CN106012103B - A kind of preparation method of high intensity alginate fibre - Google Patents
A kind of preparation method of high intensity alginate fibre Download PDFInfo
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- CN106012103B CN106012103B CN201610533173.9A CN201610533173A CN106012103B CN 106012103 B CN106012103 B CN 106012103B CN 201610533173 A CN201610533173 A CN 201610533173A CN 106012103 B CN106012103 B CN 106012103B
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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
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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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
- 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
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
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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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- Thermal Sciences (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of preparation method of high intensity alginate fibre, its key step are as follows:Mass percent concentration is configured to as 3% 12% sodium alginate soln, and by sodium alginate soln by volume 1:3‑1:5 are divided into two parts, and nano-calcium carbonate is added in wherein portion;Then another sodium alginate soln is added, is stirred evenly, spinning solution is made;Again by the filtering of obtained spinning solution, rapidly defoaming, wet spinning is carried out by coagulating bath of calcium chloride, obtains a nanometer as-spun fibre;Then, as-spun fibre soaks to 24h 72h in deionized water, then it is post-treated to obtain the final product.The present invention in sodium alginate soln by introducing nano-calcium carbonate, utilize the Interfacial Adsorption and the principle of interface free volume increase of nano-particle, significantly reduce the viscosity of alginate fibre spinning solution, improve the spinnability of fiber, its technique is simple, easily controllable, and the fibre strength spun out is high, anti-degradability is good.
Description
Technical field
The present invention relates to a kind of preparation method of alginate fibre, more particularly to a kind of preparation side of high intensity alginate fibre
Method.
Background technology
Sodium alginate is a kind of natural polysaccharide extracted from the cell membrane of brown alga, it is by α-L- mannuronic acids
The linear natural polymer that (M units) is formed with β-D- guluronic acids (G units) by Isosorbide-5-Nitrae-glucosides key connection, mean molecule
Amount is differed thousands of between hundreds of thousands.
It is well known that due to having extremely strong intermolecular interaction between strand and strand, (hydrogen bond, electrostatic are made
With), pure sodium alginate solution even under relatively low concentration, is also showing high viscous characteristic, and is easy to gelation, causes to spin
Silk can not carry out.
Therefore, in the sodium alginate fiber wet spinning forming technology of the prior art, to ensure spinnability index, it is necessary to set
Method reduces the viscosity of spinning solution.
At present, general method is to control the concentration of sodium alginate soln in a relatively low concentration range, lead to
Often it is 3wt%-6wt%.Since in the sodium alginate soln of low concentration, sodium alginate component content is relatively fewer, spinning process
In, specific yield needs to consume substantial amounts of spinning solution, causes spinning technique inefficiency.
In the prior art, in order to control the viscosity index of sodium alginate spinning solution, improve sodium alginate fiber and be spun to
Shape efficiency, the sodium alginate spinning solution viscosity reduction technology generally used mainly include two major classes, its mechanism is by making seaweed
Sour sodium is degraded to a certain extent, to realize the reduction of its solution viscosity index.Wherein:One kind is added in sodium alginate soln
Add the oxidants such as hydrogen peroxide, sodium hypochlorite;It is another kind of to be, using sodium alginate soln is heated up, the method for stewing process.
Undeniable to be, the two technology for efficiently solving the reduction of sodium alginate dope viscosity index is asked
Topic.But accompanying problem is that, this method by reducing the sodium alginate degree of polymerization merely, necessarily causes final institute
Obtained alginate fibre mechanical performance index different degrees of reduction or loss.
Therefore, develop that " negative effect " is relatively small (to fiber physical property Index Influence) or there is no " negative
The sodium alginate spinning solution viscosity reduction technology of face effect ", to ensure being smoothed out of spinning technique, promote sodium alginate fiber
The raising of spinning technique efficiency, the production for sodium alginate (or alginate) fiber, is of great practical significance.
The content of the invention
The object of the present invention is to provide a kind of preparation method of high-strength alginate fibre, its technique is simple, easily-controllable, spinnability
It is good;Obtained alginate fiber intensity is high, anti-degradability is good.
