CN106480544B - A kind of preparation method of Cuttlefish Ink-alginate composite fiber - Google Patents
A kind of preparation method of Cuttlefish Ink-alginate composite fiber Download PDFInfo
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/04—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of alginates
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/04—Pigments
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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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- Multicomponent Fibers (AREA)
Abstract
The invention discloses a kind of preparation methods of Cuttlefish Ink-alginate composite fiber comprising the preparation of squid ink extracts, the preparation of Cuttlefish Ink-sodium alginate spinning solution, Cuttlefish Ink-three processing steps of alginate composite fiber spinning and post-processing.It is mixed water-insoluble squid ink extracts with sodium alginate soln by emulsifier, forms sodium alginate emulsion；By the natural stabilization of sodium alginate macromolecular, emulsifier to the plasticization of sodium alginate soln, and the hydrogen bond action between squid ink extracts and sodium alginate macromolecular, make mixing stable homogeneous, Cuttlefish Ink-sodium alginate spinning solution suitable for wet spinning technology requirement.The present invention have the characteristics that technique is easily-controllable, spinning technique process does not break end and silk less, pigment be lost in less, product quality stabilization, good color fastness, dry fracture strength it is high, suitable for scale industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of alginate fiber more particularly to a kind of Cuttlefish Ink-alginate are compound
The preparation method of fiber.
Background technology
Alginate fibre has good biocompatibility, and pure alginate fibre is white, soft touch, and surface is smooth light
Pool has good drapability, there is unique excellent properties better than traditional fibre.Alginate fibre is in addition to self flame retardance, height
Outside the typical excellent properties such as hygroscopicity, biodegradation and compatibility, gel blockage, shielding property and high oxygen permeability, also
With the excellent performance such as excellent bacteriostasis antibiosis, hemostatic, absorption minerals.So that alginate fibre is in civilian clothes, day
Change and hygiene article sector has huge market application prospect.
Cuttlefish Ink is synthesized by the gland in ink sac, is stored in ink sac, Cuttlefish Ink evidence《Bencao Shiyi》It is described, it can lead
Blood thorn is pained.It is now used as a kind of Chinese medicine, mainly as hemostat, treats hemorrhagic disease, such as functional uterine bleeding, gastrorrhagia
Deng.Correlative study in recent years also found that Cuttlefish Ink has antitumor action, the effect being also improved to the immunity of human body.Cuttlefish Ink
Antitumor action be to be generated by the intermediary of immune system, principle active component may be one group of mucopolysaccharide, but be worth
It is to be noted that the country begins one's study when Cuttlefish Ink, acquire the condition of Cuttlefish Ink there is no said before so stringent, but still
Effectively, illustrate that anticancer component therein can may under general condition extract.
It is believed that Cuttlefish Ink-alginate composite fiber will have good market application value and promotion prospect：One
Aspect, Cuttlefish Ink-alginate composite fiber can degradable, with general alginate fiber superperformance；On the other hand,
In Cuttlefish Ink-alginate composite fiber, contained squid ink extracts and alginate all have good antibacterial bacteriostatic
Function, squid ink extracts ingredient especially therein also have good hemostatic function and effect；Furthermore Cuttlefish Ink-alginic acid
Salt composite fibre is a kind of coloured fiber, enriches the color of alginate fiber, improves the industry of alginate fiber
Added value.
Invention content
Easily-controllable, spinning technique process that it is an object of the present invention to provide a kind of techniques do not break end and silk less, pigment be lost in less,
The preparation method of product quality stabilization, good color fastness, the high Cuttlefish Ink-alginate composite fiber of dry fracture strength.
