CN106435817B - A kind of preparation method of functional regeneration cellulose fibre - Google Patents

A kind of preparation method of functional regeneration cellulose fibre Download PDF

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Publication number
CN106435817B
CN106435817B CN201610838054.4A CN201610838054A CN106435817B CN 106435817 B CN106435817 B CN 106435817B CN 201610838054 A CN201610838054 A CN 201610838054A CN 106435817 B CN106435817 B CN 106435817B
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cellulose
functional
powder
mother liquor
spinning
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CN106435817A (en
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张玉梅
王华平
王朝生
陈烨
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Donghua University
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Donghua University
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/02Preparation of spinning solutions
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D13/00Complete machines for producing artificial threads
    • D01D13/02Elements of machines in combination
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/06Wet spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/07Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof

Abstract

The present invention relates to a kind of preparation method of functional regeneration cellulose fibre, includes the following steps: to dissolve low polymerization degree cellulose using cellulose solvent, the carrier solution of functional powder is made;The Strong shear effect provided by mixing plant, functional powder is mixed with carrier solution, function aqueous mother liquor is made;Function aqueous mother liquor is injected into cellulose spinning fluid in a manner of adding online, spinning solution is squeezed out, solidification forming is functional regeneration cellulose fibre.The present invention can overcome conventional method functional powder to mix difficulty with spinning solution, disperse non-uniform problem, and mother liquor carrier used is shaped with fibre solidification, and no Additional auxiliaries enter solvent and coagulating bath system.Manufacturing process of the invention is simple, flexible, efficient, and the production of functional regeneration cellulose fibre can be realized based on conventional production line.

Description

A kind of preparation method of functional regeneration cellulose fibre
Technical field
The present invention relates to a kind of preparation methods of functional regeneration cellulose fibre.
Background technique
Regenerated celulose fibre is the cellulose fibre using native cellulose as raw material, through regeneration preparation.Regenerated cellulose Fibrous raw material is renewable, good hygroscopicity, snugness of fit are high, is the main species of chemical fibre.Since the fusing point of cellulose is high In decomposition temperature, the production of regenerated celulose fibre is mainly using the method for wet spinning or dry-jet wet spinning.According to life The difference of production. art, the regenerated celulose fibre of commercialization mainly include viscose rayon, Lyocell fibers, copper ammonia fiber etc..
With the development of regenerated celulose fibre technology, functional regeneration cellulose fibre becomes new developing direction.Wherein, Spinning solution is added in functional additive, and then extrusion, solidification forming are one of preparation methods.Such as the preparation of flame retardant viscose fiber Inorganic fire-retarded powder or small organic molecule fire retardant are added spinning solution with powder, and then squeeze out simultaneously solidification forming by process (patent No.: ZL201110287745.7, a kind of composite silicon-based flame-retardant viscose fiber and its production method).Fire-retardant powder directly with Spinning solution mixing causes powder dispersion process difficulty big, the high requirements on the equipment since cellulose solution viscosity is high.Additionally deposit It is easy to deposit in powder, reunite, mixes non-uniform problem, causes the unstable of spinneret hole plug and fibre property.In order to mention The dispersing uniformity of high functional additive and spinning solution has patent to carry out fire-retardant powder and surfactant, dispersing agent pre- Mixing, is made suspension or emulsion.Suspension, emulsion are mixed with cellulose spinning fluid can be improved functional additive Dispersing uniformity (a kind of patent No.: phosphor nitrogen fire retardant dispersion of ZL201110252275.0 and preparation method thereof), however table The auxiliary agents such as face activating agent can enter coagulating bath, influence the normal recycling of solvent and coagulator, increase cost recovery.Remain in fiber In auxiliary agent also will affect every physicochemical property of fiber, there is also the possibility of auxiliary agent exudation in use process.
Polymer composite fiber is prepared by melt spinning, the method for currently generalling use functional agglomerate addition, specifically Refer to that the functional additive of high-content and substrate macromolecule material are blended means through reinforcing and the finely dispersed pellet of powder, spinning are made Process mixes master batch with matrix macromolecule and extrusion molding.Master-batch techniques disperse functional form additive and matrix macromolecule more Flexibly and conveniently, it is easier to improve the dispersing uniformity of the two, while improving production efficiency, equipment cost and energy is greatly reduced Consumption.
Solution blending prepares regenerated cellulose composite fibre and also rarely has cellulose solution, solution of cellulose derivative at present The technology of mother liquor is mixed and made into functional powder, the relevant technologies have to be developed.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of functional regeneration cellulose fibre, obvious characteristic of the invention is Functional powder is uniformly mixed with low polymerization degree cellulose solution, function aqueous mother liquor is made.Function aqueous mother liquor to add online Method inject cellulose spinning fluid, functional regeneration cellulose fibre is made in and then spinning technique.
A kind of preparation method of functional regeneration cellulose fibre of the invention, includes the following steps:
(1) low polymerization degree cellulose is dissolved using cellulose solvent, the carrier solution of functional powder is made;
(2) functional powder and carrier solution are stirred, function aqueous mother liquor is made;
(3) function aqueous mother liquor is injected in cellulose spinning fluid in a manner of adding online, functionality spinning solution is made, so By extrusion, solidification and drawing-off, functional regeneration cellulose fibre is made.
The preparation method of functional regeneration cellulose fibre as described above, the degree of polymerization of the low polymerization degree cellulose are 200-500, the degree of polymerization of cellulosic material is 500-1500 in the cellulose spinning fluid.
The preparation method of functional regeneration cellulose fibre as described above, the functional powder refers to inorganic or organic Powder is antibacterial, fire retardant functionality powder, and is not dissolved in solidification used in the coagulation step of cellulose solvent and fiber Agent;For the functional powder average grain diameter less than 1 μm, the coagulator is water.
