle size of 500nm, wherein the bioactive material is a silicon dioxide porous material with the microencapsulated particles loaded in the pores.
The silica had a specific surface area of 90m2/g and an average pore diameter of 80 nm.
Wherein the microencapsulated particles: silicon dioxide: the mass ratio of the methylene dinaphthalene sodium sulfonate is 4: 1: 3.
the melt spinning comprises the steps of uniformly mixing a bioactive material and a PE slice in a mass ratio of 1:9 to obtain a skin layer material, uniformly mixing the bioactive material and the PET slice in a mass ratio of 1:30 to obtain a core layer material, respectively placing the skin layer material and the core layer material into corresponding screw extruder hoppers to extrude a skin layer melt and a core layer melt, compounding the skin layer melt and the core layer melt in a composite spinning assembly, and then ejecting a skin-core layer structure fiber through a spinneret plate.
The mass ratio of the skin layer material to the core layer material in the melt spinning process is 1: 2.
the melt temperature of the skin layer material in the melt extrusion process is 105 ℃; the melt temperature of the melting screw B is 180-195 ℃.
And air cooling, namely cooling and solidifying the fiber trickle subjected to melt spinning by circular air blowing, and feeding cold air in a deformation area 0mm below a spinning assembly plate at the air speed of 0.8 m/s, the side air temperature of 18 ℃, the air humidity of 50% and the air speed of 1.8 m/s.
The drafting is carried out by adopting a drafting machine, the drafting multiple is 7 times, and the drafting speed is 20 m/min;
and the curling is carried out in a curling machine, the curling pressure is 0.1MPa, the curling degree is 4.5 percent, and the fiber after the curling is finished is cut into broken filaments.
Example 2
A method for preparing ES macrobiological fiber containing active ingredients of pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis comprises preparing bioactive ingredients, preparing master batch containing bioactive ingredients, melt spinning, air cooling, drafting and crimping.
The preparation of the bioactive components comprises extraction, drying, grinding, microencapsulation, grinding modification and porosification.
The extraction comprises the steps of uniformly mixing the dried orange peel, the orange peel and the shaddock peel, drying at 70 ℃ until the water content is lower than 7%, then placing the mixture into a crusher to be crushed into coarse powder with the particle size of 2mm, adding absolute ethyl alcohol, and carrying out continuous countercurrent ultrasonic extraction at 60 ℃ for 105min to obtain an ethanol ultrasonic extracting solution, wherein the ultrasonic frequency is 60 KHz; carrying out high-temperature high-pressure concentration on the ethanol ultrasonic extracting solution to obtain a concentrated solution, wherein the temperature in the high-temperature high-pressure process is 92 ℃, and the pressure is 0.3 MPa; and then adding activated carbon into the concentrated solution for decolorization and then filtering to obtain purified concentrated solution.
And drying, namely performing spray drying on the purified concentrated solution to obtain concentrated particles.
And grinding, namely grinding the concentrated particles to obtain concentrated powder with the particle size of 6 microns.
Microencapsulation, namely uniformly mixing concentrated powder, lecithin and deionized water, and then stirring at 65 ℃, wherein the stirring speed is 370rpm, and the stirring time is 25 min; adding zinc stearate, trehalose and xanthan gum after stirring, heating to 47 ℃, putting into a high shearing machine, shearing and emulsifying at 6800rpm for 17min, and then performing spray drying to obtain microencapsulated particles.
Wherein the mass ratio of the concentrated powder to the lecithin to the deionized water is 3: 4: 70.
wherein the mass ratio of the concentrated powder, the zinc stearate, the trehalose and the xanthan gum is 10: 3: 6: 7.
and grinding modification, namely adding the microencapsulated particles into a ball mill for grinding to obtain the ground microencapsulated particles with the average particle size of 45 nm.
And (2) carrying out porosification, namely mixing the microencapsulated particles with silicon dioxide, adding the mixture into absolute ethyl alcohol, then adding sodium methylene dinaphthalene sulfonate, and stirring for 3.5 hours at 320rpm, so that the microencapsulated particles are fully dispersed into the pore diameter of the silicon dioxide to form a bioactive material with the average particle size of 550nm, wherein the bioactive material is a silicon dioxide porous material with the microencapsulated particles loaded in the pores.
