CN114892301B - Preparation method of antibacterial and anti-inflammatory mint polyester fiber - Google Patents
Preparation method of antibacterial and anti-inflammatory mint polyester fiber Download PDFInfo
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- CN114892301B CN114892301B CN202210526505.6A CN202210526505A CN114892301B CN 114892301 B CN114892301 B CN 114892301B CN 202210526505 A CN202210526505 A CN 202210526505A CN 114892301 B CN114892301 B CN 114892301B
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 87
- 239000000835 fiber Substances 0.000 title claims abstract description 56
- 235000006679 Mentha X verticillata Nutrition 0.000 title claims abstract description 51
- 235000002899 Mentha suaveolens Nutrition 0.000 title claims abstract description 51
- 235000001636 Mentha x rotundifolia Nutrition 0.000 title claims abstract description 51
- 229920000728 polyester Polymers 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 230000003110 anti-inflammatory effect Effects 0.000 title claims abstract description 39
- 238000002156 mixing Methods 0.000 claims abstract description 68
- 238000009987 spinning Methods 0.000 claims abstract description 43
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000011812 mixed powder Substances 0.000 claims abstract description 13
- 239000000284 extract Substances 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 238000002844 melting Methods 0.000 claims abstract description 5
- 230000008018 melting Effects 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims description 76
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims description 51
- 229910001701 hydrotalcite Inorganic materials 0.000 claims description 51
- 229960001545 hydrotalcite Drugs 0.000 claims description 51
- 238000001354 calcination Methods 0.000 claims description 48
- 229940105902 mint extract Drugs 0.000 claims description 39
- 239000003607 modifier Substances 0.000 claims description 35
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 230000004913 activation Effects 0.000 claims description 24
- 238000002788 crimping Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 15
- 229920002635 polyurethane Polymers 0.000 claims description 13
- 239000004814 polyurethane Substances 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 229910000278 bentonite Inorganic materials 0.000 claims description 9
- 239000000440 bentonite Substances 0.000 claims description 9
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 7
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 7
- 239000004571 lime Substances 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 6
- 239000008267 milk Substances 0.000 claims description 6
- 210000004080 milk Anatomy 0.000 claims description 6
- 235000013336 milk Nutrition 0.000 claims description 6
- 235000020737 peppermint extract Nutrition 0.000 claims description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000002137 ultrasound extraction Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 abstract description 13
- 230000004048 modification Effects 0.000 abstract description 6
- 238000012986 modification Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 6
- 239000005020 polyethylene terephthalate Substances 0.000 description 26
- 230000006870 function Effects 0.000 description 16
- 238000005406 washing Methods 0.000 description 11
- 239000004744 fabric Substances 0.000 description 7
- 239000004753 textile Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 241000191967 Staphylococcus aureus Species 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- 241000222122 Candida albicans Species 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 3
- 229940095731 candida albicans Drugs 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 206010061218 Inflammation Diseases 0.000 description 2
- 241000700605 Viruses Species 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 230000003467 diminishing effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000004054 inflammatory process Effects 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000255925 Diptera Species 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 235000016257 Mentha pulegium Nutrition 0.000 description 1
- 244000246386 Mentha pulegium Species 0.000 description 1
- 235000004357 Mentha x piperita Nutrition 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000001050 hortel pimenta Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001846 repelling effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention discloses preparation of PET antibacterial function master batch, which comprises the following steps: blending 20-40 parts of mixed powder containing mint extracts, 60-80 parts of PET slices and 1-5 parts of mutual agent, melting and extruding by a double screw extruder, and granulating to obtain PET antibacterial function master batch; the preparation method of the antibacterial and anti-inflammatory mint polyester fiber comprises the following steps: mixing 2% -4% of PET antibacterial function master batch into PET slices, and spinning according to the polyester slice spinning production process and flow to obtain the antibacterial and anti-inflammatory mint polyester fiber. According to the preparation method of the antibacterial and anti-inflammatory mint fiber, disclosed by the invention, the effective components of mint are stable, the loss is less in the preparation and use processes of the fiber, the modification effect on the polyester fiber is good, and the stability of the modification effect is better.
Description
Technical Field
The invention relates to the technical field of antibacterial polyester fibers, in particular to a preparation method of antibacterial and anti-inflammatory mint polyester fibers.
Background
With the enhancement of environmental protection concepts and health consciousness of people in recent years, the requirements on textiles are not cold protection and shielding, the pursuit of colors is not satisfied, and the functions, health and environmental protection of textile fibers are more important. The large number of microorganisms and germs in daily life brings a lot of trouble to the life of people and causes great threat to the health of human bodies, so that the textile closely contacted with the skin of the human bodies is required to be more and more, the textile with the antibacterial function is required, and the textile with the antibacterial function has wide market prospect.
