CN103981588B - A kind of antibacterial and deodouring cellulose fibre and preparation method thereof - Google Patents
A kind of antibacterial and deodouring cellulose fibre and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of antibacterial and deodouring cellulose fibre, the aluminosilicate slow-release microcapsule wherein containing 1 ~ 10wt%, the bamboo charcoal nano-powder of 1 ~ 5wt%, dry fracture strength are 1.80 ~ 2.60cN/dtex, and wet breaking strength is 0.90 ~ 1.50cN/dtex; Preparation method comprises: the preparation of modified rayon and spinning and post processing, add aluminosilicate slow-release microcapsule in described spinning and last handling process.The present invention has that wearability is excellent, textile process performance is good, anti-antibacterial and deodorization functions is given prominence to; Bamboo charcoal nano pulp is added from rear dissolving and stirs, alumino-silicate powder is made slow-release microcapsule, employing is spun front injection system and is added before spinning, the existence of microcapsules avoids that strong acid-base directly contacts alumino-silicate and the active principle that causes decomposes and runs off and structural deterioration, in fabric, alumino-silicate microcapsules discharge active ingredient slowly along with acid bath is shaping or friction is broken, bamboo charcoal nano powder adsorb peculiar smell, plays that Long-term Anti is antibacterial, the effect of deodorizing.
Description
Technical field
The present invention relates to modified cellulose technical field, particularly relate to a kind of antibacterial and deodouring cellulose fibre and preparation method thereof.
Background technology
Along with the progress of society and the raising of people's living standard, the idea of people's dressing is also constantly upgrading, and has higher requirement to the Comfortable attractive of the functional of textiles and product.And the production of the natural fabrics such as cotton, fiber crops, silk, hair is owing to striving the impact of ground contradiction by natural climate and grain and cotton, increase of production is very slow, far away can not practical requirement.
Occurring in nature cellulose not only storage level is large, and is a kind of inexhaustible, nexhaustible renewable resource.This raw material also only has at present and is a littlely made into fiber.That is familiar with nature along with the mankind deepens continuously, and cellulosic utilization also will expand gradually.In contrast to this, the raw material (oil, coal, natural gas etc.) that synthetic fiber are mainly formed by the different geologic(al) period is produced, although the storage capacity of these raw materials is very large, it is consuming gradually, and is difficult to recover.Have scholarly forecast, tellurian petroleum resources will be used up to mid-term 21st century.And cellulosic resource is unlimited, it is with the constantly natural synthesis of huge speed.
The epoch that 21 century is the further protection of the environment of requirement and makes rational use of resources.Cellulose fibre is owing to can be changed into steam and carbon dioxide by biological decomposition or safe combustion, and the welding problem caused by discarded object is few.As can be seen here, no matter from the degree of enriching of resource, process from discarded object, and many-sidedly to consider from the comfortableness of dress and elegant in appearance grade, it is very necessary for developing cellulose fibre.
Current China viscose kind majority is general fibre, and functional fiber, fibre in differentiation are little.Though the domestic production technology having known color fibre, fire resistance fibre, superfine denier fiber, the producer forming mass production capabilities is few.Analyze according to insider, China's fibre in differentiation is in quality and quantitatively with abroad still have gap.Domesticly at present can not meet the needs of export market due to plurality of raw materials, garment exportation fabric 70% is by import.One of the main reasons is new technology, new product development ability, high-caliber differentialand functional fiber limited amount.According to statistics, Europe, the United States, Deng developed country per capita viscose consumption figure are 1.3 kilograms, are 6 ~ 7 times of developing country.This shows that fibre in differentiation not only has domestic market widely, and has wide international market.Therefore be necessary Devoting Major Efforts To Developing high-performance, differential kind, meet domestic and international market demand, improving product competitiveness.
The various antibacterial fabrics (comprising knitted fabric, woven and nonwoven fabric) seen in the market, substantially three kinds of methods are adopted to produce: one is first added in spinning material by antiseptic to make anti-bacterial fibre, then make various antibacterial fabric, this method is commonly used to produce chemical synthetic fiber series products; Two is add antiseptic (being often called as antibacterial finishing agent) in fabric printing Final finishing process, then various antibacterial fabric is made, this method both can produce pure natural fiber or pure chemistry synthetic fiber series products, also blend fibre series products can be produced, wide adaptability, therefore the production of most antibacterial fabric is adopted in this way; Three is first added in spinning material by antiseptic to make anti-bacterial fibre, then adds antibacterial finishing agent in fabric printing Final finishing process, and then make various antibacterial fabric, this method only uses in the specialities with very high antibacterial performance requirement.
The antimicrobial technology of current China has achieved larger development, but antimicrobial product also also exists some problems, most organic antiseptic all has certain excitant and toxic and side effect to human body skin, and mineral-type antiseptic is often containing heavy metal ion, very easily by being absorbed by the body with contact human skin, high risks is caused to the health of human body.
Antibacterial wide spectrum problem can be solved better, develop the antiseptic of wide spectrum more, improve antibacterial durability, fabric is made still to have good antibacterial effect through repeatedly washing, can selectively anti-bacteria breeding and make clump count remain on harmless level, instead of simply utterly destroy all bacteriums.It is particularly urgent that the solution of this series of problems becomes.