Present invention technical solution used for the above purpose is, a kind of Cuttlefish Ink-alginate composite fiber
Preparation method, which is characterized in that include the following steps：
The first step, the preparation of squid ink extracts
By mass fraction, 60~100 parts of sodium alginate powder, 5 parts of cuttlefish ink sac, 1 part of emulsifier are weighed respectively, it is spare；
Taken cuttlefish ink sac is placed in homogenizer, 0 DEG C of water with quality such as taken cuttlefish ink sacs, homogenization is added
10min；Then, it filters, it is thick to obtain squid ink extracts；
It after gained squid ink extracts crude product is frozen into solid-state, is placed in freeze drier, in -40 DEG C of condenser temperature
Under, then freeze-drying 10h using grinding pump circular grinding 15min, obtains squid ink extracts highly finished product；
Second step, the preparation of Cuttlefish Ink-sodium alginate spinning solution
It is 4%~8% sodium alginate soln that taken sodium alginate powder, which is configured to mass percent concentration, in stirring shape
Emulsifier is added under state, standing and defoaming 10h obtains sodium alginate emulsified solution；
Squid ink extracts highly finished product and sodium alginate emulsified solution are added in dynamic mixer, after mixing,
Obtain Cuttlefish Ink-sodium alginate spinning solution；
Third walks, Cuttlefish Ink-alginate composite fiber spinning and post-processing
Gained Cuttlefish Ink-sodium alginate spinning solution is subjected to wet spinning, and passes through coagulating bath solidification forming, drawing-off successively
Cuttlefish Ink-alginate composite fiber is made after sizing, drying.
The technical effect brought directely by the technical proposal is that preparation process is simple, production cost is low；It is worth relatively high
One of main material ingredient squid ink extracts, be lost in production process few.Reason is：
In above-mentioned technical proposal, squid ink extracts (water-insoluble) are directly used to simple machinery under low temperature water environment
Method is extracted, to the minimum of the damage control of the active ingredient of raw material.The study found that prepared Chinese ink is the black by being invisible to the naked eye
The thick suspension that grain is constituted, Cuttlefish Ink particle balling preparation type, diameter is between 90-250nm.It is only filtered when therefore filtering
Fall the effect of ink the tissue substance of capsule, effectively at Cuttlefish Ink particle do not lose.
The mesh of grinding pump circular grinding it is to further ensure that the larger particles ground in crude extract, when preventing spinning
The quality for influencing spun fiber, in combination with freeze-drying, low temperature concentrated extract mixed liquor improves extract purity.
Meanwhile " it was found that and utilizing " sodium alginate macromolecular has natural " emulsification and stabilization " this objective rule
Rule, in conjunction with the addition of emulsifier, further stabilizes uniform dispersed of the insoluble Cuttlefish Ink in sodium alginate spinning solution
State remains the ecosystem nanometer bead state of Cuttlefish Ink particle.
That is, in above-mentioned technical proposal, need to only be stablized by easy mechanical extraction, dynamic mixing, composite emulsifying,
It can achieve the purpose that prepare high quality Cuttlefish Ink-sodium alginate spinning solution.
In follow-up spinning, since extract is or not Cuttlefish Ink active ingredient (Cuttlefish Ink melanin and proteoglycan compound)
It is dissolved in water, and adds and easily forms hydrogen bond between active ingredient and sodium alginate macromolecular so that is present in the crow on as-spun fibre surface layer
Crafty ink takes object ingredient to not easily run off in coagulation bath.
Since in spinning solution, squid ink extracts are uniformly dynamically mixed with sodium alginate, after subsequent solidification forming,
Squid ink extracts ingredient will be evenly distributed in the inside and surface layer of fiber.Fiber prepared by above-mentioned technical proposal,
Quality uniformity and stability are good.
It is worth noting that in the technical solution, the addition of small molecule water soluble emulsifier, not only in the preparation of spinning solution
In play the role of stable emulsifying dispersion liquid system, and in spinning process while alginate fiber curing molding, by
It is that soluble small molecular one end is hydrophilic in naturally occurring emulsifying agent, one end oleophylic, while fibre solidification shapes, emulsifier will be with spinning
Moisture content part in silk liquid spills into the surface of as-spun fibre, and hydrophilic one end can form hydrogen with alginate fiber surface
Key associates, and only exposes one end of oleophylic, to form one layer of hydrophobic protective layer on the surface of as-spun fibre, it is possible to prevente effectively from
Doubling phenomena between as-spun fibre and as-spun fibre caused by the formation of hydrogen bond.
In addition, in above-mentioned technical proposal, due to organic solvent-free and synthetic material；And raw material sources are easy, production
Flow is uncomplicated, working substance extraction efficiency is high when extraction, after spinning working substance retain it is more.Therefore, the preparation of above-mentioned technical proposal
Method is not only adapted to industrialized production, and meets the requirement of clean manufacturing.
Preferably, above-mentioned coagulating bath is the calcium chloride solution that mass percent concentration is 4~8%.
What the optimal technical scheme was directly brought has the technical effect that, selects the calcium chloride solution of higher concentration as solidification
Bath, in order to accelerate the replacement rate of sodium ion, and then improve the sodium ion replacement rate in the unit interval, reach preferably
Crosslinking degree, and then ensure that final fiber product has preferable fracture strength performance indicator.