The polyester fiber is used as the synthetic fiber with the largest worldwide output, has compact macromolecular structure arrangement, has good performance characteristics, high strength and good elasticity, and can improve the application range of polyester when being prepared with the antibacterial performance. At present, antibacterial researches on polyester fibers mainly comprise antibacterial fabrics formed by adding an antibacterial finishing agent through post-finishing processing, wherein the processing method comprises surface coating, resin finishing and a microcapsule method, but the defects of poor antibacterial effect and poor durability of the fabrics are found. The antibacterial fiber can be prepared by adding an antibacterial agent into the spinning solution in the spinning process, so that the defect of the antibacterial fabric prepared by the after-finishing method can be greatly overcome, and the durable antibacterial effect is achieved. Inorganic antibacterial agents commonly used for preparing antibacterial master batches are Ag-based, cu-based and Zn-based. The addition amount is too large in the use process, which is easy to cause the color change of the fabric.
Natural products extracted from peppermint have certain inhibiting effect on bacillus and various viruses by extracting effective components. The safety is high, no toxic or side effect is generated on the human body, the degradation is easy, no long-term residue in the natural world is generated, and the problems of potential toxic effect, drug resistance, enrichment through food chains and the like of the synthetic functional agent on the human body are avoided. Meets the development requirement of ecological textiles.
The mint is adopted to extract the effective components and is loaded on a specific carrier, and the effective components are prepared into specific functional master batches, but the loading effect is not ideal, the combination is not firm, and the loss of the effective components of the mint simultaneously causes the functional reduction.
Based on the method, the invention provides a preparation method of antibacterial and anti-inflammatory mint polyester fiber.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of antibacterial and anti-inflammatory mint polyester fiber, which aims to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a preparation method of antibacterial and anti-inflammatory mint polyester fiber, which comprises the following steps:
step one, preparation of a mint extract:
s1, extracting, filtering and purifying a mint extract;
the coarse powder adopts ethanol solution with volume concentration of 60-90%, ultrasonic extraction time is 30-60min, wherein the mass ratio of the coarse powder of the peppermint extract to the ethanol is 1:4-10, and then filtering and purifying;
s2, preparing a mint extract-containing functional modifier:
carrying out ultrasonic treatment on the load modifier for 20-40min under the power condition of 1000-1200w, and then mixing in a high-pressure homogenizer for 20-30min;
s3, mixing:
mixing the mint extract functional modifier and the mint extract according to the weight ratio of 1:3 to obtain mixed powder containing the mint extract;
step two, preparing PET antibacterial function master batch:
blending 20-40 parts of mixed powder containing mint extracts, 60-80 parts of PET slices and 1-5 parts of mutual agent, melting and extruding by a double screw extruder, and granulating to obtain PET antibacterial function master batch;
the mixing temperature is 250-280 ℃, the mixing time is 30-50min, the screw rotating speed is 100-160rpm, and the extrusion pressure is 100-170kgf/cm < 3 >;
step three, preparing antibacterial and anti-inflammatory mint polyester fibers:
mixing 2% -4% of PET antibacterial function master batch into PET slices, and spinning according to the polyester slice spinning production process and flow to obtain the antibacterial and anti-inflammatory mint polyester fiber.
Preferably, the preparation method of the load modifier comprises the following steps:
s1: delivering hydrotalcite into a grinder for grinding at a grinding speed of 1000-1500r/min for 10-20min, and grinding with 500-1000 meshes to obtain first-grade hydrotalcite;
s2: preparation of grinding aid: stirring 30-40 parts of polyurethane emulsion prepared by mixing 10-20 parts of polyethylene glycol, polyurethane and acetone in a ratio of 1:3 at a rotating speed of 100-500r/min for 30-40min, and obtaining a grinding aid after stirring;
s3: mixing the first-stage hydrotalcite with a grinding aid in a ratio of 10:1, and carrying out secondary grinding, wherein the grinding speed is 600-900r/min, and the grinding time is 15-25min, so as to obtain secondary hydrotalcite;
s4: mixing the second-stage hydrotalcite with lime milk, and further carrying out tertiary grinding, wherein the tertiary grinding speed is 500-700r/min, and the grinding time is 10-20min, so as to obtain coated hydrotalcite;
s5: and (3) sending the coated hydrotalcite into a calciner for calcination treatment, wherein the calcination temperature is 400-500 ℃, the calcination time is 15-25min, and naturally cooling to room temperature after the calcination is finished, so as to obtain the load modifier.