In recent years, occurred utilizing natural macromolecular material to carry out the antibacterial deodourizing processing of textiles for antiseptic, meet the requirement of textiles safety, healthy and environmental protection, chitin kind fiber becomes main a member.Because chitin fiber brute force is low, fragility is large, fiber band look and expensive etc., affects quality and the cost of goods, can not absorb decomposition for the foul smell produced, cause and be difficult to penetration and promotion.
Application number be 200510073503.2 Chinese patent disclose a kind of deodorization fiber and preparation method thereof, comprise the steps: to add dioxide photocatalyst titanium by after phthalocyanine iron and nodeless mesh water alumina silicate mixed grinding, be uniformly mixed with the coupling agent prepared and add polypropylene and EVA resin and stir, add surfactant and dispersant, mix with carrier polypropylene after the obtained deodorant of stirring concentrates master batch drying and obtain deodorization fiber through melt spinning.Application number be 201110219501.5 Chinese patent disclose a kind of antibacterial and deodouring modified polyester fibre, cut into slices and antiseptic-antibacterial zeolite particles by PET, deodorant is made up of phthalocyanine iron, alumina silicate and dioxide photocatalyst titanium and mixes, the antiseptic of 4-10% and the deodorant of 10-15% are joined in PET section in 200-230 DEG C, produce by common terylene chips spinning process and flow process, obtained antibacterial and deodouring modified polyester fibre product.Application number is the Chinese patent of 201210098266.5, disclose a kind of Deodorization polyamide fiber and preparation method thereof, the parts by weight of raw material components and each component are: polyamide fiber 100-300 part, 2-bromo-2-nitro-1,3-propylene glycol 0.5-2 part, solvent 200-500 part, dehydrating agent 0.05-0.2 part and catalyst 0.1-0.2 part.The 2-bromo-2-nitro-1,3-propylene glycol and polyamide fiber with deodorization functions are reacted, makes the hydroxyl in 2-bromo-2-nitro-1,3-propylene glycol molecule and the carboxyl in polyamide molecule carry out condensation reaction, and then obtain the polyamide fiber with deodorization functions.
Deodorizing antibiotic fibrid disclosed above all belongs to the category of synthetic fiber, and on the one hand, synthetic fiber mostly rely on petroleum resources, and along with the exhaustion day by day of the energy, exploitation will inevitably be restricted; On the other hand, although synthetic fiber brute force is outstanding, sucting wet air permeability is poor, and wear uncomfortable property, discomfort is fit to do underclothes dressing, and therefore the performance of antibacterial and deodouring performance is also had a greatly reduced quality.
Application number is the PCT patent of 00803554.7, disclose a kind of deodorization fiber and preparation method thereof, treatment fluid is adopted to contain the chitin of de-acetyl and/or the deacetyl chitin of modification, carboxylic acid polyalcohol, zinc oxide and binder resin process native cellulose or synthetic fiber.Application number be 00805580.7 PCT patent discloses a kind of fibrous structure thing with deodorizing or antibiotic property, fiber surface has the fibrous structure thing of composite oxides that titanium and silicon forms and adhesive.Application number is the Chinese patent of 201010185033.X, discloses a kind of fabric with antibacterial and deodorizing function, this fabric adopts deodorant composition and organic antibacterial agent process is padded or coating machining obtains.Deodorant composition is formed by least two kinds in the deodorant being main component with silica, zinc oxide or titanium dioxide, and organic antibacterial agent is row Quaternary Silicone Polymers class antiseptic.
Deodorizing antibiotic fibrid disclosed above all belongs to fabric post-treatment technique, although the antibacterial and deodouring function ratio of Final finishing fabric is more excellent, price also relative moderate is convenient to promote, and washability is poor, because the feel that there is fabric of adhesive is hardened, be not suitable for very much the underclothes making summer.
Application number be 201310097045.0 Chinese patent disclose a kind of method for making with natural antibacterial, deodorizing and anion function bamboo cellulose fibre, appropriate waste coffee dregs is first added bamboo pulp as raw material by system, add oxidation methyl agate beautiful jade solvent again, after making its phase mixed dissolution become mucus, with dry spray wet-spinning, this mucus is squeezed out from spinning mouth, and in coagulating bath, solidify regeneration silk, finally by washing, dry, oil and batch supervisor after, can obtain and there is natural antibacterial, deodorizing and anion function bamboo cellulose fibre.This patent adopts novel dissolvent method sky silk technique to prepare cellulose fibre, due to the recoverable not only spinning technique environmental protection of solvent, but also effectively make use of discarded coffee grounds as functional additive, but the production cost of fiber is higher, is unfavorable for that large batch of industrialization is produced and promotes.
