CN106283268A - A kind of preparation method of cellulose/calcium alginate blended fiber - Google Patents
A kind of preparation method of cellulose/calcium alginate blended fiber Download PDFInfo
- Publication number
- CN106283268A CN106283268A CN201610848098.5A CN201610848098A CN106283268A CN 106283268 A CN106283268 A CN 106283268A CN 201610848098 A CN201610848098 A CN 201610848098A CN 106283268 A CN106283268 A CN 106283268A
- Authority
- CN
- China
- Prior art keywords
- cellulose
- calcium alginate
- blended fiber
- preparation
- spinning
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
-
- 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
-
- 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
- D01D5/04—Dry spinning methods
-
- 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
-
- 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
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
-
- 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
-
- 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
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/12—Applications used for fibers
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Manufacturing & Machinery (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention relates to the preparation method of a kind of cellulose/calcium alginate blended fiber, particularly relate to the preparation method of a kind of Wound dressing cellulose/calcium alginate blended fiber.Key step includes: (1) is uniform with N methyl morpholine N oxide (NMMO) aqueous solution by cellulose, mixes with sodium alginate soln, be simultaneously introduced calcium chloride and prepare cellulose/calcium alginate blend solution after complete swelling.(2) thin film evaporation mode is used to prepare cellulose/calcium alginate spinning liquid.(3) use dry-jet wet-spinning to accompany by ultrasonication and prepare cellulose/calcium alginate blended fiber.This blended fiber is used for manufacturing wound dressing, feature is that the calcium alginate of blended fiber is evenly distributed, grain size is less than 100nm, filament number is 1.3～3.5dtex, dry break strength 2.0～3.5cN/dtex, wet break strength is 1.5～3.0cN/dtex, and saturated moisture absorption regain is 20～30%, and water retention is 70～80%.
Description
Technical field
The invention belongs to blended fiber technical field, relate to the preparation method of a kind of cellulose/calcium alginate blended fiber,
Particularly relate to the preparation method of a kind of Wound dressing cellulose/calcium alginate blended fiber.
Background technology
Calcium alginate fibre with there is gel characteristic natural sea calcium alginate as raw material, it is possible to absorb a large amount of wound fluid
And keep wound surface moist environment, it is used as novel Wound dressing.But calcium alginate fibre hygrometric state mechanical strength is poor, and wound surface is wet
Under environment, fibre structure destroys, and have impact on the scope of application and the ease of use of calcium alginate dressing.Cellulose is nature storage
The natural polymer that amount is maximum, the cellulose fibre such as cotton, viscose rayon is widely used traditional dressing material.But cellulose
Fiber dressing air-moisture-permeable, is unfavorable for the holding of wound moist environment, causes wound surface incrustation and dressing to bond.Set fiber element is fine
Structural intergrity under dimension hygrometric state condition will be the desirable feedstock of dressing with the fibrous material of alginic acid fibre moisture-absorbing moisture-keeping function.
The exploitation of cellulose/calcium alginate blended fiber is the feasible method realizing above-mentioned requirements.Current published money
In material, sodium alginate soln is blended by Patents with cellulose xanthate ester, alkali cellulose, with the process route of viscose rayon
Prepare cellulose/calcium alginate blended fiber (patent No.: 200610044596 cellulose/alginate composite fibers and system thereof
Preparation Method；The patent No.: the preparation method of 201,010,501,609 1 kinds of alginate/cellulose composite fibres).Prepared by this kind of method
Cellulose/calcium alginate blended fiber, performance of keeping humidity is better than viscose rayon, and hygrometric state mechanical strength is better than calcium alginate fibre.
But owing to the fracture strength of viscose rayon self is limited, (common binder fiber dry break strength is 1.6～2.7cN/dtex, wet
State fracture strength be its about 50%), the mechanical strength of blended fiber is the most on the low side, and (wet break strength is less than 1.2cN/
dtex).The pollution hidden trouble that cellulose viscose manufacturing technique exists also is the obstacle of its sustainable development.