Preferably, the calcination treatment is carried out by adopting pressure of 10-20 Mpa.
Preferably, the pressure of the holding pressure is 15MPa.
Preferably, the preparation method of the intergranular agent comprises the following steps:
step one: feeding bentonite into a calciner for calcination, wherein the calcination temperature is 350-450 ℃, the calcination time is 20-30min, then reducing the temperature to 220-300 ℃ at the speed of 1-3 ℃/min, and continuing to keep the temperature for 25-35min;
step two: then placing the mixture into an active solution for activation treatment, wherein the activation rotating speed is 500-1000r/min, the activation time is 10-30min, and the mutual agent is obtained after the activation is finished, water washing and drying.
Preferably, the active liquid is prepared by mixing sodium dodecyl sulfate and deionized water according to a weight ratio of 1:5, then adding hydrochloric acid, adjusting the pH to 4.5-5.5, then adding lanthanum chloride accounting for 10-30% of the total amount of the sodium dodecyl sulfate, and stirring until the mixture is fully stirred to obtain the active liquid.
Preferably, the mass fraction of the lanthanum chloride is 10-20%.
Preferably, the mass fraction of lanthanum chloride is 15%.
Preferably, the supply amount of the spinning metering pump is 600-900g/min, the spinning temperature is 280-300 ℃, the spinning speed is 500-1000m/min, the draft multiple is 2-5 times, the crimping pressure is 0.2-0.4Mpa, and the crimping degree is 2.5-5%.
Preferably, the supply amount of the spinning metering pump is 750g/min, the spinning temperature is 290 ℃, the spinning speed is 750m/min, the draft multiple is 3.5 times, the crimping pressure is 0.3Mpa, and the crimping degree is 3.5%.
Compared with the prior art, the invention has the following beneficial effects:
1. the mint extract used in the invention is a natural plant function modifier, and has the characteristics of safety, no toxicity, no side effect, environment friendliness and no pollution to the environment, and is friendly to human and livestock.
2. The antibacterial anti-inflammatory mint fiber prepared by the invention has excellent antibacterial effect, and has 99% of antibacterial rate to staphylococcus aureus, 99% of antibacterial rate to escherichia coli and more than 95% of antibacterial rate to candida albicans.
3. According to the preparation method of the antibacterial and anti-inflammatory mint fiber, disclosed by the invention, the effective components of mint are stable, the loss is less in the preparation and use processes of the fiber, the modification effect on the polyester fiber is good, and the stability of the modification effect is better.
4. The antibacterial anti-inflammatory mint fiber and the fabric thereof prepared by the invention have excellent antibacterial property after 50 times of washing, and can not lose effect due to washing, and the antibacterial durability and the washing fastness are good.
5. The antibacterial anti-inflammatory mint fiber prepared by the invention also has the effects of inhibiting viruses, diminishing inflammation, repelling mosquitoes and the like, and the fabric prepared by the fiber has good comfort and good cool feeling.
6. The preparation method of the antibacterial and anti-inflammatory mint polyester fiber provided by the invention has the advantages of simple process and reasonable process, and meets the requirement of large-scale production of functional polyester fibers.
The loading modifier adopts lamellar hydrotalcite as a matrix, the hydrotalcite is firstly subjected to grinding treatment, so as to realize a modified body, in grinding, polyurethane of a grinding aid is adopted to modify the hydrotalcite so as to enable the hydrotalcite to have a chain structure, so that the loading capacity of a mint extract is improved, and the added lime cream is subjected to grinding cladding treatment, so that the generated calcium carbonate modifies the hydrotalcite matrix in a certain shape, and spherical, cubic and other shapes are provided; thus, a large working space is provided for loading the mint extract, the intergranular agent is calcined by bentonite and activated by activating solution, the lamellar function of the bentonite is enhanced, and the bentonite is matched with the loaded modifier and is blended into the terylene fiber body, so that the functionality of the product is improved, and the effects of resisting bacteria, diminishing inflammation and the like of the product are further improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The preparation method of the antibacterial and anti-inflammatory mint polyester fiber comprises the following steps:
step one, preparation of a mint extract:
s1, extracting, filtering and purifying a mint extract;
the coarse powder adopts ethanol solution with volume concentration of 60-90%, ultrasonic extraction time is 30-60min, wherein the mass ratio of the coarse powder of the peppermint extract to the ethanol is 1:4-10, and then filtering and purifying;
s2, preparing a mint extract-containing functional modifier:
carrying out ultrasonic treatment on the load modifier for 20-40min under the power condition of 1000-1200w, and then mixing in a high-pressure homogenizer for 20-30min;
s3, mixing:
mixing the mint extract functional modifier and the mint extract according to the weight ratio of 1:3 to obtain mixed powder containing the mint extract;
step two, preparing PET antibacterial function master batch:
blending 20-40 parts of mixed powder containing mint extracts, 60-80 parts of PET slices and 1-5 parts of mutual agent, melting and extruding by a double screw extruder, and granulating to obtain PET antibacterial function master batch;
the mixing temperature is 250-280 ℃, the mixing time is 30-50min, the screw rotating speed is 100-160rpm, and the extrusion pressure is 100-170kgf/cm < 3 >;
step three, preparing antibacterial and anti-inflammatory mint polyester fibers:
mixing 2% -4% of PET antibacterial function master batch into PET slices, and spinning according to the polyester slice spinning production process and flow to obtain the antibacterial and anti-inflammatory mint polyester fiber.
