CN104005110A - Regenerated cellulose fiber containing microencapsulated anti-mite medicine and preparation method thereof - Google Patents

Regenerated cellulose fiber containing microencapsulated anti-mite medicine and preparation method thereof Download PDF

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Publication number
CN104005110A
CN104005110A CN201410187341.4A CN201410187341A CN104005110A CN 104005110 A CN104005110 A CN 104005110A CN 201410187341 A CN201410187341 A CN 201410187341A CN 104005110 A CN104005110 A CN 104005110A
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mite
borneol
microencapsulation
essential oil
wormwood essential
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CN104005110B (en
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毛军
陈红霞
陆鹏
丁可敬
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JIANGSU GOLDSUN TEXTILE TECHNOLOGY CO., LTD.
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Jiangsu Gold Cloth Capable Of Reflecting Sun Infrared And Ultraviolet Rays Industry Co Ltd
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Abstract

The invention provides regenerated cellulose fiber containing a microencapsulated anti-mite medicine and a preparation method thereof. The regenerated cellulose fiber comprises a viscose-rayon spinning solution and the microencapsulated anti-mite medicine, the microencapsulated anti-mite medicine accounts for 0.05-2% by mass of methyl cellulose in the viscose-rayon spinning solution, methyl cellulose accounts for 99.95-98% by mass of dry regenerated cellulose fiber, and borneol and argy wormwood essential oil are taken as a capsule core. The preparation method comprises: firstly preparing a solution of borneol and argy wormwood essential oil, then preparing microcapsules from the solution of borneol and argy wormwood essential oil through a microencapsulation technology, adding the microcapsules into the viscose-rayon spinning solution, mixing uniformly, and finally utilizing a viscose-rayon wet spinning technology to prepare the regenerated cellulose fiber containing the microencapsulated anti-mite medicine. The regenerated cellulose fiber containing microencapsulated anti-mite medicine has the repelling rate on dermatophagoides farina of 95% or more, and has extremely strong anti-mite effect, and has the antibacterial rate on staphylococcus aureus, escherichia coli and other pathogens of 90% or more.

Description

Regenerated celulose fibre that contains microencapsulation mite-proof medicine and preparation method thereof
Technical field
The invention belongs to weaving production technical field, be specifically related to a kind of regenerated celulose fibre that contains microencapsulation mite-proof medicine and preparation method thereof.
Background technology
Acarid is a kind of small-sized arthropod, body length is generally 0.1~0.5mm, to the harm of human body be mainly reflected in parasitism, sting thorn, poison is stung, suck blood, anaphylactia, the aspect such as spread disease, can cause the various diseases such as asthma, rhinitis, dermatitis, ringworm of the body, the mankind healthy caused to serious harm.
Natural borneol is in the resin of Dipterocarpaceae magaphanerophytes kapur and volatile oil, to extract the crystallization obtaining, also claims in " borneol " or " Borneolum ", and be to be close to pure dextrorotation triterpenoid.The isomer synthetic through chemical method specifies for " synthetic borneol " its QUALITY STANDARD should meet Chinese Pharmacopoeia.Borneol, nature and flavor are arduous, are slightly cold, and have logical all keys, and loose stagnated fire, goes screen improving eyesight, effect of swelling and pain relieving.In treatment, keep silent in air port, pyreticosis coma, and aphtha, tympanitis, carbuncle is swollen, hemorrhoid, conjunctivitis.In the time of the solution state of 0.5% mass fraction, staphylococcus, streptococcus, Diplococcus pneumopniae, Escherichia coli and the pathogenic dermatophyte of part etc. are had to inhibitory action.GB2760-1996 specifies that borneol is the flavorant that allows use, be mainly used in preparing peppermint, rosemary, Xue MingRosma rinus officinalis, the type essence such as lavender, also for the special additive of cleaning agent, washing agent, insect-proof agent, therapeutic cosmetic, and for the anti-mite medicament of pharmaceuticals industry.
Modern medicine study proves, contains extremely abundant and complicated chemical composition in wormwood, and main component is volatile oil and tannin class, flavonoids, alcohols, polysaccharide and microelement kind etc.Pharmacological evaluation also proved wormwood have antibacterial, antiviral, relieving asthma, antibechic, misfortune phlegm, antiallergy, hemostasis and anticoagulation, enhancing immunity, protect the effects such as liver cholagogic, antipyretic calmness and step-down.In the present invention, wormwood essential oil be from wormwood through extracting technique of Chinese medicine purification gained, mainly utilize its antibacterial action.