To achieve the above object, required technical problems to be solved are not carry out what drop was gathered to sodium alginate to the present invention
Under the premise of, how to make modest viscosity, the spinning solution suitable for wet spinning technology.
The present invention is solution above-mentioned technical problem the technical scheme adopted is that a kind of preparation side of high intensity alginate fibre
Method, it is characterised in that comprise the following steps:
The ratio of the first step, in mass ratio 100 ︰ 0.1-2, weighs sodium alginate and nano-calcium carbonate respectively, spare;
Second step, taken sodium alginate is dissolved in water, be stirred at room temperature 3-6 it is small when, then, be warming up at 50 DEG C,
Continue stir 2-5 it is small when, be configured to mass percent concentration be 3%-12% sodium alginate soln;
And sodium alginate soln is divided into two parts of A, B, nano-calcium carbonate is added in A parts, it is small to be continuously stirred at room temperature 3
When, be then sonicated 0.5-2 it is small when, obtain mixed solution;
Then, B parts are added into above-mentioned mixed solution, stirred evenly, it is former that nano-calcium carbonate-sodium alginate spinning is made
Liquid;
3rd step, passes through filtering by obtained nano-calcium carbonate-sodium alginate spinning solution, is 100Pa in vacuum
Under, rapidly defoaming, it is 20-55 DEG C to control spinning solution temperature, and wet spinning is carried out by coagulating bath of calcium chloride, obtain it is chemical into
It is divided into the as-spun fibre of nano-calcium carbonate-sodium alginate;
4th step, as-spun fibre is placed in deionization water-bath and soaks 24h-72h;Pass through pre-add heating bath successively again, leading
Stretch and drafting forming and oiling treatment are carried out in bath, to obtain the final product;
Above-mentioned pre-add heating bath, drawing-off bath and drafting forming temperature are respectively 30-60 DEG C, 60-120 DEG C and 110-150 DEG C;It is fine
The draw ratio of dimension is 100%-300%;
Above-mentioned A parts is 1 with B parts of volume ratio:3-1:5.
The technical effect brought directely by the technical proposal is that using the skin effect and bulk effect of nano-calcium carbonate,
Increased by the Interfacial Adsorption and interface free volume of nano-calcium carbonate, effectively reduce the viscous of alginate fibre spinning solution
Degree, improves the spinnability of alginate fibre;
Simultaneously as slow release of the nano-calcium carbonate in fibrous inside so that the sodium alginate strand of fibrous inside
Further crosslinking, can be effectively improved mechanical property, the anti-degradability of reinforcing fiber of fiber;Also, it is beneficial to follow-up drawing-off
Process is smoothed out and the stabilization of drawing-off effect and raising.
Calcium carbonate is widely used in the preparation of polymer-based composite as a kind of common reinforcing agent, and particle diameter has pole
Wide scope (10nm-10um), can effectively adjust suspension viscosity.And calcium carbonate indissoluble in aqueous, can slowly discharge
Calcium ion, so as to form certain crosslinking between sodium alginate strand and strand.
In above-mentioned technical proposal, why as-spun fibre is carried out to the immersion treatment (24- of long period in deionized water
72h), it is intended that so that nano-calcium carbonate fully discharges, and then the crosslinking to the sodium alginate strand of fibrous inside is more filled
Point.In this way, the intensity index of product can be effectively improved.
In above-mentioned technical proposal, during the rapidly defoaming of spinning solution, why control in the very high (vacuum of vacuum
Spend to carry out under 100).The reason is that, on the premise of deaeration effect is ensured, the time of bubble removal step is shortened as far as possible, with
The excessive release of nano-calcium carbonate is avoided, and then causes the part sodium alginate (quilt) in spinning solution to be crosslinked, so that spinning
Silk stock solution viscosity raises.