Further preferably, mentioned emulsifier is one or more of gum arabic, xanthans or bassora gum mixture.
What the optimal technical scheme was directly brought has the technical effect that, gum arabic, xanthans or bassora gum raw material are easy to
It obtains, emulsifying effectiveness is good and can natural degradation.
Further preferably, main technologic parameters are as follows for above-mentioned wet spinning：
Spinning temperature is 20~35 DEG C, and coagulation bath temperature is 20~35 DEG C, and draw ratio is 180%~230%；
What the optimal technical scheme was directly brought has the technical effect that, spinning temperature is 20~35 DEG C, and coagulation bath temperature is
20~35 DEG C, be conducive to the stability of the blend spinning liquid system of squid ink extracts and sodium alginate soln, while conducive to crow
The stability of crafty ink extract；
Draw ratio is conducive to the spinning moulding of the fiber under higher concentration for 180%~230%, ensures the dry of final products
The stability of fracture strength index.
Drying temperature is 40 DEG C, time 1.5h.
Further preferably, the preparation method of above-mentioned Cuttlefish Ink-alginate composite fiber, obtained Cuttlefish Ink-sea
The color fastness to water of alginates composite fibre is 4~5 grades；Dye value >=14.6 K/S；Dry fracture strength is 3.24~3.56cN/
dtex。
What the optimal technical scheme was directly brought has the technical effect that, suitable for all kinds of clothes, the requirements of weaving process of material is defended, for patch
The human body compatibility of body clothing obtains effective guarantee.
Supplementary explanation：In above-mentioned technical proposal, by the quality for controlling both sodium alginate ingredient and squid ink extracts
Than the addition of Cuttlefish Ink highly finished product (in short, control), can obtaining the composite fibre of serial color, (color color includes ash
Color, black, and the various gradual change colors between grey to black).
In conclusion the present invention is compared with the existing technology, have that technique is easily-controllable, spinning technique process does not break end and silk less,
Pigment is lost in less, product quality stabilization, good color fastness, does fracture strength height；It is environmental friendly, have suitable for scale industrial production etc.
Beneficial effect.
Description of the drawings
Fig. 1 is the transmission electron microscope photo of Cuttlefish Ink-sodium alginate spinning solution of embodiment 1；
Fig. 2 is formed by hydrogen bond structure schematic diagram between the sodium alginate strand and squid ink extracts for the present invention.
Specific implementation mode
With reference to embodiment, the present invention is described in detail.
Explanation：
One, in following embodiment, raw materials used quality and source are as follows：
1, sodium alginate powder：Relative molecular mass >=100,000, commercial product or are extracted in natural seaweed plant；
2, cuttlefish ink sac is fresh or freezing primary agricultural products；
3,0 DEG C of water is prepared using deionized water or softened water.
Two, the detection of properties of product and the method for inspection are as follows：
1, fracture strength is done：Reference《GB/T 14337-2008 man-made staple fibres Wellas stretch method for testing performance》
2, resistance to water colour jail element：Reference《GBT 5713-1997 textile color stabilities test color fastness to water》
Embodiment 1
Preparation method is as follows：
The first step, the preparation of squid ink extracts
By mass fraction, 60 parts of sodium alginate powder, 5 parts of ink sac (containing prepared Chinese ink), emulsifier gum arabic 1 are weighed respectively
Part；
Ink sac is added to the ice water of mass fractions such as being added in homogenizer, homogenization 10min；By the mixing of gained
Liquid obtains squid ink extracts crude product after two layers of filtered through gauze.
It after gained squid ink extracts crude product is frozen into solid-state, is placed in freeze drier, in -40 DEG C of condenser temperature
Under, then freeze-drying 10h using grinding pump circular grinding 15min, obtains squid ink extracts highly finished product；
Second step, the preparation of Cuttlefish Ink-sodium alginate spinning solution
It is 8% sodium alginate soln that taken sodium alginate powder, which is configured to mass percent concentration, under stirring
Emulsifier is added, standing and defoaming 10h obtains sodium alginate emulsified solution；,
Squid ink extracts highly finished product and sodium alginate emulsified solution are added in dynamic mixer, after mixing,
Obtain Cuttlefish Ink-sodium alginate spinning solution；
Third walks, Cuttlefish Ink-alginate composite fiber spinning and post-processing
Gained Cuttlefish Ink-sodium alginate spinning solution is subjected to wet spinning, and passes through coagulating bath solidification forming, drawing-off successively
Cuttlefish Ink-alginate composite fiber is made after sizing, drying.