The preparation method of functional regeneration cellulose fibre as described above, the antiseptic powder be metallic silver, copper, The powder of zinc and its oxide, or also include silica or the work of negative Ag-bearing, copper, zinc and its oxide further Property charcoal powder;The fire retardant functionality powder is that the fire retardant functionality powder is organic fire-retardant pyrophosphoric acid esters, specifically, 2,2 '-oxos bis- (- 2,2 '-disulphide of 5,5- dimethyl -1,3,2- dioxathion alkane), (2- oxo -5,5- diformazan of 1,2- bis- Base -1,3,2- dioxy phosphorus heterocycle hex- 2- amino) ethane or the (thio -5,5- dimethyl -1,3,2- dioxy phosphorus heterocycle of 2- of N, N '-two Hexyl) ethylenediamine.
The preparation method of functional regeneration cellulose fibre as described above, the cellulose solvent are N-methylmorpholine-N- Oxide (NMMO)/water or ionic liquid;
N-methylmorpholine-N- oxide/the aqueous systems, wherein ratio shared by water is less than 15wt%.
The ionic liquid is 1- butyl -3- methylimidazole villaumite, 1- ethyl-3-methylimidazole acetate or 1- butyl - 3- methylimidazole bromide;
The preparation method of functional regeneration cellulose fibre as described above, low polymerization degree cellulose in the carrier solution Concentration is 6~15wt%;The mass ratio of the low polymerization degree cellulose and functional powder is 1-10:1;The cellulose spinning The concentration of cellulosic material is 6~15wt% in liquid.
The preparation method of functional regeneration cellulose fibre as described above, the equipment of the stirring are screw extruder or pinch Conjunction machine, the rate of the stirring are 100-300 revs/min, the stirring when it is 0.5-1 hours a length of.
The preparation method of functional regeneration cellulose fibre as described above, it is described that function aqueous mother liquor is injected into cellulose spinning Mode in liquid is that function aqueous mother liquor is injected into cellulose spinning fluid in a manner of adding online, specially in the fibre of production line It ties up and installs the online adding set of function aqueous mother liquor additional on plain spinning solution transfer pipeline, wherein cellulose spinning fluid and function aqueous mother liquor Mass ratio is 1-20:1.
The preparation method of functional regeneration cellulose fibre as described above, the functionality spinning solution are prepared into functional regeneration The technique of cellulose fibre is wet spinning technology or dry-jet wet spinning technique.
Functional regeneration cellulose fibre produced by the present invention, characterized in that when the functional powder added in step (2) is When antiseptic powder, the functional regeneration cellulose fibre is antibacterial regenerated celulose fibre, the antibacterial regenerated fiber Cellulose fiber filament number is 0.9-4.8dtex, breaking strength 1.7-4.5cN/dtex, according to GB/T 20944.3-2008's Method carries out antibiotic property test, to antibiotic rate >=93% of Escherichia coli, to antibiotic rate >=95% of staphylococcus aureus;
When the functional powder added in step (2) is fire retardant functionality powder, the functional regeneration cellulose fibre For fire-retardant regenerated cellulose fiber, the fire-retardant regenerated cellulose filament fineness is 1.3-4.9dtex, and breaking strength is 1.5-3.5cN/dtex, limit oxygen index >=25.0%.
The principle of the present invention:
Cellulose is made of D- glucopyranosyl, belongs to stiff chain structure, and the hydroxyl on cellulose molecular chain is dividing Hydrogen bond is formed with molecule interchain in subchain.The viscosity of the characteristics of due to cellulose molecular structure, cellulose solution are higher, for example, Cellulosic degree of polymerization is 569, and concentration is cellulose/NMMO/H of 12.9wt%2O solution, Zero shear viscosity when temperature is 85 DEG C For 8670Pa.s;Cellulosic degree of polymerization is 569, and concentration is cellulose/1- butyl -3- methylimidazole villaumite of 10.4wt% ([BMIM] Cl) solution, Zero shear viscosity when temperature is 85 DEG C reach 7920Pa.s (Kosan B, Michels C, Meister F.Dissolution and forming of cellulose with ionic liquids[J].Cellulose,2008, 15(1):59-66.).It is evenly dispersed in cellulose solution that high viscosity characteristic is difficult to functional powder, wants to mixing apparatus Ask also more harsh.
Predictably, it is easier to uniformly mix with functional powder compared with the cellulose solution of low viscosity.Cellulose gathers Right reduction, the viscosity decline of cellulose solution.In addition, the molecular structure of the cellulose in low polymerization degree cellulose and spinning solution Unanimously, dissolving each other for molecular level may be implemented in the two.
Therefore the present invention selects carrying body of the low polymerization degree cellulose as functional powder, as functional powder and fibre Tie up the mixed uniformly bridge of plain spinning solution.It is easier to using low polymerization degree cellulose uniform with functional powder, cellulose solution The characteristics of mixing, plays intermediation, the mixing of promotion functions powder and cellulose spinning fluid.
The utility model has the advantages that
(1) it is lower than cellulose spinning fluid using the viscosity of low polymerization degree cellulose solution, is easier to uniform with functional powder Mixed advantage selects low polymerization degree cellulose as the matrix of function aqueous mother liquor, be prepared for functional powder be uniformly dispersed, property The stable function aqueous mother liquor of matter.Function aqueous mother liquor can inject the spinning of generally conventional regenerated celulose fibre by online adding set Silk liquid transportation system, easily and flexibly manufactures functional regeneration cellulose fibre.
(2) molecular structure of low polymerization degree cellulose is similar to cellulose, and dissolving each other for molecular level may be implemented in the two.It is solidifying Gu process is with cellulose together solidification forming and does not enter coagulating bath, no additional additive enters coagulating bath, do not increase solvent with The burden of coagulating bath recycling.According to the present invention, only it need to increase online adding set on conventional regeneration cellulose fibre production line The production of functional regeneration cellulose fibre can be realized, method is succinctly flexible, strong operability.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited Fixed range.