Why it is 1 by volume by sodium alginate raw material in above-mentioned technical proposal:3-1:5 are divided into two parts of A, B, be because
For component A is ultrasonically treated, is the fine dispersion for nano-calcium carbonate, still, in ultrasonication, can not be kept away
It will cause a degree of degraded of sodium alginate with exempting from.A parts that accounting is lacked in selection carry out ultrasonic disperse processing, are blended into afterwards
B parts more than accounting, not only may insure that nano-calcium carbonate obtained good dispersion effect, but also can reduce supersound process to greatest extent
The degraded of sodium alginate caused by process, in turn results in final fiber product physical performance index (particularly intensity index)
Harmful effect.
Preferably, the particle diameter of above-mentioned nano-calcium carbonate is 5nm-100nm.
What the optimal technical scheme was directly brought has the technical effect that, the calcium carbonate of small particle can be well dispersed in first
In sodium alginate soln, secondly the calcium carbonate of small particle plays the role of nano-particle, due to Interfacial Adsorption, interface free volume
Increase, can reduce the resistance of motion of sodium alginate strand, so as to reduce the viscosity of sodium alginate spinning solution.
Further preferably, the mass percent concentration of calcium chloride is 3%-8% in above-mentioned coagulating bath;The temperature of coagulating bath is
25-65℃。
What the optimal technical scheme was directly brought has the technical effect that, power of the technological parameter in spinning process to gained fiber
Performance is learned to have a significant impact.Ours experience have shown that:
1st, the crosslinking of the higher card sodium alginate of calcium chloride concentration is faster, crosslinking is more abundant, but excessive calcium chloride concentration
The crosslinking of sodium alginate can be caused uneven;
2nd, higher solidification bath temperature can cause the activity increase of sodium alginate strand, and drawability is stronger.It is but excessive
Temperature can also cause the degraded of sodium alginate strand.
In conclusion the present invention has the alginate fiber that technology controlling and process is simple, is spun out relative to the prior art
The beneficial effects such as intensity is high, anti-degradability is good.
Embodiment
With reference to embodiment, the present invention is described in detail.
Illustrate, in following embodiment:
1st, raw materials used is commercial product;
2nd, the particle diameter of nano-calcium carbonate is 5nm-100nm;
3rd, the average molecular weight of sodium alginate is 200kDa-500kDa;
4th, the detection method of dope viscosity and properties of product
Dope viscosity:MCR-301 rotational rheometers;
Fiber tensile strength:The full-automatic monofilament tester of FAVIMAT AIROBOT types, alginate fiber is cut to
The short fibre of 6cm or so, takes mass of fibers 50 samples to be stretched with the fiber number, intensity, fracture of full-automatic monofilament tester test fiber
Long rate;
Anti- degradability:Certain filament is weighed, is put into hydrogenperoxide steam generator (1mol/L), observes at regular intervals
Fibre morphology, with observation occur the time of fracture of wire, the time of fibrous fracture, Fibrinolysis time.The above-mentioned time is longer, represents
The anti-degradability of fiber is better.
Embodiment 1
Preparation method comprises the following steps:
The first step, in mass ratio 100:0.1 ratio, weighs 3g sodium alginates and the nano-calcium carbonate of 0.003g respectively,
It is spare;
Second step, taken sodium alginate is added in the deionized water of 100ml and is dissolved, be stirred at room temperature 3 it is small when, so
Afterwards, be warming up at 50 DEG C, continue stirring 2 it is small when, be configured to mass percent concentration be 3% sodium alginate soln;
And by above-mentioned sodium alginate soln according to 1:5 ratio is divided into two parts of A, B, and 0.003g nano-sized carbons are added in A parts
Sour calcium, be continuously stirred at room temperature 3 it is small when, be then sonicated 0.5 it is small when, obtain mixed solution;
Then, B parts are added into above-mentioned mixed solution, stirred evenly, it is former that nano-calcium carbonate-sodium alginate spinning is made
Liquid;
3rd step, passes through filtering by obtained nano-calcium carbonate-sodium alginate spinning solution, is 150Pa in vacuum
Under, rapidly defoaming, it is 20-55 DEG C to control spinning solution temperature, carries out wet spinning by coagulating bath of calcium chloride, obtains nano-sized carbon
Sour calcium-sodium alginate as-spun fibre;
4th step, as-spun fibre is placed in deionization water-bath and soaks 24h;Bathed successively by pre-add heating bath, in drawing-off again
Middle progress drafting forming and oiling treatment, to obtain the final product;
Above-mentioned pre-add heating bath, drawing-off bath and drafting forming temperature are respectively 45 DEG C, 75 DEG C and 125 DEG C;The draw ratio of fiber
For 200%;
The mass percent concentration of calcium chloride is 5% in above-mentioned coagulating bath;The temperature of coagulating bath is 45 DEG C.