Existing anti-mite cellulose fibre is generally that the pesticide of synthetic pesticide class or commercially available mite-proof agent are joined and in fiber, be spun into fiber.Pesticide pesticide toxicity is larger, and people is known from experience and causes potential harm.At present, the anti-mite of artificial fibre is processed the post-processing approach of mainly taking fiber to carry out medicine dipping and medicine spraying, because medicine is poor to artificial fibre internal penetration, surface drug can cause drug effect to go down because of washing, Exposure to Sunlight, affects the persistence of anti-mite effect.
Publication number is that the patent documentation that CN102517910B, name are called " a kind of anti-mite polyamide fiber and preparation method thereof " discloses a kind of anti-mite polyamide fiber and preparation method thereof, this invention is reacted chrysanthemumic acid compounds with polyamide fiber, and then obtains having the polyamide fiber of anti-mite function.This fiber is synthetic fiber, and chrysanthemumic acid is synthetic drug, have human body irritant, be unfavorable for promote.
Publication number is that patent documentation that CN101168864A, name are called " a kind of polypropylene fiber of highly effective acarid-proof " discloses a kind of anti-mite polypropylene fiber made from PP section blend melt spinning after nanometer grade powder that commercially available mite-proof agent is ground into, polypropylene fiber is synthetic fiber, the not clear and definite active ingredient of commercially available mite-proof agent, cannot judge its bio-toxicity and ecological security, be unfavorable for promoting.
Publication number is that patent documentation that CN101168867A, name are called " a kind of highly effective acarid-proof and have the viscose of antibacterial action " provides a kind of and adds the mite-resistant cellulose viscose of making through wet spinning in rayon spinning stoste after commercially available mite-proof agent is ground into nanometer grade powder.Wherein the not clear and definite active ingredient of commercially available mite-proof agent, cannot judge its bio-toxicity and ecological security, is unfavorable for promoting; And Powdered mite-proof agent manufacture craft difficulty is large, be difficult to be uniformly dispersed, and cost is higher.
Publication number is that patent documentation that CN100558953C, name are called " a kind of preparation method of acarus-proof antibiotic cellulose fiber " provides to know clearly and a kind ofly joins as mite-proof agent the anti-mite cellulose fibre of making in fiber afterwards using composite to Hexythiazox, buprofezin, fenpyroximate and various auxiliary agents etc., drug ingedient complexity wherein, preparing process is loaded down with trivial details; And these active ingredients all belong to pesticide pesticide, not only eye is had to minimal irritation effect, long-term use is unfavorable for health and the ecological balance, and such agricultural chemicals just has miticidal effect while only having contact acarid, can not walk quickly and keep away effect to acarid generation.
Borneol not only can contact and kill acarid, can also walk quickly and keep away effect to the acarid generation that does not contact borneol; And borneol external application is nontoxic to human body, pollution-free to ecological environment.Through literature search, do not occur thering is health care at present, drive mite, the borneol of antibacterial triple effects joins as mite-proof medicine the technology and the product that in cellulose spinning fluid, are spun into the regenerated celulose fibre that has anti-mite function and human body is had no side effect.
Summary of the invention
The object of this invention is to provide a kind of regenerated celulose fibre that contains microencapsulation mite-proof medicine and preparation method thereof, scattering ratio >=95% of gained regenerated celulose fibre to dust mite, there is extremely strong anti-mite effect, the bacteriostasis rate of the germ such as staphylococcus aureus, Escherichia coli is reached more than 90%, there is extremely strong antibiotic effect.
A kind of regenerated celulose fibre that contains microencapsulation mite-proof medicine, comprise rayon spinning stoste and microencapsulation mite-proof medicine, wherein microencapsulation mite-proof medicine quality accounts for 0.05~2% of methylcellulose quality in rayon spinning stoste, and methylcellulose quality accounts for 98~99.5% of regenerated celulose fibre dry weight; Capsule-core made by borneol and wormwood essential oil by described microencapsulation mite-proof medicine.