Lyocell fiber is with N-methylmorpholine-N-oxide (NMMO)/H2O solution is direct solvent, dry-jet wet-spinning system
Standby regenerated celulose fibre, the dry break strength of Lyocell fiber is 3.0～5.0cN/dtex, and wet break strength is
They are 70～80% years old.On this basis, Lyocell fiber main manufacturer Lenzing company that Sargassum granule is mixed into cellulose is molten
Liquid, is prepared for cellulose/Sargassum composite fibre.The skin compatible material such as multiple alginate, protein are contained, compound fibre due to Sargassum
Dimension is favored by user in the field of taking.But this kind of composite fibre be not for the Demand Design production of Wound dressing, and Sargassum becomes
Divide complexity, be not particularly suited for wound surface.Also there is the patent (patent No.: 200910016898 bacterial cellulose/sodium alginate composite fibers
And preparation method thereof) direct solvent using ionic liquid as cellulose is proposed, sodium alginate micro-nano powder is mixed into fiber
Element/ionic liquid solution, dry-jet wet-spinning prepares cellulose/sodium alginate blended fiber.What above two preparation method existed asks
Topic is, i.e. Sargassum and the difficult and full-bodied cellulose solution of sodium alginate powder body is dispersed, Sargassum or sodium alginate powder body
It is prone to reunite, affects the stability of fiber forming process and properties of product.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of cellulose/calcium alginate blended fiber.The present invention's is obvious
Feature is that uniformly and the NMMO aqueous solution that cellulose and water content are 40～60wt% is made cellulose complete swelling；By molten
Swollen thing mixes with sodium alginate soln, and addition calcium chloride prepares cellulose/calcium alginate blend in mixed process；Use
Thin film evaporation mode makes the moisture of mixed liquor be reduced to below 15wt%, prepares cellulose/calcium alginate spinning liquid；Use dry spray
Wet spinning accompanies by ultrasonication and prepares cellulose/calcium alginate blended fiber.
The preparation method of a kind of cellulose/calcium alginate blended fiber of the present invention comprises the steps:
(1) cellulose pulp uniformly and is made cellulose complete swelling with NMMO aqueous solution；Meanwhile, preparation alginic acid
Sodium solution；
(2) swelling thing is mixed with sodium alginate soln, and in mixed process, add calcium chloride；
(3) moisture making step gained mixed liquor is reduced to below 15wt%, prepares cellulose/calcium alginate spinning liquid；
(4) through dry-jet wet-spinning, cellulose/calcium alginate blended fiber is prepared.
As preferred technical scheme:
The preparation method of a kind of cellulose/calcium alginate blended fiber as above, in described dry-jet wet-spinning, fiber
Element/calcium alginate spinning liquid accompanies by ultrasonication when spinneret orifice is extruded.
The preparation method of a kind of cellulose/calcium alginate blended fiber as above, described ultrasonication uses ultrasonic
Generator, supersonic frequency is 20～35kHz, and power is 20～300W.
The preparation method of a kind of cellulose/calcium alginate blended fiber as above, fiber in described cellulose pulp
The degree of polymerization of element is 400～1000, and the water content of cellulose pulp is 4～6wt%；The water content of described NMMO aqueous solution is 40
～60wt%；Described swelling temperature is 60～80 DEG C.
The preparation method of a kind of cellulose/calcium alginate blended fiber as above, described sodium alginate soln dense
Degree is 0.5～5wt%；The amount of described sodium alginate is 0.1～15wt% of cellulose in described cellulose pulp；Described chlorination
Calcium is 1:2 with the mol ratio of sodium ion in described sodium alginate soln；Described calcium chloride can add with the form of powder body or aqueous solution
Entering, the grain size of calcium chloride powder body is less than 1 μm, and the concentration of calcium chloride solution is 2～5wt%.
The preparation method of a kind of cellulose/calcium alginate blended fiber as above, described moisture is reduced to thin film and steams
Originating party formula, specifically uses membrane evaporator, and technological parameter is: solution temperature is 85～120 DEG C, and vacuum is-8.0 × 10-4～-
9.0×10-4Pa。
The preparation method of a kind of cellulose/calcium alginate blended fiber as above, described cellulose/calcium alginate spins
In silk liquid, the total amount of cellulose and calcium alginate accounts for the 6～15wt% of spinning liquid.