Wherein, in wet spinning process, spinning temperature is 35 DEG C, and coagulation bath temperature is 35 DEG C, the chlorination that coagulating bath is 8%
Calcium solution；Draw ratio is 230%；
The drying of fiber is carried out in vacuum drier, and the temperature in vacuum drier is 40 DEG C, drying time 1.5
Hour.Properties of product testing result：
Obtained fiber product color fastness to water reach 4~5 grades, K/S values be 17.7, dry fracture strength is 3.20N/
dtex。
Embodiment 2
Preparation method is as follows：
The first step, the preparation of squid ink extracts
By mass fraction, weigh 70 parts of sodium alginate powder, 5 parts of ink sac (contain prepared Chinese ink) respectively, 1 part of emulsifier (wherein, Ah
Draw uncle gummy 0.5 part, 0.5 part of xanthans)；
Ink sac is added to the ice water of mass fractions such as being added in homogenizer, homogenization 10min；By the mixing of gained
Liquid obtains squid ink extracts crude product after two layers of filtered through gauze.
It after gained squid ink extracts crude product is frozen into solid-state, is placed in freeze drier, in -40 DEG C of condenser temperature
Under, then freeze-drying 10h using grinding pump circular grinding 15min, obtains squid ink extracts highly finished product；Second step, crow
The preparation of crafty ink-sodium alginate spinning solution
It is 7% sodium alginate soln that taken sodium alginate powder, which is configured to mass percent concentration, under stirring
Emulsifier is added, standing and defoaming 10h obtains sodium alginate emulsified solution；,
Squid ink extracts highly finished product and sodium alginate emulsified solution are added in dynamic mixer, after mixing,
Obtain Cuttlefish Ink-sodium alginate spinning solution；
Third walks, Cuttlefish Ink-alginate composite fiber spinning and post-processing
Gained Cuttlefish Ink-sodium alginate spinning solution is subjected to wet spinning, and passes through coagulating bath solidification forming, drawing-off successively
Cuttlefish Ink-alginate composite fiber is made after sizing, drying.
Wherein, in wet spinning process, spinning temperature is 30 DEG C, and coagulation bath temperature is 30 DEG C, the chlorination that coagulating bath is 7%
Calcium solution；Draw ratio is 217%；
The drying of fiber is carried out in vacuum drier, and the temperature in vacuum drier is 40 DEG C, drying time 1.5
Hour.Properties of product testing result：
Obtained fiber product color fastness to water reach 4~5 grades, K/S values be 16.3, dry fracture strength is 3.11N/
dtex。
Embodiment 3
Preparation method is as follows：
The first step, the preparation of squid ink extracts
By mass fraction, weigh 80 parts of sodium alginate powder, 5 parts of ink sac (contain prepared Chinese ink) respectively, 1 part of emulsifier (wherein, Ah
Draw 0.5 part of uncle's natural gum, 0.3 part of xanthans, 0.2 part of bassora gum)；
Ink sac is added to the ice water of mass fractions such as being added in homogenizer, homogenization 10min；By the mixing of gained
Liquid obtains squid ink extracts crude product after two layers of filtered through gauze.
It after gained squid ink extracts crude product is frozen into solid-state, is placed in freeze drier, in -40 DEG C of condenser temperature
Under, then freeze-drying 10h using grinding pump circular grinding 15min, obtains squid ink extracts highly finished product；Second step, crow
The preparation of crafty ink-sodium alginate spinning solution
It is 6% sodium alginate soln that taken sodium alginate powder, which is configured to mass percent concentration, under stirring
Emulsifier is added, standing and defoaming 10h obtains sodium alginate emulsified solution；,
Squid ink extracts highly finished product and sodium alginate emulsified solution are added in dynamic mixer, after mixing,
Obtain Cuttlefish Ink-sodium alginate spinning solution；
Third walks, Cuttlefish Ink-alginate composite fiber spinning and post-processing
Gained Cuttlefish Ink-sodium alginate spinning solution is subjected to wet spinning, and passes through coagulating bath solidification forming, drawing-off successively
Cuttlefish Ink-alginate composite fiber is made after sizing, drying.
