CN109972233A - The preparation method of the biodegradable alginic acid fibre with high-intensity and high-tenacity - Google Patents
The preparation method of the biodegradable alginic acid fibre with high-intensity and high-tenacity Download PDFInfo
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- CN109972233A CN109972233A CN201910120944.5A CN201910120944A CN109972233A CN 109972233 A CN109972233 A CN 109972233A CN 201910120944 A CN201910120944 A CN 201910120944A CN 109972233 A CN109972233 A CN 109972233A
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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
- 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
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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
- 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
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Abstract
The invention discloses a kind of preparation methods of biodegradable alginic acid fibre with high-intensity and high-tenacity, belong to the preparation technical field of alginic acid fibre.The preparation method includes: that raw material sodium alginate and cellulose ether are dissolved in deionized water first, is arranged to co-blended spinning liquid A；Then poly- polysaccharide nano dispersion fluid is prepared, and gained co-blended spinning liquid A and the poly- polysaccharide nano dispersion fluid of gained are sufficiently mixed, the compound of polysorbas20, monoglyceride or both is added thereto, co-blended spinning liquid B is obtained after successively agitated, deaeration；Finally co-blended spinning liquid B is placed in coagulating bath, using wet spinning technology, up to alginic acid fibre after drawing-off, washing, immersion, drying.The present invention has the beneficial effects such as easily-controllable simple process, energy conservation and environmental protection, good product quality.
Description
Technical field
The present invention relates to the preparation technical fields of alginic acid fibre, and in particular to a kind of to select environmentally protective matter biomaterial
The method for preparing high-intensity and high-tenacity alginate fibre.
Background technique
China be the first big country of algae culturing and seaweed processing big country, cultivation with processing seaweed account for the whole world 70% with
On.Algal polysaccharides have wide development and application prospect, can produce large quantities of measurers by material base of cheap algal polysaccharides
There are important value and high value-added product.The natural polysaccharide sodium alginate extracted from seaweed can be used as raw material, by wet
Method spinning technique prepares alginic acid fibre, and research finds that alginic acid fibre has many excellent performances, such as high-hygroscopicity, hemostasis
Property, high oxygen permeability, gel blockage, biological degradability and biocompatibility etc., can be used for making non-woven fabrics and fabric, for curing
With gauze, bandage, dressing and facial mask etc..But alginic acid fibre ultimate strength is low, and extension at break is small, easily broken in spinning process
It splits, belongs to typical brittle fracture, greatly limit its application range.
Based on above-mentioned the technical problems existing in the prior art, the researchers in the field are more absorbed in correlative study
Improve the mechanical property of alginic acid fibre, and improve the method for alginic acid fibre mechanical property mainly by alginic acid into
Row is modified, and method of modifying mainly includes physical modification and chemical modification.Wherein physical modification mainly has the methods of blending, filling,
Chemical modification mainly includes the means such as copolymerization, grafting.
Mainly have about above-mentioned correlative study report: adding inorganic nanoparticles in spinning solution, such as adds nanometer two
Silica, nano montmorillonite, nano-titanium dioxide, nano-aluminum hydroxide etc. prepare alginic acid/inorganic nano by wet spinning
Particle composite fibre utilizes the good characteristics such as the high intensity, high rigidity, high-specific surface area of inorganic nanoparticles itself, enhancing sea
The tension failure strength of alginate fibre.Some promotes alginic acid fibre big using epoxychloropropane preparation crosslinking alginic acid fibre
Crosslinking between molecule；Or calcium alginate fibre is impregnated using copper-bath, by the way that there is higher sequestering power with oxygen atom
Copper ion and calcium ion occur ion-exchanged calcium alginate fibre.
If 106012103 A of CN discloses a kind of preparation method of high-intensitive alginate fibre, in sodium alginate soln
It joined nanometer calcium carbonate and spinning solution be made, by the spinning solution through filtering, rapidly defoaming, carried out by coagulating bath of calcium chloride
Wet spinning obtains a nanometer as-spun fibre；Then, as-spun fibre impregnates to -72h for 24 hours in deionized water, then it is post-treated i.e.
?.
106149099 A of CN discloses a kind of preparation method of high-intensitive alginate fibre, has produced alginate first
Spinning solution is done then alginate spinning solution is obtained after alginate and polyvinyl alcohol blending or crosslinking through spinning, microwave
High-intensitive alginate fibre is prepared after dry and etc..