The preparation method of a kind of cellulose/calcium alginate blended fiber as above, described dry-jet wet-spinning, make spinning thin
In flowing out spinneret orifice 50mm, temperature is reduced to 5～10 DEG C；Be specially use ring coldblast, the pathogenic wind-warm of described ring coldblast be-5～
5 DEG C, blowing flow is 200～400L/min, and humidity is 10～60%.
The preparation method of a kind of cellulose/calcium alginate blended fiber as above, the technique ginseng of described dry-jet wet-spinning
Number is: the extrusion temperature of spinning liquid is 85～120 DEG C, and air layer a length of 10～100mm, air layer temperature is-5～5 DEG C；Solidifying
Gu bath consists of NMMO and water, NMMO content is 1～10wt%, and coagulation bath temperature scope is 5～25 DEG C；Baking temperature be 70～
150℃。
The preparation method of a kind of cellulose/calcium alginate blended fiber as above, described cellulose/calcium alginate is common
The calcium alginate of combined filament is evenly distributed, and grain size is less than 100nm, and filament number is 1.3～3.5dtex, and dry state fracture is strong
Degree 2.0～3.5cN/dtex, wet break strength is 1.5～3.0cN/dtex, and saturated moisture absorption regain is 20～30%, water conservation
Rate is 70～80%.
The present invention adds calcium chloride at the swelling thing of cellulose with sodium alginate soln mix stages, and its principle is as follows, is blended
The Blending Processes of thing is the dynamic process of " dispersion " and " gathering ", and screw extruder provides Strong shear active force can make point
Dephasing ruptures, and phase size reduces.Add calcium chloride in the process, the sodium alginate under Strong shear power effect can be made to be cured as
Calcium alginate nano-particle, is effectively improved the dispersing uniformity of cellulose and calcium alginate, is prepared for grain size and is less than
The calcium alginate granule of 100nm.
The spinning liquid spinneret orifice extrusion of the present invention accompanies by ultrasound functions, and its principle is as follows, cellulose/calcium alginate spinning liquid
In calcium alginate nano-particle specific surface area and surface can be big, it is easy to reunite.For the problems referred to above, spinning liquid spray webbing of the present invention
Hole extrusion accompanies by ultrasound wave, and the powerful shearing force produced by ultrasound wave " ultrasonic cavitation " phenomenon destroys calcium alginate nano-particle
Reunion.
Beneficial effect
Compared with the prior art, the cellulose of the present invention/calcium alginate blended fiber two phase dispersing uniformity is good, dispersion phase
Phase size is little, and therefore the mechanical strength of fiber is high, moisture-absorbing moisture-keeping performance is good.
The present invention without changing the composition of Lyocell fiber coagulating bath, the recovery of beneficially NMMO solvent.Existing Lyocell
Fiberline just can be used for the production of fiber of the present invention through simple transformation.
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/calcium alginate blended fiber, under the conditions of 60 DEG C, by the fibre of water content 4wt%
Dimension element pulp uniformly and makes cellulose complete swelling with the NMMO aqueous solution of water content 40wt%, fiber in cellulose pulp
The degree of polymerization of element is 400；Swelling thing is mixed with the sodium alginate soln that concentration is 0.5wt%, and adds in mixed process
Grain size is that the calcium chloride powder body of 0.8um prepares cellulose/calcium alginate blend solution, and the amount of sodium alginate is cellulose slurry
The 1wt% of cellulose in the dregs of rice, calcium chloride is 1:2 with the mol ratio of sodium ion in sodium alginate soln；It is 85 DEG C in solution temperature,
Vacuum is-8.0 × 10-4Under conditions of Pa, membrane evaporator is used to be reduced by the moisture of cellulose/calcium alginate blend solution
Preparing cellulose/calcium alginate spinning liquid to 15wt%, the total amount of cellulose and calcium alginate accounts for the 6wt% of spinning liquid.
Use dry-jet wet-spinning that cellulose/calcium alginate spinning liquid is prepared as cellulose/calcium alginate blended fiber, spinning
Liquid accompanies by ultrasonication when spinneret orifice is extruded, and ultrasonication uses ultrasonic generator, and supersonic frequency is 20kHz, and power is
20W；The extrusion temperature of spinning liquid is 85 DEG C；The a length of 10mm of air layer, air layer temperature is-5 DEG C；Ring coldblast is used to make to spin
When silk thread goes out spinneret orifice 25mm, temperature is reduced to 5 DEG C, and the pathogenic wind-warm of ring coldblast is-5 DEG C, and blowing flow is 200L/min, wet
Degree is 10%；Spinning liquid thread passes air layer, enters the coagulating bath being made up of NMMO and water, and solidification forming is fiber, NMMO
Content be 1wt%, coagulation bath temperature scope is 5 DEG C；Fiber, after drawing-off, washing, is dried under the conditions of 70 DEG C.Test table
Bright, the calcium alginate of the cellulose of preparation/calcium alginate blended fiber is evenly distributed, and grain size is 100nm, and filament number is
1.3dtex, dry break strength 2.0cN/dtex, wet break strength is 1.5cN/dtex, and saturated moisture absorption regain is 20%,
Water retention is 70%.
