CN106149080A - A kind of preparation method of cellulose/Calamina composite fibre - Google Patents
A kind of preparation method of cellulose/Calamina composite fibre Download PDFInfo
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- CN106149080A CN106149080A CN201610838005.0A CN201610838005A CN106149080A CN 106149080 A CN106149080 A CN 106149080A CN 201610838005 A CN201610838005 A CN 201610838005A CN 106149080 A CN106149080 A CN 106149080A
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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 the preparation method of a kind of cellulose/Calamina composite fibre, comprise the steps: to use cellulose solvent to dissolve cellulose esters, prepare the carrier solution of Calamina powder body；The Strong shear effect provided by mixing plant, is mixed Calamina powder body with carrier solution, prepares Calamina mother solution；In the way of online interpolation, Calamina mother solution is injected cellulose spinning fluid, and spinning liquid is extruded, solidification forming and drawing-off, prepares cellulose/Calamina composite fibre.The present invention is directed to Calamina powder body difficult with the mixed uniformly problem of high viscosity spinning liquid, use Calamina mother solution to inject spinning liquid, and then the mode of spinning technique prepare cellulose/Calamina composite fibre.Mother solution carrier used by the present invention shapes with fibre solidification, enters solvent and coagulating bath system without Additional auxiliaries.The manufacturing process of the present invention is simple, flexible, efficient, can realize the production of cellulose/Calamina composite fibre based on conventional production line.
Description
Technical field
The present invention relates to regenerated fiber field, be specifically related to the preparation method of a kind of cellulose/Calamina composite fibre.
Background technology
The cellulose fibres such as cotton, viscose rayon, lyocell fiber have excellent pro-skin performance, are widely used in next to the skin
Medicated clothing.In order to increase the function of cellulose fibre, patent ZL201010511031.5 (calamine cellulose fiber and preparation side thereof
Method) propose the preparation method of a kind of functional fibre cellulose fiber, concrete grammar is by Calamina slurry and cellulose/ion liquid
Spinning liquid mixes, and prepares cellulose/Calamina composite fibre through wet spinning shaping.Owing to Calamina is to multiple contact dermatitis
Having therapeutical effect, functional fibre can prevent dermopathic generation, also can alleviate the severe pruritus dermatoses such as urticaria, miliaria
Symptom.
Being mixed with cellulose spinning fluid by the Calamina powder body such as Calamina, both mixing uniformity are asking of overriding concern
Topic.Owing to cellulose solution viscosity is high, cause powder body dispersive process difficulty big, high to equipment requirements.Additionally, there may be powder body easy
In depositing, reunite, mix uneven problem, cause the instability of spinneret orifice blocking and fibre property.In order to improve Calamina
With the dispersing uniformity of spinning solution, patent ZL201010511031.5 by Calamina and amine cation type surfactant,
Silicon system cationoid surfactant, sodium tripolyphosphate carry out premixing, make suspension or the Calamina slurry of emulsion state.
Suspension, emulsion are mixed with cellulose spinning fluid the dispersing uniformity that can improve functional additive, but surface activity
The auxiliary agents such as agent can enter coagulating bath, affects the normal recovery of solvent and coagulator, increases cost recovery.Residual helping in the fibre
Agent also can affect every physicochemical property of fiber, there is also the possibility that auxiliary agent oozes out during use.
Realize the dispersed of Calamina powder body the most efficiently, reduce Calamina powder body adding procedure to original shaping work
The interference of skill, is that cellulose/Calamina composite fibre produces the technical bottleneck needing to break through.
Summary of the invention
The present invention be directed to the deficiencies in the prior art, it is provided that the preparation method of a kind of cellulose/Calamina composite fibre, will
Calamina powder body is mixed homogeneously with cellulose ester solution, prepares Calamina mother solution, by Calamina mother solution with the online method added
Inject cellulose spinning fluid, and then spinning technique, prepare cellulose/Calamina composite fibre.