The preparation method of the load modifier in the embodiment comprises the following steps:
s1: delivering hydrotalcite into a grinder for grinding at a grinding speed of 1000-1500r/min for 10-20min, and grinding with 500-1000 meshes to obtain first-grade hydrotalcite;
s2: preparation of grinding aid: stirring 30-40 parts of polyurethane emulsion prepared by mixing 10-20 parts of polyethylene glycol, polyurethane and acetone in a ratio of 1:3 at a rotating speed of 100-500r/min for 30-40min, and obtaining a grinding aid after stirring;
s3: mixing the first-stage hydrotalcite with a grinding aid in a ratio of 10:1, and carrying out secondary grinding, wherein the grinding speed is 600-900r/min, and the grinding time is 15-25min, so as to obtain secondary hydrotalcite;
s4: mixing the second-stage hydrotalcite with lime milk, and further carrying out tertiary grinding, wherein the tertiary grinding speed is 500-700r/min, and the grinding time is 10-20min, so as to obtain coated hydrotalcite;
s5: and (3) sending the coated hydrotalcite into a calciner for calcination treatment, wherein the calcination temperature is 400-500 ℃, the calcination time is 15-25min, and naturally cooling to room temperature after the calcination is finished, so as to obtain the load modifier.
The calcination treatment in this example was carried out using a pressure of 10 to 20 MPa.
The pressure of the holding pressure in this example was 15MPa.
The preparation method of the intergranular agent of the embodiment comprises the following steps:
step one: feeding bentonite into a calciner for calcination, wherein the calcination temperature is 350-450 ℃, the calcination time is 20-30min, then reducing the temperature to 220-300 ℃ at the speed of 1-3 ℃/min, and continuing to keep the temperature for 25-35min;
step two: then placing the mixture into an active solution for activation treatment, wherein the activation rotating speed is 500-1000r/min, the activation time is 10-30min, and the mutual agent is obtained after the activation is finished, water washing and drying.
The active liquid of the embodiment is prepared by mixing sodium dodecyl sulfate and deionized water according to a weight ratio of 1:5, then adding hydrochloric acid, adjusting the pH value to 4.5-5.5, then adding lanthanum chloride accounting for 10-30% of the total amount of the sodium dodecyl sulfate, and stirring until the mixture is fully stirred to obtain the active liquid.
The mass fraction of lanthanum chloride in the embodiment is 10-20%.
The mass fraction of lanthanum chloride in this example was 15%.
The spinning metering pump of the embodiment has the supply amount of 600-900g/min, the spinning temperature of 280-300 ℃, the spinning speed of 500-1000m/min, the drafting multiple of 2-5 times, the crimping pressure of 0.2-0.4Mpa and the crimping degree of 2.5-5%.
The spinning metering pump of this example had a supply of 750g/min, a spinning temperature of 290℃and a spinning speed of 750m/min, a draft multiple of 3.5 times, a crimping pressure of 0.3MPa and a crimping degree of 3.5%.
Example 1.