Although above method can be effectively improved the mechanical property of alginate fibre, it, which is only absorbed in, improves seaweed fibre
The intensity of dimension lacks the green environmental protection of used material and considers, as the addition of inorganic nano-particle may be to alginic acid fibre
The biocompatibility and degradability of dimension generate adverse effect, also will affect other performances such as its moisture-absorbing moisture-keeping.
Summary of the invention
The purpose of the present invention is to provide a kind of systems of biodegradable alginic acid fibre with high-intensity and high-tenacity
Preparation Method, which not only reduces problem of environmental pollutions caused by preparation process, moreover it is possible to while improving the mechanics of alginic acid fibre
Performance.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of biodegradable alginic acid fibre, which is characterized in that successively the following steps are included:
Raw material sodium alginate and cellulose ether are dissolved in deionized water by a, the sodium alginate and cellulose ether
Mass ratio is 3~5:1, and configuration obtains the co-blended spinning liquid A that mass percent is 6~12%；
B weighs a certain amount of poly- polysaccharide nano-crystalline, and is dissolved in deionized water, at 25 DEG C, 800~1000w function
Ultrasonic wave disperses 2~3h under rate, obtains poly- polysaccharide nano dispersion fluid；
Poly- polysaccharide nano dispersion fluid obtained by co-blended spinning liquid A obtained by step a and step b is sufficiently mixed by c, and is added thereto
Enter the substance D that mass fraction is 0.05~0.5%, co-blended spinning liquid B is obtained after successively agitated, deaeration；
Co-blended spinning liquid B described in step c is placed in coagulating bath by d, using wet spinning technology, through drawing-off, washing, leaching
Up to alginic acid fibre after bubble, drying；
The cellulose ether be water soluble anionic or non-ionic, the substance D be polysorbas20, monoglyceride or
The compound of the two.
The direct bring of the optimal technical scheme has the technical effect that
(1) present invention utilizes poly- polysaccharide nano-crystalline large specific surface area, and good biocompatibility is environmental-friendly, reproducible excellent
Point, after poly- polysaccharide nano-crystalline is added in alginic acid matrix, special orientation, three-dimensional net structure and interfacial structure are not only
Strong hydrogen bond can be formed with alginic acid matrix, load is undertaken in alginic acid fibre drawing process, and can play rivet
Effect, prevents the diffusion of crackle, spreads stress to different directions, to improve the strength and toughness of alginic acid fibre material；
In addition, the addition of cellulose ether can form molecular entanglement with alginic acid, the tensile toughness of alginic acid fibre is effectively improved, because
This can by the poly- polysaccharide nano-crystalline of control addition and the amount of cellulose ether, so as to adjust the balance between strength and toughness,
Meet the different application demand of alginic acid fibre.
(2) raw material selected by the present invention do not use any harmful chemicals, entirely degradable green
Environment-friendly materials do not have any damage to the Green performance of alginic acid.
(3) present invention process is simple, and power consumption of polymer processing is low, and the industrialization that can be perfectly suitable for alginic acid fibre is continuously given birth to
It produces.
It is of the invention for ease of understanding, it is described further below with reference to reaction mechanism of the Fig. 4 to above-mentioned technical proposal.
Cellulose ether macromolecular is added in alginic acid matrix, entangled to each other between alginic acid and cellulose ether macromolecular,
And intermolecular hydrogen bonding is formed, and poly- polysaccharide nano-crystalline is evenly spread in two kinds of macromolecular network structures, and keep network more complicated, at
Three-dimensional structure, by after calcium chloride coagulation bath, the combination of alginic acid molecular rearrangement, G unit in macromolecular with
Calcium ion chelates to form eggshell structure, between macromolecular relative close arrange, tangle reductions, at this time cellulose ether macromolecular with gather
Polysaccharide nano-crystalline plays the role of its tensile property vital, and cellulose ether macromolecular can be between alginic acid macromolecular
Entanglement effect is played, when alginic acid fibre receives stretching, after alginic acid fibre weak section fracture, still has cellulose ether to divide greatly
Son plays a part of support frame, in addition, between the hydroxyl in cellulose ether macromolecular and the polar group of alginic acid macromolecular
There are hydrogen bond action, poly- polysaccharide nano-crystalline is shown in there is hydrogen bond action with two kinds of macromoleculars in the base, draws in alginic acid fibre
Load is undertaken during stretching, and rivet can be played the role of, prevents the diffusion of crackle, spreads stress to different directions, two
Person's synergistic effect, preferably improves the strength and toughness of alginic acid fibre.