The preparation method of a kind of cellulose/Calamina composite fibre of the present invention, comprises the steps:
(1) use cellulose solvent to dissolve cellulose esters, prepare the carrier solution of Calamina powder body；
(2) Calamina powder body is mixed with carrier solution stirring, prepare Calamina mother solution；
(3) Calamina mother solution is injected in cellulose spinning fluid, prepare functional spinning liquid, then through squeezing
Go out, solidify and drawing-off, prepare cellulose/Calamina composite fibre.
The preparation method of cellulose/Calamina composite fibre as above, described cellulose esters is cellulose acetate, vinegar
Acid cellulose propionate or acetylbutyrylcellulose, the degree of polymerization of described cellulose esters is 200-1000, and total esterification degree is 2.3-
2.5；In described cellulose spinning fluid, the degree of polymerization of cellulosic material is 500-1500.
The preparation method of cellulose/Calamina composite fibre as above, described Calamina powder body mean diameter is less than
0.2μm。
The preparation method of cellulose/Calamina composite fibre as above, described cellulose solvent be N-methylmorpholine-
N-oxide water or ionic liquid；
Described N-methylmorpholine-N-oxide/aqueous systems, wherein, the ratio shared by water is less than 15wt%；
Described ionic liquid be 1-butyl-3-Methylimidazole. villaumite, 1-ethyl-3-methylimidazole acetate or 1-butyl-
3-Methylimidazole. bromide.
The preparation method of cellulose/Calamina composite fibre as above, in described carrier solution, cellulose esters is dense
Degree is 6～15wt%；Described cellulose esters is 1-10:1 with the mass ratio of Calamina powder body；Fiber in described cellulose spinning fluid
The concentration of element raw material is 6～15wt%.
The preparation method of cellulose/Calamina composite fibre as above, the equipment of described stirring is Screw Extrusion
Machine or kneader, the speed of described stirring is 100-300 rev/min, described stirring time a length of 0.5-1 hour.
The preparation method of cellulose/Calamina composite fibre as above, described Calamina mother solution injects cellulose and spins
Mode in silk liquid is to inject in cellulose spinning fluid by Calamina mother solution in the way of online interpolation, is specially on a production line
Cellulose spinning fluid transfer pipeline on install the online adding set of Calamina mother solution additional, wherein cellulose spinning fluid is female with Calamina
Liquid mass ratio is 3-20:1.
The preparation method of cellulose/Calamina composite fibre as above, described functional spinning liquid prepare cellulose/
The technique of Calamina composite fibre is wet spinning technology or dry-jet wet spinning technique.
Cellulose/Calamina composite fibre that the preparation method of cellulose/Calamina composite fibre as above prepares,
Described cellulose/Calamina composite fibre filament number is 0.9-4.8dtex, and dry break strength is 1.7-4.5cN/dtex.
Cellulose/Calamina composite fibre as above, described composite fibre has auxiliary to skin pruritus, scytitis
Therapeutical effect.
The principle of the present invention:
Cellulose is made up 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.Due to cellulose molecular structure, the viscosity of cellulose solution is higher, such as,
Cellulosic degree of polymerization is 569, and concentration is the cellulose/NMMO/H of 12.9wt%2O solution, temperature is Zero shear viscosity when 85 DEG C
For 8670Pa.s；Cellulosic degree of polymerization is 569, and concentration is the cellulose/1-butyl-3-Methylimidazole. villaumite of 10.4wt%
([BMIM] Cl) solution, temperature is that Zero shear viscosity when 85 DEG C reaches 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 dispersed that high viscosity characteristic makes Calamina powder body be difficult in cellulose solution, mixing apparatus
Ask the harshest.
Owing to the hydroxyl quantity on cellulose esters strand is less than the hydroxyl on cellulose molecular chain, cellulose esters strand
The interior interaction also phase factor with molecule interchain reduces, and therefore the viscosity of cellulose ester solution is less than cellulose solution.Additionally, it is fine
Dimension element ester is close to consistent with the structure of cellulose, and both are capable of dissolving each other of molecular level.