Wherein, in wet spinning process, spinning temperature is 28 DEG C, and coagulation bath temperature is 28 DEG C, the chlorination that coagulating bath is 6%
Calcium solution；Draw ratio is 207%；
The drying of fiber is carried out in vacuum drier, and the temperature in vacuum drier is 40 DEG C, drying time 1.5
Hour.Properties of product testing result：
Obtained fiber product color fastness to water reach 4~5 grades, K/S values be 15.6, dry fracture strength is 3.06N/
dtex。
Embodiment 4
Preparation method is as follows：
The first step, the preparation of squid ink extracts
By mass fraction, weigh 90 parts of sodium alginate powder, 5 parts of ink sac (contain prepared Chinese ink) respectively, 1 part of emulsifier (wherein, Ah
Draw uncle gummy 0.5 part, 0.5 part of bassora gum)；
Ink sac is added to the ice water of mass fractions such as being added in homogenizer, homogenization 10min；By the mixing of gained
Liquid obtains squid ink extracts crude product after two layers of filtered through gauze.
It after gained squid ink extracts crude product is frozen into solid-state, is placed in freeze drier, in -40 DEG C of condenser temperature
Under, then freeze-drying 10h using grinding pump circular grinding 15min, obtains squid ink extracts highly finished product；
Second step, the preparation of Cuttlefish Ink-sodium alginate spinning solution
It is 5% sodium alginate soln that taken sodium alginate powder, which is configured to mass percent concentration, under stirring
Emulsifier is added, standing and defoaming 10h obtains sodium alginate emulsified solution；,
Squid ink extracts highly finished product and sodium alginate emulsified solution are added in dynamic mixer, after mixing,
Obtain Cuttlefish Ink-sodium alginate spinning solution；
Third walks, Cuttlefish Ink-alginate composite fiber spinning and post-processing
Gained Cuttlefish Ink-sodium alginate spinning solution is subjected to wet spinning, and passes through coagulating bath solidification forming, drawing-off successively
Cuttlefish Ink-alginate composite fiber is made after sizing, drying.
Wherein, in wet spinning process, spinning temperature is 23 DEG C, and coagulation bath temperature is 23 DEG C, the chlorination that coagulating bath is 5%
Calcium solution；Draw ratio is 191%；
The drying of fiber is carried out in vacuum drier, and the temperature in vacuum drier is 40 DEG C, drying time 1.5
Hour.Properties of product testing result：
Obtained fiber product color fastness to water reach 4~5 grades, K/S values be 14.7, dry fracture strength is 2.99N/
dtex。
Embodiment 5
Preparation method is as follows：
The first step, the preparation of squid ink extracts
By mass fraction, 100 parts of sodium alginate powder, 5 parts of ink sac (containing prepared Chinese ink), 1 part of emulsifier xanthans are weighed respectively；
Ink sac is added to the ice water of mass fractions such as being added in homogenizer, homogenization 10min；By the mixing of gained
Liquid obtains squid ink extracts crude product after two layers of filtered through gauze.
It after gained squid ink extracts crude product is frozen into solid-state, is placed in freeze drier, in -40 DEG C of condenser temperature
Under, then freeze-drying 10h using grinding pump circular grinding 15min, obtains squid ink extracts highly finished product；
Second step, the preparation of Cuttlefish Ink-sodium alginate spinning solution
It is 4% sodium alginate soln that taken sodium alginate powder, which is configured to mass percent concentration, under stirring
Emulsifier is added, standing and defoaming 10h obtains sodium alginate emulsified solution；,
Squid ink extracts highly finished product and sodium alginate emulsified solution are added in dynamic mixer, after mixing,
Obtain Cuttlefish Ink-sodium alginate spinning solution；
Third walks, Cuttlefish Ink-alginate composite fiber spinning and post-processing
Gained Cuttlefish Ink-sodium alginate spinning solution is subjected to wet spinning, and passes through coagulating bath solidification forming, drawing-off successively
Cuttlefish Ink-alginate composite fiber is made after sizing, drying.
Wherein, in wet spinning process, spinning temperature is 20 DEG C, and coagulation bath temperature is 20 DEG C, the chlorination that coagulating bath is 4%
Calcium solution；Draw ratio is 180%；
The drying of fiber is carried out in vacuum drier, and the temperature in vacuum drier is 40 DEG C, drying time 1.5
Hour.Properties of product testing result：
Obtained fiber product color fastness to water reach 4~5 grades, K/S values be 14.6, dry fracture strength is 2.91N/
dtex。
To more fully understand the technical characterstic of the present invention, below in conjunction with the accompanying drawings, the present invention is further illustrated.
