CN105442073A - Preparation method of anti-mite and antibacterial regenerative cellulosic fibers - Google Patents
Preparation method of anti-mite and antibacterial regenerative cellulosic fibers Download PDFInfo
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- CN105442073A CN105442073A CN201510998349.3A CN201510998349A CN105442073A CN 105442073 A CN105442073 A CN 105442073A CN 201510998349 A CN201510998349 A CN 201510998349A CN 105442073 A CN105442073 A CN 105442073A
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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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
-
- 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
- D01D5/06—Wet spinning methods
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Abstract
The invention provides a preparation method of anti-mite and antibacterial regenerative cellulosic fibers. The preparation method comprises the following steps: mixing and then microencapsulating neem oil and photocatalyst assistant anatase nano TiO2, dispersing obtained microcapsules, spinning with a viscose spinning solution, and preparing the regenerative cellulosic fibers with a mite resistance function. According to the preparation method, viscose fibers obtained by spinning in the spinning solution added with the microcapsules containing azadirachtin and nano TiO2 have a better mite expelling and bacterium inhibition effect; the compatibility is higher, and a better synergistic effect can be achieved.
Description
Technical field
The invention belongs to textile industry material technology field, be specifically related to the preparation method of the antibacterial regenerated celulose fibre of a kind of anti-mite.
Background technology
Acarid is the segmental appendage class parasite that a class build is less, body size is usually at about 0.5mm, huge number, wherein dirt mite grows usually in the household articless such as mattress, down toy, sofa, bed clothes, cushion, pillow, with the sweat of the mankind, secretion, exuviae bits feeding.The corpse of acarid, secretion and excreta are all the anaphylactogens that can cause a disease, and now there are some researches show, the adult of 97% can be caused a disease because of mite infection, common disease comprise breathe heavily, rhinitis, dermatitis, ringworm of the body etc.
Print chinaberry system Meliaceae Melia arbor, originates in India and Burma, extensively plants in tropical and subtropical region, plants in the existing distribution of more than 70 countries of Southern Asia, Africa and South America.What find from print chinaberry plant plants insecticide active substance based on more than 400 of nimbin A, more than 400 can be prevented and treated and plant agricultural, warehouse and sanitary insect pest, little on natural enemy impact, obvious toxicity is not had to plant and vertebrate, degraded rapidly in the environment, aboundresources, reproducible utilization is more perfect pesticide.In addition, nimbin also medical value widely, as anti-malarial, bring down a fever, expelling parasite, conk etc. in suppression animal and human body.Current nimbin has been widely applied in the field such as agricultural chemicals, cosmetics.
Mostly current mite-assistant fiber is on the market in the spinning solution added by the auxiliary agent of synthesis class, then spinning moulding obtains mite-assistant fiber, the weak point of this fibrid: directly added in fiber by this analog assistant on the one hand, these auxiliary agents easily contact with human skin, affects human body healthy; On the other hand, the anti-mite auxiliary agent toxicity of synthesis class is comparatively large, also even more serious to the injury of human body.Some mite-assistant fiber are then the methods by Final finishing in addition, anti-mite auxiliary agent is arranged on each fibrid, thus there is the effect of anti-mite, the shortcoming of these class methods not only can affect the quality of fiber own by the mode of Final finishing, finally cause the feel of fabric not good enough, the auxiliary agent washability of Final finishing is poor simultaneously, and the anti-mite duration is shorter, cannot meet consumer demand.
Patent CN101168867A provide a kind of commercially available mite-proof agent is ground into nanometer grade powder after add the mite-resistant cellulose viscose made through wet spinning in rayon spinning stoste, the not clear and definite active ingredient of this commercially available mite-proof agent, its bio-toxicity and ecological security cannot be judged, be unfavorable for promoting; And Powdered mite-proof agent manufacture craft difficulty is large, be difficult to be uniformly dispersed, cost is higher.Patent CN100558953C discloses and a kind ofly joins as mite-proof agent the mite-assistant fiber cellulose fiber made in fiber afterwards using composite to Hexythiazox, buprofezin, fenpyroximate and various auxiliary agents etc., its drug ingedient is complicated, preparing process is loaded down with trivial details, and these active ingredients all belong to pesticide pesticide, not only there is minimal irritation effect to eye, Long-Time Service is unfavorable for health and the ecological balance, and such agricultural chemicals only has during contact acarid and just has miticidal effect, can not produce walk quickly and keep away effect to acarid.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art and the preparation method providing the antibacterial regenerated celulose fibre of a kind of anti-mite, gained fiber not only has and good drives mite fungistatic effect, and elasticity and strength character are improved.