Based on this, the present invention select cellulose esters as the carrying body of Calamina powder body, as Calamina powder body and fiber
The element mixed uniformly bridge of spinning liquid.Cellulose esters is utilized to be more easy to and Calamina powder body, the mixed uniformly feature of cellulose solution,
Play intermediation, promote the mixing of Calamina powder body and cellulose spinning fluid.
Beneficial effect:
(1) utilize the viscosity of cellulose ester solution less than cellulose spinning fluid, be more easy to mixed uniformly with Calamina powder body
Advantage, select cellulose esters as the matrix of Calamina mother solution, be prepared for Calamina powder body be uniformly dispersed, the stove of stable in properties sweet
Stone mother solution.Calamina mother solution can inject the spinning liquid delivery system of generally conventional regenerated celulose fibre by online adding set
System, manufactures cellulose/Calamina composite fibre easily and flexibly.
(2) molecular structure of cellulose esters is similar to cellulose, and both can realize dissolving each other of molecular level.Process of setting
With cellulose in the lump solidification forming and do not enter coagulating bath, enter coagulating bath without extra additive, do not increase solvent and coagulating bath
The burden reclaimed.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/Calamina composite fibre, method brief introduction, workable.
(3) cellulose/Calamina composite fibre can prevent dermopathic generation, has auxiliary to skin pruritus, scytitis
Help therapeutical effect.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate this
Bright rather than limit the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, art technology
The present invention can be made various changes or modifications by personnel, and these equivalent form of values fall within the application appended claims equally and limited
Fixed scope.
Embodiment 1
The preparation method of a kind of cellulose/Calamina composite fibre, comprises the steps:
(NMMO)/(wherein the ratio shared by water is water to use cellulose solvent N-methylmorpholine-N-oxide
13.8wt%) dissolving the degree of polymerization is 200, and total esterification degree is the cellulose acetate of 2.3, and preparing cellulose acetate concentration is 6wt%
The carrier solution of Calamina powder body；Then screw rod is used to squeeze with carrier solution the Calamina powder body that mean diameter is 0.19 μm
Go out machine stirring mixing, the speed wherein stirred is 100 revs/min, stirring time a length of 0.5 hour, cellulose acetate and Calamina
The mass ratio of powder body is 1:1, prepares Calamina mother solution；Finally in the way of online interpolation, Calamina mother solution being injected the degree of polymerization is
500, concentration is in the cellulose spinning fluid of 6wt%, is specially on cellulose spinning fluid transfer pipeline on a production line and installs additional
The online adding set of Calamina mother solution, wherein cellulose spinning fluid is 3:1 with the mass ratio of Calamina mother solution, prepares functional spinning
Silk liquid, the then extrusion in wet spinning technology, solidification and drafting step, prepare cellulose/Calamina composite fibre.
Test shows, the filament number of cellulose/Calamina composite fibre is 0.9dtex, and dry break strength is
1.7cN/dtex。
Embodiment 2
The preparation method of a kind of cellulose/Calamina composite fibre, comprises the steps:
(NMMO)/(wherein the ratio shared by water is water to use cellulose solvent N-methylmorpholine-N-oxide
13.4wt%) dissolving the degree of polymerization is 1000, and total esterification degree is the cellulose acetate propionate of 2.5, prepares cellulose acetate propionate dense
Degree is the carrier solution of the Calamina powder body of 15wt%；Then by Calamina powder body that mean diameter is 0.18 μm and carrier solution
Use kneader stirring mixing, the speed wherein stirred is 300 revs/min, stirring time a length of 1 hour, cellulose acetate propionate
It is 9:1 with the mass ratio of Calamina powder body, prepares Calamina mother solution；Finally Calamina mother solution is injected in the way of online interpolation
The degree of polymerization is 1500, and concentration is in the cellulose spinning fluid of 15wt%, is specially cellulose spinning fluid conveying on a production line
Installing the online adding set of Calamina mother solution on pipeline additional, wherein cellulose spinning fluid is 20:1 with the mass ratio of Calamina mother solution,
Prepare functional spinning liquid, the then extrusion in dry-jet wet spinning technique, solidification and drafting step, prepare cellulose/stove
Calamina composite fibre.