The preparation method of the antibacterial and anti-inflammatory mint polyester fiber comprises the following steps:
step one, preparation of a mint extract:
s1, extracting, filtering and purifying a mint extract;
the coarse powder adopts ethanol solution with volume concentration of 60%, the ultrasonic extraction time is 3min, wherein the mass ratio of the coarse powder of the peppermint extract to the ethanol is 1:4, filtering and purifying;
s2, preparing a mint extract-containing functional modifier:
carrying out ultrasonic treatment on the load modifier for 20min under the power condition of 1000w, and then mixing in a high-pressure homogenizer for 20min;
s3, mixing:
mixing the mint extract functional modifier and the mint extract according to the weight ratio of 1:3 to obtain mixed powder containing the mint extract;
step two, preparing PET antibacterial function master batch:
blending 20 parts of mixed powder containing mint extracts, 60 parts of PET slices and 1 part of mutual agent, carrying out melt extrusion by a double-screw extruder, and granulating to obtain PET antibacterial function master batch;
the mixing temperature is 250 ℃, the mixing time is 30min, the screw rotating speed is 100rpm, and the extrusion pressure is 100kgf/cm < 3 >;
step three, preparing antibacterial and anti-inflammatory mint polyester fibers:
mixing 2% of PET antibacterial master batch into PET slices, and spinning according to the polyester slice spinning production process and flow to obtain the antibacterial and anti-inflammatory mint polyester fiber.
The preparation method of the load modifier in the embodiment comprises the following steps:
s1: feeding hydrotalcite into a grinder for grinding, wherein the grinding speed is 1000r/min, the grinding time is 10min, and the hydrotalcite is ground by 500 meshes to obtain first-grade hydrotalcite;
s2: preparation of grinding aid: stirring 30 parts of polyurethane emulsion prepared by mixing 10 parts of polyethylene glycol, polyurethane and acetone in a ratio of 1:3 at a rotating speed of 100-500r/min for 30min, and obtaining a grinding aid after the stirring is finished;
s3: mixing the first-stage hydrotalcite with a grinding aid in a ratio of 10:1, and carrying out secondary grinding, wherein the grinding speed is 600r/min, and the grinding time is 15min, so as to obtain secondary hydrotalcite;
s4: mixing the second-stage hydrotalcite with lime milk, and further carrying out tertiary grinding, wherein the tertiary grinding speed is 500r/min, and the grinding time is 10min, so as to obtain coated hydrotalcite;
s5: and (3) sending the coated hydrotalcite into a calciner for calcination treatment, wherein the calcination temperature is 400 ℃, the calcination time is 15min, and the coated hydrotalcite is naturally cooled to room temperature after the calcination is finished, so as to obtain the load modifier.
In the calcination treatment of this example, a pressure of 10Mpa was used for the pressure maintaining treatment.
The preparation method of the intergranular agent of the embodiment comprises the following steps:
step one: feeding bentonite into a calciner for calcination, wherein the calcination temperature is 350 ℃, the calcination time is 20min, then reducing the temperature to 220 ℃ at the speed of 1 ℃/min, and continuing to keep the temperature for 25-35min;
step two: then placing the mixture into an active solution for activation treatment, wherein the activation rotating speed is 5000r/min, the activation time is 10min, and after the activation is finished, washing and drying the mixture to obtain the intergranular agent.
The active liquid of the embodiment is prepared by mixing sodium dodecyl sulfate and deionized water according to a weight ratio of 1:5, then adding hydrochloric acid, adjusting the pH value to 4.5, then adding lanthanum chloride accounting for 10% of the total amount of the sodium dodecyl sulfate, and stirring to be full, thus obtaining the active liquid.
The mass fraction of lanthanum chloride in this example was 10%.
The spinning metering pump of this example had a supply of 600g/min, a spinning temperature of 280℃and a spinning speed of 500m/min, a draft multiple of 2 times, a crimping pressure of 0.2MPa and a crimping degree of 2.5%.
Example 2.
The preparation method of the antibacterial and anti-inflammatory mint polyester fiber comprises the following steps:
step one, preparation of a mint extract:
s1, extracting, filtering and purifying a mint extract;
the coarse powder adopts ethanol solution with volume concentration of 90%, the ultrasonic extraction time is 60min, wherein the mass ratio of the coarse powder of the peppermint extract to the ethanol is 1:10, filtering and purifying;
s2, preparing a mint extract-containing functional modifier:
carrying out ultrasonic treatment on the load modifier for 40min under the power condition of 1200w, and then mixing for 30min in a high-pressure homogenizer;
s3, mixing:
mixing the mint extract functional modifier and the mint extract according to the weight ratio of 1:3 to obtain mixed powder containing the mint extract;
step two, preparing PET antibacterial function master batch:
blending 40 parts of mixed powder containing mint extracts, 80 parts of PET slices and 5 parts of mutual agent, carrying out melt extrusion by a double-screw extruder, and granulating to obtain PET antibacterial function master batch;
the mixing temperature is 280 ℃, the mixing time is 50min, the screw rotating speed is 160rpm, and the extrusion pressure is 170kgf/cm < 3 >;
step three, preparing antibacterial and anti-inflammatory mint polyester fibers:
mixing 4% of PET antibacterial master batch into PET slices, and spinning according to the polyester slice spinning production process and flow to obtain the antibacterial and anti-inflammatory mint polyester fiber.