Application number be 200680008036.8 PCT patent discloses a kind of deodorizing and antibacterial fiber product, the invention provides the deodorizing and antibacterial fiber product of cancrinite class mineral, clay mineral, coniferous tree bleached kraft pulp and the bleached hardwood kraft pulp comprised containing the metal with antibiotic property.Application number be 201210349910.1 Chinese patent disclose one and to disappear bad smell of perspiration viscose and preparation method thereof, the invention belongs to technical field of fiber preparation, relate to silicate mineral and acid, functional viscose fiber that salt amphiprotic substance is produced, particularly a kind of bad smell of perspiration viscose and preparation method thereof that disappears containing short rayon fiber and viscose filament yarn.Utilize natural aluminosilicate for deodorization absorbent is to prepare cellulose fibre although above patent all belongs to, if adopt traditional cellulose fiber terylene short fiber production technology, as knowledge, pulp is through soda-dip, add alkali lye after carbon disulfide yellow and make rayon spinning liquid, through deaeration, adopt wet spinning spinning process shaping after maturation, coagulating bath is sulfuric acid, the existence of a large amount of acid-alkali salt will certainly cause the loss of the effective mineral matter of major part, the antibacterial and deodouring having badly influenced finished fiber is functional, test shows, adding the fine content of first from rear dissolving is 7% aluminosilicate powder, mix rear spinning after refining procedure, the content adopting residue on ignition method to detect aluminosilicate in final fiber is about 1.9%, aluminosilicate active principle more than 5% is run off by NaOH and sulfuric acid decomposition.
Summary of the invention
First technical problem to be solved by this invention is: the deficiency existed for prior art, provides the cellulose fibre that a kind of wearability is excellent, textile process performance is good, it is antibacterial to resist and deodorization functions is given prominence to.
Second technical problem to be solved by this invention is: the deficiency existed for prior art, when not affecting normal spinning, bamboo charcoal nano pulp is added from rear dissolving and stirs, alumino-silicate powder is made slow-release microcapsule, employing is spun front injection system and is added before spinning, the existence of microcapsules avoids that strong acid-base directly contacts alumino-silicate and the active principle that causes decomposes and runs off and structural deterioration, in fabric, alumino-silicate microcapsules discharge active ingredient slowly along with acid bath is shaping or friction is broken, bamboo charcoal nano powder adsorb peculiar smell, play Long-term Anti antibacterial, the effect of deodorizing, and the fibre wearability produced is excellent, the preparation method of the antibacterial and deodouring cellulose fibre that textile process performance is good.
Technical solution of the present invention is, following a kind of antibacterial and deodouring cellulose fibre is provided, aluminosilicate slow-release microcapsule containing 1 ~ 10wt% in described fiber, bamboo charcoal nano-powder containing 1 ~ 5wt%, the dry fracture strength of described fiber is 1.80 ~ 2.60cN/dtex, wet breaking strength is 0.90 ~ 1.50cN/dtex, dry elongation at break is 16 ~ 22%, to ammonia removal rate >=92.0%, acetic acid clearance >=92.0%, isovaleric acid clearance >=93.0%, bactericidal activity logarithm value >=0, bacteriostatic activity logarithm value >=2.
A preparation method for antibacterial and deodouring cellulose fibre, step comprises: the preparation of modified rayon and spinning and post processing, add aluminosilicate slow-release microcapsule in described spinning and last handling process.
Concrete technology step is as follows:
(1) preparation of modified rayon: take cellulose pulp as raw material, viscose glue is obtained through comprising dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step, in dissolving step, add the denaturant accounting for chemical cellulose 0.5 ~ 1.2wt% in viscose glue, add bamboo charcoal nano pulp stirring 2 ~ 4h and obtain modified rayon;
(2) spinning and post processing: by spinning front injecting systems, aluminosilicate microcapsules are joined blender by measuring pump, modified rayon liquid joins blender by viscose glue flowmeter simultaneously, mix rear quick introducing coagulating bath spinning moulding, then obtain antibacterial and deodouring cellulose fibre through strand drawing-off and post-processing step.
As preferably, described coagulating bath comprises sulfuric acid 80 ~ 130g/l, zinc sulfate 8 ~ 13.5g/l, sodium sulphate 320 ~ 350g/l.
As preferably, the preparation of described bamboo charcoal nano pulp is that to join concentration be in the sodium hydroxide solution of 4.0 ~ 6.0wt% for the bamboo-carbon powder of 200 ~ 900 nanometers by particle diameter, stir 40 ~ 60 minutes at the temperature of 40 ± 3 DEG C, dispersant is added after filtration, add that quality is bamboo charcoal nano-powder quality 0.02 ~ 0.10% of dispersant, stir after 60 ~ 80 minutes under the high speed rotating of 500 ~ 1000 turns/min, obtain the stable slurry containing bamboo-carbon powder 30 ~ 40wt%.
As preferably, the preparation of described aluminosilicate slow-release microcapsule comprises:
(1) preliminary treatment: natural aluminosilicate being joined concentration is in the aqueous slkali of 3.0 ~ 5.0wt%, soak at the temperature of 32 ± 2 DEG C after 30 ~ 40 minutes, then wash when temperature is 40 ± 2 DEG C, dry at the temperature of 80 ± 3 DEG C after filtration, the aluminosilicate powder of last precomminution to 0.9 ~ 1.8 micron;
(2) preparation of slow-release microcapsule: gelatin and soft water in proportion 1:24 ~ 30 add in reactor, control temperature 80 ~ 86 DEG C of heating for dissolving, then 50 ± 1 DEG C are cooled to, slowly add aluminosilicate powder prepared by preliminary treatment afterwards, use high speed dispersor high-speed stirred, mixing speed is 100 ~ 150 revolutions per seconds, adjust ph is to acid, reaction 15 ~ 20min, be cooled to 10 ~ 12 DEG C of Post RDBMS, adjust ph is to alkalescence, reaction 40 ~ 50min, reduce mixing speed to 10 ~ 15 revolutions per second, after reaction 60 ~ 80min, suction filtration obtains " containing microcapsules 25 ~ 30wt%, particle diameter D90≤2.0 micron, be greater than particle≤1% of 4 microns, core wall is than for 3:1 " homogeneous latex emulsion.