Test shows, the filament number of cellulose/Calamina composite fibre is 4.8dtex, and dry break strength is
1.7cN/dtex。
Embodiment 3
The preparation method of a kind of cellulose/Calamina composite fibre, comprises the steps:
Using cellulose solvent 1-butyl-3-Methylimidazole. villaumite to dissolve the degree of polymerization is 300, and total esterification degree is the vinegar of 2.4
Acid cellulose butyrate, prepares the carrier solution of the Calamina powder body that acetylbutyrylcellulose concentration is 7wt%；Then by average particle
Footpath is that Calamina powder body and the carrier solution of 0.19 μm use screw extruder stirring to mix, the speed wherein stirred is 200 turns/
Point, stirring time a length of 0.6 hour, the mass ratio of acetylbutyrylcellulose and Calamina powder body is 10:1, prepares Calamina female
Liquid；Calamina mother solution finally injecting in the way of online interpolation the degree of polymerization for 600, concentration is the cellulose spinning fluid of 8wt%
In, it is specially on cellulose spinning fluid transfer pipeline on a production line and installs the online adding set of Calamina mother solution additional, wherein fine
Dimension element spinning liquid is 7:1 with the mass ratio of Calamina mother solution, prepares functional spinning liquid, then squeezing through wet spinning technology
Go out, solidify and drafting step, prepare cellulose/Calamina composite fibre.
Test shows, the filament number of cellulose/Calamina composite fibre is 0.9dtex, and dry break strength is
4.5cN/dtex。
Embodiment 4
The preparation method of a kind of cellulose/Calamina composite fibre, comprises the steps:
Using cellulose solvent 1-ethyl-3-methylimidazole acetate to dissolve the degree of polymerization is 400, and total esterification degree is 2.35
Acetylbutyrylcellulose, prepares the carrier solution of the Calamina powder body that acetylbutyrylcellulose concentration is 8wt%；Then will be average
Particle diameter is that Calamina powder body and the carrier solution of 0.192 μm use kneader stirring to mix, the speed wherein stirred is 150 turns/
Point, stirring time a length of 0.7 hour, the mass ratio of acetylbutyrylcellulose and Calamina powder body is 5:1, prepares Calamina female
Liquid；Calamina mother solution finally injecting in the way of online interpolation the degree of polymerization for 900, concentration is the cellulose spinning fluid of 7wt%
In, it is specially on cellulose spinning fluid transfer pipeline on a production line and installs the online adding set of Calamina mother solution additional, wherein fine
Dimension element spinning liquid is 7:1 with the mass ratio of Calamina mother solution, prepares functional spinning liquid, then in dry-jet wet spinning technique
Extrusion, solidification and drafting step, prepare cellulose/Calamina composite fibre.
Test shows, the filament number of cellulose/Calamina composite fibre is 2dtex, and dry break strength is 3cN/
dtex。
Embodiment 5
The preparation method of a kind of cellulose/Calamina composite fibre, comprises the steps:
Using cellulose solvent 1-ethyl-3-methylimidazole acetate to dissolve the degree of polymerization is 400, and total esterification degree is 2.39
Acetylbutyrylcellulose, prepares the carrier solution of the Calamina powder body that acetylbutyrylcellulose concentration is 10wt%；Then will be flat
All particle diameters are that the Calamina powder body of 0.189 μm uses screw extruder stirring to mix with carrier solution, and the speed wherein stirred is
250 revs/min, stirring time a length of 0.8 hour, the mass ratio of acetylbutyrylcellulose and Calamina powder body is 8:1, prepares stove sweet
Stone mother solution；Calamina mother solution finally injecting in the way of online interpolation the degree of polymerization for 900, concentration is that the cellulose of 9wt% spins
In silk liquid, it is specially on cellulose spinning fluid transfer pipeline on a production line and installs the online adding set of Calamina mother solution additional, its
Middle cellulose spinning fluid is 6:1 with the mass ratio of Calamina mother solution, prepares functional spinning liquid, then in wet spinning technology
Extrusion, solidification and drafting step, prepare cellulose/Calamina composite fibre.