The silica had a specific surface area of 95m2/g and an average pore diameter of 90 nm.
Wherein the microencapsulated particles: silicon dioxide: the mass ratio of the methylene dinaphthalene sodium sulfonate is 4: 1: 2.
the melt spinning comprises the steps of uniformly mixing a bioactive material and a PE slice in a mass ratio of 1:10 to obtain a skin layer material, uniformly mixing the bioactive material and the PET slice in a mass ratio of 1:32 to obtain a core layer material, respectively placing the skin layer material and the core layer material into corresponding screw extruder hoppers to extrude a skin layer melt and a core layer melt, compounding the skin layer melt and the core layer melt in a composite spinning assembly, and then ejecting a skin-core layer structure fiber through a spinneret plate.
The mass ratio of the skin layer material to the core layer material in the melt spinning process is 1: 2.2.
the melt temperature of the skin layer material in the melt extrusion process is 110 ℃; the melt temperature of the melting screw B was 190 ℃.
And air cooling, namely cooling and solidifying the fiber trickle subjected to melt spinning by circular air blowing, and feeding cold air in a deformation area of 100mm below a spinning assembly plate, wherein the air speed is 0.9 m/s, the air temperature of side air blowing is 20 ℃, the air humidity is 52% and the air speed is 2 m/s.
The drafting is carried out by adopting a drafting machine, the drafting multiple is 8 times, and the drafting speed is 22 m/min;
and (3) curling in a curling machine, wherein the curling pressure is 0.12MPa, the curling degree is 5%, and the fiber after the curling is finished is cut into broken filaments.
Example 3
A method for preparing ES macrobiological fiber containing active ingredients of pericarpium Citri Tangerinae, fructus Citri Junoris and fructus Citri Grandis comprises preparing bioactive ingredients, preparing master batch containing bioactive ingredients, melt spinning, air cooling, drafting and crimping.
The preparation of the bioactive components comprises extraction, drying, grinding, microencapsulation, grinding modification and porosification.
The extraction comprises the steps of uniformly mixing the dried orange peel, the orange peel and the shaddock peel, drying at 75 ℃ until the water content is lower than 7%, then placing the mixture into a crusher to be crushed into coarse powder with the particle size of 3mm, adding absolute ethyl alcohol, and carrying out continuous countercurrent ultrasonic extraction at 65 ℃ for 110min to obtain an ethanol ultrasonic extracting solution, wherein the ultrasonic frequency is 65 KHz; carrying out high-temperature high-pressure concentration on the ethanol ultrasonic extracting solution to obtain a concentrated solution, wherein the temperature in the high-temperature high-pressure process is 95 ℃, and the pressure is 0.4 MPa; and then adding activated carbon into the concentrated solution for decolorization and then filtering to obtain purified concentrated solution.
And drying, namely performing spray drying on the purified concentrated solution to obtain concentrated particles.
And grinding, namely grinding the concentrated particles to obtain concentrated powder with the particle size of 7 microns.
Microencapsulation, namely uniformly mixing concentrated powder, lecithin and deionized water, and then stirring at 75 ℃, wherein the stirring speed is 420rpm, and the stirring time is 30 min; adding zinc stearate, trehalose and xanthan gum after stirring, heating to 50 ℃, putting into a high shearing machine, shearing and emulsifying at 7200rpm for 18min, and then performing spray drying to obtain microencapsulated particles.
Wherein the mass ratio of the concentrated powder to the lecithin to the deionized water is 3: 5: 75.
wherein the mass ratio of the concentrated powder, the zinc stearate, the trehalose and the xanthan gum is 10: 4: 7: 8.
and grinding modification, namely adding the microencapsulated particles into a ball mill for grinding to obtain the ground microencapsulated particles with the average particle size of 50 nm.