As preferably, described dispersant is neopelex.
As preferably, described denaturant is alkyl polyamine.
Adopt the beneficial effect of the technical program: in antibacterial and deodouring cellulose fibre of the present invention, the content of alumino-silicate active ingredient runs off less, add the adsorption function that bamboo charcoal nano-powder is powerful, anti-antibacterial, the deodorization functions more lasting stability of finished fiber, therefore the absorption of the existing native cellulose fibre of antibacterial and deodouring cellulose fibre of the present invention breathe freely, comfortable and easy to wear, discarded after can the advantage of natural degradation, have again anti-antibacterial, deodorization functions is strong, effect is lasting advantage.
Detailed description of the invention
For ease of illustrating, below antibacterial and deodouring cellulose fibre of the present invention and preparation method thereof is elaborated.
Embodiment 1:
Preparation 0.78dtex × 32mm antibacterial and deodouring cellulose fibre:
(1) bamboo charcoal nano pulp is prepared for subsequent use
The preparation of bamboo charcoal nano pulp is that 200 ~ 900 bamboo charcoal nano powders join in the sodium hydroxide solution of 5.0wt% by particle diameter, be stir 45 minutes under the condition of 41 DEG C in temperature, dispersant DBSA is added after filtration, the quality adding dispersant is the 0.08wt% of bamboo charcoal nano-powder quality, stir under 800 turns/min rotating speed after 70 minutes, obtain the stable slurry containing bamboo-carbon powder 35wt%, i.e. bamboo charcoal nano pulp.
(2) aluminosilicate slow-release microcapsule is prepared for subsequent use
The preparation of aluminosilicate slow-release microcapsule comprises:
(1) preliminary treatment: natural aluminosilicate is joined in the aqueous slkali of 4.0wt%, be 32 DEG C in temperature and soak after 35 minutes, be 41 DEG C in temperature and wash, dry after filtration at 80 DEG C, then precomminution is to the aluminosilicate powder of D90=1.8 micron;
(2) preparation of slow-release microcapsule: gelatin and soft water in proportion 1:27 add in reactor, control temperature 85 DEG C of heating for dissolving, then 51 DEG C are cooled to, slowly add aluminosilicate powder prepared by preliminary treatment afterwards, use high speed dispersor high-speed stirred, mixing speed is 120 revolutions per seconds, adjust ph is to acid, reaction 18min, solidification is added after being cooled to 11 DEG C, adjust ph is to alkalescence, reaction 45min, reduce mixing speed to 10 revolutions per second, after reaction 70min, suction filtration obtains containing " microcapsules 28wt%, particle diameter D90≤2.0 micron, be greater than particle≤1% of 4 microns, core wall is than for 3:1 " homogeneous latex emulsion, i.e. aluminosilicate spansule.
The preparation method of preparation 0.78dtex × 32mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: take cellulose pulp as raw material, viscose glue is obtained through comprising dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step, in dissolving step, add the denaturant alkyl polyamine accounting for chemical cellulose 0.8wt% in viscose glue, add the above-mentioned bamboo charcoal nano pulp for preparing of the 2wt% accounting for finished fiber quality and stir 3h and obtain modified rayon.
2. spinning and post processing: by spinning front injecting systems, the above-mentioned aluminosilicate microcapsules prepared are joined blender by measuring pump, aluminosilicate microcapsules account for the 8wt% of finished fiber quality, modified rayon liquid joins blender by viscose glue flowmeter simultaneously, mix rear quick introducing coagulating bath spinning moulding, described coagulating bath consist of sulfuric acid 90g/l, zinc sulfate 11.5g/l, sodium sulphate 330g/l, then obtain antibacterial and deodouring cellulose fibre through strand drawing-off and post-processing step.
Through detecting 0.78dtex × 32mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 1 obtains, wherein the testing result of leading indicator is as shown in following table:
Note: the antibacterial value described in upper table and sterilizing value are according to Japanese Industrial Standards JISL1902:2008.
Embodiment 2:
Preparation 1.11dtex × 32mm antibacterial and deodouring cellulose fibre:
(1) bamboo charcoal nano pulp is prepared for subsequent use
The preparation of bamboo charcoal nano pulp is that 200 ~ 900 bamboo charcoal nano powders join in the sodium hydroxide solution of 4.0wt% by particle diameter, stir 60 minutes at 40 DEG C, add dispersant after filtration and enter DBSA, dispersant add the 0.10wt% that quality is bamboo charcoal nano-powder quality, stir under 500 turns/min rotating speed after 80 minutes, obtain the stable slurry containing bamboo-carbon powder 30wt%, i.e. bamboo charcoal nano pulp.