A preparation method for the antibacterial regenerated celulose fibre of anti-mite is mixed with rayon spinning liquid by the mode spinning forward slip value by Nim oil micro capsule, and wet spinning obtains the regenerated celulose fibre containing Nim oil micro capsule.
Further, described Nim oil micro capsule adds in form of an aqueous solutions.
Further, described Nim oil micro capsule content is in aqueous 10 ~ 20wt%.
Further, also containing dispersant in the described aqueous solution, the consumption of dispersant is 1 ~ 3wt% of Nim oil micro capsule consumption.
Further, described dispersant is the one in calgon, tristerin or stearate.
Further, the capsule-core of described Nim oil micro capsule comprises nim oil, photocatalyst auxiliary agent and base oil, and the consumption of nim oil is 10 ~ 15wt%, and the consumption of photocatalyst auxiliary agent is 3 ~ 5wt%, and the consumption of base oil is 80 ~ 87wt%.
Further, described base oil is the one in rose hip oil, grape-kernel oil, olive oil, wheat-germ oil, SIMMONDSIA CHINENSIS SEED OIL, Avocado Oil or macadamia nut oil.
Further, described photocatalyst auxiliary agent is dichloride in anatase type TiO
2, its particle diameter is 0 ~ 20nm.
Further, described Nim oil micro capsule is slow-release type microcapsule, and particle diameter is 0.1 ~ 1 μm.
Further, the consumption of described Nim oil micro capsule is 2 ~ 4wt% of the fine content of first in rayon spinning liquid.
The present invention is first by nim oil and photocatalyst auxiliary agent dichloride in anatase type TiO
2microencapsulation after mixing, carries out spinning, the obtained regenerated celulose fibre with anti-mite function by mixing with rayon spinning liquid after obtained microcapsules dispersion again.The anti-mite effect of the natural nim oil of this fiber utilization and photocatalyst auxiliary agent nano-TiO
2combination, nim oil is compared with the anti-mite auxiliary agent of conventional synthesis, and toxicity is lower, healthy advantageously in the mankind, also has wide material sources, environment friendly and pollution-free feature simultaneously; And photocatalyst auxiliary agent nano-TiO
2can light-catalyzed reaction be caused under irradiation by sunlight, thus around it, form a large amount of hydroxyl free radicals (-OH) and negative oxygen ion (O
2-) carry out each type organic of oxidation Decomposition, comprise bacterium, make fiber have bacteriostasis property.
Because the character of nim oil is stable not, especially under the condition of illumination, the ultraviolet in sunshine can cause it to decompose, and nano-TiO
2the some ultra violet rays of sunshine can be absorbed, thus can not be decomposed under the condition of illumination by available protecting nim oil, ensure the persistence of anti-mite effect.Photocatalyst material is under the irradiation of ultraviolet simultaneously, and after reaction, itself produces one group and is respectively with plus-minus electric hole and electronics, contacts, can produce hydroxyl free radical (-OH) and the negative oxygen ion (O of Strong oxdiative power with the hydrone in air
2 -), thus the various organic compound of potent decomposition and part inorganic matter, destroy the cell membrane of bacterium and the protein of solidification virus, can form permanent antifouling coat at material surface, has extremely strong antifouling, sterilization and deodorization functions.
Detailed description of the invention:
Below by detailed description of the invention, the present invention is described in further detail.But it will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting scope of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition (such as with reference to " dyeing and finishing technology and principle " that Zhao Tao writes, China Textiles Press, 2009) or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
In the liquid of rayon spinning described in the present invention, first fibre refers to: alpha cellulose is also known as alpha-cellulose.Cellulosic material to be dipped in the sodium hydroxide solution of 17.5% ~ 18% undissolved part after 45 minutes at 20 DEG C.