Embodiment 1
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
Use cellulose solvent N-methylmorpholine-N- oxide (NMMO)/water (wherein ratio shared by water for The function that low polymerization degree cellulose concentration is 6wt% is made in 13.8wt%) the low polymerization degree cellulose that the dissolution degree of polymerization is 200 Property powder carrier solution;Then by average grain diameter less than 1 μm, and it is not dissolved in institute in the coagulation step of cellulose solvent and fiber The silver-colored antiseptic powder and carrier solution of coagulator are stirred using screw extruder, wherein the rate stirred is 100 revs/min, stirring when it is 0.5 hour a length of, the mass ratio of low polymerization degree cellulose and silver-colored functional powder is 1:1, is made anti- Bacterium function aqueous mother liquor;It is 500 that antibacterial functions aqueous mother liquor is finally injected the degree of polymerization in a manner of adding online, concentration 6wt% Cellulose spinning fluid in, on cellulose spinning fluid transfer pipeline specially in the production line install additional function aqueous mother liquor add online Feeder apparatus, wherein cellulose spinning fluid and the mass ratio of antibacterial functions aqueous mother liquor are 17:1, antiseptic spinning solution are made, so By extrusion, solidification and the drafting step in wet spinning technology, antibacterial regenerated celulose fibre is made.
Test shows that antibacterial regenerated celulose fibre filament number is 0.9dtex, and breaking strength 1.7cN/dtex is pressed Antibiotic property test is carried out according to the method for GB/T 20944.3-2008, the antibiotic rate to Escherichia coli is 93%, to golden yellow grape The antibiotic rate of coccus is 95%.
Embodiment 2
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
Use cellulose solvent N-methylmorpholine-N- oxide (NMMO)/water (wherein ratio shared by water for The function that low polymerization degree cellulose concentration is 15wt% is made in 13.4wt%) the low polymerization degree cellulose that the dissolution degree of polymerization is 500 Property powder carrier solution;Then by average grain diameter less than 1 μm, and it is not dissolved in institute in the coagulation step of cellulose solvent and fiber The copper functional powder and carrier solution of coagulator are stirred using kneader, wherein the rate stirred be 300 turns/ Point, stirring when it is 1 hour a length of, the mass ratio of low polymerization degree cellulose and copper functional powder is 9:1, and antiseptic is made Mother liquor;It is 1500 that antibacterial functions aqueous mother liquor is finally injected the degree of polymerization in a manner of adding online, and concentration is the fiber of 15wt% Function aqueous mother liquor is installed additional in plain spinning solution, on cellulose spinning fluid transfer pipeline specially in the production line adds dress online It sets, wherein cellulose spinning fluid and the mass ratio of antibacterial functions aqueous mother liquor are 4:1, and antiseptic spinning solution is made, then passes through Antibacterial regenerated celulose fibre is made in extrusion, solidification and drafting step in dry-jet wet spinning technique.
Test shows that antibacterial regenerated celulose fibre filament number is 4.8dtex, and breaking strength 4.5cN/dtex is pressed Antibiotic property test is carried out according to the method for GB/T 20944.3-2008, the antibiotic rate to Escherichia coli is 93.6%, to golden yellow Portugal The antibiotic rate of grape coccus is 95.5%.
Embodiment 3
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
It uses the cellulose solvent 1- butyl -3- methylimidazole villaumite dissolution degree of polymerization for 300 low polymerization degree cellulose, makes Obtain the functional powder carrier solution that low polymerization degree cellulose concentration is 7wt%;Then by average grain diameter less than 1 μm, and it is insoluble The zinc functional powder and carrier solution of solution coagulator used in the coagulation step of cellulose solvent and fiber use screw rod Extruder is stirred, wherein the rate stirred be 200 revs/min, stirring when it is 0.6 hour a length of, low polymerization degree cellulose with The mass ratio of zinc functional powder is 10:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial functions aqueous mother liquor to add online Mode to inject the degree of polymerization be 600, concentration is in the cellulose spinning fluid of 8wt%, and cellulose specially in the production line is spun The online adding set of function aqueous mother liquor is installed additional on silk liquid transfer pipeline, wherein the matter of cellulose spinning fluid and antibacterial functions aqueous mother liquor Amount is made antiseptic spinning solution, then the extrusion through wet spinning technology, solidification and drafting step, is made anti-than being 7:1 Bacterium regenerated celulose fibre.
Test show antibacterial regenerated celulose fibre filament number be 1dtex, breaking strength 1.8cN/dtex, according to The method of GB/T 20944.3-2008 carries out antibiotic property test, and the antibiotic rate to Escherichia coli is 94%, to Staphylococcus aureus The antibiotic rate of bacterium is 95.6%.
Embodiment 4
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
Use cellulose solvent 1- ethyl-3-methylimidazole acetate dissolution the degree of polymerization for 400 low polymerization degree cellulose, The functional powder carrier solution that low polymerization degree cellulose concentration is 8wt% is made;Then by average grain diameter less than 1 μm, and not The silver oxide functional powder for being dissolved in coagulator used in the coagulation step of cellulose solvent and fiber is adopted with carrier solution It is stirred with kneader, wherein the rate stirred is 150 revs/min, when 0.7 hour a length of, the low polymerization degree cellulose of stirring Mass ratio with silver oxide functional powder is 5:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial functions aqueous mother liquor with online It is 900 that the mode of addition, which injects the degree of polymerization, and concentration is fiber specially in the production line in the cellulose spinning fluid of 7wt% Install the online adding set of function aqueous mother liquor on plain spinning solution transfer pipeline additional, wherein the matter of cellulose spinning fluid and function aqueous mother liquor Antiseptic spinning solution is made than being 7:1 in amount, then through extrusion, solidification and the drafting step in dry-jet wet spinning technique, Antibacterial regenerated celulose fibre is made.