(2) aluminosilicate slow-release microcapsule is prepared for subsequent use
The preparation of aluminosilicate slow-release microcapsule comprises:
(1) preliminary treatment: natural aluminosilicate is joined in the aqueous slkali of 3.0wt%, be 30 DEG C in temperature and soak after 30 minutes, be 38 DEG C in temperature and wash, dry after filtration at 77 DEG C, then precomminution is to the aluminosilicate powder of D90=1.2 micron;
(2) preparation of slow-release microcapsule: gelatin and soft water in proportion 1:24 add in reactor, control temperature 82 DEG C of heating for dissolving, then 49 DEG C are cooled to, slowly add aluminosilicate powder prepared by preliminary treatment afterwards, use high speed dispersor high-speed stirred, speed is 150 revolutions per seconds, adjust ph is to acid, reaction 20min, solidification is added after being cooled to 10 DEG C, adjust ph is to alkalescence, reaction 40min, reduce mixing speed to 12 revolutions per second, after reaction 80min, suction filtration obtains " containing microcapsules 30wt%, particle diameter D90≤2.0 micron, be greater than particle≤1% of 4 microns, core wall is than for 3:1 " homogeneous latex emulsion, i.e. aluminosilicate spansule.
The preparation method of preparation 1.11dtex × 32mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: take cellulose pulp as raw material, viscose glue is obtained through comprising dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step, in dissolving step, add the denaturant alkyl polyamine accounting for chemical cellulose 0.5wt% in viscose glue, add the above-mentioned bamboo charcoal nano pulp stirring 2h prepared of the 1wt% accounting for finished fiber quality and obtain modified rayon.
2. spinning and post processing: by spinning front injecting systems, the above-mentioned aluminosilicate microcapsules prepared are joined blender by measuring pump, aluminosilicate microcapsules account for the 1wt% of finished fiber quality, modified rayon liquid joins blender by viscose glue flowmeter simultaneously, mix rear quick introducing coagulating bath spinning moulding, described coagulating bath consist of sulfuric acid 120g/l, zinc sulfate 8.5g/l, sodium sulphate 320g/l, then obtain antibacterial and deodouring cellulose fibre through strand drawing-off and post-processing step.
Through detecting 1.11dtex × 32mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 2 obtains, wherein the testing result of leading indicator is as shown in following table:
Note: the antibacterial value described in upper table and sterilizing value are according to Japanese Industrial Standards JISL1902:2008.
Embodiment 3:
Preparation 1.33dtex × 38mm antibacterial and deodouring cellulose fibre:
(1) bamboo charcoal nano pulp is prepared for subsequent use
The preparation of bamboo charcoal nano pulp is that 200 ~ 900 bamboo charcoal nano powders join in the sodium hydroxide solution of 6.0wt% by particle diameter, stir 50 minutes at 43 DEG C, dispersant DBSA is added after filtration, dispersant add the 0.02wt% that quality is bamboo charcoal nano-powder quality, stir under 600 turns/min rotating speed after 60 minutes, obtain the stable slurry containing bamboo-carbon powder 40wt%, i.e. bamboo charcoal nano pulp.
(2) aluminosilicate slow-release microcapsule is prepared for subsequent use
The preparation of aluminosilicate slow-release microcapsule comprises:
(1) preliminary treatment: natural aluminosilicate is joined in the aqueous slkali of 5.0wt%, be 34 DEG C in temperature and soak after 40 minutes, be 42 DEG C in temperature and wash, dry after filtration at 83 DEG C, then precomminution is to the aluminosilicate powder of D90=1.6 micron;
(2) preparation of slow-release microcapsule: gelatin and soft water in proportion 1:30 add in reactor, control temperature 80 DEG C of heating for dissolving, then 50 DEG C are cooled to, slowly add aluminosilicate powder prepared by preliminary treatment afterwards, use high speed dispersor high-speed stirred, speed is 100 revolutions per seconds, adjust ph is to acid, reaction 15min, solidification is added after being cooled to 12 DEG C, adjust ph is to alkalescence, reaction 50min, reduce mixing speed to 15 revolutions per second, after reaction 60min, suction filtration obtains " containing microcapsules 25wt%, particle diameter D90≤2.0 micron, be greater than particle≤1% of 4 microns, core wall is than for 3:1 " homogeneous latex emulsion, i.e. aluminosilicate spansule.
The preparation method of preparation 1.33dtex × 38mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: take cellulose pulp as raw material, viscose glue is obtained through comprising dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step, in dissolving step, add the denaturant alkyl polyamine accounting for chemical cellulose 1.2wt% in viscose glue, add the above-mentioned bamboo charcoal nano pulp stirring 4h prepared of the 4wt% accounting for finished fiber quality and obtain modified rayon.
2. spinning and post processing: by spinning front injecting systems, the above-mentioned aluminosilicate microcapsules prepared are joined blender by measuring pump, aluminosilicate microcapsules account for the 7wt% of finished fiber quality, modified rayon liquid joins blender by viscose glue flowmeter simultaneously, mix rear quick introducing coagulating bath spinning moulding, described coagulating bath consist of sulfuric acid 80g/l, zinc sulfate 10.5g/l, sodium sulphate 340g/l, then obtain antibacterial and deodouring cellulose fibre through strand drawing-off and post-processing step.
