Background technology
Along with social progress and the raising of people's living standard, the idea of people's dressing is also constantly being upgraded, and the Comfortable attractive of the functional and product to textiles is had higher requirement.And the production of the natural fabrics such as cotton, fiber crops, silk, hair due to be subject to natural climate and grain and cotton strive ground contradiction impact, 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 a little fiber that is made at present.Along with deepening continuously that the mankind are familiar with nature, cellulosic utilization also will expand gradually.In contrast to this, synthetic fiber are mainly to be produced by the raw material (oil, coal, natural gas etc.) that the different geologic(al) periods form, 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 constantly natural synthetic with huge speed.
21 century is the further protection of the environment of requirement and the epoch of making rational use of resources.Cellulose fibre is owing to being changed into steam and carbon dioxide by biological decomposition or safe combustion, and the welding problem being caused by discarded object is few.As can be seen here, no matter from the degree of enriching of resource, from the processing of discarded object, and many-sidedly consider from the comfortableness of dress and elegant in appearance grade, it is very necessary developing cellulose fibre.
At present China's viscose kind majority is general fibre, and functional fiber, fibre in differentiation are little.Though the domestic production technology of having grasped coloured fiber, fire resistance fibre, superfine denier fiber, the producer that forms mass production capabilities is few.According to insider analyze, China's fibre in differentiation quality with quantitatively with still have gap abroad.At present domestic because plurality of raw materials can not meet the needs of export market, 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) of seeing in the market, substantially adopt three kinds of methods to produce: the one, first antiseptic is added and in spinning material, make anti-bacterial fibre, then make various antibacterial fabrics, this method is commonly used to produce chemical synthetic fiber series products; The 2nd, after fabric printing, in arrangement process, add antiseptic (being often called as antibacterial finishing agent), then make various antibacterial fabrics, this method both can have been produced pure natural fiber or pure chemistry synthetic fiber series products, also can produce blend fibre series products, wide adaptability, therefore the production of most antibacterial fabrics is to adopt in this way; The 3rd, first antiseptic is added and in spinning material, make anti-bacterial fibre, then in arrangement process, add antibacterial finishing agent after fabric printing, then make various antibacterial fabrics, this method is only used in the specialities with very high antibacterial performance requirement.
The antimicrobial technology of China has obtained larger development at present, but antimicrobial product also exists some problems, most organic antiseptics all have certain excitant and toxic and side effect to human body skin, and mineral-type antiseptic often contains heavy metal ion, very easily, by contacting and be absorbed by the body with human body skin, the health of human body is caused to very big harm.
Can solve better antibacterial wide spectrum problem, develop the antiseptic of wide spectrum more, improve antibacterial durability, make fabric through repeatedly washing and still there is good antibacterial effect, the breeding of anti-bacteria selectively also makes 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 for antiseptic carries out the antibacterial deodourizing processing of textiles, met the requirement of textiles safety, health 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 having produced, and causes and is difficult to penetration and promotion.
Application number is that 200510073503.2 Chinese patent discloses a kind of deodorization fiber and preparation method thereof, comprise the steps: by phthalocyanine iron with without adding dioxide photocatalyst titanium after crystallization water alumina silicate mixed grinding, be uniformly mixed and add polypropylene and EVA resin and stir with the coupling agent preparing, add surfactant and dispersant, stir to make after the concentrated master batch of deodorant is dried and mix through melt spinning and make deodorization fiber with carrier polypropylene.Application number is that 201110219501.5 Chinese patent discloses a kind of antibacterial and deodouring modified polyester fibre, by PET section and antiseptic-antibacterial zeolite particles, deodorant is formed and is mixed by phthalocyanine iron, alumina silicate and dioxide photocatalyst titanium, the deodorant of the antiseptic of 4-10% and 10-15% is joined in PET section in 200-230 DEG C, produce by common terylene chips spinning process and flow process, make antibacterial and deodouring modified polyester fibre product.Application number is 201210098266.5 Chinese patent, a kind of deodorizing polyamide fiber and preparation method thereof is disclosed, 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 with deodorization functions is reacted with polyamide fiber, make the carboxyl in hydroxyl and the polyamide molecule in 2-bromo-2-nitro-1,3-propylene glycol molecule carry out condensation reaction, and then obtain having the polyamide fiber of deodorization functions.