Test shows, the filament number of cellulose/Calamina composite fibre is 2.8dtex, and dry break strength is
3.5cN/dtex。
Embodiment 6
The preparation method of a kind of cellulose/Calamina composite fibre, comprises the steps:
Using cellulose solvent 1-butyl-3-Methylimidazole. bromide to dissolve the degree of polymerization is 850, and total esterification degree is the vinegar of 2.3
Acid cellulose butyrate, prepares the carrier solution of the Calamina powder body that acetylbutyrylcellulose concentration is 11wt%；Then will be average
Particle diameter is that the Calamina powder body of 0.191 μm uses screw extruder stirring to mix with carrier solution, and the speed wherein stirred is 200
Rev/min, stirring time a length of 0.7 hour, the mass ratio of acetylbutyrylcellulose and Calamina powder body is 7:1, prepares Calamina
Mother solution；Calamina mother solution finally injecting in the way of online interpolation the degree of polymerization for 900, concentration is the cellulose spinning of 12wt%
In liquid, it is specially on cellulose spinning fluid transfer pipeline on a production line and installs the online adding set of Calamina mother solution additional, wherein
Cellulose spinning fluid is 12:1 with the mass ratio of Calamina mother solution, prepares functional spinning liquid, then through dry-jet wet spinning work
Extrusion, solidification and drafting step in skill, prepares cellulose/Calamina composite fibre.
Test shows, the filament number of cellulose/Calamina composite fibre is 3.8dtex, and dry break strength is
2.5cN/dtex。
Embodiment 7
The preparation method of a kind of cellulose/Calamina composite fibre, comprises the steps:
Using cellulose solvent 1-ethyl-3-methylimidazole acetate to dissolve the degree of polymerization is 450, and total esterification degree is 2.45
Cellulose acetate propionate, prepares the carrier solution of the Calamina powder body that cellulose acetate propionate concentration is 14wt%；Then will be flat
All particle diameters are that the Calamina powder body of 0.19 μm uses screw extruder stirring to mix with carrier solution, and the speed wherein stirred is
250 revs/min, stirring time a length of 0.8 hour, the mass ratio of cellulose acetate propionate and Calamina powder body is 3:1, prepares stove sweet
Stone mother solution；Calamina mother solution finally injecting in the way of online interpolation the degree of polymerization for 1300, concentration is the cellulose of 14wt%
In spinning liquid, it is specially on cellulose spinning fluid transfer pipeline on a production line and installs the online adding set of Calamina mother solution additional,
Wherein cellulose spinning fluid is 10:1 with the mass ratio of Calamina mother solution, prepares functional spinning liquid, then through dry spray Wet-spinning
Extrusion, solidification and drafting step in silk technique, prepares cellulose/Calamina composite fibre.
Test shows, the filament number of cellulose/Calamina composite fibre is 1.8dtex, and dry break strength is
2.5cN/dtex。
Embodiment 8
The preparation method of a kind of cellulose/Calamina composite fibre, comprises the steps:
Using cellulose solvent 1-butyl-3-Methylimidazole. bromide to dissolve the degree of polymerization is 900, and total esterification degree is the vinegar of 2.3
Acid cellulose propionate, prepares the carrier solution of the Calamina powder body that cellulose acetate propionate concentration is 14wt%；Then will be average
Particle diameter is that Calamina powder body and the carrier solution of 0.194 μm use kneader stirring to mix, the speed wherein stirred is 200 turns/
Point, stirring time a length of 0.9 hour, the mass ratio of cellulose acetate propionate and Calamina powder body is 6:1, prepares Calamina female
Liquid；Calamina mother solution finally injecting in the way of online interpolation the degree of polymerization for 1400, concentration is the cellulose spinning of 12wt%
In liquid, it is specially on cellulose spinning fluid transfer pipeline on a production line and installs the online adding set of Calamina mother solution additional, wherein
Cellulose spinning fluid is 14:1 with the mass ratio of Calamina mother solution, prepares functional spinning liquid, then in wet spinning technology
Extrusion, solidification and drafting step, prepare cellulose/Calamina composite fibre.