Through detecting 1.33dtex × 38mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 3 obtains, wherein the testing result of leading indicator is as shown in following table:
Note: the antibacterial value described in upper table and sterilizing value are according to Japanese Industrial Standards JISL1902:2008.
Embodiment 4:
Preparation 1.67dtex × 38mm antibacterial and deodouring cellulose fibre:
(1) bamboo charcoal nano pulp is prepared for subsequent use
The preparation of bamboo charcoal nano pulp is that 200 ~ 900 bamboo charcoal nano powders join in the sodium hydroxide solution of 6.0wt% by particle diameter, stir 50 minutes at 43 DEG C, dispersant DBSA is added after filtration, dispersant add the 0.02wt% that quality is bamboo charcoal nano-powder quality, stir under 900 turns/min rotating speed after 60 minutes, obtain the stable slurry containing bamboo-carbon powder 40wt%, i.e. bamboo charcoal nano pulp.
(2) aluminosilicate slow-release microcapsule is prepared for subsequent use
The preparation of aluminosilicate slow-release microcapsule comprises:
(1) preliminary treatment: natural aluminosilicate is joined in the aqueous slkali of 5.0wt%, be 34 DEG C in temperature and soak after 40 minutes, be 42 DEG C in temperature and wash, dry after filtration at 83 DEG C, then precomminution is to the aluminosilicate powder of D90=1.6 micron;
(2) preparation of slow-release microcapsule: gelatin and soft water in proportion 1:30 add in reactor, control temperature 80 DEG C of heating for dissolving, then 50 DEG C are cooled to, slowly add aluminosilicate powder prepared by preliminary treatment afterwards, use high speed dispersor high-speed stirred, speed is 100 revolutions per seconds, adjust ph is to acid, reaction 15min, solidification is added after being cooled to 12 DEG C, adjust ph is to alkalescence, reaction 50min, reduce mixing speed to 14 revolutions per second, after reaction 60min, suction filtration obtains " containing microcapsules 25wt%, particle diameter D90≤2.0 micron, be greater than particle≤1% of 4 microns, core wall is than for 3:1 " homogeneous latex emulsion, i.e. aluminosilicate spansule.
The preparation method of preparation 1.67dtex × 38mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: take cellulose pulp as raw material, viscose glue is obtained through comprising dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step, in dissolving step, add the denaturant alkyl polyamine accounting for chemical cellulose 1.2wt% in viscose glue, add the above-mentioned bamboo charcoal nano pulp stirring 4h prepared of the 4wt% accounting for finished fiber quality and obtain modified rayon.
2. spinning and post processing: by spinning front injecting systems, the above-mentioned aluminosilicate microcapsules prepared are joined blender by measuring pump, aluminosilicate microcapsules account for the 7wt% of finished fiber quality, modified rayon liquid joins blender by viscose glue flowmeter simultaneously, mix rear quick introducing coagulating bath spinning moulding, described coagulating bath consist of sulfuric acid 80g/l, zinc sulfate 10.5g/l, sodium sulphate 340g/l, then obtain antibacterial and deodouring cellulose fibre through strand drawing-off and post-processing step.
Through detecting 1.67dtex × 38mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 4 obtains, wherein the testing result of leading indicator is as shown in following table:
Note: the antibacterial value described in upper table and sterilizing value are according to Japanese Industrial Standards JISL1902:2008.
Embodiment 5:
Preparation 2.22dtex × 51mm antibacterial and deodouring cellulose fibre:
(1) bamboo charcoal nano pulp is prepared for subsequent use
The preparation of bamboo charcoal nano pulp is that 200 ~ 900 bamboo charcoal nano powders join in the sodium hydroxide solution of 4.4wt% by particle diameter, stir 58 minutes at 42 DEG C, DBSA dispersant is added after filtration, quality is the 0.03wt% of bamboo charcoal nano-powder quality, stir under 1000 turns/min rotating speed after 72 minutes, obtain the stable slurry containing bamboo-carbon powder 32wt%, i.e. bamboo charcoal nano pulp.
(2) aluminosilicate slow-release microcapsule is prepared for subsequent use:
The preparation of aluminosilicate slow-release microcapsule comprises:
(1) preliminary treatment: natural aluminosilicate is joined in the aqueous slkali of 3.7wt%, be 33 DEG C in temperature and soak after 34 minutes, be 39 DEG C in temperature and wash, dry after filtration at 79 DEG C, then precomminution is to the aluminosilicate powder of D90=1.3 micron;
(2) preparation of slow-release microcapsule: gelatin and soft water in proportion 1:29 add in reactor, control temperature 82 DEG C of heating for dissolving, then 49 DEG C are cooled to, slowly add aluminosilicate powder prepared by preliminary treatment afterwards, use high speed dispersor high-speed stirred, speed is 135 revolutions per seconds, adjust ph is to acid, reaction 17min, solidification is added after being cooled to 11 DEG C, adjust ph is to alkalescence, reaction 48min, reduce mixing speed to 13 revolutions per second, after reaction 75min, suction filtration obtains " containing microcapsules 27wt%, particle diameter D90≤2.0 micron, be greater than particle≤1% of 4 microns, core wall is than for 3:1 " homogeneous latex emulsion, i.e. aluminosilicate spansule.