Falling ball method: the time that 2mm steel ball falls needed for 20cm from described viscose solution.
Capsule of nano of the present invention utilizes conventional microcapsule coated technology to make.
Embodiment 1
The preparation of rayon spinning liquid
Raw material to be the degree of polymerization be 500 ~ 600 Cotton Pulp, the fine content of its first is greater than 90%, and according to following process route glue: dipping, squeezing, pulverize, experienced, yellow, continuous-dissolution, filtration, deaeration.
According to above-mentioned manufacture technics, to form the fine content of rayon spinning liquid first be 8.8%, NaOH mass fraction is 5.9%, and viscosity is (falling ball method) 58s, and ripe degree is (10%NH
4cl) 8.6mL.
The preparation of dispersion of microcapsules system
In reactor, be the dispersion of microcapsules system of 10% with distilled water preparation mass fraction, nim oil, nano-TiO in capsule-core
2with the component of rose hip oil than being 10:4:86, adding the glyceryl tristearate dispersant accounting for microcapsules quality 1%, fully stirring and can obtain comparatively uniform micro-capsule dispersion liquid.Adopt sheet frame filter to filter through double-deck fine cloth, pressure, at below 0.2Mpa, obtains uniform micro-capsule dispersion liquid.
Viscose solution mixes with capsule of nano dispersion emulsion
Micro-capsule dispersion liquid adds in above-mentioned stand-by viscose solution by adoption rate pump quantitatively, and mixes.Micro-capsule dispersion liquid adopts syringe pump with the speed injection of 6 liters/min in dynamic mixer, and the flow of viscose solution is 50 liters/min, leaves standstill 1h under normal temperature.Wherein, the quality of microcapsules is 0%, 1%, 2%, 3%, 4%, 5% of the fine weight of first.
The mixed solution of microcapsules and viscose glue is sent into wet spinning operation and is carried out spinning by wet spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 52 DEG C, and plasticizing-bath temperature is 95 DEG C.Coagulation bath composition is: sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
The leading indicator of the fiber prepared through above-mentioned steps is as follows:
As can be seen from the table, introduce Nim oil micro capsule in rayon spinning liquid after, can significantly improve and drive mite fungistatic effect, and modified fibre has better elasticity and strength character.
Comparative example 1
Not containing nim oil in the microcapsules added by spinning solution.Testing result: fiber number 1.69dtex; Dry strong 1.97cN/dtex; Wet strong 1.35cN/dtex; Dryly stretch 17.1%; Bacteriostasis rate 98.5%; Acarid walks quickly and keeps away rate 0%.
Comparative example 2
Not containing photocatalyst auxiliary agent in the microcapsules added by spinning solution.Testing result: fiber number 1.65dtex; Dry strong 2.43cN/dtex; Wet strong 1.55cN/dtex; Dryly stretch 16.9%; Bacteriostasis rate 0%; Acarid walks quickly and keeps away rate 88.8%.
From above result, containing nimbin and nano-TiO
2microcapsules add spinning in spinning solution to and obtain viscose and have and drive mite fungistatic effect preferably, the compatibility of the two is better, can play good synergy simultaneously.
Embodiment 2
The preparation of rayon spinning liquid
Raw material to be the degree of polymerization be 500 ~ 600 wood pulps, the fine content of its first is greater than 90%, and according to following process route glue: dipping, squeezing, pulverize, experienced, yellow, continuous-dissolution, filtration, deaeration.
According to above-mentioned manufacture technics, to form the fine content of rayon spinning liquid first be 9.0%, NaOH mass fraction is 5.8%, and viscosity is (falling ball method) 60s, and ripe degree is (10%NH
4cl) 8.9mL.
The preparation of dispersion of microcapsules system
In reactor, be the dispersion of microcapsules system of 5%, 10%, 15%, 20%, 25% with distilled water preparation mass fraction, nim oil, nano-TiO in capsule-core
2with the component of olive oil oil than being 12:3:85, adding the glyceryl tristearate dispersant accounting for microcapsules quality 2%, fully stirring and can obtain comparatively uniform micro-capsule dispersion liquid.Adopt sheet frame filter to filter through double-deck fine cloth, pressure, at below 0.2Mpa, obtains uniform micro-capsule dispersion liquid.