Embodiment 2
The preparation method of a kind of cellulose/calcium alginate blended fiber, under the conditions of 65 DEG C, by water content 4.5wt%
Cellulose pulp uniformly and makes cellulose complete swelling with the NMMO aqueous solution of water content 45wt%, fine in cellulose pulp
The degree of polymerization of dimension element is 550；Swelling thing is mixed with the sodium alginate soln that concentration is 1.5wt%, and adds in mixed process
Entering the calcium chloride powder body that grain size is 1um and prepare cellulose/calcium alginate blend solution, the amount of sodium alginate is cellulose slurry
The 3.8wt% of cellulose in the dregs of rice, calcium chloride is 1:2 with the mol ratio of sodium ion in sodium alginate soln；It is 94 in solution temperature
DEG C, vacuum is-8.2 × 10-4Under conditions of Pa, use membrane evaporator by the moisture of cellulose/calcium alginate blend solution
Being reduced to 14wt% and prepare cellulose/calcium alginate spinning liquid, the total amount of cellulose and calcium alginate accounts for spinning liquid
8.3wt%.
Use dry-jet wet-spinning that cellulose/calcium alginate spinning liquid is prepared as cellulose/calcium alginate blended fiber, spinning
Liquid accompanies by ultrasonication when spinneret orifice is extruded, and ultrasonication uses ultrasonic generator, and supersonic frequency is 24kHz, and power is
90W；The extrusion temperature of spinning liquid is 94 DEG C；The a length of 33mm of air layer, air layer temperature is-2.5 DEG C；Ring coldblast is used to make
Dynamic analysis of spinning goes out temperature at spinneret orifice 28mm and is reduced to 6.3 DEG C, and the pathogenic wind-warm of ring coldblast is-2.5 DEG C, and blowing flow is 250L/
Min, humidity is 23%；Spinning liquid thread passes air layer, enters the coagulating bath being made up of NMMO and water, and solidification forming is fine
Dimension, the content of NMMO is 3.3wt%, and coagulation bath temperature scope is 10 DEG C；Fiber is after drawing-off, washing, dry under the conditions of 90 DEG C
Dry.Test shows, the calcium alginate of the cellulose of preparation/calcium alginate blended fiber is evenly distributed, and grain size is 90nm, single
Silk size is 1.8dtex, dry break strength 2.4cN/dtex, and wet break strength is 1.9cN/dtex, and saturated moisture absorption gets damp again
Rate is 22%, and water retention is 72%.
Embodiment 3
The preparation method of a kind of cellulose/calcium alginate blended fiber, under the conditions of 70 DEG C, by the fibre of water content 5wt%
Dimension element pulp uniformly and makes cellulose complete swelling with the NMMO aqueous solution of water content 50wt%, fiber in cellulose pulp
The degree of polymerization of element is 700；Swelling thing is mixed with the sodium alginate soln that concentration is 2.25wt%, and adds in mixed process
Concentration is that the calcium chloride solution of 2wt% prepares cellulose/calcium alginate blend solution, and the amount of sodium alginate is in cellulose pulp
The 7.5wt% of cellulose, calcium chloride is 1:2 with the mol ratio of sodium ion in sodium alginate soln；It is 103 DEG C in solution temperature,
Vacuum is-8.5 × 10-4Under conditions of Pa, membrane evaporator is used to be reduced by the moisture of cellulose/calcium alginate blend solution
Preparing cellulose/calcium alginate spinning liquid to 13wt%, the total amount of cellulose and calcium alginate accounts for the 10.5wt% of spinning liquid.