Dope viscosity, the testing result of properties of product are as follows:
Dope viscosity testing result
Sample (mass percentage content) | Sodium alginate (3%) | Sodium alginate (3%)+nano-calcium carbonate (0.003%) |
η0[Pa.s] | 12.5 | 10.6 |
Fibre strength testing result
Anti- degradability testing result
Embodiment 2
Preparation method comprises the following steps:
The ratio of the first step, in mass ratio 100 ︰ 0.5, weighs 5g sodium alginates and the nano-calcium carbonate of 0.0.025g respectively
Calcium, it is spare;
Second step, taken sodium alginate is dissolved in water, be stirred at room temperature 4 it is small when, then, be warming up at 50 DEG C, after
When continuous stirring 3.5 is small, the sodium alginate soln that mass percent concentration is 5% is configured to;
And by sodium alginate soln according to 1:4 ratio is divided into two parts of A, B, and 0.025g nano-calcium carbonates are added in A parts,
Be continuously stirred at room temperature 3 it is small when, be then sonicated 1 it is small when, obtain mixed solution;
Then, B parts are added into above-mentioned mixed solution, stirred evenly, it is former that nano-calcium carbonate-sodium alginate spinning is made
Liquid;
3rd step, passes through filtering by obtained nano-calcium carbonate-sodium alginate spinning solution, is 100Pa in vacuum
Under, rapidly defoaming, it is 35 DEG C to control spinning solution temperature, carries out wet spinning by coagulating bath of calcium chloride, obtains nano-calcium carbonate
Calcium-sodium alginate as-spun fibre;
4th step, as-spun fibre is placed in deionization water-bath and soaks 36h;Bathed successively by pre-add heating bath, in drawing-off again
Middle progress drafting forming and oiling treatment, to obtain the final product;
Above-mentioned pre-add heating bath, drawing-off bath and drafting forming temperature are respectively 35 DEG C, 65 DEG C and 115 DEG C;The draw ratio of fiber
For 150%;
The mass percent concentration of calcium chloride is 4% in above-mentioned coagulating bath;The temperature of coagulating bath is 55 DEG C.
Dope viscosity, the testing result of properties of product are as follows:
Dope viscosity testing result
Sample (mass percentage content) | Sodium alginate (5%) | Sodium alginate (5%)+nano-calcium carbonate (0.025%) |
η0[Pa.s] | 55.6 | 43.2 |
Fibre strength testing result
Anti- degradability testing result
Embodiment 3
Preparation method comprises the following steps:
The ratio of the first step, in mass ratio 100 ︰ 1, weighs 7g sodium alginates and the nano-calcium carbonate of 0.07g respectively, standby
With;
Second step, taken sodium alginate is dissolved in water, be stirred at room temperature 5 it is small when, then, be warming up at 50 DEG C, after
When continuous stirring 4 is small, the sodium alginate soln that mass percent concentration is 7% is configured to;
And by sodium alginate soln according to 1:4 ratio is divided into A, B parts, and 0.07g nano-calcium carbonates are added in A parts,
At room temperature persistently stirring 3 it is small when, be then sonicated 1.5 it is small when, obtain mixed solution;
Then, B parts are added into above-mentioned mixed solution, stirred evenly, it is former that nano-calcium carbonate-sodium alginate spinning is made
Liquid;
3rd step, passes through filtering by obtained nano-calcium carbonate-sodium alginate spinning solution, is 100Pa in vacuum
Under, rapidly defoaming, it is 45 DEG C to control spinning solution temperature, carries out wet spinning by coagulating bath of calcium chloride, obtains nano-calcium carbonate
Calcium-sodium alginate as-spun fibre;
4th step, as-spun fibre is placed in deionization water-bath and soaks 48h;Bathed successively by pre-add heating bath, in drawing-off again
Middle progress drafting forming and oiling treatment, to obtain the final product;
Above-mentioned pre-add heating bath, drawing-off bath and drafting forming temperature are respectively 40 DEG C, 60 DEG C and 100 DEG C;The draw ratio of fiber
For 300%;
The mass percent concentration of calcium chloride is 6% in above-mentioned coagulating bath;The temperature of coagulating bath is 40 DEG C.
