CN106149080B - A kind of preparation method of cellulose/calamine composite fibre - Google Patents
A kind of preparation method of cellulose/calamine composite fibre Download PDFInfo
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- CN106149080B CN106149080B CN201610838005.0A CN201610838005A CN106149080B CN 106149080 B CN106149080 B CN 106149080B CN 201610838005 A CN201610838005 A CN 201610838005A CN 106149080 B CN106149080 B CN 106149080B
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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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/30—Zinc; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
- A61K47/38—Cellulose; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/70—Web, sheet or filament bases ; Films; Fibres of the matrix type containing drug
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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
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Abstract
The present invention relates to a kind of cellulose/calamine composite fibre preparation methods, include the following steps：Cellulose esters is dissolved using cellulose solvent, the carrier solution of calamine powder is made；The Strong shear effect provided by mixing plant, calamine powder is mixed with carrier solution, calamine mother liquor is made；Calamine mother liquor is injected into cellulose spinning fluid in a manner of adding online, cellulose/calamine composite fibre is made through extrusion, solidification forming and drawing-off in spinning solution.The present invention injects spinning solution for calamine powder difficulty and the mixed uniformly problem of high viscosity spinning solution, using calamine mother liquor, and then the mode of spinning technique prepares cellulose/calamine composite fibre.Mother liquor carrier used in the present invention 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 cellulose/calamine composite fibre can be realized based on conventional production line.
Description
Technical field
The present invention relates to regenerated fiber fields, and in particular to a kind of preparation method of cellulose/calamine composite fibre.
Background technique
The cellulose fibres such as cotton, viscose rayon, lyocell fiber have excellent skin affinity, are widely used in personal
Clothing.In order to increase the function of cellulose fibre, patent ZL201010511031.5 (calamine cellulose fiber and its preparation side
Method) a kind of preparation method of functional fibre cellulose fiber is proposed, specific method is by calamine slurry and cellulose/ion liquid
Spinning solution mixing, prepares cellulose/calamine composite fibre through wet spinning forming.Since calamine is to a variety of contact dermatitis
There is therapeutic effect, functional fibre can prevent dermopathic generation, can also mitigate the acute pruritic skin diseases such as nettle rash, prickly heat
Symptom.
The calamines powder such as calamine is mixed with cellulose spinning fluid, the mixing uniformity of the two is asking for overriding concern
Topic.Since cellulose solution viscosity is high, cause powder dispersion process difficulty big, the high requirements on the equipment.It is easy to additionally, there may be powder
In deposition, reunion, the non-uniform problem of mixing, the unstable of spinneret hole plug and fibre property is caused.In order to improve calamine
With the dispersing uniformity of spinning solution, patent ZL201010511031.5 by calamine and amine cation type surfactant,
Silicon systems cationoid surfactant, sodium tripolyphosphate are pre-mixed, and the calamine slurry of suspension or milkiness liquid status is made.
Suspension, emulsion mixes to the dispersing uniformity that functional additive can be improved with cellulose spinning fluid, however surface-active
The auxiliary agents such as agent can enter coagulating bath, influence the normal recycling of solvent and coagulator, increase cost recovery.Residual helping in the fibre
Agent also will affect every physicochemical property of fiber, and there is also the possibility of auxiliary agent exudation in use process.
How efficiently to realize the evenly dispersed of calamine powder, reduces calamine powder adding procedure to original forming work
The interference of skill is the technical bottleneck that cellulose/calamine composite fibre production needs to break through.
Summary of the invention
The present invention be directed to the deficiencies in the prior art, provide a kind of preparation method of cellulose/calamine composite fibre, will
Calamine powder is uniformly mixed with cellulose ester solution, and calamine mother liquor, the method that calamine mother liquor is added online is made
Cellulose spinning fluid, and then spinning technique are injected, cellulose/calamine composite fibre is made.
A kind of cellulose/calamine composite fibre preparation method of the invention, includes the following steps：
(1) cellulose esters is dissolved using cellulose solvent, the carrier solution of calamine powder is made；
(2) calamine powder is stirred with carrier solution, calamine mother liquor is made；
(3) calamine mother liquor is injected in cellulose spinning fluid, functionality spinning solution is made, then through squeezing
Out, cellulose/calamine composite fibre is made in solidification and drawing-off.
The preparation method of cellulose/calamine composite fibre as described above, the cellulose esters are cellulose acetate, vinegar
Sour cellulose propionate or acetylbutyrylcellulose, the degree of polymerization of the cellulose esters are 200-1000, and total esterification degree is 2.3-
2.5；The degree of polymerization of cellulosic material is 500-1500 in the cellulose spinning fluid.