Use dry-jet wet-spinning that cellulose/calcium alginate spinning liquid is prepared as cellulose/calcium alginate blended fiber, spinning
Liquid accompanies by ultrasonication when spinneret orifice is extruded, and ultrasonication uses ultrasonic generator, and supersonic frequency is 28kHz, and power is
160W；The extrusion temperature of spinning liquid is 103 DEG C；The a length of 55mm of air layer, air layer temperature is 0 DEG C；Ring coldblast is used to make
Dynamic analysis of spinning goes out temperature at spinneret orifice 35mm and is reduced to 7.5 DEG C, and the pathogenic wind-warm of ring coldblast is 0 DEG C, and blowing flow is 300L/min,
Humidity is 35%；Spinning liquid thread passes air layer, enters the coagulating bath being made up of NMMO and water, and solidification forming is fiber,
The content of NMMO is 5.5wt%, and coagulation bath temperature scope is 15 DEG C；Fiber, after drawing-off, washing, is dried under the conditions of 110 DEG C.
Test shows, the calcium alginate of the cellulose of preparation/calcium alginate blended fiber is evenly distributed, and grain size is 85nm, monofilament
Fiber number is 2.4dtex, dry break strength 2.8cN/dtex, and wet break strength is 2.3cN/dtex, saturated moisture absorption regain
Being 25%, water retention is 75%.
Embodiment 4
The preparation method of a kind of cellulose/calcium alginate blended fiber, under the conditions of 75 DEG C, by water content 5.5wt%
Cellulose pulp uniformly and makes cellulose complete swelling with the NMMO aqueous solution of water content 55wt%, fine in cellulose pulp
The degree of polymerization of dimension element is 850；Swelling thing is mixed with the sodium alginate soln that concentration is 3.5wt%, and adds in mixed process
Entering the calcium chloride solution that concentration is 3wt% and prepare cellulose/calcium alginate blend solution, the amount of sodium alginate is cellulose pulp
The 11wt% of middle cellulose, calcium chloride is 1:2 with the mol ratio of sodium ion in sodium alginate soln；It is 112 DEG C in solution temperature,
Vacuum is-8.8 × 10-4Under conditions of Pa, membrane evaporator is used to be reduced by the moisture of cellulose/calcium alginate blend solution
Preparing cellulose/calcium alginate spinning liquid to 13wt%, the total amount of cellulose and calcium alginate accounts for the 12.8wt% of spinning liquid.
Use dry-jet wet-spinning that cellulose/calcium alginate spinning liquid is prepared as cellulose/calcium alginate blended fiber, spinning
Liquid accompanies by ultrasonication when spinneret orifice is extruded, and ultrasonication uses ultrasonic generator, and supersonic frequency is 32kHz, and power is
230W；The extrusion temperature of spinning liquid is 112 DEG C；The a length of 77mm of air layer, air layer temperature is 2.5 DEG C；Use ring coldblast
Making dynamic analysis of spinning go out temperature at spinneret orifice 42mm and be reduced to 8.8 DEG C, the pathogenic wind-warm of ring coldblast is 2.5 DEG C, and blowing flow is 350L/
Min, humidity is 47%；Spinning liquid thread passes air layer, enters the coagulating bath being made up of NMMO and water, and solidification forming is fine
Dimension, the content of NMMO is 7.8wt%, and coagulation bath temperature scope is 20 DEG C；Fiber is after drawing-off, washing, dry under the conditions of 130 DEG C
Dry.Test shows, the calcium alginate of the cellulose of preparation/calcium alginate blended fiber is evenly distributed, and grain size is 80nm, single
Silk size is 3.0dtex, dry break strength 3.2cN/dtex, and wet break strength is 2.7cN/dtex, and saturated moisture absorption gets damp again
Rate is 28%, and water retention is 78%.
Embodiment 5
The preparation method of a kind of cellulose/calcium alginate blended fiber, under the conditions of 80 DEG C, by the fibre of water content 6wt%
Dimension element pulp uniformly and makes cellulose complete swelling with the NMMO aqueous solution of water content 60wt%, fiber in cellulose pulp
The degree of polymerization of element is 1000；Swelling thing is mixed with the sodium alginate soln that concentration is 5wt%, and adds dense in mixed process
Degree prepares cellulose/calcium alginate blend solution for the calcium chloride solution of 5wt%, and the amount of sodium alginate is fine in cellulose pulp
The 15wt% of dimension element, calcium chloride is 1:2 with the mol ratio of sodium ion in sodium alginate soln；It is 120 DEG C in solution temperature, vacuum
Degree is for-9.0 × 10-4Under conditions of Pa, membrane evaporator is used to be reduced to by the moisture of cellulose/calcium alginate blend solution
13wt% prepares cellulose/calcium alginate spinning liquid, and the total amount of cellulose and calcium alginate accounts for the 15wt% of spinning liquid.