Disclosed deodorizing antibiotic fibrid all belongs to the category of synthetic fiber above, 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 are powerful outstanding, sucting wet air permeability is poor, wears uncomfortable property, and 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 00803554.7 PCT patent, a kind of deodorization fiber and preparation method thereof is disclosed, adopt treatment fluid to contain the de-chitin of acetyl and/or the deacetyl chitin of modification, carboxylic acid polyalcohol, zinc oxide and binder resin are processed native cellulose or synthetic fiber.Application number is that 00805580.7 PCT patent discloses a kind of fibrous structure thing with deodorizing or antibiotic property, has composite oxides that titanium and silicon forms and the fibrous structure thing of adhesive on fiber surface.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 that is main component with silica, zinc oxide or titanium dioxide, and organic antibacterial agent is row Quaternary Silicone Polymers class antiseptic.
Disclosed deodorizing antibiotic fibrid all belongs to fabric post-treatment technique above, although the antibacterial and deodouring function ratio of rear finish fabric is better, price also relatively cheap being convenient to is promoted, and washability is poor, because the feel that has fabric of adhesive is hardened, be not suitable for very much making the underclothes in summer.
Application number is that 201310097045.0 Chinese patent discloses a kind of method for making with natural antibacterial, deodorizing and anion function bamboo cellulose fibre, system first adds bamboo pulp as raw material appropriate waste coffee dregs, add again oxidation methyl agate beautiful jade solvent, its phase mixed dissolution is become after mucus, to do spray wet-spinning, this mucus is squeezed out from spin mouth, and in coagulating bath, solidify regeneration silk, there is natural antibacterial, deodorizing and anion function bamboo cellulose fibre finally by washing, be dried, oil and batch after supervisor, can making.This patent is to adopt novel dissolvent method sky silk technique to prepare cellulose fibre, due to the not only spinning technique environmental protection of recoverable of solvent, but also effectively utilize discarded coffee grounds as functional additive, but the production cost of fiber is higher, be unfavorable for large batch of industrialization production popularization.
Application number is that 200680008036.8 PCT patent discloses a kind of deodorizing and antibacterial fiber product, the invention provides the deodorizing and antibacterial fiber product that comprises the cancrinite class mineral, clay mineral, coniferous tree bleached kraft pulp and the bleached hardwood kraft pulp that contain the metal with antibiotic property.Application number is that 201210349910.1 Chinese patent discloses the one bad smell of perspiration viscose and preparation method thereof that disappears, the invention belongs to fiber preparing technical field, relate to the functional viscose fiber of silicate mineral and acid, the production of salt amphiprotic substance, particularly a kind of bad smell of perspiration viscose and preparation method thereof that disappears containing short rayon fiber and viscose filament yarn.Although all belonging to, above patent utilize natural aluminosilicate to prepare cellulose fibre for deodorization absorbent, if adopt traditional cellulose fibre production technology, as knowledge, pulp floods through alkali lye, after carbon disulfide yellow, add alkali lye to make rayon spinning liquid, through deaeration, after maturation, adopt wet spinning spray silk technological forming, coagulating bath is sulfuric acid, the existence of a large amount of acid-alkali salts will certainly cause most of effectively loss of mineral matter, the antibacterial and deodouring that has 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 that adopts calcination residue method to detect aluminosilicate in final fiber is 1.9% left and right, exceeding 5% aluminosilicate active principle is decomposed and runs off by NaOH and sulfuric acid.
Summary of the invention
First technical problem to be solved by this invention is: the deficiency existing for prior art, provides that a kind of wearability is good, textile process performance is good, anti-antibacterial and cellulose fibre that deodorization functions is outstanding.