As the further improvement of foregoing invention, in described capsule-core, the mass concentration of borneol is 5%~15%, and the mass concentration of wormwood essential oil is 85%~95%.
As the further improvement of foregoing invention, described borneol is natural drug borneol or the synthetic borneol that has equal effect with it.
The preparation method of the above-mentioned regenerated celulose fibre that contains microencapsulation mite-proof medicine, comprises the following steps:
Step 1, is dissolved in borneol in wormwood essential oil, obtains borneol-wormwood essential oil;
Step 2, by microencapsulation technology, prepares the microcapsules that capsule-core-softgel shell mass ratio is 1:1 by step 1 gained borneol-wormwood essential oil solution;
Step 3, adds step 2 gained microcapsules the rayon spinning stoste of premix, mixes, and obtains microcapsules premix spinning solution;
Step 4, obtains through wet spinning, coagulation forming, washing, non-oxide desulfurization and drying production process the regenerated celulose fibre that contains microencapsulation mite-proof medicine by step 3 gained spinning solution.
As the further improvement of foregoing invention, in described step 2, microencapsulation technology used is interfacial polymerization.
As the further improvement of foregoing invention, the concrete steps of described interfacial polymerization are: first borneol-wormwood essential oil Solution Dispersion is prepared to oil phase in capsule material, again gained oil phase is added in the aqueous solution of emulsifying agent, after emulsify at a high speed, add auxiliary agent, then rinse gained slurries, after being dried, can obtain microcapsules.
As the further improvement of foregoing invention, in step 4, non-oxide desulfurization is for adopting desulfurizing agent Na2S or Na2SO3 to carry out desulfurization post processing.
Borneol is a kind of organic solid medicine, hardness is less, be difficult to be crushed to micron, Nano grade as inoganic solids medicine, the present invention does not use medicine crushing technology, but be first dissolved in the wormwood essential oil with antibacterial functions, be prepared into the microcapsules that average grain diameter is 2 μ m, the fibre diameter of common viscose glue approximately 20 μ m, do not affect the spinning technique of viscose glue again.
The present invention's mite-proof agent used be can be used for medicine and food, to the nontoxic borneol of human body and wormwood essential oil, not only there is the effect of mite-proofing and antimicrobial, also there is refrigerant aromatic odor and health-care effect.In addition, because borneol and wormwood essential oil are scattered in fabric integer with capsule state, its release and volatilization have slow release effect, and persistence is good.After testing, its scattering ratio >=95% to dust mite, has extremely strong anti-mite effect.Bacteriostasis rate to the germ such as staphylococcus aureus, Escherichia coli reaches more than 90%.
Detailed description of the invention
Embodiment 1
The extract borneol that is 99% by the purity that comes from natural plants kapur is dissolved in wormwood essential oil, makes borneol mass concentration and be borneol-wormwood essential oil of 5%.
In weight portion, get 2 parts of toluene di-isocyanate(TDI)s and 4 parts of borneol-wormwood essential oil solution mix composition oil phase, this oil phase is dropped into containing in 10 parts of water of wt1% emulsifying agent polyvinyl alcohol (Mw1500), adopt high-speed emulsifying machine to carry out emulsification, rotating speed 9200-9600r/min, emulsification 5min, obtains O/w emulsion.For making emulsion-stabilizing, add 10 parts of the aqueous solution that contain wt0.13% dispersant sodium alginate, add 4.6 parts of polyethylene glycol (Mw400-600) and 1% catalyst dibutyl tin dilaurate simultaneously, under room temperature, stir 2 hours, then temperature rises to 70 DEG C, add chain extender ethylenediamine, and continue to stir 1 hour, wall material is cured.Gained slurries are removed the wormwood essential oil on unreacted toluene di-isocyanate(TDI) and wall material surface with the alcohol flushing of wt30%, under room temperature, be dried and can obtain microcapsules in 24 hours.
Be that in rayon spinning liquid, 0.05% ratio of methylcellulose content joins in rayon spinning liquid by above-mentioned microcapsules according to microcapsules consumption, the microcapsules that contain borneol and wormwood essential oil are evenly spread in spinning solution.
By above-mentioned spinning solution through wet spinning, coagulation forming, washing, non-oxide desulfurization and≤105 DEG C of temperature under drying production process make, spinning technique is conventional viscose glue wet spinning technology, employing desulfurizing agent is sodium sulfite.