Use dry-jet wet-spinning that cellulose/calcium alginate spinning liquid is prepared as cellulose/calcium alginate blended fiber, spinning
Liquid accompanies by ultrasonication when spinneret orifice is extruded, and ultrasonication uses ultrasonic generator, and supersonic frequency is 35kHz, and power is
300W；The extrusion temperature of spinning liquid is 120 DEG C；The a length of 100mm of air layer, air layer temperature is 5 DEG C；Ring coldblast is used to make
Dynamic analysis of spinning goes out temperature at spinneret orifice 41mm and is reduced to 10 DEG C, and the pathogenic wind-warm of ring coldblast is 5 DEG C, and blowing flow is 400L/min,
Humidity is 60%；Spinning liquid thread passes air layer, enters the coagulating bath being made up of NMMO and water, and solidification forming is fiber,
The content of NMMO is 10wt%, and coagulation bath temperature scope is 15 DEG C；Fiber, after drawing-off, washing, is dried under the conditions of 150 DEG C.
Test shows, the calcium alginate of the cellulose of preparation/calcium alginate blended fiber is evenly distributed, and grain size is 90nm, monofilament
Fiber number is 3.5dtex, dry break strength 3.5cN/dtex, and wet break strength is 3.0cN/dtex, saturated moisture absorption regain
Being 30%, water retention is 80%.
Claims (10)
1. a preparation method for cellulose/calcium alginate blended fiber, is characterized in that comprising the following steps:
(1) cellulose pulp uniformly and is made cellulose complete swelling with NMMO aqueous solution；Meanwhile, preparation sodium alginate is molten
Liquid；
(2) swelling thing is mixed with sodium alginate soln, and in mixed process, add calcium chloride；
(3) moisture making step gained mixed liquor is reduced to below 15wt%, prepares cellulose/calcium alginate spinning liquid；
(4) through dry-jet wet-spinning, cellulose/calcium alginate blended fiber is prepared.
The preparation method of a kind of cellulose/calcium alginate blended fiber the most according to claim 1, it is characterised in that institute
Stating in dry-jet wet-spinning, described cellulose/calcium alginate spinning liquid accompanies by ultrasonication when spinneret orifice is extruded.
The preparation method of a kind of cellulose/calcium alginate blended fiber the most according to claim 2, it is characterised in that institute
Stating ultrasonication and use ultrasonic generator, supersonic frequency is 20～35kHz, and power is 20～300W.
The preparation method of a kind of cellulose/calcium alginate blended fiber the most according to claim 1, it is characterised in that institute
Stating the degree of polymerization of cellulose in cellulose pulp is 400～1000, and the water content of described cellulose pulp is 4～6wt%；Described
The water content of NMMO aqueous solution is 40～60wt%；Described swelling temperature is 60～80 DEG C.
The preparation method of a kind of cellulose/calcium alginate blended fiber the most according to claim 1, it is characterised in that institute
The concentration stating sodium alginate soln is 0.5～5wt%；The amount of sodium alginate be cellulose in described cellulose pulp 0.1～
15wt%；Calcium chloride is 1:2 with the mol ratio of sodium ion in described sodium alginate soln.
The preparation method of a kind of cellulose/calcium alginate blended fiber the most according to claim 1, it is characterised in that institute
Stating moisture and be reduced to thin film evaporation mode, specifically use membrane evaporator, technological parameter is: solution temperature is 85～120 DEG C, very
Reciprocal of duty cycle is-8.0 × 10-4～-9.0 × 10-4Pa。
The preparation method of a kind of cellulose/calcium alginate blended fiber the most according to claim 1, it is characterised in that institute
Stating in cellulose/calcium alginate spinning liquid, the total amount of cellulose and calcium alginate accounts for the 6～15wt% of spinning liquid.