The preparation method of cellulose/calamine composite fibre as described above, the calamine powder average grain diameter are less than
0.2μm。
The preparation method of cellulose/calamine composite fibre as described above, the cellulose solvent are N-methylmorpholine-
N- oxide 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 cellulose/calamine composite fibre as described above, cellulose esters is dense in the carrier solution
Degree is 6~15wt%；The mass ratio of the cellulose esters and calamine powder is 1-10:1；Fiber in the cellulose spinning fluid
The concentration of plain raw material is 6~15wt%.
The preparation method of cellulose/calamine composite fibre as described above, the equipment of the stirring is Screw Extrusion
Machine or kneader, 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 cellulose/calamine composite fibre as described above, the calamine mother liquor injection cellulose are spun
Mode in silk liquid is to inject calamine mother liquor in cellulose spinning fluid in a manner of adding online, specially in the production line
Cellulose spinning fluid transfer pipeline on install the online adding set of calamine mother liquor additional, wherein cellulose spinning fluid and calamine are female
Liquid mass ratio is 3-20:1.
The preparation method of cellulose/calamine composite fibre as described above, the functionality spinning solution prepare cellulose/
The technique of calamine composite fibre is wet spinning technology or dry-jet wet spinning technique.
Cellulose/calamine composite fibre made from the preparation method of cellulose/calamine composite fibre as described above,
The cellulose/calamine composite fibre filament number is 0.9-4.8dtex, dry break strength 1.7-4.5cN/dtex.
Cellulose/calamine composite fibre as described above, the composite fibre have auxiliary to pruitus, scytitis
Therapeutic effect.
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 calamine powder, wants to mixing apparatus
Ask also more harsh.
Since the hydroxyl quantity on cellulose esters strand is less than the hydroxyl on cellulose molecular chain, cellulose esters strand
Also phase factor reduces for the interior interaction with molecule interchain, therefore the viscosity of cellulose ester solution is less than cellulose solution.In addition, fine
The structure for tieing up plain ester and cellulose is almost consistent, and the two can be realized dissolving each other for molecular level.
Based on this, the present invention selects cellulose esters as the carrying body of calamine powder, as calamine powder and fiber
The plain mixed uniformly bridge of spinning solution.Using cellulose esters be easier to calamine powder, the mixed uniformly feature of cellulose solution,
Intermediation is played, the mixing of calamine powder and cellulose spinning fluid is promoted.
Beneficial effect：
(1) it is lower than cellulose spinning fluid using the viscosity of cellulose ester solution, is easier to mixed uniformly with calamine powder
Advantage selects cellulose esters that it is sweet to be prepared for the furnace that calamine powder is uniformly dispersed, property is stable as the matrix of calamine mother liquor
Stone mother liquor.Calamine mother liquor can inject the spinning solution delivery system of generally conventional regenerated celulose fibre by online adding set
System easily and flexibly manufactures cellulose/calamine composite fibre.
(2) molecular structure of cellulose esters is similar to cellulose, and dissolving each other for molecular level may be implemented in the two.Process of setting
Coagulating bath is not entered with cellulose together solidification forming and, no additional additive enters coagulating bath, does not increase solvent and coagulating bath
The burden of recycling.According to the present invention, only need to increase online adding set on conventional regeneration cellulose fibre production line can be real
Now tie up the production of element/calamine composite fibre, method brief introduction, strong operability.
(3) cellulose/calamine composite fibre can prevent dermopathic generation, have to pruitus, scytitis auxiliary
Help therapeutic effect.
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 cellulose/calamine composite fibre, includes the following steps：
Use cellulose solvent N-methylmorpholine-N- oxide (NMMO)/water (wherein ratio shared by water for
13.8wt%) the dissolution degree of polymerization is 200, the cellulose acetate that total esterification degree is 2.3, and it is 6wt% that cellulose acetate concentration, which is made,
Calamine powder carrier solution；Then average grain diameter is squeezed for 0.19 μm of calamine powder and carrier solution using screw rod
Machine is stirred out, wherein the rate stirred is 100 revs/min, when 0.5 hour a length of, cellulose acetate and the calamine of stirring
The mass ratio of powder is 1:1, calamine mother liquor is made；Calamine mother liquor is finally injected the degree of polymerization in a manner of adding online is
500, concentration is to install additional on cellulose spinning fluid transfer pipeline specially in the production line in the cellulose spinning fluid of 6wt%
The online adding set of calamine mother liquor, wherein the mass ratio of cellulose spinning fluid and calamine mother liquor is 3:1, it is made functional and spins
Cellulose/calamine composite fibre is made then through extrusion, solidification and the drafting step in wet spinning technology in silk liquid.