Test shows that antibacterial regenerated celulose fibre filament number is 2.3dtex, and breaking strength 2.5cN/dtex is pressed Antibiotic property test is carried out according to the method for GB/T 20944.3-2008, the antibiotic rate to Escherichia coli is 93.7%, to golden yellow Portugal The antibiotic rate of grape coccus is 95.4%.
Embodiment 5
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
Use cellulose solvent 1- ethyl-3-methylimidazole acetate dissolution the degree of polymerization for 400 low polymerization degree cellulose, The functional powder carrier solution that low polymerization degree cellulose concentration is 10wt% is made;Then by average grain diameter less than 1 μm, and not The copper oxide functional powder for being dissolved in coagulator used in the coagulation step of cellulose solvent and fiber is adopted with carrier solution It is stirred with screw extruder, wherein the rate stirred is 250 revs/min, when 0.8 hour a length of, the low polymerization degree fibre of stirring The mass ratio of dimension element and copper oxide functional powder is 8:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial functions aqueous mother liquor with It is 900 that the mode added online, which injects the degree of polymerization, and concentration is in the cellulose spinning fluid of 9wt%, specially in the production line Install the online adding set of function aqueous mother liquor on cellulose spinning fluid transfer pipeline additional, wherein cellulose spinning fluid and antiseptic The mass ratio of mother liquor is 6:1, antiseptic spinning solution is made, then through extrusion, solidification and the drawing-off in wet spinning technology Antibacterial regenerated celulose fibre is made in step.
Test shows that antibacterial regenerated celulose fibre filament number is 3dtex, breaking strength 3cN/dtex, according to GB/ The method of T 20944.3-2008 carries out antibiotic property test, and the antibiotic rate to Escherichia coli is 93.8%, to Staphylococcus aureus The antibiotic rate of bacterium is 95.6%.
Embodiment 6
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
It uses the cellulose solvent 1- butyl -3- methylimidazole bromide dissolution degree of polymerization for 250 low polymerization degree cellulose, makes Obtain the functional powder carrier solution that low polymerization degree cellulose concentration is 11wt%;Then by average grain diameter less than 1 μm, and it is insoluble The zinc oxide functional powder and carrier solution of solution coagulator used in the coagulation step of cellulose solvent and fiber use Screw extruder is stirred, wherein the rate stirred is 200 revs/min, when 0.7 hour a length of, the low polymerization degree fiber of stirring The mass ratio of element and zinc oxide functional powder is 7:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial functions aqueous mother liquor with It is 900 that the mode of line addition, which injects the degree of polymerization, and concentration is fibre specially in the production line in the cellulose spinning fluid of 12wt% It ties up and installs the online adding set of function aqueous mother liquor additional on plain spinning solution transfer pipeline, wherein cellulose spinning fluid and antibacterial functions sexupara The mass ratio of liquid is 12:1, and antiseptic spinning solution is made, then through in dry-jet wet spinning technique extrusion, solidify and lead Step is stretched, antibacterial regenerated celulose fibre is made.
Test show antibacterial regenerated celulose fibre filament number be 4dtex, breaking strength 3.8cN/dtex, according to The method of GB/T 20944.3-2008 carries out antibiotic property test, and the antibiotic rate to Escherichia coli is 93.5%, to golden yellow grape The antibiotic rate of coccus is 96%.
Embodiment 7
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
Use cellulose solvent 1- ethyl-3-methylimidazole acetate dissolution the degree of polymerization for 450 low polymerization degree cellulose, The functional powder carrier solution that low polymerization degree cellulose concentration is 14wt% is made;Then by average grain diameter less than 1 μm, and not Silicon-dioxide powdery and the carrier for being dissolved in the load silver of coagulator used in the coagulation step of cellulose solvent and fiber are molten Liquid is stirred using screw extruder, wherein the rate stirred is 250 revs/min, when 0.8 hour a length of, the oligomerization of stirring The mass ratio for spending the silicon-dioxide powdery of cellulose and load silver is 3:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial functions It is 1300 that aqueous mother liquor injects the degree of polymerization in a manner of adding online, and concentration is specially to exist in the cellulose spinning fluid of 14wt% On cellulose spinning fluid transfer pipeline on production line install additional the online adding set of function aqueous mother liquor, wherein cellulose spinning fluid with The mass ratio of antibacterial functions aqueous mother liquor is 10:1, antiseptic spinning solution is made, then through in dry-jet wet spinning technique Extrusion, solidification and drafting step, are made antibacterial regenerated celulose fibre.
Test shows that antibacterial regenerated celulose fibre filament number is 4.7dtex, and breaking strength 4.4cN/dtex is pressed Antibiotic property test is carried out according to the method for GB/T 20944.3-2008, the antibiotic rate to Escherichia coli is 93.8%, to golden yellow Portugal The antibiotic rate of grape coccus is 95.4%.
Embodiment 8
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
It uses the cellulose solvent 1- butyl -3- methylimidazole bromide dissolution degree of polymerization for 400 low polymerization degree cellulose, makes Obtain the functional powder carrier solution that low polymerization degree cellulose concentration is 14wt%;Then by average grain diameter less than 1 μm, and it is insoluble The silicon-dioxide powdery and carrier solution of the supported copper of solution coagulator used in the coagulation step of cellulose solvent and fiber It is stirred using kneader, wherein the rate stirred is 200 revs/min, when 0.9 hour a length of, the low polymerization degree fiber of stirring The mass ratio of element and the silicon-dioxide powdery of supported copper is 6:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial functions aqueous mother liquor It is 1400 that the degree of polymerization is injected in a manner of adding online, and concentration is in the cellulose spinning fluid of 12wt%, specially in production line On cellulose spinning fluid transfer pipeline on install the online adding set of function aqueous mother liquor additional, wherein cellulose spinning fluid and antibacterial function Can aqueous mother liquor mass ratio be 14:1, be made antiseptic spinning solution, then through in wet spinning technology extrusion, solidification and Antibacterial regenerated celulose fibre is made in drafting step.