The preparation method of a kind of cellulose/calcium alginate blended fiber the most according to claim 1, it is characterised in that institute
Stating dry-jet wet-spinning, in making dynamic analysis of spinning go out spinneret orifice 50mm, temperature is reduced to 5～10 DEG C；It is specially and uses ring coldblast, described
The pathogenic wind-warm of ring coldblast is-5～5 DEG C, and blowing flow is 200～400L/min, humidity is 10～60%.
The preparation method of a kind of cellulose/calcium alginate blended fiber the most according to claim 1, it is characterised in that institute
The technological parameter stating dry-jet wet-spinning is: the extrusion temperature of spinning liquid is 85～120 DEG C, air layer a length of 10～100mm, air
Layer temperature is-5～5 DEG C；Coagulation bath composition is NMMO and water, and NMMO content is 1～10wt%, coagulation bath temperature scope be 5～
25℃；Baking temperature is 70～150 DEG C.
The preparation method of a kind of cellulose/calcium alginate blended fiber the most according to claim 1, it is characterised in that institute
The calcium alginate stating cellulose/calcium alginate blended fiber is evenly distributed, grain size be less than 100nm, filament number be 1.3～
3.5dtex, dry break strength 2.0～3.5cN/dtex, wet break strength is 1.5～3.0cN/dtex, and saturated moisture absorption is returned
Tide rate is 20～30%, and water retention is 70～80%.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2016102650677 | 2016-04-25 | ||
| CN201610265067.7A CN105839222A (en) | 2016-04-25 | 2016-04-25 | Preparation method of cellulose/calcium alginate blend fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106283268A true CN106283268A (en) | 2017-01-04 |
| CN106283268B CN106283268B (en) | 2019-01-29 |
Family
ID=56590370
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610265067.7A Pending CN105839222A (en) | 2016-04-25 | 2016-04-25 | Preparation method of cellulose/calcium alginate blend fiber |
| CN201610848098.5A Active CN106283268B (en) | 2016-04-25 | 2016-09-26 | A kind of preparation method of cellulose/calcium alginate blended fiber |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610265067.7A Pending CN105839222A (en) | 2016-04-25 | 2016-04-25 | Preparation method of cellulose/calcium alginate blend fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN105839222A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110359101A (en) * | 2019-07-19 | 2019-10-22 | 嘉兴学院 | A kind of gel spinning process manufacturing chitin fiber |
| WO2022252955A1 (en) * | 2021-05-31 | 2022-12-08 | 南京林业大学 | Hydroxylated alginate fiber and preparation method therefor |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7094796B2 (en) * | 2017-06-30 | 2022-07-04 | オーミケンシ株式会社 | Rayon fiber |
| CN108532013A (en) * | 2018-04-26 | 2018-09-14 | 俞小峰 | A kind of preparation method of long-acting type anti-bacteria fabric fibrous material |
| CN109162096B (en) * | 2018-08-31 | 2021-01-26 | 山东绿纤工程设计有限公司 | Method for preparing flame-retardant Lyocell cellulose fiber based on post-treatment method |
| CN109267318B (en) * | 2018-09-17 | 2021-12-17 | 山东绿纤工程设计有限公司 | Flame-retardant lyocell fiber and preparation method thereof |
| CN109429806B (en) * | 2018-12-14 | 2021-03-30 | 重庆城市管理职业学院 | Water storage gardening flowerpot |
| CN110359110B (en) * | 2019-07-19 | 2021-11-05 | 嘉兴学院 | Alginate modified regenerated cellulose fiber and preparation method thereof |
| CN113493934A (en) * | 2020-04-01 | 2021-10-12 | 苏州合祥纺织科技有限公司 | Preparation method of agar fibers |
| CN112127009B (en) * | 2020-09-11 | 2022-10-14 | 嘉兴学院 | Cellulose/calcium alginate blend fiber with skin-core structure and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1858312A (en) * | 2006-05-29 | 2006-11-08 | 山东海龙股份有限公司 | Cellulose/alginate composite fiber and its preparing method |
| CN101168869A (en) * | 2007-11-08 | 2008-04-30 | 山东海龙股份有限公司 | Soybean protein/alginate /cellulose fibre and preparation method thereof |
| CN101660215A (en) * | 2009-09-23 | 2010-03-03 | 陈福库 | Protein and cellulose composite fiber and manufacturing method thereof |
-
2016
- 2016-04-25 CN CN201610265067.7A patent/CN105839222A/en active Pending