The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.67dtex; Dry strong 1.7cN/dtex; Wet strong 1.0cN/dtex; Dryly stretch 20%; In fiber, microcapsules quality accounts for 0.05% of methylcellulose content in rayon spinning liquid, and methylcellulose quality accounts for 99.95% of fiber dry weight.
Embodiment 2
Be that 98% synthetic borneol is dissolved in wormwood essential oil by coming from purity, make borneol mass concentration and be borneol-wormwood essential oil of 10%.
In weight portion, get 5 parts of toluene di-isocyanate(TDI)s and 5 parts of borneol-wormwood essential oil solution mix composition oil phase, this oil phase is dropped into containing in 12 parts of water of wt1.2% emulsifying agent polyvinyl alcohol (Mw1500), adopt high-speed emulsifying machine to carry out emulsification, rotating speed 9200-9600r/min, emulsification 5min, obtains O/w emulsion.For making emulsion-stabilizing, add 10 parts of the aqueous solution that contain wt0.15% dispersant sodium alginate, add 5.4 parts of polyethylene glycol (Mw400-600) and 1% catalyst dibutyl tin dilaurate simultaneously, under room temperature, stir 2 hours, then temperature rises to 70 DEG C, add chain extender ethylenediamine, and continue to stir 1 hour, wall material is cured.Gained slurries are removed the wormwood essential oil on unreacted toluene di-isocyanate(TDI) and wall material surface with 30% alcohol flushing, under room temperature, be dried and can obtain microcapsules in 24 hours.
Be that in rayon spinning liquid, 1% ratio of methylcellulose content joins in rayon spinning liquid by above-mentioned microcapsules according to microcapsules consumption, the microcapsules that contain borneol and wormwood essential oil are evenly spread in spinning solution.
By above-mentioned spinning solution through wet spinning, coagulation forming, washing, non-oxide desulfurization and≤105 DEG C of temperature under drying production process make, spinning technique is conventional viscose glue wet spinning technology, employing desulfurizing agent is sodium sulfite.
The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.59dtex; Dry strong 1.8cN/dtex; Wet strong 1.1cN/dtex; Dryly stretch 18%; In fiber, microcapsules quality accounts for 1% of methylcellulose content in rayon spinning liquid, and methylcellulose quality accounts for 99% of fiber dry weight.
Embodiment 3
The extract borneol that is 99% by the purity that comes from natural plants kapur is dissolved in wormwood essential oil, makes borneol mass concentration and be borneol-wormwood essential oil of 5%.
In weight portion, get 2 parts of toluene di-isocyanate(TDI)s and 4 parts of borneol-wormwood essential oil solution mix composition oil phase, this oil phase is dropped into containing in 10 parts of water of wt1% emulsifying agent polyvinyl alcohol (Mw1500), adopt high-speed emulsifying machine to carry out emulsification, rotating speed 9200-9600r/min, emulsification 5min, obtains O/w emulsion.For making emulsion-stabilizing, add 10 parts of the aqueous solution that contain wt0.13% dispersant sodium alginate, add 4.6 parts of polyethylene glycol (Mw400-600) and 1% catalyst dibutyl tin dilaurate simultaneously, under room temperature, stir 2 hours, then temperature rises to 70 DEG C, add chain extender ethylenediamine, and continue to stir 1 hour, wall material is cured.Gained slurries are removed the wormwood essential oil on unreacted toluene di-isocyanate(TDI) and wall material surface with the alcohol flushing of wt30%, under room temperature, be dried and can obtain microcapsules in 24 hours.
Be that in rayon spinning liquid, 0.05% ratio of methylcellulose content joins in rayon spinning liquid by above-mentioned microcapsules according to microcapsules consumption, the microcapsules that contain borneol and wormwood essential oil are evenly spread in spinning solution.
By above-mentioned spinning solution through wet spinning, coagulation forming, washing, non-oxide desulfurization and≤105 DEG C of temperature under drying production process make, spinning technique is conventional viscose glue wet spinning technology, employing desulfurizing agent is sodium sulfite.