Dope viscosity, the testing result of properties of product are as follows:
Dope viscosity testing result
Sample (mass percentage content) | Sodium alginate (7%) | Sodium alginate (7%)+nano-calcium carbonate (0.07%) |
η0[Pa.s] | 210.6 | 163.5 |
Fibre strength testing result
Anti- degradability testing result
Embodiment 4
Preparation method comprises the following steps:
The ratio of the first step, in mass ratio 100 ︰ 2, weighs the sodium alginate of 9g and the nano-calcium carbonate of 0.18g respectively, standby
With;
Second step, taken sodium alginate is dissolved in water, be stirred at room temperature 6 it is small when, then, be warming up at 50 DEG C, after
When continuous stirring 4 is small, the sodium alginate soln that mass percent concentration is 9% is configured to;
And by sodium alginate soln according to 1:3 ratio is divided into two parts of A, B, and 0.18g nano-calcium carbonates are added in A parts,
Be continuously stirred at room temperature 3 it is small when, be then sonicated 2 it is small when, obtain mixed solution;
Then, B parts are added into above-mentioned mixed solution, stirred evenly, it is former that nano-calcium carbonate-sodium alginate spinning is made
Liquid;
3rd step, passes through filtering by obtained nano-calcium carbonate-sodium alginate spinning solution, is 100Pa in vacuum
Under, rapidly defoaming, it is 30 DEG C to control spinning solution temperature, carries out wet spinning by coagulating bath of calcium chloride, obtains nano-calcium carbonate
Calcium-sodium alginate as-spun fibre;
4th step, as-spun fibre is placed in deionization water-bath and soaks 72h;Bathed successively by pre-add heating bath, in drawing-off again
Middle progress drafting forming and oiling treatment, to obtain the final product;
Above-mentioned pre-add heating bath, drawing-off bath and drafting forming temperature are respectively 40 DEG C, 80 DEG C and 130 DEG C;The draw ratio of fiber
For 100%;
The mass percent concentration of calcium chloride is 3% in above-mentioned coagulating bath;The temperature of coagulating bath is 25 DEG C.
Dope viscosity, the testing result of properties of product are as follows:
Dope viscosity testing result
Fibre strength testing result
Anti- degradability testing result
Sample (mass percentage content) | There is the time (h) of fracture of wire | The time (h) of fibrous fracture | The time (h) of Fibrinolysis |
Sodium alginate (9%) | 3.5 | 25.5 | 29 |
Sodium alginate (9%)+nano-calcium carbonate (0.18%) | 4 | 28 | 35 |
Embodiment 5
Preparation method comprises the following steps:
The ratio of the first step, in mass ratio 100 ︰ 1, weighs the sodium alginate of 12g and the nano-calcium carbonate of 0.12g respectively,
It is spare;
Second step, taken sodium alginate is dissolved in water, be stirred at room temperature 6 it is small when, then, be warming up at 50 DEG C, after
When continuous stirring 5 is small, the sodium alginate soln that mass percent concentration is 12% is configured to;
And by sodium alginate soln according to 1:3 ratio is divided into two parts of A, B, and 0.18g nano-calcium carbonates are added in A parts,
Be continuously stirred at room temperature 2 it is small when, be then sonicated 1 it is small when, obtain mixed solution;
Then, B parts are added into above-mentioned mixed solution, stirred evenly, it is former that nano-calcium carbonate-sodium alginate spinning is made
Liquid;
3rd step, passes through filtering by obtained nano-calcium carbonate-sodium alginate spinning solution, is 100Pa in vacuum
Under, rapidly defoaming, it is 30 DEG C to control spinning solution temperature, carries out wet spinning by coagulating bath of calcium chloride, obtains nano-calcium carbonate
Calcium-sodium alginate as-spun fibre;