Viscose solution mixes with capsule of nano dispersion emulsion:
Micro-capsule dispersion liquid adds in above-mentioned stand-by viscose solution by adoption rate pump quantitatively, and mixes.Micro-capsule dispersion liquid adopts syringe pump with the speed injection of 6 liters/min in dynamic mixer, and the flow of viscose solution is 50 liters/min, leaves standstill 1h under normal temperature.Wherein, the quality of microcapsules is 3% of the fine weight of first.
The mixed solution of microcapsules and viscose glue is sent into wet spinning operation and is carried out spinning by wet spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 52 DEG C, and plasticizing-bath temperature is 95 DEG C.Coagulation bath composition is: sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
The leading indicator of the fiber prepared through above-mentioned steps is as follows.
| Nim oil micro capsule concentration | 5％ | 10％ | 15％ | 20％ | 25％ |
| Fiber number dtex | 1.64 | 1.65 | 1.70 | 1.69 | 1.69 |
| Dry strong cN/dtex | 2.25 | 2.29 | 2.21 | 2.33 | 1.88 |
| Wet strong cN/dtex | 1.32 | 1.31 | 1.40 | 1.36 | 1.32 |
| Dryly stretch % | 17.1 | 18.3 | 17.7 | 18.0 | 16.1 |
| Bacteriostasis rate (%) | 54.3 | 95.2 | 93.7 | 92.6 | 69.5 |
| Acarid walks quickly and keeps away rate (%) | 12.8 | 64.7 | 57.1 | 53.7 | 17.6 |
It can be seen from the table, Nim oil micro capsule concentration is regulated and controled when preferable range, can improve significantly and drive mite fungistatic effect, and modified fibre has better elasticity and strength character.
Embodiment 3
The preparation of rayon spinning liquid
Raw material to be the degree of polymerization be 500 ~ 600 bamboo pulp, the fine content of its first is greater than 90%, and according to following process route glue: dipping, squeezing, pulverize, experienced, yellow, continuous-dissolution, filtration, deaeration.
According to above-mentioned manufacture technics, to form the fine content of rayon spinning liquid first be 8.9%, NaOH mass fraction is 6.0%, and viscosity is (falling ball method) 59s, and ripe degree is (10%NH
4cl) 8.7mL.
The preparation of dispersion of microcapsules system
In reactor, with the dispersion of microcapsules system that distilled water preparation mass fraction is 20%, in capsule-core, nim oil and wheat-germ oil mass ratio are 10:90, add the calgon dispersant accounting for microcapsules quality 0%, 1%, 2%, 3%, 4%, 5%, fully stir and can obtain comparatively uniform micro-capsule dispersion liquid.Adopt sheet frame filter to filter through double-deck fine cloth, pressure, at below 0.2Mpa, obtains uniform micro-capsule dispersion liquid.
Viscose solution mixes with capsule of nano dispersion emulsion
Micro-capsule dispersion liquid adds in above-mentioned stand-by viscose solution by adoption rate pump quantitatively, and mixes.Micro-capsule dispersion liquid adopts syringe pump with the speed injection of 6 liters/min in dynamic mixer, and the flow of viscose solution is 50 liters/min, leaves standstill 1h under normal temperature.Wherein, the quality of microcapsules is 10% of the fine weight of first.
The mixed solution of microcapsules and viscose glue is sent into wet spinning operation and is carried out spinning by wet spinning.Spinning head specification is 21000 holes × 0.06mm, and spinning speed is 55m/min, and coagulation bath temperature is 52 DEG C, and plasticizing-bath temperature is 95 DEG C.Coagulation bath composition is: sulfuric acid 115g/L, sodium sulphate 325g/L, zinc sulfate 11.5g/L.