The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.61dtex; Dry strong 1.9cN/dtex; Wet strong 1.3cN/dtex; Dryly stretch 21%, in fiber, borneol quality accounts for 1.5% of fiber dry weight, and methylcellulose quality accounts for 98.5% of fiber dry weight.
Embodiment 4
Be that 98% synthetic borneol is dissolved in wormwood essential oil by coming from purity, make borneol mass concentration and be borneol-wormwood essential oil of 20%.
In weight portion, get 5 parts of toluene di-isocyanate(TDI)s and 5 parts of borneol-wormwood essential oil solution mix composition oil phase, this oil phase is dropped into containing in 12 parts of water of wt1.2% emulsifying agent polyvinyl alcohol (Mw1500), adopt high-speed emulsifying machine to carry out emulsification, rotating speed 9200-9600r/min, emulsification 5min, obtains O/w emulsion.For making emulsion-stabilizing, add 10 parts of the aqueous solution that contain wt0.15% dispersant sodium alginate, add 5.4 parts of polyethylene glycol (Mw400-600) and 1% catalyst dibutyl tin dilaurate simultaneously, under room temperature, stir 2 hours, then temperature rises to 70 DEG C, add chain extender ethylenediamine, and continue to stir 1 hour, wall material is cured.Gained slurries are removed the wormwood essential oil on unreacted toluene di-isocyanate(TDI) and wall material surface with 30% alcohol flushing, under room temperature, be dried and can obtain microcapsules in 24 hours.
Be that in rayon spinning liquid, 0.08% ratio of methylcellulose content joins in rayon spinning liquid by above-mentioned microcapsules according to microcapsules consumption, the microcapsules that contain borneol and wormwood essential oil are evenly spread in spinning solution.
By above-mentioned spinning solution through wet spinning, coagulation forming, washing, non-oxide desulfurization and≤105 DEG C of temperature under drying production process make, spinning technique is conventional viscose glue wet spinning technology, employing desulfurizing agent is sodium sulfite.
The leading indicator of the fiber of preparing through above-mentioned steps is as follows: fiber number 1.65dtex; Dry strong 2.0cN/dtex; Wet strong 1.3cN/dtex; Dryly stretch 23%; In fiber, microcapsules quality accounts for 2% of methylcellulose content in rayon spinning liquid, and methylcellulose quality accounts for 98% of fiber dry weight.
Reference examples 1
The difference of the present embodiment and embodiment 4 is: the present embodiment adopts and is crushed to nano level borneol and adds in wormwood essential oil to replace borneol-wormwood essential oil microcapsules to add to and in rayon spinning liquid, carry out spinning.
The mite-proofing and antimicrobial test data of table 1 acarus-proof antibiotic
The mite-proofing and antimicrobial test data of table 2 acarus-proof antibiotic
As seen from the above table, add the anti-mite biocidal property of fiber that in rayon spinning liquid, spinning obtains to be better than being crushed to the prepared fiber of nano level borneol-wormwood essential oil after borneol-wormwood essential oil being made to microcapsules.
Reference examples 2
The difference of the present embodiment and embodiment 3 is: in the present embodiment, in microcapsules capsule-core, the mass concentration of borneol is 20%, and the mass concentration of wormwood essential oil is 80%.
The leading indicator of the fiber preparing is as follows: fiber number 0.95dtex; Dry strong 1.1cN/dtex; Wet strong 0.7cN/dtex; Dryly stretch 12%.
Reference examples 3
The difference of the present embodiment and embodiment 3 is: in the present embodiment, in microcapsules capsule-core, the mass concentration of borneol is 25%, and the mass concentration of wormwood essential oil is 75%.
The leading indicator of the fiber preparing is as follows: fiber number 0.86dtex; Dry strong 0.8cN/dtex; Wet strong 0.5cN/dtex; Dryly stretch 9%.
Reference examples 2,3 is known compared with embodiment 3 gained fibers, and when borneol mass concentration is 5%~15%, gained fibre property is good.
Because the mite-proof agent of borneol, wormwood essential oil composition has excellent security, the anti-mite bacteriostasis property of broad-spectrum high efficacy and refrigerant faint scent of calming the nerves, it is not only the jinx of acarid and germ, can also bring certain health-care effect and refrigerant sense.The present invention can be used for producing the core pad class bedding with anti-mite, antibacterial, fragrant, health care, deodorization functions, can also make core pad fabric after making yarn.The prepared fiber that adds of this drug microcapsule meets GB/T18383-2007 wadding fibre current techique standard.

