CN106435817B - A kind of preparation method of functional regeneration cellulose fibre - Google Patents
A kind of preparation method of functional regeneration cellulose fibre Download PDFInfo
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- 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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D13/00—Complete machines for producing artificial threads
- D01D13/02—Elements of machines in combination
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
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Abstract
本发明涉及一种功能再生纤维素纤维的制备方法，包括下述步骤：采用纤维素溶剂溶解低聚合度纤维素，制得功能性粉体的载体溶液；通过搅拌设备提供的强剪切作用，将功能性粉体与载体溶液混合，制得功能性母液；将功能性母液以在线添加的方式注入纤维素纺丝液，纺丝液经挤出、凝固成形为功能再生纤维素纤维。本发明能够克服传统方法功能性粉体与纺丝液混合困难，分散不均匀的问题，所用的母液载体随纤维凝固成形，无额外助剂进入溶剂与凝固浴体系。本发明的成形方法简单、灵活、高效，基于常规生产线即可实现功能再生纤维素纤维的生产。The invention relates to a method for preparing functional regenerated cellulose fibers, comprising the following steps: dissolving cellulose with a low degree of polymerization by using a cellulose solvent to obtain a carrier solution of functional powder; The functional powder is mixed with the carrier solution to obtain a functional mother solution; the functional mother solution is injected into the cellulose spinning solution in the way of online addition, and the spinning solution is extruded and solidified to form functional regenerated cellulose fibers. The invention can overcome the problems of difficulty in mixing the functional powder and spinning solution and uneven dispersion in the traditional method. The forming method of the invention is simple, flexible and efficient, and can realize the production of functional regenerated cellulose fibers based on a conventional production line.
Description
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%.
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