Second technical problem to be solved by this invention is: the deficiency existing for prior art, in the situation that not affecting normal spinning, bamboo charcoal nano pulp is added and stirred from rear dissolving, alumino-silicate powder is made to slow-release microcapsule, employing is spun front injection system and is added before spinning, the active principle that the existence of microcapsules has avoided strong acid-base to cause the direct contact of alumino-silicate decomposes loss and structural deterioration, in fabric, alumino-silicate microcapsules are along with acid bath moulding or friction are broken and discharged slowly active ingredient, bamboo charcoal nano powder absorption peculiar smell, play Long-term Anti antibacterial, the effect of deodorizing, and the fibre wearability of producing is good, 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, in described fiber, contain the aluminosilicate slow-release microcapsule of 1~10wt%, the bamboo charcoal nano-powder that contains 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: taking cellulose pulp as raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step make viscose glue, in dissolving step, add the denaturant that accounts for chemical cellulose 0.5~1.2wt% in viscose glue, add bamboo charcoal nano pulp to stir 2 ~ 4h and make modified rayon;
(2) spinning and post processing: by spinning front injecting systems, aluminosilicate microcapsules are joined to 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 bamboo-carbon powder that the preparation of described bamboo charcoal nano pulp is is 200 ~ 900 nanometers by particle diameter joins in the sodium hydroxide solution that concentration is 4.0 ~ 6.0wt%, at the temperature of 40 ± 3 DEG C, stir 40 ~ 60 minutes, after filtration, add dispersant, the quality that adds of dispersant is 0.02 ~ 0.10% of bamboo charcoal nano-powder quality, under the high speed rotating of turn 500 ~ 1000/min, stir after 60 ~ 80 minutes, 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 is joined in the aqueous slkali that concentration is 3.0~5.0wt%, at the temperature of 32 ± 2 DEG C, soak after 30~40 minutes, then in the time that being 40 ± 2 DEG C, temperature washes, after filtration, at the temperature of 80 ± 3 DEG C, dry 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 80 ~ 86 DEG C of heating for dissolving of temperature, then be cooled to 50 ± 1 DEG C, the aluminosilicate powder that slowly adds afterwards preliminary treatment to prepare, use high speed dispersor high-speed stirred, mixing speed is 100~150 revolutions per seconds, regulate pH value to acid, reaction 15 ~ 20 min, after being cooled to 10 ~ 12 DEG C, solidify, regulate pH value to alkalescence, reaction 40 ~ 50 min, reduce mixing speed to 10 ~ 15 revolutions per second, after reaction 60 ~ 80 min, 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 more lasting stability of deodorization functions of finished fiber, therefore the advantage that the absorption of the existing native cellulose fibre of antibacterial and deodouring cellulose fibre of the present invention can natural degradation after ventilative, comfortable and easy to wear, discarded, has again anti-antibacterial, deodorization functions is strong, effect is lasting advantage.
Detailed description of the invention
For ease of explanation, below antibacterial and deodouring cellulose fibre of the present invention and preparation method thereof is elaborated.
Embodiment 1:
Prepare 0.78 dtex × 32mm antibacterial and deodouring cellulose fibre:
(1) prepare bamboo charcoal nano pulp for subsequent use
The preparation of bamboo charcoal nano pulp is to be that 200 ~ 900 bamboo charcoal nano powders join in the sodium hydroxide solution of 5.0wt% by particle diameter, be to stir 45 minutes under the condition of 41 DEG C in temperature, after filtration, add dispersant DBSA, the quality that adds dispersant is the 0.08wt% of bamboo charcoal nano-powder quality, under 800 turn/min rotating speeds, stir after 70 minutes, obtain the stable slurry containing bamboo-carbon powder 35wt%, i.e. bamboo charcoal nano pulp.
(2) prepare aluminosilicate slow-release microcapsule 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 soak after 35 minutes in temperature, be 41 DEG C in temperature and wash, dry at 80 DEG C after filtration, 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 85 DEG C of heating for dissolving of temperature, then be cooled to 51 DEG C, the aluminosilicate powder that slowly adds afterwards preliminary treatment to prepare, use high speed dispersor high-speed stirred, mixing speed is 120 revolutions per seconds, regulate pH value to acid, reaction 18min, after being cooled to 11 DEG C, add curing, regulate pH value 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, it is aluminosilicate spansule.
Prepare the preparation method of 0.78 dtex × 32mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: taking cellulose pulp as raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step make viscose glue, in dissolving step, add the denaturant alkyl polyamine that accounts for chemical cellulose 0.8wt% in viscose glue, add to account for the above-mentioned bamboo charcoal nano pulp preparing of 2wt% of finished fiber quality and stir 3h to make modified rayon.
2. spinning and post processing: by spinning front injecting systems, the above-mentioned aluminosilicate microcapsules that prepare are joined to 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.
Detect through 0.78dtex × 32mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 1 is made, 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 the JIS L1902:2008 of Japanese Industrial Standards.
Embodiment 2:
Preparation 1.11dtex × 32mm antibacterial and deodouring cellulose fibre:
(1) prepare bamboo charcoal nano pulp for subsequent use
The preparation of bamboo charcoal nano pulp is to be 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, after filtration, add dispersant and enter DBSA, the quality that adds of dispersant is the 0.10wt% of bamboo charcoal nano-powder quality, under 500 turn/min rotating speeds, stir after 80 minutes, obtain the stable slurry containing bamboo-carbon powder 30wt%, i.e. bamboo charcoal nano pulp.