Test shows that antibacterial regenerated celulose fibre filament number is 3.8dtex, and breaking strength 4.2cN/dtex is pressed Antibiotic property test is carried out according to the method for GB/T 20944.3-2008, the antibiotic rate to Escherichia coli is 93.3%, to golden yellow Portugal The antibiotic rate of grape coccus is 95.6%.
Embodiment 9
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
It uses the cellulose solvent 1- butyl -3- methylimidazole bromide dissolution degree of polymerization for 350 low polymerization degree cellulose, makes Obtain the functional powder carrier solution that low polymerization degree cellulose concentration is 12wt%;Then by average grain diameter less than 1 μm, and it is insoluble The silicon-dioxide powdery and carrier solution of the zinc supported of solution coagulator used in the coagulation step of cellulose solvent and fiber It is stirred using kneader, wherein the rate stirred is 200 revs/min, when 0.9 hour a length of, the low polymerization degree fiber of stirring The mass ratio of element and the silicon-dioxide powdery of zinc supported is 8:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial functions aqueous mother liquor It is 800 that the degree of polymerization is injected in a manner of adding online, and concentration is in the cellulose spinning fluid of 12wt%, specially in the production line Cellulose spinning fluid transfer pipeline on install the online adding set of function aqueous mother liquor, wherein cellulose spinning fluid and antibacterial functions additional The mass ratio of aqueous mother liquor is 5:1, and antiseptic spinning solution is made, then through the extrusion in dry-jet wet spinning technique, solidification And drafting step, antibacterial regenerated celulose fibre is made.
Test show antibacterial regenerated celulose fibre filament number be 4dtex, breaking strength 4.2cN/dtex, according to The method of GB/T 20944.3-2008 carries out antibiotic property test, and the antibiotic rate to Escherichia coli is 93.4%, to golden yellow grape The antibiotic rate of coccus is 95.6%.
Embodiment 10
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
It uses the cellulose solvent 1- butyl -3- methylimidazole villaumite dissolution degree of polymerization for 400 low polymerization degree cellulose, makes Obtain the functional powder carrier solution that low polymerization degree cellulose concentration is 13wt%;Then by average grain diameter less than 1 μm, and it is insoluble The absorbent charcoal powder body of the zinc supported of solution coagulator used in the coagulation step of cellulose solvent and fiber is adopted with carrier solution It is stirred with screw extruder, wherein the rate stirred is 200 revs/min, when 0.7 hour a length of, the low polymerization degree fibre of stirring The mass ratio of dimension element and the absorbent charcoal powder body of zinc supported is 4:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial functions aqueous mother liquor It is 1000 that the degree of polymerization is injected in a manner of adding online, and concentration is in the cellulose spinning fluid of 8wt%, specially in the production line Cellulose spinning fluid transfer pipeline on install the online adding set of function aqueous mother liquor, wherein cellulose spinning fluid and antibacterial functions additional The mass ratio of aqueous mother liquor is 5:1, and antiseptic spinning solution is made, then through in wet spinning technology extrusion, solidify and lead Step is stretched, antibacterial regenerated celulose fibre is made.
Test shows that antibacterial regenerated celulose fibre filament number is 4.5dtex, and breaking strength 3.5cN/dtex is pressed Antibiotic property test is carried out according to the method for GB/T 20944.3-2008, the antibiotic rate to Escherichia coli is 93.5%, to golden yellow Portugal The antibiotic rate of grape coccus is 95.8%.
Embodiment 11
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
It uses the cellulose solvent 1- butyl -3- methylimidazole villaumite dissolution degree of polymerization for 400 low polymerization degree cellulose, makes Obtain the functional powder carrier solution that low polymerization degree cellulose concentration is 9wt%;Then by average grain diameter less than 1 μm, and it is insoluble The absorbent charcoal powder body of the supported copper of solution coagulator used in the coagulation step of cellulose solvent and fiber is adopted with carrier solution It is stirred with screw extruder, wherein the rate stirred is 200 revs/min, when 0.9 hour a length of, the low polymerization degree fibre of stirring The mass ratio of dimension element and the absorbent charcoal powder body of supported copper is 10:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial functions sexupara It is 1400 that liquid injects the degree of polymerization in a manner of adding online, and concentration is specially to produce in the cellulose spinning fluid of 14wt% Install the online adding set of function aqueous mother liquor on cellulose spinning fluid transfer pipeline on line additional, wherein cellulose spinning fluid and antibacterial The mass ratio of function aqueous mother liquor be 8:1, be made antiseptic spinning solution, then through in dry-jet wet spinning technique extrusion, Antibacterial regenerated celulose fibre is made in solidification and drafting step.
Test shows that antibacterial regenerated celulose fibre filament number is 4.5dtex, and breaking strength 4.2cN/dtex is pressed Antibiotic property test is carried out according to the method for GB/T 20944.3-2008, the antibiotic rate to Escherichia coli is 93.2%, to golden yellow Portugal The antibiotic rate of grape coccus is 95.6%.