Test shows that cellulose/calamine composite fibre filament number is 0.9dtex, and dry break strength is
1.7cN/dtex。
Embodiment 2
A kind of preparation method of cellulose/calamine composite fibre, includes the following steps：
Use cellulose solvent N-methylmorpholine-N- oxide (NMMO)/water (wherein ratio shared by water for
13.4wt%) the dissolution degree of polymerization is 1000, and it is dense that cellulose acetate propionate is made in the cellulose acetate propionate that total esterification degree is 2.5
Degree is the carrier solution of the calamine powder of 15wt%；Then the calamine powder and carrier solution for being 0.18 μm by average grain diameter
It is stirred using kneader, wherein the rate stirred is 300 revs/min, when 1 hour a length of, the cellulose acetate propionate of stirring
Mass ratio with calamine powder is 9:1, calamine mother liquor is made；Finally calamine mother liquor is injected in a manner of adding online
The degree of polymerization is 1500, and concentration is in the cellulose spinning fluid of 15wt%, and cellulose spinning fluid specially in the production line conveys
Install the online adding set of calamine mother liquor on pipeline additional, wherein the mass ratio of cellulose spinning fluid and calamine mother liquor is 20:1,
Functionality spinning solution is made, then through extrusion, solidification and the drafting step in dry-jet wet spinning technique, cellulose/furnace is made
Sweet stone composite fibre.
Test shows that cellulose/calamine composite fibre filament number is 4.8dtex, and dry break strength is
1.7cN/dtex。
Embodiment 3
A kind of preparation method of cellulose/calamine composite fibre, includes the following steps：
Use cellulose solvent 1- butyl -3- methylimidazole villaumite dissolution the degree of polymerization be 300, total esterification degree for 2.4 vinegar
The carrier solution for the calamine powder that acetylbutyrylcellulose concentration is 7wt% is made in sour cellulose butyrate；It then will average grain
Diameter be 0.19 μm calamine powder and carrier solution be stirred using screw extruder, wherein the rate stirred be 200 turns/
Point, stirring when it is 0.6 hour a length of, the mass ratio of acetylbutyrylcellulose and calamine powder is 10:1, it is female that calamine is made
Liquid；It is 600 that calamine mother liquor is finally injected the degree of polymerization in a manner of adding online, and concentration is the cellulose spinning fluid of 8wt%
In, the online adding set of calamine mother liquor is installed on cellulose spinning fluid transfer pipeline specially in the production line additional, wherein fine
The mass ratio for tieing up plain spinning solution and calamine mother liquor is 7:1, functionality spinning solution is made, then squeezing through wet spinning technology
Out, cellulose/calamine composite fibre is made in solidification and drafting step.
Test shows that cellulose/calamine composite fibre filament number is 0.9dtex, and dry break strength is
4.5cN/dtex。
Embodiment 4
A kind of preparation method of cellulose/calamine composite fibre, includes the following steps：
Using the cellulose solvent 1- ethyl-3-methylimidazole acetate dissolution degree of polymerization is 400, and total esterification degree is 2.35
The carrier solution for the calamine powder that acetylbutyrylcellulose concentration is 8wt% is made in acetylbutyrylcellulose；Then it will be averaged
Partial size be 0.192 μm calamine powder and carrier solution be stirred using kneader, wherein the rate stirred be 150 turns/
Point, stirring when it is 0.7 hour a length of, the mass ratio of acetylbutyrylcellulose and calamine powder is 5:1, it is female that calamine is made
Liquid；It is 900 that calamine mother liquor is finally injected the degree of polymerization in a manner of adding online, and concentration is the cellulose spinning fluid of 7wt%
In, the online adding set of calamine mother liquor is installed on cellulose spinning fluid transfer pipeline specially in the production line additional, wherein fine
The mass ratio for tieing up plain spinning solution and calamine mother liquor is 7:1, functionality spinning solution is made, then through in dry-jet wet spinning technique
Extrusion, solidification and drafting step, be made cellulose/calamine composite fibre.