The preparation method of preparation 2.22dtex × 51mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: take cellulose pulp as raw material, viscose glue is obtained through comprising dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step, in dissolving step, add the denaturant alkyl polyamine accounting for chemical cellulose 0.9wt% in viscose glue, add the above-mentioned bamboo charcoal nano pulp stirring 2.5h prepared of the 3wt% accounting for finished fiber quality and obtain modified rayon.
2. spinning and post processing: by spinning front injecting systems, above-mentioned prepare aluminosilicate microcapsules are joined blender by measuring pump, aluminosilicate microcapsules account for the 8wt% of finished fiber quality, modified rayon liquid joins blender by viscose glue flowmeter simultaneously, mix rear quick introducing coagulating bath spinning moulding, described coagulating bath consist of sulfuric acid 105g/l, zinc sulfate 10.5g/l, sodium sulphate 330g/l, then obtain antibacterial and deodouring cellulose fibre through strand drawing-off and post-processing step.
Through detecting 2.22dtex × 51mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 5 obtains, wherein the testing result of leading indicator is as shown in following table:
Note: the antibacterial value described in upper table and sterilizing value are according to Japanese Industrial Standards JISL1902:2008.
Embodiment 6:
Preparation 3.33dtex × 60mm antibacterial and deodouring cellulose fibre:
(1) bamboo charcoal nano pulp is prepared for subsequent use
The preparation of bamboo charcoal nano pulp is that 200 ~ 900 bamboo charcoal nano powders join in the sodium hydroxide solution of 4.9wt% by particle diameter, stir 49 minutes at 42 DEG C, DBSA dispersant is added after filtration, quality is the 0.09wt% of bamboo charcoal nano-powder quality, stir under 700 turns/min rotating speed after 71 minutes, obtain the stable slurry containing bamboo-carbon powder 32.6wt%, i.e. bamboo charcoal nano pulp.
(2) aluminosilicate slow-release microcapsule is prepared for subsequent use
The preparation of aluminosilicate slow-release microcapsule comprises:
(1) preliminary treatment: natural aluminosilicate is joined in the aqueous slkali of 4.1wt%, be 33 DEG C in temperature and soak after 36 minutes, be 40 DEG C in temperature and wash, dry after filtration at 82 DEG C, then precomminution is to the aluminosilicate powder of D90=0.9 micron;
(2) preparation of slow-release microcapsule: gelatin and soft water in proportion 1:25 add in reactor, control temperature 83 DEG C of heating for dissolving, then 51 DEG C are cooled to, slowly add aluminosilicate powder prepared by preliminary treatment afterwards, use high speed dispersor high-speed stirred, speed is 143 revolutions per seconds, adjust ph is to acid, reaction 18min, solidification is added after being cooled to 11 DEG C, adjust ph is to alkalescence, reaction 43min, reduce mixing speed to 11 revolutions per second, after reaction 75min, suction filtration obtains " containing microcapsules 27wt%, particle diameter D90≤2.0 micron, be greater than particle≤1% of 4 microns, core wall is than for 3:1 " homogeneous latex emulsion, i.e. aluminosilicate spansule.
The preparation method of preparation 3.33dtex × 60mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: take cellulose pulp as raw material, viscose glue is obtained through comprising dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step, in dissolving step, add the denaturant alkyl polyamine accounting for chemical cellulose 1.1wt% in viscose glue, add the above-mentioned bamboo charcoal nano pulp stirring 3.6h prepared of the 5wt% accounting for finished fiber quality and obtain modified rayon.
2. spinning and post processing: by spinning front injecting systems, the above-mentioned aluminosilicate microcapsules prepared are joined blender by measuring pump, aluminosilicate microcapsules account for the 10wt% of finished fiber quality, modified rayon liquid joins blender by viscose glue flowmeter simultaneously, mix rear quick introducing coagulating bath spinning moulding, described coagulating bath consist of sulfuric acid 113g/l, zinc sulfate 12.5g/l, sodium sulphate 348g/l, then obtain antibacterial and deodouring cellulose fibre through strand drawing-off and post-processing step.
Through detecting 3.33dtex × 60mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 6 obtains, wherein the testing result of leading indicator is as shown in following table:
Note: the antibacterial value described in upper table and sterilizing value are according to Japanese Industrial Standards JISL1902:2008.
Through detecting the antibacterial and deodouring cellulose fibre prepared by above-described embodiment 1 ~ 5, the dry fracture strength of prepared cellulose fibre is 1.80 ~ 2.60cN/dtex, wet breaking strength is 0.90 ~ 1.50cN/dtex, dry elongation at break is 16 ~ 22%, to ammonia removal rate >=92.0%, and acetic acid clearance >=92.0%, isovaleric acid clearance >=93.0%, bactericidal activity logarithm value >=0, bacteriostatic activity logarithm value >=2, all meet instructions for use.In addition, although the specification of the cellulose fibre prepared by embodiment 1 ~ 5 is different, the analysis found that, the short fiber of cellulose cost prepared by embodiment 4 drops into lower, and the cellulose fibre combination property of preparation is the highest, is a kind of production and processing method of optimum.