4th step, as-spun fibre is placed in deionization water-bath and soaks 72h;Bathed successively by pre-add heating bath, in drawing-off again
Middle progress drafting forming and oiling treatment, to obtain the final product;
Above-mentioned pre-add heating bath, drawing-off bath and drafting forming temperature are respectively 45 DEG C, 85 DEG C and 135 DEG C;The draw ratio of fiber
For 100%;
The mass percent concentration of calcium chloride is 5% in above-mentioned coagulating bath;The temperature of coagulating bath is 25 DEG C.Spinning solution glues
Degree, product dope viscosity, the testing result of properties of product are as follows:
Dope viscosity testing result
Sample (mass percentage content) | Sodium alginate (12%) | Sodium alginate (12%)+nano-calcium carbonate (0.12%) |
η0[Pa.s] | 2600 | 2310 |
Fibre strength testing result
Anti- degradability testing result
Claims (3)
1. a kind of preparation method of high intensity alginate fibre, it is characterised in that comprise the following steps:
The ratio of the first step, in mass ratio 100 ︰ 0.1-2, weighs sodium alginate and nano-calcium carbonate respectively, spare;
Second step, taken sodium alginate is dissolved in water, be stirred at room temperature 3-6 it is small when, then, be warming up at 50 DEG C, continue
When stirring 2-5 is small, the sodium alginate soln that mass percent concentration is 3%-12% is configured to;
And sodium alginate soln is divided into two parts of A, B, add nano-calcium carbonate in A parts, be continuously stirred at room temperature 3 it is small when,
Be then sonicated 0.5-2 it is small when, obtain mixed solution;
Then, B parts are added into above-mentioned mixed solution, stirred evenly, nano-calcium carbonate-sodium alginate spinning solution is made;
3rd step, by obtained nano-calcium carbonate-sodium alginate spinning solution by filtering, in the case where vacuum is 100Pa, soon
Fast deaeration, it is 20-55 DEG C to control spinning solution temperature, carries out wet spinning by coagulating bath of calcium chloride, obtaining chemical composition is
The as-spun fibre of nano-calcium carbonate-sodium alginate;
4th step, as-spun fibre is placed in deionization water-bath and soaks 24h-72h;Bathed successively by pre-add heating bath, in drawing-off again
Middle progress drafting forming and oiling treatment, to obtain the final product;
Above-mentioned pre-add heating bath, drawing-off bath and drafting forming temperature are respectively 30-60 DEG C, 60-120 DEG C and 110-150 DEG C;Fiber
Draw ratio is 100%-300%;
Above-mentioned A parts is 1 with B parts of volume ratio:3-1:5.
2. the preparation method of high intensity alginate fibre according to claim 1, it is characterised in that the nano-calcium carbonate
Particle diameter is 5nm-100nm.
3. the preparation method of high intensity alginate fibre according to claim 1, it is characterised in that chlorination in the coagulating bath
The mass percent concentration of calcium is 3%-8%;The temperature of coagulating bath is 25-65 DEG C.
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CN100491612C (en) * | 2005-12-21 | 2009-05-27 | 青岛大学 | Algae fiber gel spinning preparing process |
CN100457990C (en) * | 2007-04-16 | 2009-02-04 | 青岛大学 | Producing method and use for common and functional calcium alginate fiber |
CN101768798B (en) * | 2010-01-22 | 2011-06-29 | 青岛大学 | Preparation method of sodium alga acid/ carbon nano tube composite fibre |
CN103774279A (en) * | 2012-10-24 | 2014-05-07 | 众地家纺有限公司 | Preparation method for new alginate fiber material with elasticity |
CN103741249B (en) * | 2013-12-31 | 2015-09-23 | 马海燕 | large-diameter polyvinyl alcohol monofilament and production method thereof |
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