- 2016-09-26 CN CN201610848098.5A patent/CN106283268B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1858312A (en) * | 2006-05-29 | 2006-11-08 | 山东海龙股份有限公司 | Cellulose/alginate composite fiber and its preparing method |
| CN101168869A (en) * | 2007-11-08 | 2008-04-30 | 山东海龙股份有限公司 | Soybean protein/alginate /cellulose fibre and preparation method thereof |
| CN101660215A (en) * | 2009-09-23 | 2010-03-03 | 陈福库 | Protein and cellulose composite fiber and manufacturing method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110359101A (en) * | 2019-07-19 | 2019-10-22 | 嘉兴学院 | A kind of gel spinning process manufacturing chitin fiber |
| CN110359101B (en) * | 2019-07-19 | 2020-10-02 | 嘉兴学院 | Gel spinning method for manufacturing chitosan fiber |
| WO2022252955A1 (en) * | 2021-05-31 | 2022-12-08 | 南京林业大学 | Hydroxylated alginate fiber and preparation method therefor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105839222A (en) | 2016-08-10 |
| CN106283268B (en) | 2019-01-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106283268B (en) | A kind of preparation method of cellulose/calcium alginate blended fiber | |
| CN101328626A (en) | Method for continuously preparing regenerated cellulose fibre | |
| CN103556260B (en) | A kind of bamboo-carbon viscose fibre and preparation method thereof | |
| CN103060946B (en) | Blend fibers of alginate and sodium carboxymethyl cellulose and preparation method and application thereof | |
| CN110359110B (en) | Alginate modified regenerated cellulose fiber and preparation method thereof | |
| CN105603554A (en) | Graphene functionalized cellulose fiber and preparation method thereof | |
| CN108004611A (en) | A kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice | |
| WO2007121609A1 (en) | The use of aqueous solution of sodium-hydroxide and sulfourea in producing cellulose products in pilot-scale | |
| CN103469542B (en) | Bacterial cellulose fiber containing nano-silver chloride particles and preparation method of fiber | |
| CN103031611A (en) | Polyvinyl alcohol fiber and preparation method as well as application thereof | |
| CN106048741B (en) | A kind of method that dry-wet spinning prepares cellulose fibre | |
| CN109402815A (en) | Graphene composite fibre yarn and its preparation method and application | |
| CN102008756A (en) | Preparation method of nano-fibrous silk fibroin-based porous scaffold | |
| CN106222771A (en) | A kind of preparation method of cellulose fibre | |
| CN115613151B (en) | Viscose macrobio-fiber containing mint and orange active ingredients and preparation method thereof | |
| CN103556255B (en) | A kind of bamboo charcoal cellulose fiber and preparation method thereof | |
| CN105177751A (en) | Colored anti-ultraviolet profiled fine denier polyester filament and preparation method thereof | |
| CN102443868B (en) | Method for manufacturing regenerated cellulose fibers | |
| CN101768790B (en) | Sheath core composite fibre of chitin and cellulose and preparation method thereof | |
| CN106048761A (en) | Encapsulated and networked regenerated cellulose phase-change fiber and preparation method thereof | |
| CN101555321A (en) | Solvent composition and preparation method and application thereof | |
| CN106149080B (en) | A kind of preparation method of cellulose/calamine composite fibre | |
| CN1190531C (en) | Manufacturing method for bamboo cellulose fibre by solvent method | |
| CN1255585C (en) | Process for preparing precursor fiber of cellulose base carbon fiber | |
| CN109750383A (en) | A kind of nano micro crystal cellulose composite viscose fiber and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 314031 2 building, Photovoltaic Science Park, 1288 Kang He road, Xiuzhou District, Jiaxing, Zhejiang. Applicant after: Jiaxing University Address before: 314033 Yuexiu South Road, Jiaxing, Jiaxing, Zhejiang Applicant before: Jiaxing University |
|
| CB02 | Change of applicant information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210922 Address after: 314000 No. 161, Huicheng Road, Huimin street, Jiashan County, Jiaxing City, Zhejiang Province Patentee after: ZHEJIANG SHENNAN PLASTIC Co.,Ltd. Address before: 314031 2 building, Photovoltaic Science Park, 1288 Kang He road, Xiuzhou District, Jiaxing, Zhejiang. Patentee before: JIAXING University |
|
| TR01 | Transfer of patent right |