Embodiment 12
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
It uses the cellulose solvent 1- butyl -3- methylimidazole villaumite dissolution degree of polymerization for 350 low polymerization degree cellulose, makes Obtain the functional powder carrier solution that low polymerization degree cellulose concentration is 8wt%;Then by average grain diameter less than 1 μm, and it is insoluble The absorbent charcoal powder body of the load silver of solution coagulator used in the coagulation step of cellulose solvent and fiber is adopted with carrier solution It is stirred with kneader, wherein the rate stirred is 200 revs/min, when 0.9 hour a length of, the low polymerization degree cellulose of stirring Mass ratio with the absorbent charcoal powder body of load silver is 2:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial functions aqueous mother liquor with It is 1100 that the mode of line addition, which injects the degree of polymerization, and concentration is fibre specially in the production line in the cellulose spinning fluid of 8wt% It ties up and installs the online adding set of function aqueous mother liquor additional on plain spinning solution transfer pipeline, wherein cellulose spinning fluid and antibacterial functions sexupara The mass ratio of liquid is 18:1, and antiseptic spinning solution is made, and is then walked through extrusion, solidification and the drawing-off in wet spinning technology Suddenly, antibacterial regenerated celulose fibre is made.
Test shows that antibacterial regenerated celulose fibre filament number is 3.8dtex, and breaking strength 3.5cN/dtex is pressed Antibiotic property test is carried out according to the method for GB/T 20944.3-2008, the antibiotic rate to Escherichia coli is 93.2%, to golden yellow Portugal The antibiotic rate of grape coccus is 95.2%.
Embodiment 13
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
It uses the cellulose solvent 1- butyl -3- methylimidazole villaumite dissolution degree of polymerization for 400 low polymerization degree cellulose, makes Obtain the functional powder carrier solution that low polymerization degree cellulose concentration is 12wt%;Then by average grain diameter less than 1 μm, and it is insoluble The absorbent charcoal powder body and carrier of the load silver oxide of solution coagulator used in the coagulation step of cellulose solvent and fiber are molten Liquid is stirred using kneader, wherein the rate stirred is 250 revs/min, when 0.8 hour a length of, the low polymerization degree fibre of stirring The mass ratio of dimension element and the absorbent charcoal powder body of load silver oxide is 7:1, and antibacterial functions aqueous mother liquor is made;Finally by antiseptic It is 800 that mother liquor injects the degree of polymerization in a manner of adding online, and concentration is specially to produce in the cellulose spinning fluid of 10wt% Install the online adding set of function aqueous mother liquor on cellulose spinning fluid transfer pipeline on line additional, wherein cellulose spinning fluid and antibacterial The mass ratio of function aqueous mother liquor be 15:1, be made antiseptic spinning solution, then through in dry-jet wet spinning technique extrusion, Antibacterial regenerated celulose fibre is made in solidification and drafting step.
Test shows that antibacterial regenerated celulose fibre filament number is 2.8dtex, and breaking strength 4.5cN/dtex is pressed Antibiotic property test is carried out according to the method for GB/T 20944.3-2008, the antibiotic rate to Escherichia coli is 93.5%, to golden yellow Portugal The antibiotic rate of grape coccus is 95.8%.
Embodiment 14
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
Use cellulose solvent 1- ethyl-3-methylimidazole acetate dissolution the degree of polymerization for 400 low polymerization degree cellulose, The functional powder carrier solution that low polymerization degree cellulose concentration is 10wt% is made;Then by average grain diameter less than 1 μm, and not It is dissolved in the absorbent charcoal powder body and carrier of the loaded copper oxide of coagulator used in the coagulation step of cellulose solvent and fiber Solution is stirred using kneader, wherein the rate stirred is 220 revs/min, when 1 hour a length of, the low polymerization degree fibre of stirring The mass ratio of dimension element and the absorbent charcoal powder body of loaded copper oxide is 1:1, and antibacterial functions aqueous mother liquor is made;Finally by antiseptic It is 1100 that mother liquor injects the degree of polymerization in a manner of adding online, and concentration is in the cellulose spinning fluid of 12wt%, specially in life Install the online adding set of function aqueous mother liquor on cellulose spinning fluid transfer pipeline in producing line additional, wherein cellulose spinning fluid and anti- The mass ratio of bacterium function aqueous mother liquor is 16:1, antibacterial functions aqueous mother liquor functionality spinning solution is made, then through dry-jet wet spinning Antibacterial functions aqueous mother liquor functional regeneration cellulose fibre is made in extrusion, solidification and drafting step in technique.
Test show antibacterial regenerated celulose fibre filament number be 4.2dtex, breaking strength 4cN/dtex, according to The method of GB/T 20944.3-2008 carries out antibiotic property test, and the antibiotic rate to Escherichia coli is 93.2%, to golden yellow grape The antibiotic rate of coccus is 95.6%.
Embodiment 15
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
Use cellulose solvent 1- ethyl-3-methylimidazole acetate dissolution the degree of polymerization for 450 low polymerization degree cellulose, The functional powder carrier solution that low polymerization degree cellulose concentration is 12.5wt% is made;Then by average grain diameter less than 1 μm, and It is not dissolved in the absorbent charcoal powder body and load of the load zinc oxide of coagulator used in the coagulation step of cellulose solvent and fiber Liquid solution is stirred using kneader, wherein the rate stirred is 250 revs/min, when 0.8 hour a length of, the oligomerization of stirring The mass ratio spent cellulose and load the absorbent charcoal powder body of zinc oxide is 3:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial function It is 1100 that energy aqueous mother liquor injects the degree of polymerization in a manner of adding online, and concentration is in the cellulose spinning fluid of 11wt%, specially Install the online adding set of function aqueous mother liquor on cellulose spinning fluid transfer pipeline in the production line additional, wherein cellulose spinning fluid Mass ratio with antibacterial functions aqueous mother liquor is 8:1, antiseptic spinning solution is made, then through in dry-jet wet spinning technique Extrusion, solidification and drafting step, are made antibacterial regenerated celulose fibre.