Test shows that cellulose/calamine composite fibre filament number is 2dtex, dry break strength 3cN/
dtex。
Embodiment 5
A kind of preparation method of cellulose/calamine composite fibre, includes the following steps：
Using the cellulose solvent 1- ethyl-3-methylimidazole acetate dissolution degree of polymerization is 400, and total esterification degree is 2.39
The carrier solution for the calamine powder that acetylbutyrylcellulose concentration is 10wt% is made in acetylbutyrylcellulose；Then it will put down
The calamine powder and carrier solution that equal partial size is 0.189 μm are stirred using screw extruder, wherein the rate stirred is
250 revs/min, stirring when it is 0.8 hour a length of, the mass ratio of acetylbutyrylcellulose and calamine powder is 8:1, it is sweet that furnace is made
Stone mother liquor；It is 900 that calamine mother liquor is finally injected the degree of polymerization in a manner of adding online, and the cellulose that concentration is 9wt% is spun
In silk liquid, the online adding set of calamine mother liquor is installed on cellulose spinning fluid transfer pipeline specially in the production line additional,
The mass ratio of middle cellulose spinning fluid and calamine mother liquor is 6:1, functionality spinning solution is made, then through in wet spinning technology
Extrusion, solidification and drafting step, be made cellulose/calamine composite fibre.
Test shows that cellulose/calamine composite fibre filament number is 2.8dtex, and dry break strength is
3.5cN/dtex。
Embodiment 6
A kind of preparation method of cellulose/calamine composite fibre, includes the following steps：
Use cellulose solvent 1- butyl -3- methylimidazole bromide dissolution the degree of polymerization be 850, total esterification degree for 2.3 vinegar
The carrier solution for the calamine powder that acetylbutyrylcellulose concentration is 11wt% is made in sour cellulose butyrate；Then it will be averaged
The calamine powder and carrier solution that partial size is 0.191 μm are stirred using screw extruder, wherein the rate stirred is 200
Rev/min, stirring when it is 0.7 hour a length of, the mass ratio of acetylbutyrylcellulose and calamine powder is 7:1, calamine is made
Mother liquor；It is 900 that calamine mother liquor is finally injected the degree of polymerization in a manner of adding online, and concentration is the cellulose spinning of 12wt%
In liquid, the online adding set of calamine mother liquor is installed on cellulose spinning fluid transfer pipeline specially in the production line additional, wherein
The mass ratio of cellulose spinning fluid and calamine mother liquor is 12:1, functionality spinning solution is made, then through dry-jet wet spinning work
Cellulose/calamine composite fibre is made in extrusion, solidification and drafting step in skill.
Test shows that cellulose/calamine composite fibre filament number is 3.8dtex, and dry break strength is
2.5cN/dtex。
Embodiment 7
A kind of preparation method of cellulose/calamine composite fibre, includes the following steps：
Using the cellulose solvent 1- ethyl-3-methylimidazole acetate dissolution degree of polymerization is 450, and total esterification degree is 2.45
The carrier solution for the calamine powder that cellulose acetate propionate concentration is 14wt% is made in cellulose acetate propionate；Then it will put down
The calamine powder and carrier solution that equal partial size is 0.19 μm are stirred using screw extruder, wherein the rate stirred is
250 revs/min, stirring when it is 0.8 hour a length of, the mass ratio of cellulose acetate propionate and calamine powder is 3:1, it is sweet that furnace is made
Stone mother liquor；It is 1300 that calamine mother liquor is finally injected the degree of polymerization in a manner of adding online, and concentration is the cellulose of 14wt%
In spinning solution, the online adding set of calamine mother liquor is installed on cellulose spinning fluid transfer pipeline specially in the production line additional,
Wherein the mass ratio of cellulose spinning fluid and calamine mother liquor is 10:1, functionality spinning solution is made, then through dry spray Wet-spinning
Extrusion, solidification and drafting step in silk technique, are made cellulose/calamine composite fibre.
Test shows that cellulose/calamine composite fibre filament number is 1.8dtex, and dry break strength is
2.5cN/dtex。
Embodiment 8
A kind of preparation method of cellulose/calamine composite fibre, includes the following steps：
Use cellulose solvent 1- butyl -3- methylimidazole bromide dissolution the degree of polymerization be 900, total esterification degree for 2.3 vinegar
The carrier solution for the calamine powder that cellulose acetate propionate concentration is 14wt% is made in sour cellulose propionate；Then it will be averaged
Partial size be 0.194 μm calamine powder and carrier solution be stirred using kneader, wherein the rate stirred be 200 turns/
Point, stirring when it is 0.9 hour a length of, the mass ratio of cellulose acetate propionate and calamine powder is 6:1, it is female that calamine is made
Liquid；It is 1400 that calamine mother liquor is finally injected the degree of polymerization in a manner of adding online, and concentration is the cellulose spinning of 12wt%
In liquid, the online adding set of calamine mother liquor is installed on cellulose spinning fluid transfer pipeline specially in the production line additional, wherein
The mass ratio of cellulose spinning fluid and calamine mother liquor is 14:1, functionality spinning solution is made, then through in wet spinning technology
Extrusion, solidification and drafting step, be made cellulose/calamine composite fibre.