In the above-described embodiments, preferred forms of the present invention is described, obviously, under inventive concept of the present invention, still can make a lot of change.At this, should illustrate, any change made under inventive concept of the present invention all will fall within the scope of protection of the present invention.
Claims (4)
1. an antibacterial and deodouring cellulose fibre, is characterized in that: the aluminosilicate slow-release microcapsule containing 1 ~ 10wt% in described fiber, the bamboo charcoal nano-powder containing 1 ~ 5wt%,
The preparation of described aluminosilicate slow-release microcapsule comprises:
(1) preliminary treatment: natural aluminosilicate being joined concentration is in the aqueous slkali of 3.0 ~ 5.0wt%, soak at the temperature of 32 ± 2 DEG C after 30 ~ 40 minutes, then wash when temperature is 40 ± 2 DEG C, dry at the temperature of 80 ± 3 DEG C after filtration, the aluminosilicate powder of last precomminution to 0.9 ~ 1.8 micron;
(2) preparation of slow-release microcapsule: gelatin and soft water in proportion 1:24 ~ 30 add in reactor, control temperature 80 ~ 86 DEG C of heating for dissolving, then 50 ± 1 DEG C are cooled to, slowly add aluminosilicate powder prepared by preliminary treatment afterwards, use high speed dispersor high-speed stirred, mixing speed is 100 ~ 150 revolutions per seconds, adjust ph is to acid, reaction 15 ~ 20min, be cooled to 10 ~ 12 DEG C of Post RDBMS, adjust ph, to alkalescence, reacts 40 ~ 50min, reduce mixing speed to 10 ~ 15 revolutions per second, after reaction 60 ~ 80min, suction filtration obtains the homogeneous latex emulsion of slow-release microcapsule;
The aluminosilicate slow-release microcapsule of described preparation is containing microcapsules 25 ~ 30wt%, particle diameter D90≤2.0 micron, is greater than particle≤1% of 4 microns, and core wall is than being 3:1.
2. antibacterial and deodouring cellulose fibre according to claim 1, is characterized in that: the dry fracture strength of described fiber is 1.80 ~ 2.60cN/dtex, and wet breaking strength is 0.90 ~ 1.50cN/dtex, and dry elongation at break is 16 ~ 22%.
3. antibacterial and deodouring cellulose fibre according to claim 2, is characterized in that: described fiber to ammonia removal rate >=92.0%, acetic acid clearance >=92.0%, isovaleric acid clearance >=93.0%.
4. antibacterial and deodouring cellulose fibre according to claim 3, is characterized in that: described fiber bactericidal activity logarithm value >=0, bacteriostatic activity logarithm value >=2.
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| CN105123749B (en) * | 2015-06-16 | 2018-11-13 | 浙江工业大学 | A kind of modification bamboo charcoal composite material and its application in preparing antiseptic |
| CN106637456A (en) * | 2015-07-24 | 2017-05-10 | 众地家纺有限公司 | Antibacterial, deodorant and efficient deodorizing cellulose fibers and preparation method thereof |
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| CN106757460B (en) * | 2016-11-30 | 2020-05-22 | 中科纺织研究院（青岛）有限公司 | Regenerated cellulose fiber containing active ingredients and capable of inhibiting aged odor and preparation method of regenerated cellulose fiber |
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| TWI706975B (en) * | 2018-12-25 | 2020-10-11 | 南亞塑膠工業股份有限公司 | Deodorizing fiber and its deodorizing masterbatch |
| CN110359108A (en) * | 2019-08-05 | 2019-10-22 | 北京宇田相变储能科技有限公司 | A kind of functional fiber cellulose fiber and the preparation method and application thereof |
| CN110468466A (en) * | 2019-08-16 | 2019-11-19 | 上海昕亚新材料科技有限公司 | A kind of fiber containing the removable active substance microcapsule of shell material |
| CN110843275B (en) * | 2019-11-29 | 2021-12-10 | 广州市新荔缘鞋业有限公司 | Preparation method of high-breathability antibacterial functional composite fabric |
| CN112914174B (en) * | 2021-01-26 | 2023-06-30 | 成都中医药大学 | Antibacterial deodorizing mask and preparation method thereof |
| CN117942281B (en) * | 2024-03-14 | 2024-06-14 | 广州天玺生物科技有限公司 | Double-coating system for inhibiting or preventing metal ions from overflowing and preparation method and application thereof |
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Address after: 266001 room 2204, block B, Jinhua apartment, 100 Nanjing Road, Shinan District, Qingdao, Shandong. Patentee after: Aoshima Yoshikanon Technology Co., Ltd. Address before: 266001 room 2204, block B, Jinhua apartment, 100 Nanjing Road, Shinan District, Qingdao, Shandong. Patentee before: Qingdao Jia Shenglong trade Co., Ltd |
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Denomination of invention: Antibacterial and deodorization cellulosic fiber and preparation method thereof Effective date of registration: 20181015 Granted publication date: 20160113 Pledgee: Qingdao high technology financing Company limited by guarantee Pledgor: Aoshima Yoshikanon Technology Co., Ltd. Registration number: 2018370010110 |
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