(2) prepare aluminosilicate slow-release microcapsule 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 soak after 30 minutes in temperature, be 38 DEG C in temperature and wash, dry at 77 DEG C after filtration, 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 82 DEG C of heating for dissolving of temperature, then be cooled to 49 DEG C, the aluminosilicate powder that slowly adds afterwards preliminary treatment to prepare, use high speed dispersor high-speed stirred, speed is 150 revolutions per seconds, regulate pH value to acid, reaction 20min, after being cooled to 10 DEG C, add curing, regulate pH value 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, it is aluminosilicate spansule.
The preparation method of preparation 1.11dtex × 32mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: taking cellulose pulp as raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step make viscose glue, in dissolving step, add the denaturant alkyl polyamine that accounts for chemical cellulose 0.5wt% in viscose glue, add the above-mentioned bamboo charcoal nano pulp stirring 2h preparing of 1wt% that accounts for finished fiber quality to make modified rayon.
2. spinning and post processing: by spinning front injecting systems, the above-mentioned aluminosilicate microcapsules that prepare are joined to 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.
Detect through 1.11dtex × 32mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 2 is made, 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 the JIS L1902:2008 of Japanese Industrial Standards.
Embodiment 3:
Preparation 1.33dtex × 38mm antibacterial and deodouring cellulose fibre:
(1) prepare bamboo charcoal nano pulp for subsequent use
The preparation of bamboo charcoal nano pulp is to be 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, after filtration, add dispersant DBSA, the quality that adds of dispersant is the 0.02wt% of bamboo charcoal nano-powder quality, under 600 turn/min rotating speeds, stir after 60 minutes, obtain the stable slurry containing bamboo-carbon powder 40wt%, i.e. bamboo charcoal nano pulp.
(2) prepare aluminosilicate slow-release microcapsule 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 soak after 40 minutes in temperature, be 42 DEG C in temperature and wash, dry at 83 DEG C after filtration, 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 80 DEG C of heating for dissolving of temperature, then be cooled to 50 DEG C, the aluminosilicate powder that slowly adds afterwards preliminary treatment to prepare, use high speed dispersor high-speed stirred, speed is 100 revolutions per seconds, regulate pH value to acid, reaction 15min, after being cooled to 12 DEG C, add curing, regulate pH value 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, it is aluminosilicate spansule.
The preparation method of preparation 1.33dtex × 38mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: taking cellulose pulp as raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step make viscose glue, in dissolving step, add the denaturant alkyl polyamine that accounts for chemical cellulose 1.2wt% in viscose glue, add the above-mentioned bamboo charcoal nano pulp stirring 4h preparing of 4wt% that accounts for finished fiber quality to make modified rayon.
2. spinning and post processing: by spinning front injecting systems, the above-mentioned aluminosilicate microcapsules that prepare are joined to 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.
Detect through 1.33dtex × 38mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 3 is made, 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 the JIS L1902:2008 of Japanese Industrial Standards.
Embodiment 4:
Preparation 1.67dtex × 38mm antibacterial and deodouring cellulose fibre:
(1) prepare bamboo charcoal nano pulp for subsequent use
The preparation of bamboo charcoal nano pulp is to be 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, after filtration, add dispersant DBSA, the quality that adds of dispersant is the 0.02wt% of bamboo charcoal nano-powder quality, under 900 turn/min rotating speeds, stir after 60 minutes, obtain the stable slurry containing bamboo-carbon powder 40wt%, i.e. bamboo charcoal nano pulp.
(2) prepare aluminosilicate slow-release microcapsule 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 soak after 40 minutes in temperature, be 42 DEG C in temperature and wash, dry at 83 DEG C after filtration, 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 80 DEG C of heating for dissolving of temperature, then be cooled to 50 DEG C, the aluminosilicate powder that slowly adds afterwards preliminary treatment to prepare, use high speed dispersor high-speed stirred, speed is 100 revolutions per seconds, regulate pH value to acid, reaction 15min, after being cooled to 12 DEG C, add curing, regulate pH value 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, it is aluminosilicate spansule.
The preparation method of preparation 1.67dtex × 38mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: taking cellulose pulp as raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step make viscose glue, in dissolving step, add the denaturant alkyl polyamine that accounts for chemical cellulose 1.2wt% in viscose glue, add the above-mentioned bamboo charcoal nano pulp stirring 4h preparing of 4wt% that accounts for finished fiber quality to make modified rayon.