The preparation method of the load modifier in the embodiment comprises the following steps:
s1: feeding hydrotalcite into a grinder for grinding, wherein the grinding speed is 1500r/min, the grinding time is 20min, and the hydrotalcite is ground by 1000 meshes to obtain first-grade hydrotalcite;
s2: preparation of grinding aid: stirring 40 parts of polyurethane emulsion prepared by mixing 20 parts of polyethylene glycol, polyurethane and acetone in a ratio of 1:3 at a rotating speed of 500r/min for 40min, and obtaining a grinding aid after the stirring is finished;
s3: mixing the first-stage hydrotalcite with a grinding aid in a ratio of 10:1, and carrying out secondary grinding, wherein the grinding speed is 900r/min, and the grinding time is 25min, so as to obtain secondary hydrotalcite;
s4: mixing the second-stage hydrotalcite with lime milk, and further carrying out tertiary grinding, wherein the tertiary grinding speed is 700r/min, and the grinding time is 20min, so as to obtain coated hydrotalcite;
s5: and (3) sending the coated hydrotalcite into a calciner for calcination treatment, wherein the calcination temperature is 500 ℃, the calcination time is 25min, and naturally cooling to room temperature after the calcination is finished, so as to obtain the load modifier.
The calcination treatment in this example was carried out using a pressure of 20 MPa.
The preparation method of the intergranular agent of the embodiment comprises the following steps:
step one: feeding bentonite into a calciner for calcination, wherein the calcination temperature is 450 ℃, the calcination time is 30min, then reducing the temperature to 300 ℃ at the speed of 3 ℃/min, and continuing to keep the temperature for 35min;
step two: then placing the mixture into an active solution for activation treatment, wherein the activation rotating speed is 1000r/min, the activation time is 30min, and after the activation is finished, washing and drying the mixture to obtain the intergranular agent.
The active liquid of the embodiment is prepared by mixing sodium dodecyl sulfate and deionized water according to a weight ratio of 1:5, then adding hydrochloric acid, adjusting the pH value to 5.5, then adding lanthanum chloride accounting for 30% of the total amount of the sodium dodecyl sulfate, and stirring to be full, thus obtaining the active liquid.
The mass fraction of lanthanum chloride in this example was 20%.
The spinning metering pump of this example had a supply of 900g/min, a spinning temperature of 300℃and a spinning speed of 1000m/min, a draft multiple of 5 times, a crimping pressure of 0.4MPa and a crimping degree of 5%.
Example 3:
the preparation method of the antibacterial and anti-inflammatory mint polyester fiber comprises the following steps:
step one, preparation of a mint extract:
s1, extracting, filtering and purifying a mint extract;
the coarse powder adopts ethanol solution with volume concentration of 75%, the ultrasonic extraction time is 45min, wherein the mass ratio of the coarse powder of the peppermint extract to the ethanol is 1:7, filtering and purifying;
s2, preparing a mint extract-containing functional modifier:
carrying out ultrasonic treatment on the load modifier for 30min under the power condition of 1100w, and then mixing for 25min in a high-pressure homogenizer;
s3, mixing:
mixing the mint extract functional modifier and the mint extract according to the weight ratio of 1:3 to obtain mixed powder containing the mint extract;
step two, preparing PET antibacterial function master batch:
blending 30 parts of mixed powder containing mint extracts, 70 parts of PET slices and 3 parts of mutual agent, melting and extruding by a double-screw extruder, and granulating to obtain PET antibacterial master batch;
the mixing temperature is 270 ℃, the mixing time is 30-50min, the screw rotating speed is 130rpm, and the extrusion pressure is 135kgf/cm < 3 >;
step three, preparing antibacterial and anti-inflammatory mint polyester fibers:
mixing 3% of PET antibacterial master batch into PET slices, and spinning according to the polyester slice spinning production process and flow to obtain the antibacterial and anti-inflammatory mint polyester fiber.
The spinning metering pump of this example had a supply of 750g/min, a spinning temperature of 290℃and a spinning speed of 750m/min, a draft multiple of 3.5 times, a crimping pressure of 0.3MPa and a crimping degree of 3.5%.