Test shows, the filament number of cellulose/Calamina composite fibre is 3dtex, and dry break strength is 2.4cN/
dtex。
Embodiment 9
The preparation method of a kind of cellulose/Calamina composite fibre, comprises the steps:
Using cellulose solvent 1-butyl-3-Methylimidazole. bromide to dissolve the degree of polymerization is 350, and total esterification degree is the vinegar of 2.3
Acid cellulose propionate, prepares the carrier solution of the Calamina powder body that cellulose acetate propionate concentration is 12wt%；Then will be average
Particle diameter is that Calamina powder body and the carrier solution of 0.18 μm use kneader stirring to mix, the speed wherein stirred is 200 turns/
Point, stirring time a length of 0.9 hour, the mass ratio of cellulose acetate propionate and Calamina powder body is 8:1, prepares Calamina female
Liquid；Calamina mother solution finally injecting in the way of online interpolation the degree of polymerization for 800, concentration is the cellulose spinning fluid of 12wt%
In, it is specially on cellulose spinning fluid transfer pipeline on a production line and installs the online adding set of Calamina mother solution additional, wherein fine
Dimension element spinning liquid is 5:1 with the mass ratio of Calamina mother solution, prepares functional spinning liquid, then in dry-jet wet spinning technique
Extrusion, solidification and drafting step, prepare cellulose/Calamina composite fibre.
Test shows, the filament number of cellulose/Calamina composite fibre is 3.2dtex, and dry break strength is
2.1cN/dtex。
Embodiment 10
The preparation method of a kind of cellulose/Calamina composite fibre, comprises the steps:
Using cellulose solvent 1-butyl-3-Methylimidazole. villaumite to dissolve the degree of polymerization is 600, and total esterification degree is the vinegar of 2.3
Acid cellulose, prepares the carrier solution of the Calamina powder body that cellulose acetate concentration is 13wt%；Then by mean diameter it is
The Calamina powder body of 0.195 μm uses screw extruder stirring to mix with carrier solution, and the speed wherein stirred is 200 revs/min,
Stirring time a length of 0.7 hour, wherein a diameter of 1.2nm of Calamina powder body, a length of 4 μm, Calamina powder body a diameter of
28nm, length 4.5 μm, cellulose acetate and calamine stone body mass ratio are 4:1, prepare Calamina mother solution；Finally by Calamina
Mother solution injects the degree of polymerization for 1000 in the way of online interpolation, and concentration is in the cellulose spinning fluid of 8wt%, is specially and is producing
Installing the online adding set of Calamina mother solution on cellulose spinning fluid transfer pipeline on line additional, wherein cellulose spinning fluid is sweet with stove
The mass ratio of stone mother solution is 5:1, prepares functional spinning liquid, the then extrusion in wet spinning technology, solidification and drawing-off step
Suddenly, cellulose/Calamina composite fibre is prepared.
Test shows, the filament number of cellulose/Calamina composite fibre is 2.5dtex, and dry break strength is
3.4cN/dtex。
Embodiment 11
The preparation method of a kind of cellulose/Calamina composite fibre, comprises the steps:
Using cellulose solvent 1-butyl-3-Methylimidazole. villaumite to dissolve the degree of polymerization is 500, and total esterification degree is the vinegar of 2.44
Acid cellulose, prepares the carrier solution of the Calamina powder body that cellulose acetate concentration is 9wt%；Then by mean diameter it is
The Calamina powder body of 0.196 μm uses screw extruder stirring to mix with carrier solution, and the speed wherein stirred is 200 revs/min,
Stirring time a length of 0.9 hour, wherein a diameter of 1.8nm of Calamina powder body, a length of 3.8 μm, the diameter of Calamina powder body
For 24nm, length 4.1 μm, cellulose acetate and calamine stone body mass ratio are 10:1, prepare Calamina mother solution；Finally that stove is sweet
Stone mother solution injects the degree of polymerization for 1400 in the way of online interpolation, and concentration is in the cellulose spinning fluid of 14wt%, is specially and exists
Install the online adding set of Calamina mother solution on cellulose spinning fluid transfer pipeline on production line additional, wherein cellulose spinning fluid with
The mass ratio of Calamina mother solution is 8:1, prepares functional spinning liquid, the then extrusion in dry-jet wet spinning technique, solidification
And drafting step, prepare cellulose/Calamina composite fibre.