Test shows that cellulose/calamine composite fibre filament number is 3dtex, dry break strength 2.4cN/
dtex。
Embodiment 9
A kind of preparation method of cellulose/calamine composite fibre, includes the following steps：
Use cellulose solvent 1- butyl -3- methylimidazole bromide dissolution the degree of polymerization be 350, total esterification degree for 2.3 vinegar
The carrier solution for the calamine powder that cellulose acetate propionate concentration is 12wt% is made in sour cellulose propionate；Then it will be averaged
Partial size be 0.18 μm calamine powder and carrier solution be stirred using kneader, wherein the rate stirred be 200 turns/
Point, stirring when it is 0.9 hour a length of, the mass ratio of cellulose acetate propionate and calamine powder is 8:1, it is female that calamine is made
Liquid；It is 800 that calamine mother liquor is finally injected the degree of polymerization in a manner of adding online, and concentration is the cellulose spinning fluid of 12wt%
In, the online adding set of calamine mother liquor is installed on cellulose spinning fluid transfer pipeline specially in the production line additional, wherein fine
The mass ratio for tieing up plain spinning solution and calamine mother liquor is 5:1, functionality spinning solution is made, then through in dry-jet wet spinning technique
Extrusion, solidification and drafting step, be made cellulose/calamine composite fibre.
Test shows that cellulose/calamine composite fibre filament number is 3.2dtex, and dry break strength is
2.1cN/dtex。
Embodiment 10
A kind of preparation method of cellulose/calamine composite fibre, includes the following steps：
Use cellulose solvent 1- butyl -3- methylimidazole villaumite dissolution the degree of polymerization be 600, total esterification degree for 2.3 vinegar
The carrier solution for the calamine powder that cellulose acetate concentration is 13wt% is made in acid cellulose；Then it is by average grain diameter
0.195 μm of calamine powder and carrier solution is stirred using screw extruder, wherein the rate stirred is 200 revs/min,
Stirring when it is 0.7 hour a length of, wherein the diameter of calamine powder is 1.2nm, and length is 4 μm, and the diameter of calamine powder is
28nm, 4.5 μm of length, cellulose acetate and calamine stone body mass ratio are 4:1, calamine mother liquor is made；Finally by calamine
It is 1000 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 8wt%
Install the online adding set of calamine mother liquor on cellulose spinning fluid transfer pipeline on line additional, wherein cellulose spinning fluid and furnace are sweet
The mass ratio of stone mother liquor is 5:1, functionality spinning solution is made, is then walked through extrusion, solidification and the drawing-off in wet spinning technology
Suddenly, cellulose/calamine composite fibre is made.
Test shows that cellulose/calamine composite fibre filament number is 2.5dtex, and dry break strength is
3.4cN/dtex。
Embodiment 11
A kind of preparation method of cellulose/calamine composite fibre, includes the following steps：
Use cellulose solvent 1- butyl -3- methylimidazole villaumite dissolution the degree of polymerization be 500, total esterification degree for 2.44 vinegar
The carrier solution for the calamine powder that cellulose acetate concentration is 9wt% is made in acid cellulose；Then it is by average grain diameter
0.196 μm of calamine powder and carrier solution is stirred using screw extruder, wherein the rate stirred is 200 revs/min,
Stirring when it is 0.9 hour a length of, wherein the diameter of calamine powder be 1.8nm, length be 3.8 μm, the diameter of calamine powder
For 24nm, 4.1 μm of length, cellulose acetate and calamine stone body mass ratio are 10:1, calamine mother liquor is made；It is finally that furnace is sweet
It is 1400 that stone 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 calamine mother liquor, wherein cellulose spinning fluid with
The mass ratio of calamine mother liquor is 8:1, functionality spinning solution is made, then through the extrusion in dry-jet wet spinning technique, solidification
And drafting step, cellulose/calamine composite fibre is made.