The preparation method of the load modifier in the embodiment comprises the following steps:
s1: feeding hydrotalcite into a grinder for grinding, wherein the grinding speed is 1250r/min, the grinding time is 15min, and the hydrotalcite is ground through 750 meshes to obtain first-grade hydrotalcite;
s2: preparation of grinding aid: stirring 35 parts of polyurethane emulsion prepared by mixing 15 parts of polyethylene glycol, polyurethane and acetone in a ratio of 1:3 at a rotating speed of 300r/min for 35min, and obtaining a grinding aid after the stirring is finished;
s3: mixing the first-stage hydrotalcite with a grinding aid in a ratio of 10:1, and carrying out secondary grinding, wherein the grinding speed is 700r/min, and the grinding time is 20min, so as to obtain secondary hydrotalcite;
s4: mixing the second-stage hydrotalcite with lime milk, and further carrying out tertiary grinding, wherein the tertiary grinding speed is 600r/min, and the grinding time is 15min, so as to obtain coated hydrotalcite;
s5: and (3) sending the coated hydrotalcite into a calciner for calcination treatment, wherein the calcination temperature is 450 ℃, the calcination time is 20min, and naturally cooling to room temperature after the calcination is finished, so as to obtain the load modifier.
In the calcination treatment of this example, a pressure of 15Mpa was used for the pressure maintaining treatment.
The preparation method of the intergranular agent of the embodiment comprises the following steps:
step one: feeding bentonite into a calciner for calcination, wherein the calcination temperature is 400 ℃, the calcination time is 25min, then reducing the temperature to 260 ℃ at the speed of 2 ℃/min, and continuing to keep the temperature for 30min;
step two: then placing the mixture into an active solution for activation treatment, wherein the activation rotating speed is 500-1000r/min, the activation time is 20min, and after the activation is finished, washing and drying the mixture to obtain the intergranular agent.
The active liquid of the embodiment is prepared by mixing sodium dodecyl sulfate and deionized water according to a weight ratio of 1:5, then adding hydrochloric acid, adjusting the pH value to 5.0, then adding lanthanum chloride accounting for 20% of the total amount of the sodium dodecyl sulfate, and stirring to be full, thus obtaining the active liquid.
The mass fraction of lanthanum chloride in this example was 15%.
Comparative example 1:
the preparation method of the polyester fiber provided in the embodiment is approximately the same as that of the embodiment 3, and the main difference is that the raw material does not contain a load modifier.
Comparative example 2:
the preparation method of the polyester fiber provided in the embodiment is approximately the same as that of the embodiment 3, and the main difference is that the polyester fiber does not contain a mutual agent.
Evaluation of antimicrobial Properties of textiles according to GB/T20944.3-2008 part 3: the test of the oscillation method is used for testing the bacteriostasis rate of staphylococcus aureus, escherichia coli and candida albicans;
the performance measurements for examples 1-3 and comparative examples 1-2 are as follows:
antibacterial property test
TABLE 1
The antibacterial and anti-inflammatory mint polyester fiber prepared by adopting the technical scheme of the embodiment 3 has excellent antibacterial effect, and has 99% of antibacterial rate on staphylococcus aureus, 99% of antibacterial rate on escherichia coli and more than 95% of antibacterial rate on candida albicans. The antibacterial anti-inflammatory mint fiber and the fabric thereof have excellent antibacterial property after 50 times of washing, and can not lose effect due to washing, and the antibacterial durability and the washing fastness are good. The added mint active ingredient is stable, the loss is less in the preparation and use processes of the fiber, the modification effect on the polyester fiber is good, and the modification effect is stable.