2. spinning and post processing: by spinning front injecting systems, the above-mentioned aluminosilicate microcapsules that prepare are joined to 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.
Detect through 1.67dtex × 38mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 4 is made, 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 the JIS L1902:2008 of Japanese Industrial Standards.
Embodiment 5:
Preparation 2.22dtex × 51mm antibacterial and deodouring cellulose fibre:
(1) prepare bamboo charcoal nano pulp for subsequent use
The preparation of bamboo charcoal nano pulp is to be 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, after filtration, add DBSA dispersant, quality is the 0.03wt% of bamboo charcoal nano-powder quality, under 1000 turn/min rotating speeds, stir after 72 minutes, obtain the stable slurry containing bamboo-carbon powder 32wt%, i.e. bamboo charcoal nano pulp.
(2) prepare aluminosilicate slow-release microcapsule 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 soak after 34 minutes in temperature, be 39 DEG C in temperature and wash, dry at 79 DEG C after filtration, 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 82 DEG C of heating for dissolving of temperature, then be cooled to 49 DEG C, the aluminosilicate powder that slowly adds afterwards preliminary treatment to prepare, use high speed dispersor high-speed stirred, speed is 135 revolutions per seconds, regulate pH value to acid, reaction 17min, after being cooled to 11 DEG C, add curing, regulate pH value 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, it is aluminosilicate spansule.
The preparation method of preparation 2.22dtex × 51mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: taking cellulose pulp as raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step make viscose glue, in dissolving step, add the denaturant alkyl polyamine that accounts for chemical cellulose 0.9wt% in viscose glue, add the above-mentioned bamboo charcoal nano pulp stirring 2.5h preparing of 3wt% that accounts for finished fiber quality to make modified rayon.
2. spinning and post processing: by spinning front injecting systems, above-mentioned prepare aluminosilicate microcapsules are joined to 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.
Detect through 2.22dtex × 51mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 5 is made, 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 the JIS L1902:2008 of Japanese Industrial Standards.
Embodiment 6:
Preparation 3.33dtex × 60mm antibacterial and deodouring cellulose fibre:
(1) prepare bamboo charcoal nano pulp for subsequent use
The preparation of bamboo charcoal nano pulp is to be 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, after filtration, add DBSA dispersant, quality is the 0.09wt% of bamboo charcoal nano-powder quality, under 700 turn/min rotating speeds, stir after 71 minutes, obtain the stable slurry containing bamboo-carbon powder 32.6wt%, i.e. bamboo charcoal nano pulp.
(2) prepare aluminosilicate slow-release microcapsule 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 soak after 36 minutes in temperature, be 40 DEG C in temperature and wash, dry at 82 DEG C after filtration, 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 83 DEG C of heating for dissolving of temperature, then be cooled to 51 DEG C, the aluminosilicate powder that slowly adds afterwards preliminary treatment to prepare, use high speed dispersor high-speed stirred, speed is 143 revolutions per seconds, regulate pH value to acid, reaction 18min, after being cooled to 11 DEG C, add curing, regulate pH value 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, it is aluminosilicate spansule.
The preparation method of preparation 3.33dtex × 60mm antibacterial and deodouring cellulose fibre:
1. the preparation of modified rayon: taking cellulose pulp as raw material, through comprising that dipping, squeezing, pulverizing, experienced, yellow, dissolving, mixing and maturation step make viscose glue, in dissolving step, add the denaturant alkyl polyamine that accounts for chemical cellulose 1.1wt% in viscose glue, add the above-mentioned bamboo charcoal nano pulp stirring 3.6h preparing of 5wt% that accounts for finished fiber quality to make modified rayon.
2. spinning and post processing: by spinning front injecting systems, the above-mentioned aluminosilicate microcapsules that prepare are joined to 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.
Detect through 3.33dtex × 60mm antibacterial and deodouring cellulosic fibrous product that the preparation method described in embodiment 6 is made, 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 the JIS L1902:2008 of Japanese Industrial Standards.
Through the prepared antibacterial and deodouring cellulose fibre of above-described embodiment 1 ~ 5 is detected, 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 prepared cellulose fibre of embodiment 1 ~ 5 is different, the analysis found that, the prepared short fiber of cellulose cost of 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 variations.At this, should illustrate, any change of making under inventive concept of the present invention all will fall within the scope of protection of the present invention.