Selection embodiment 1 is representative embodiment, and the spinning solution sampling in its preparation process is carried out transmission electron microscope observation,
To confirm dispersity of the squid ink extracts in spinning solution.
In Fig. 1, circular black spot is the squid ink extracts (insoluble) being dispersed in sodium alginate soln.
As shown in Figure 1, squid ink extracts are in more satisfactory dispersity in spinning solution, working substance ingredient retains
It is more, and insoluble characteristic is shown, effective composition granule is at spheroidal, and grain size is at tens nanometers.
Explanation：The addition of emulsifier and the stabilization of sodium alginate are bright to the evenly dispersed effect of insoluble working substance
It is aobvious.
Fig. 2 is formed by hydrogen bond structure schematic diagram between sodium alginate strand and squid ink extracts.
In Fig. 2,5,6- dihydroxy indoles, 5,6- dihydroxy indole -2- carboxylic acids and protein substance extract for Cuttlefish Ink
Object.
As shown in Fig. 2, the electricity on the working substance ingredient of part of hydroxyl and squid ink extracts on sodium alginate strand
The big oxygen atom of negativity, forms hydrogen bond；
Electron deficient hydrogen on part carboxyl on sodium alginate strand, with the working substance ingredient of squid ink extracts,
Form hydrogen bond.
Explanation：Obtained Cuttlefish Ink-sodium alginate composite fiber product has preferable color fastness to water.
Claims (4)
1. a kind of preparation method of Cuttlefish Ink-alginate composite fiber, which is characterized in that include the following steps：
The first step, the preparation of squid ink extracts
By mass fraction, 60~100 parts of sodium alginate powder, 5 parts of cuttlefish ink sac, 1 part of emulsifier are weighed respectively, it is spare；
Taken cuttlefish ink sac is placed in homogenizer, 0 DEG C of water with quality such as taken cuttlefish ink sacs, homogenization 10min is added；
Then, it filters, obtains squid ink extracts crude product；
After gained squid ink extracts crude product is frozen into solid-state, it is placed in freeze drier, it is cold at -40 DEG C of condenser temperature
Dry 10h is lyophilized, then, using grinding pump circular grinding 15min, obtains squid ink extracts highly finished product；
Second step, the preparation of Cuttlefish Ink-sodium alginate spinning solution
It is 4%~8% sodium alginate soln that taken sodium alginate powder, which is configured to mass percent concentration, under stirring
Emulsifier is added, standing and defoaming 10h obtains sodium alginate emulsified solution；
Squid ink extracts highly finished product and sodium alginate emulsified solution are added in dynamic mixer, after mixing, are obtained
Cuttlefish Ink-sodium alginate spinning solution；
Third walks, Cuttlefish Ink-alginate composite fiber spinning and post-processing
Gained Cuttlefish Ink-sodium alginate spinning solution is subjected to wet spinning, and fixed by coagulating bath solidification forming, drawing-off successively
Cuttlefish Ink-alginate composite fiber is made after type, drying；
The emulsifier is one or more of gum arabic, xanthans or bassora gum mixture.
2. the preparation method of Cuttlefish Ink-alginate composite fiber according to claim 1, which is characterized in that described solidifying
Gu bath is the calcium chloride solution that mass percent concentration is 4%~8%.
3. according to the preparation method of any Cuttlefish Ink-alginate composite fibers of claim 1-2, which is characterized in that
Main technologic parameters are as follows for the wet spinning：
Spinning temperature is 20~35 DEG C, and coagulation bath temperature is 20~35 DEG C, and draw ratio is 180%~230%；
Drying temperature is 40 DEG C, drying time is 1.5 hours.
4. the preparation method of Cuttlefish Ink-alginate composite fiber according to claim 3, which is characterized in that obtained
Cuttlefish Ink-alginate composite fiber color fastness to water be 4~5 grades；
Dye value >=14.6 K/S；
Dry fracture strength is 3.24~3.56cN/dtex.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610838486.5A CN106480544B (en) | 2016-09-21 | 2016-09-21 | A kind of preparation method of Cuttlefish Ink-alginate composite fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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