Test show antibacterial regenerated celulose fibre filament number be 4dtex, breaking strength 3.8cN/dtex, according to The method of GB/T 20944.3-2008 carries out antibiotic property test, and the antibiotic rate to Escherichia coli is 93.5%, to golden yellow grape The antibiotic rate of coccus is 95.4%.
Embodiment 16
A kind of preparation method of antibacterial regenerated celulose fibre, includes the following steps:
Use cellulose solvent 1- ethyl-3-methylimidazole acetate dissolution the degree of polymerization for 350 low polymerization degree cellulose, The functional powder carrier solution that low polymerization degree cellulose concentration is 14wt% is made;Then by average grain diameter less than 1 μm, and not It is dissolved in the absorbent charcoal powder body and carrier of the load silver oxide of coagulator used in the coagulation step of cellulose solvent and fiber Solution is stirred using screw extruder, wherein the rate stirred be 280 revs/min, stirring when it is 0.9 hour a length of, it is oligomeric The mass ratio of the absorbent charcoal powder body of DP cellulose and load silver oxide is 5:1, and antibacterial functions aqueous mother liquor is made;Finally by antibacterial It is 1300 that function aqueous mother liquor injects the degree of polymerization in a manner of adding online, and concentration is in the cellulose spinning fluid of 9wt%, specially Install the online adding set of function aqueous mother liquor on cellulose spinning fluid transfer pipeline in the production line additional, wherein cellulose spinning fluid Mass ratio with antibacterial functions aqueous mother liquor is 10:1, antiseptic spinning solution is made, then through in dry-jet wet spinning technique Extrusion, solidification and drafting step, be made antibacterial regenerated celulose fibre.
Test show antibacterial regenerated celulose fibre filament number be 4dtex, breaking strength 4.2cN/dtex, according to The method of GB/T 20944.3-2008 carries out antibiotic property test, and the antibiotic rate to Escherichia coli is 93.4%, to golden yellow grape The antibiotic rate of coccus is 95.3%.
Embodiment 17
A kind of preparation method of flame retarding function regenerated celulose fibre, includes the following steps:
Using cellulose solvent N-methylmorpholine-N- oxide (NMMO)/water, (wherein ratio shared by water is 14wt%) The low polymerization degree cellulose that the degree of polymerization is 300 is dissolved, the functional powder that low polymerization degree cellulose concentration is 12wt% is made and carries Liquid solution;Then by average grain diameter less than 1 μm, and it is not dissolved in solidification used in the coagulation step of cellulose solvent and fiber Oxo bis- (- 2,2 '-disulphide of 5,5- dimethyl -1,3,2- dioxathion alkane) powders in the 2,2 ' of agent-are used with carrier solution and are pinched Conjunction machine is stirred, wherein the rate stirred is 200 revs/min, when 0.9 hour a length of, the low polymerization degree cellulose and 2 of stirring, The mass ratio of bis- (5,5- dimethyl -1,3,2- dioxathion alkane -2, the 2 '-disulphide) powders of 2 '-oxos is 8:1, is made fire-retardant Function aqueous mother liquor;It is 1200 that flame retarding function aqueous mother liquor is finally injected the degree of polymerization in a manner of adding online, concentration 12wt% Cellulose spinning fluid in, on cellulose spinning fluid transfer pipeline specially in the production line install additional function aqueous mother liquor add online Feeder apparatus, wherein cellulose spinning fluid and the mass ratio of flame retarding function aqueous mother liquor are 1:1, fire retardant functionality spinning solution are made, so By extrusion, solidification and the drafting step in wet spinning technology, flame retarding function regenerated celulose fibre is made.
Test shows that the filament number of fire-retardant regenerated cellulose fiber obtained is 1.3dtex, breaking strength 1.5cN/ Dtex, limit oxygen index 25.0%.
Embodiment 18
A kind of preparation method of flame retarding function regenerated celulose fibre, includes the following steps:
Use cellulose solvent N-methylmorpholine-N- oxide (NMMO)/water (wherein ratio shared by water for The function that low polymerization degree cellulose concentration is 6wt% is made in 13.8wt%) the low polymerization degree cellulose that the dissolution degree of polymerization is 500 Property powder carrier solution;Then by average grain diameter less than 1 μm, and it is not dissolved in institute in the coagulation step of cellulose solvent and fiber (2- oxo -5,5- dimethyl -1,3,2- dioxy phosphorus heterocycle hex- 2- amino) the ethane powder of 1,2- bis- and carrier of coagulator Solution is stirred using kneader, wherein the rate stirred is 200 revs/min, when 0.5 hour a length of, the low polymerization degree of stirring The mass ratio of cellulose and 1,2- bis- (2- oxo -5,5- dimethyl -1,3,2- dioxy phosphorus heterocycle hex- 2- amino) ethane powder is Flame retarding function aqueous mother liquor is made in 9:1;It is 500 that flame retarding function aqueous mother liquor is finally injected the degree of polymerization in a manner of adding online, dense Degree is to install additional on cellulose spinning fluid transfer pipeline specially in the production line functional in the cellulose spinning fluid of 15wt% The online adding set of mother liquor, wherein cellulose spinning fluid and the mass ratio of flame retarding function aqueous mother liquor are 15:1, and flame retarding function is made Property spinning solution then through extrusion, solidification and the drafting step in dry-jet wet spinning technique flame retarding function regenerated cellulose is made Fiber.
Test shows that the filament number of fire-retardant regenerated cellulose fiber obtained is 4.9dtex, breaking strength 3.5cN/ Dtex, limit oxygen index 27.0%.