The leading indicator of the fiber prepared through above-mentioned steps is as follows.
| Dispersant concentration | 0％ | 1％ | 2％ | 3％ | 4％ | 5％ |
| Fiber number dtex | 1.69 | 1.72 | 1.63 | 1.75 | 1.69 | 1.67 |
| Dry strong cN/dtex | 1.90 | 2.01 | 2.24 | 2.11 | 1.88 | 1.95 |
| Wet strong cN/dtex | 1.32 | 1.45 | 1.60 | 1.35 | 1.32 | 1.43 |
| Dryly stretch % | 14.7 | 15.8 | 18.1 | 16.2 | 16.1 | 17.4 |
| Bacteriostasis rate (%) | 78.5 | 95.2 | 93.7 | 92.6 | 69.5 | 59.4 |
| Acarid walks quickly and keeps away rate (%) | 43.2 | 64.7 | 57.1 | 53.7 | 17.6 | 18.2 |
It can be seen from the table, dispersant concentration is regulated and controled when preferable range, can improve significantly and drive mite fungistatic effect, and modified fibre has better elasticity and strength character.
Claims (10)
1. a preparation method for the antibacterial regenerated celulose fibre of anti-mite, is characterized in that: mixed with rayon spinning liquid by the mode spinning forward slip value by Nim oil micro capsule, and wet spinning obtains the regenerated celulose fibre containing Nim oil micro capsule.
2. the preparation method of the antibacterial regenerated celulose fibre of anti-mite according to claim 1, is characterized in that: described Nim oil micro capsule adds in form of an aqueous solutions.
3. the preparation method of the antibacterial regenerated celulose fibre of anti-mite according to claim 2, is characterized in that: described Nim oil micro capsule content is in aqueous 10 ~ 20wt%.
4. the preparation method of the antibacterial regenerated celulose fibre of anti-mite according to claim 2, is characterized in that: also containing dispersant in the described aqueous solution, the consumption of dispersant is 1 ~ 3wt% of Nim oil micro capsule consumption.
5. the preparation method of the antibacterial regenerated celulose fibre of anti-mite according to claim 4, is characterized in that: described dispersant is the one in calgon, tristerin or stearate.
6. the preparation method of the antibacterial regenerated celulose fibre of anti-mite according to claim 1, it is characterized in that: the capsule-core of described Nim oil micro capsule comprises nim oil, photocatalyst auxiliary agent and base oil, the consumption of nim oil is 10 ~ 15wt%, the consumption of photocatalyst auxiliary agent is 3 ~ 5wt%, and the consumption of base oil is 80 ~ 87wt%.
7. the preparation method of the antibacterial regenerated celulose fibre of anti-mite according to claim 6, is characterized in that: described base oil is the one in rose hip oil, grape-kernel oil, olive oil, wheat-germ oil, SIMMONDSIA CHINENSIS SEED OIL, Avocado Oil or macadamia nut oil.
8. the preparation method of the antibacterial regenerated celulose fibre of anti-mite according to claim 6, is characterized in that: described photocatalyst auxiliary agent is dichloride in anatase type TiO
2, its particle diameter is 0 ~ 20nm.
9. the preparation method of the antibacterial regenerated celulose fibre of anti-mite according to claim 1, it is characterized in that: described Nim oil micro capsule is slow-release type microcapsule, particle diameter is 0.1 ~ 1 μm.
10. the preparation method of the antibacterial regenerated celulose fibre of anti-mite according to claim 1, is characterized in that: the consumption of described Nim oil micro capsule is 2 ~ 4wt% of the fine content of first in rayon spinning liquid.
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Cited By (5)
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| CN105696325A (en) * | 2016-04-20 | 2016-06-22 | 吴江市林旺纺织厂 | Antifungal anti-mite textile material and preparation method thereof |
| CN107981766A (en) * | 2017-11-15 | 2018-05-04 | 吴家淡 | A kind of antibacterial anti-mite net skin towel |
| 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 |
| CN111671181A (en) * | 2020-06-04 | 2020-09-18 | 中国制浆造纸研究院有限公司 | Mask and preparation method thereof |
| CN111733531A (en) * | 2020-06-04 | 2020-10-02 | 中国制浆造纸研究院有限公司 | Multifunctional mask and preparation method thereof |
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| CN111733531A (en) * | 2020-06-04 | 2020-10-02 | 中国制浆造纸研究院有限公司 | Multifunctional mask and preparation method thereof |
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