Test shows, the filament number of cellulose/Calamina composite fibre is 0.9dtex, and dry break strength is 4cN/
dtex。
Claims (9)
1. a preparation method for cellulose/Calamina composite fibre, is characterized in that: comprise the steps:
(1) use cellulose solvent to dissolve cellulose esters, prepare the carrier solution of Calamina powder body；
(2) Calamina powder body is mixed with carrier solution stirring, prepare Calamina mother solution；
(3) Calamina mother solution is injected in cellulose spinning fluid, prepared functional spinning liquid, the most extruded, solidification and drawing-off,
Prepare cellulose/Calamina composite fibre.
The preparation method of cellulose the most according to claim 1/Calamina composite fibre, it is characterised in that described fiber
Element ester is cellulose acetate, cellulose acetate propionate or acetylbutyrylcellulose, and the degree of polymerization of described cellulose esters is 200-
1000, total esterification degree is 2.3-2.5；In described cellulose spinning fluid, the degree of polymerization of cellulosic material is 500-1500.
The preparation method of cellulose the most according to claim 1/Calamina composite fibre, it is characterised in that described stove is sweet
Stone powder body mean diameter is less than 0.2 μm.
The preparation method of cellulose the most according to claim 1/Calamina composite fibre, it is characterised in that described fiber
Element solvent is N-methylmorpholine-N-oxide water or ionic liquid；
Described N-methylmorpholine-N-oxide/aqueous systems, wherein, the ratio shared by water is less than 15wt%；
Described ionic liquid is 1-butyl-3-Methylimidazole. villaumite, 1-ethyl-3-methylimidazole acetate or 1-butyl-3-first
Base imidazoles bromide.
The preparation method of cellulose the most according to claim 1/Calamina composite fibre, it is characterised in that described carrier
In solution, the concentration of cellulose esters is 6～15wt%；Described cellulose esters is 1-10:1 with the mass ratio of Calamina powder body；Described
In cellulose spinning fluid, the concentration of cellulosic material is 6～15wt%.
The preparation method of cellulose the most according to claim 1/Calamina composite fibre, it is characterised in that described stirring
Equipment be screw extruder or kneader, the speed of described stirring is 100-300 rev/min, described stirring time a length of
0.5-1 hour.
The preparation method of cellulose the most according to claim 1/Calamina composite fibre, it is characterised in that described stove is sweet
It is that in the way of online interpolation, Calamina mother solution is injected cellulose spinning fluid that stone mother solution injects the mode in cellulose spinning fluid
In, it is specially on cellulose spinning fluid transfer pipeline on a production line and installs the online adding set of Calamina mother solution additional, wherein fine
Dimension element spinning liquid is 3-20:1 with the mass ratio of Calamina mother solution.
The preparation method of cellulose the most according to claim 1/Calamina composite fibre, it is characterised in that described function
The technique of cellulose/Calamina composite fibre prepared by property spinning liquid is wet spinning technology or dry-jet wet spinning technique.
9. cellulose/Calamina that the preparation method of cellulose/Calamina composite fibre as claimed in claim 1 prepares is combined
Fiber, is characterized in that: described cellulose/Calamina composite fibre filament number is 0.9-4.8dtex, and dry break strength is
1.7-4.5cN/dtex。
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