Claims (7)

1. a regenerated celulose fibre that contains microencapsulation mite-proof medicine, it is characterized in that: comprise rayon spinning stoste and microencapsulation mite-proof medicine, wherein microencapsulation mite-proof medicine quality accounts for 0.05~2% of methylcellulose quality in rayon spinning stoste, and methylcellulose quality accounts for 99.8~99.5% of regenerated celulose fibre dry weight; Capsule-core made by borneol and wormwood essential oil by described microencapsulation mite-proof medicine.
2. the regenerated celulose fibre that contains microencapsulation mite-proof medicine according to claim 1, is characterized in that: in described capsule-core, the mass concentration of borneol is 5%~15%, and the mass concentration of wormwood essential oil is 85%~95%.
3. the regenerated celulose fibre that contains microencapsulation mite-proof medicine according to claim 1, is characterized in that: described borneol is natural drug borneol or the synthetic borneol that has equal effect with it.
4. the preparation method of the regenerated celulose fibre that contains microencapsulation mite-proof medicine claimed in claim 1, is characterized in that: comprise the following steps:
Step 1, is dissolved in borneol in wormwood essential oil, obtains borneol-wormwood essential oil;
Step 2, by microencapsulation technology, prepares microcapsules by step 1 gained borneol-wormwood essential oil;
Step 3, adds step 2 gained microcapsules the rayon spinning stoste of premix, mixes, and obtains microcapsules premix spinning solution;
Step 4, obtains through wet spinning, coagulation forming, washing, non-oxide desulfurization and drying production process the regenerated celulose fibre that contains microencapsulation mite-proof medicine by step 3 gained spinning solution.
5. the preparation method of the regenerated celulose fibre that contains microencapsulation mite-proof medicine according to claim 4, is characterized in that: in step 2, microencapsulation technology used is interfacial polymerization.
6. the preparation method of the regenerated celulose fibre that contains microencapsulation mite-proof medicine according to claim 5, it is characterized in that: the concrete steps of described interfacial polymerization are: first borneol-wormwood essential oil Solution Dispersion is prepared to oil phase in capsule material, again gained oil phase is added in the aqueous solution of emulsifying agent, after emulsify at a high speed, add dispersant, catalyst and chain extender, then rinse gained slurries, after being dried, can obtain microcapsules.
7. the preparation method of the regenerated celulose fibre that contains microencapsulation mite-proof medicine according to claim 4, is characterized in that: in step 4, non-oxide desulfurization is for adopting desulfurizing agent Na 2s or Na 2sO 3carry out desulfurization post processing.
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CN105671665A (en) * 2016-02-02 2016-06-15 湖州珠力纳米材料科技开发有限公司 Microcapsule type rose-modified regenerated cellulose fiber and preparation method thereof
CN105671665B (en) * 2016-02-02 2018-05-08 湖州珠力纳米材料科技开发有限公司 A kind of microcapsule-type rose modification regeneration cellulose fibre and preparation method thereof
CN107268096A (en) * 2016-04-07 2017-10-20 河北吉藁化纤有限责任公司 A kind of preparation method of wormwood antibacterial viscose fiber
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CN107338497A (en) * 2016-08-24 2017-11-10 桐乡守敬应用技术研究院有限公司 A kind of antibacterial aloe fiber
CN108265374A (en) * 2016-12-30 2018-07-10 滨州亚光家纺有限公司 A kind of wormwood antibacterial towel and its production method
CN106835343A (en) * 2017-01-10 2017-06-13 中科纺织研究院(青岛)有限公司 A kind of plants antimicrobial cellulose fibre and preparation method thereof and the medical water proof nonwoven cloth prepared using the fiber
US20190203381A1 (en) 2017-12-29 2019-07-04 Infinitus(China) Company Ltd. A method for preparing regenerated cellulose fibers having anti-bacteria, anti-mite and anti-mould functions and the use thereof
US10563322B2 (en) 2017-12-29 2020-02-18 Infinitus (China) Company Ltd. Method for preparing regenerated cellulose fibers having anti-bacteria, anti-mite and anti-mould functions and the use thereof

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