Embodiment 19
A kind of preparation method of flame retarding function regenerated celulose fibre, includes the following steps:
Use cellulose solvent 1- ethyl-3-methylimidazole acetate dissolution the degree of polymerization for 400 low polymerization degree cellulose, The functional powder carrier solution that low polymerization degree cellulose concentration is 12wt% is made;Then by average grain diameter less than 1 μm, and not It is dissolved in the N of coagulator used in the coagulation step of cellulose solvent and fiber, N '-two (thio dimethyl-1-5,5- 2-, 3,2- dioxy phosphorus heterocycle cyclohexyls) ethylenediamine powder and carrier solution are stirred using kneader, wherein the rate stirred is 200 Rev/min, stirring when it is 1 hour a length of, low polymerization degree cellulose and N, N '-two (2- is thio -5,5- dimethyl -1,3,2- dioxy Phosphorus heterocycle cyclohexyl) ethylenediamine powder mass ratio be 7:1, be made flame retarding function aqueous mother liquor;Finally by flame retarding function aqueous mother liquor with It is 1000 that the mode added online, which injects the degree of polymerization, and concentration is in the cellulose spinning fluid of 12wt%, specially in the production line Cellulose spinning fluid transfer pipeline on install the online adding set of function aqueous mother liquor, wherein cellulose spinning fluid and flame retarding function additional The mass ratio of aqueous mother liquor is 20:1, and fire retardant functionality spinning solution is made, then through the extrusion in dry-jet wet spinning technique, solidification And drafting step, flame retarding function regenerated celulose fibre is made.
Test shows that the filament number of fire-retardant regenerated cellulose fiber obtained is 3dtex, breaking strength 2.2cN/ Dtex, limit oxygen index 25.0%.

Claims (9)

1. a kind of preparation method of functional regeneration cellulose fibre, it is characterized in that: including the following steps:
(1) low polymerization degree cellulose is dissolved using cellulose solvent, the carrier solution of functional powder is made;
(2) functional powder and carrier solution are stirred, function aqueous mother liquor is made;
(3) function aqueous mother liquor is injected in cellulose spinning fluid, functionality spinning solution is made, then through extrusion, solidification and drawing-off, Functional regeneration cellulose fibre is made;The degree of polymerization of the low polymerization degree cellulose is 200-500;In the cellulose spinning fluid The degree of polymerization of cellulosic material is 600-1500.
2. the preparation method of functional regeneration cellulose fibre according to claim 1, which is characterized in that the functionality powder Body refers to inorganic or organic powder, is antibacterial or fire retardant functionality powder, and be not dissolved in the solidifying of cellulose solvent and fiber Gu coagulator used in step;The functional powder average grain diameter is less than 1 μm.
3. the preparation method of functional regeneration cellulose fibre according to claim 2, which is characterized in that the antibacterial functions Property powder be metallic silver, copper, zinc and its oxide powder, or also include negative Ag-bearing, copper, zinc and its oxygen further The silica or absorbent charcoal powder body of compound;The fire retardant functionality powder is organic fire-retardant pyrophosphoric acid esters, specifically: 2, 2 '-oxos bis- (- 2,2 '-disulphide of 5,5- dimethyl -1,3,2- dioxathion alkane), (2- oxo -5,5- dimethyl-of 1,2- bis- 1,3,2- dioxy phosphorus heterocycle hex- 2- amino) ethane or the (thio -5,5- dimethyl -1,3,2- dioxy phospha hexamethylene of 2- of N, N '-two Base) ethylenediamine.
4. the preparation method of functional regeneration cellulose fibre according to claim 1, which is characterized in that the cellulose is molten Agent is N-methylmorpholine-N- oxide/water or ionic liquid;
The ionic liquid is 1- butyl -3- methylimidazole villaumite, 1- ethyl-3-methylimidazole acetate or 1- butyl -3- first Base imidazoles bromide;
N-methylmorpholine-N- oxide/the aqueous systems, wherein ratio shared by water is less than 15wt%.
5. the preparation method of functional regeneration cellulose fibre according to claim 1, which is characterized in that the carrier solution The concentration of middle low polymerization degree cellulose is 6~15wt%;The mass ratio of the low polymerization degree cellulose and functional powder is 1- 10:1;The concentration of cellulosic material is 6~15wt% in the cellulose spinning fluid.
6. the preparation method of functional regeneration cellulose fibre according to claim 1, which is characterized in that the stirring is set Standby is screw extruder or kneader, and the rate of the stirring is 100-300 revs/min, and when a length of 0.5-1 of the stirring is small When.
7. the preparation method of functional regeneration cellulose fibre according to claim 1, which is characterized in that it is described will be functional Mode in mother liquor injection cellulose spinning fluid is that function aqueous mother liquor is injected into cellulose spinning fluid in a manner of adding online In, install the online adding set of function aqueous mother liquor additional specially on the cellulose spinning fluid transfer pipeline of production line, wherein fiber Plain spinning solution and the mass ratio of function aqueous mother liquor are 1-20:1.
8. the preparation method of functional regeneration cellulose fibre according to claim 1, which is characterized in that the functional spinning The technique that silk liquid is successfully prepared energy regenerated celulose fibre is wet spinning technology or dry-jet wet spinning technique.
9. functional regeneration cellulose fibre made from the preparation method of functional regeneration cellulose fibre as described in claim 1, It is characterized in that: when the functional powder added in step (2) is antiseptic powder, the functional regeneration cellulose fibre For antibacterial regenerated celulose fibre, the antibacterial regenerated celulose fibre filament number is 0.9-4.8dtex, and breaking strength is 1.7-4.5cN/dtex carries out antibiotic property test according to the method for GB/T 20944.3-2008, to the antibiotic rates of Escherichia coli >= 93%, to antibiotic rate >=95% of staphylococcus aureus;
When the functional powder added in step (2) is fire retardant functionality powder, the functional regeneration cellulose fibre is resistance Regenerated celulose fibre is fired, the fire-retardant regenerated cellulose filament fineness is 1.3-4.9dtex, breaking strength 1.5- 3.5cN/dtex, limit oxygen index >=25.0%.
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