Test shows that cellulose/calamine composite fibre filament number is 0.9dtex, dry break strength 4cN/
dtex。
Claims (8)
1. a kind of cellulose/calamine composite fibre preparation method, it is characterized in that：Include the following steps：
(1) cellulose esters is dissolved using cellulose solvent, the carrier solution of calamine powder is made, the cellulose esters is acetic acid
Cellulose, cellulose acetate propionate or acetylbutyrylcellulose, the degree of polymerization of the cellulose esters are 200-450, total esterification degree
For 2.3-2.5；
(2) calamine powder is stirred with carrier solution, calamine mother liquor is made；
(3) calamine mother liquor is injected in cellulose spinning fluid, functionality spinning solution is made, then through extrusion, solidification and drawing-off,
Cellulose/calamine composite fibre is made；The degree of polymerization of cellulosic material is 500-1500 in the cellulose spinning fluid.
2. cellulose according to claim 1/calamine composite fibre preparation method, which is characterized in that the furnace is sweet
Mountain flour body average grain diameter is less than 0.2 μm.
3. cellulose according to claim 1/calamine composite fibre preparation method, which is characterized in that the fiber
Plain solvent is N-methylmorpholine-N- oxide/water or ionic liquid；
In the N-methylmorpholine-N- oxide/water, 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- first
Base imidazoles bromide.
4. cellulose according to claim 1/calamine composite fibre preparation method, which is characterized in that the carrier
The concentration of cellulose esters is 6~15wt% in solution；The mass ratio of the cellulose esters and calamine powder is 1-10:1；It is described
The concentration of cellulosic material is 6~15wt% in cellulose spinning fluid.
5. cellulose according to claim 1/calamine composite fibre preparation method, which is characterized in that the stirring
Equipment is screw extruder or kneader, and the rate of the stirring is 100-300 revs/min, the stirring when it is a length of
0.5-1 hours.
6. cellulose according to claim 1/calamine composite fibre preparation method, which is characterized in that the furnace is sweet
Mode in stone mother liquor injection cellulose spinning fluid is that calamine mother liquor is injected cellulose spinning fluid in a manner of adding online
In, the online adding set of calamine mother liquor is installed on cellulose spinning fluid transfer pipeline specially in the production line additional, wherein fine
The mass ratio for tieing up plain spinning solution and calamine mother liquor is 3-20:1.
7. cellulose according to claim 1/calamine composite fibre preparation method, which is characterized in that functionality is spun
It is wet spinning technology or dry-jet wet spinning technique that silk liquid, which prepares cellulose/calamine composite fibre technique,.
8. cellulose/calamine made from cellulose as described in claim 1/calamine composite fibre preparation method is compound
Fiber, it is characterized in that：The cellulose/calamine composite fibre filament number is 0.9-4.8dtex, and dry break strength is
1.7-4.5cN/dtex。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610838005.0A CN106149080B (en) | 2016-09-21 | 2016-09-21 | A kind of preparation method of cellulose/calamine composite fibre |
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| CN201610838005.0A CN106149080B (en) | 2016-09-21 | 2016-09-21 | A kind of preparation method of cellulose/calamine composite fibre |
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| Publication Number | Publication Date |
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| CN106149080A CN106149080A (en) | 2016-11-23 |
| CN106149080B true CN106149080B (en) | 2018-11-23 |
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| CN101736428A (en) * | 2009-12-23 | 2010-06-16 | 山东海龙股份有限公司 | Method for preparing Chinese medicinal cellulose fiber by solvent method |
| CN101851803A (en) * | 2010-05-28 | 2010-10-06 | 新乡化纤股份有限公司 | Health-care function viscose fiber and preparation method thereof |
| CN101985781A (en) * | 2010-10-19 | 2011-03-16 | 山东海龙股份有限公司 | Calamine cellulose fiber and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101736428A (en) * | 2009-12-23 | 2010-06-16 | 山东海龙股份有限公司 | Method for preparing Chinese medicinal cellulose fiber by solvent method |
| CN101851803A (en) * | 2010-05-28 | 2010-10-06 | 新乡化纤股份有限公司 | Health-care function viscose fiber and preparation method thereof |
| CN101985781A (en) * | 2010-10-19 | 2011-03-16 | 山东海龙股份有限公司 | Calamine cellulose fiber and preparation method thereof |
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| 磷系阻燃纤维素酯及其纤维的制备与阻燃性能研究;郑云波;《天津工业大学硕士学位论文》;20150730;第61页第1段、第15页最后一段 * |
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