And (2) carrying out porosification, namely mixing the microencapsulated particles with silicon dioxide, adding the mixture into absolute ethyl alcohol, then adding sodium methylene dinaphthalene sulfonate, and stirring for 4 hours at 350rpm, so that the microencapsulated particles are fully dispersed into the pore diameter of the silicon dioxide to form a bioactive material with the average particle size of 600nm, wherein the bioactive material is a silicon dioxide porous material with the microencapsulated particles loaded in the pores.
The silica had a specific surface area of 100m2/g and an average pore diameter of 100 nm.
Wherein the microencapsulated particles: silicon dioxide: the mass ratio of the methylene dinaphthalene sodium sulfonate is 5: 1: 3.
the melt spinning comprises the steps of uniformly mixing a bioactive material and a PE slice in a mass ratio of 1:12 to obtain a skin layer material, uniformly mixing the bioactive material and the PET slice in a mass ratio of 1:35 to obtain a core layer material, respectively placing the skin layer material and the core layer material into corresponding screw extruder hoppers to extrude a skin layer melt and a core layer melt, compounding the skin layer melt and the core layer melt in a composite spinning assembly, and then ejecting a skin-core layer structure fiber through a spinneret plate.
The mass ratio of the skin layer material to the core layer material in the melt spinning process is 1: 2.5.
the melt temperature of the skin layer material in the melt extrusion process is 115 ℃; the melt temperature of the melting screw B was 195 ℃.
And air cooling, namely cooling and solidifying the fiber trickle subjected to melt spinning by circular air blowing, and feeding cold air within 200mm of a deformation area below a spinning assembly plate, wherein the air speed is 1 m/s, the air temperature of side air blowing is 21 ℃, the air humidity is 55% and the air speed is 2.2 m/s.
The drafting is carried out by adopting a drafting machine, the drafting multiple is 9 times, and the drafting speed is 24 m/min;
and the curling is carried out in a curling machine, the curling pressure is 0.15MPa, the curling degree is 5.2 percent, and the fiber after the curling is finished is cut into broken filaments.
Example 4
Tests were carried out using ES macrobio fibers containing the active ingredients of orange peel, orange and grapefruit as described in examples 1-3, while setting up comparative tests 1-2 for comparison.
Comparative example 1: the preparation method of the ES macrobio fiber containing the active ingredients of the tangerine peel, the orange and the pomelo as described in the example 1 is adopted, and the difference is that: the microencapsulation step is omitted in the preparation of the bioactive component, and the concentrated powder is directly mixed with silicon dioxide after the grinding is finished to carry out grinding modification.
Comparative example 2: the preparation method of the ES macrobio fiber containing the active ingredients of the tangerine peel, the orange and the pomelo as described in the example 1 is adopted, and the difference is that: in melt spinning, no bioactive material is added to the core material.
The performance of the ES macrobio fiber containing active ingredients of tangerine peel, orange and pomelo prepared in examples 1-3 and comparative examples 1-2 is as follows:
all percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the 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 ES large biological fiber containing active ingredients of tangerine peel, orange and pomelo is characterized by comprising the steps of preparation of the active ingredients, preparation of master batches containing the active ingredients, melt spinning, air cooling, drafting and curling.
2. The method of claim 1, wherein the preparation of the bioactive component comprises extraction, drying, grinding, microencapsulation, grinding modification, and porosification.
3. The preparation method of ES macrobio-fiber containing active ingredients of tangerine peel, orange and pomelo according to claim 2, wherein the extraction comprises mixing tangerine peel, orange peel and pomelo peel uniformly, drying at 60-75 ℃ until the water content is lower than 7%, then placing in a pulverizer to pulverize into coarse powder with particle size of 1-3mm, adding absolute ethanol, and performing continuous countercurrent ultrasonic extraction at 55-65 ℃ for 110min to obtain ethanol ultrasonic extract with ultrasonic frequency of 55-65 KHz; concentrating the ethanol ultrasonic extraction solution at high temperature and high pressure to obtain a concentrated solution, wherein the temperature in the high-temperature and high-pressure process is 90-95 ℃, and the pressure is 0.25-0.4 MPa; and then adding activated carbon into the concentrated solution for decolorization and then filtering to obtain purified concentrated solution.