Antibacterial properties of the product (for example staphylococcus aureus) washed 50 times:
| staphylococcus aureus (%) | |
| Example 1 | 99.0 |
| Example 2 | 99.4 |
| Example 3 | 99.6 |
| Comparative example 1 | 89.2 |
| Comparative example 2 | 91.3 |
TABLE 2
As can be seen from examples 1-3 and comparative examples 1-2 in Table 2, the intergrating agent and the loading modifier in the product have a remarkable improvement effect on the stability of the antibacterial properties of the product.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (7)
1. The preparation method of the antibacterial and anti-inflammatory mint polyester fiber is characterized by comprising the following steps of:
step one, preparation of a mint extract:
s1, extracting, filtering and purifying a mint extract;
the coarse powder adopts ethanol solution with volume concentration of 60-90%, ultrasonic extraction time is 30-60min, wherein the mass ratio of the coarse powder of the peppermint extract to the ethanol is 1:4-10, and then filtering and purifying;
s2, preparing a mint extract-containing functional modifier:
carrying out ultrasonic treatment on the load modifier for 20-40min under the power condition of 1000-1200w, and then mixing in a high-pressure homogenizer for 20-30min;
s3, mixing:
mixing the mint extract functional modifier and the mint extract according to the weight ratio of 1:3 to obtain mixed powder containing the mint extract;
step two, preparing PET antibacterial function master batch:
blending 20-40 parts of mixed powder containing mint extracts, 60-80 parts of PET slices and 1-5 parts of mutual agent, melting and extruding by a double screw extruder, and granulating to obtain PET antibacterial function master batch;
the mixing temperature is 250-280 ℃, the mixing time is 30-50min, the screw rotating speed is 100-160rpm, and the extrusion pressure is 100-170kgf/cm < 3 >;
step three, preparing antibacterial and anti-inflammatory mint polyester fibers:
mixing 2% -4% of PET antibacterial function master batch into PET slices, and spinning according to the polyester slice spinning production process and flow to obtain antibacterial and anti-inflammatory mint polyester fibers;
the preparation method of the load modifier comprises the following steps:
s1: delivering hydrotalcite into a grinder for grinding at a grinding speed of 1000-1500r/min for 10-20min, and grinding with 500-1000 meshes to obtain first-grade hydrotalcite;
s2: preparation of grinding aid: stirring 30-40 parts of polyurethane emulsion prepared by mixing 10-20 parts of polyethylene glycol, polyurethane and acetone in a ratio of 1:3 at a rotating speed of 100-500r/min for 30-40min, and obtaining a grinding aid after stirring;
s3: mixing the first-stage hydrotalcite with a grinding aid in a ratio of 10:1, and carrying out secondary grinding, wherein the grinding speed is 600-900r/min, and the grinding time is 15-25min, so as to obtain secondary hydrotalcite;
s4: mixing the second-stage hydrotalcite with lime milk, and further carrying out tertiary grinding, wherein the tertiary grinding speed is 500-700r/min, and the grinding time is 10-20min, so as to obtain coated hydrotalcite;
s5: the coated hydrotalcite is sent into a calciner for calcination treatment, the calcination temperature is 400-500 ℃, the calcination time is 15-25min, and the loaded modifier is obtained after the natural cooling to room temperature after the calcination is finished;
the preparation method of the mutual agent comprises the following steps:
step one: feeding bentonite into a calciner for calcination, wherein the calcination temperature is 350-450 ℃, the calcination time is 20-30min, then reducing the temperature to 220-300 ℃ at the speed of 1-3 ℃/min, and continuing to keep the temperature for 25-35min;
step two: then placing the mixture into an active solution for activation treatment, wherein the activation rotating speed is 500-1000r/min, the activation time is 10-30min, and the mixture is washed and dried after the activation is finished to obtain the intergranular agent;
the active liquid is prepared by mixing sodium dodecyl sulfate and deionized water according to a weight ratio of 1:5, then adding hydrochloric acid, adjusting the pH value to 4.5-5.5, then adding lanthanum chloride accounting for 10-30% of the total amount of the sodium dodecyl sulfate, and stirring to be full, thus obtaining the active liquid.
2. The method for preparing antibacterial and anti-inflammatory mint polyester fiber according to claim 1, wherein the calcination treatment is carried out by adopting 10-20Mpa pressure.
3. The method for preparing antibacterial and anti-inflammatory mint polyester fiber according to claim 2, wherein the pressure maintaining pressure is 15MPa.
4. The method for preparing antibacterial and anti-inflammatory mint polyester fiber according to claim 1, wherein the mass fraction of lanthanum chloride is 10-20%.
5. The method for preparing antibacterial and anti-inflammatory mint polyester fiber according to claim 4, wherein the mass fraction of lanthanum chloride is 15%.
6. The method for preparing antibacterial and anti-inflammatory mint polyester fiber according to claim 1, wherein the supply amount of the spinning metering pump is 600-900g/min, the spinning temperature is 280-300 ℃, the spinning speed is 500-1000m/min, the draft multiple is 2-5 times, the crimping pressure is 0.2-0.4Mpa, and the crimping degree is 2.5-5%.
7. The method for preparing antibacterial and anti-inflammatory mint polyester fiber according to claim 6, wherein the supply amount of the spinning metering pump is 750g/min, the spinning temperature is 290 ℃, the spinning speed is 750m/min, the draft multiple is 3.5 times, the crimping pressure is 0.3Mpa, and the crimping degree is 3.5%.
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