4. The method for preparing ES macrobio fiber containing active ingredients of tangerine peel, orange and pomelo according to claim 2, wherein the drying is performed, and the purified concentrated solution is spray-dried to obtain concentrated particles.
5. The method for preparing ES macrobio fiber containing tangerine peel, orange and pomelo active ingredients according to claim 2, wherein the grinding is performed to grind the concentrated granules to obtain concentrated powder with 4-7 μm size.
6. The preparation method of ES macrobio fiber containing tangerine peel, orange and pomelo active ingredients as claimed in claim 2, wherein the microencapsulation is performed by uniformly mixing concentrated powder, lecithin and deionized water, and then stirring at 60-75 ℃, wherein the stirring speed is 350-420rpm, and the stirring time is 20-30 min; adding zinc stearate, trehalose and xanthan gum after stirring, heating to 45-50 ℃, putting into a high shearing machine, shearing and emulsifying at 6000-.
7. The method for preparing ES macrobio fiber containing tangerine peel, orange and pomelo active ingredients according to claim 2, wherein the grinding modification is carried out by adding the microencapsulated particles into a ball mill for grinding to obtain the ground microencapsulated particles with an average particle size of 40-50 nm.
8. The method for preparing ES macrobio-fiber containing active ingredients of tangerine peel, orange and pomelo according to claim 2, wherein the step of porous treatment is that the microencapsulated particles and silicon dioxide are mixed and then added into absolute ethyl alcohol, then sodium methylenedinaphthalene sulfonate is added, and then the mixture is stirred for 3-4h at the speed of 300-350rpm, so that the microencapsulated particles are fully dispersed into the pore diameter of the silicon dioxide, and a bioactive material with the average particle size of 500-600nm is formed, wherein the bioactive material is a silicon dioxide porous material with the microencapsulated particles loaded in the pores;
the specific surface area of the silicon dioxide is 90-100m2/g, and the average pore diameter is 80-100 nm;
wherein the microencapsulated particles: silicon dioxide: the mass ratio of the methylene dinaphthalene sodium sulfonate is 4-5: 1: 2-3.
9. The method for preparing the ES macrobio-fiber containing the active ingredients of tangerine peel, orange and pomelo according to claim 1, wherein the melt spinning comprises the steps of uniformly mixing the bioactive material and the PE slices in a mass ratio of 1:9-12 to obtain a skin layer material, uniformly mixing the bioactive material and the PET slices in a mass ratio of 1:30-35 to obtain a core layer material, respectively placing the skin layer material and the core layer material into corresponding hoppers of a screw extruder, extruding the skin layer melt and the core layer melt, compounding the skin layer melt and the core layer melt in a composite spinning assembly, and then spraying the skin-core layer structural fiber through a spinneret plate.
10. The method for preparing ES macrobio fiber containing active ingredients of tangerine peel, orange and pomelo according to claim 1, wherein the air cooling is to cool and solidify the fiber stream after melt spinning by circular blowing, and to send cold air with the wind speed of 0.8-1 m/s, the side blowing temperature of 18-21 ℃, the wind humidity of 50-55% and the wind speed of 1.8-2.2m/s in the deformation zone of 0-200mm under the plate of the spinning assembly.
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| CN114395817A (en) * | 2022-01-24 | 2022-04-26 | 百事基材料（青岛）股份有限公司 | A Dabiol PA56 fiber containing active ingredients of fructus Citri Junoris, herba Menthae and fructus Tiliae Miquelianae |
| CN114687004A (en) * | 2022-03-02 | 2022-07-01 | 百事基材料（青岛）股份有限公司 | A macrobiotic ES fiber containing active components of tea and orange |
| CN116065259A (en) * | 2023-02-08 | 2023-05-05 | 百事基材料（青岛）股份有限公司 | Milk ES large biological fiber and preparation method thereof |
| CN116103784A (en) * | 2023-02-23 | 2023-05-12 | 福地(石狮)新材料科技有限公司 | Degradable ES fiber and production method thereof |
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