As a preferred solution of the present invention, the cellulose ether of above-mentioned water soluble anionic is carboxymethyl cellulose,
Non-ionic cellulose ether is methylcellulose, hydroxyethyl cellulose, hydroxypropyl cellulose or hydroxypropyl methyl cellulose.
As another preferred embodiment of the invention, above-mentioned cellulose ether is hydroxypropyl methyl cellulose.
Further, in step a, the mass ratio of above-mentioned sodium alginate and cellulose ether is 4:1.
Further, in step b, it is poly- that above-mentioned poly- polysaccharide nano-crystalline is selected from Cellulose nanocrystal, nanometer starch crystal or shell
Sugar is nanocrystalline.
Further, above-mentioned poly- polysaccharide nano-crystalline is Cellulose nanocrystal.
Further, the preparation step of step d coagulating bath are as follows: a certain amount of calcium chloride is dissolved in distilled water, is produced
The calcium chloride water for being 4~6% to mass percent, coagulation bath temperature are 15~30 DEG C.
Further, in step d, three-stage draft process is taken, the multiple of every segment process drawing-off is 1.2~1.5 times, water
15~50 DEG C of temperature taken are washed, 50~70 DEG C of temperature taken are dried.
Compared with prior art, present invention offers following advantageous effects:
Firstly, the present invention has selected the combination of poly- polysaccharide nano-crystalline and cellulose ether from the selection of raw material, thus prepare
Obtained alginic acid fibre belongs to green product, can make various needles, woven fabric and non-woven fabrics, can be not only used for medical yarn
Cloth, bandage and dressing etc. have the characteristics that biological degradability and compatibility, promote wound healing, reduce wound pain, is medicine
Field provides new medical material, and increases new green fiber material to take fabric, greatly improves marine prods
Added value, while the problems such as by making full use of marine resources, alleviating tired synthetic fibers resource, environmental pollution.
In addition, in preparation method, entanglement of formation network between cellulose ethers macromolecular and alginic acid macromolecular gathers more
The nanocrystalline structure in matrix of sugar includes orientation, three-dimensional net structure and interfacial structure, is added into fiber in alginic acid matrix
After plain ether and poly- polysaccharide nano-crystalline, load can be undertaken in alginic acid fibre drawing process by forming special stereochemical structure,
Poly- polysaccharide nano-crystalline plays the role of rivet, prevents the diffusion of crackle, spreads stress to different directions, cellulose ether macromolecular
Playing the role of tangling and be buffered with fracture, the two, which acts synergistically, can greatly improve the strength and toughness of alginic acid fibre material,
In addition, the hydrogen bond between poly- polysaccharide nano-crystalline and alginic acid also enhances active force between the two to a certain extent.
Finally, the present invention is compared with prior art, have easily-controllable simple process, energy conservation and environmental protection, good product quality etc. beneficial to effect
Fruit.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawing:
Fig. 1 is pure alginic acid fibre tension failure of the invention face figure；
Fig. 2 is the tension failure face figure for the alginate fibre that following embodiments 3 are prepared；
Fig. 3 is the x-ray diffraction pattern of pure alginate fibre and embodiment 3；
Fig. 4 is reaction mechanism schematic diagram of the present invention.
Specific embodiment
The invention proposes a kind of preparation methods of biodegradable alginic acid fibre with high-intensity and high-tenacity, are
Keep advantages of the present invention, technical solution clearer, clear, elaborates combined with specific embodiments below to the present invention.
Illustrate: raw material needed for following embodiment can be bought by commercial channel and be obtained.
Cellulose ether mainly selects anionic and non-ionic, anionic: carboxymethyl cellulose (CMC)；
It is non-ionic: methylcellulose (MC), hydroxyethyl cellulose (HEC), hydroxypropyl cellulose (HPC), hydroxypropyl first
Base cellulose (HPMC)；
It is brilliant that poly- polysaccharide nano-crystalline is selected from Cellulose nanocrystal, nanometer starch crystal or chitosan nano.
Embodiment 1:
The preparation method of the biodegradable alginic acid fibre with high-intensity and high-tenacity, specifically includes the following steps:
Raw material sodium alginate and cellulose ether hydroxypropyl methyl cellulose are dissolved in deionized water, seaweed by the first step
Sour sodium and the mass ratio of hydroxypropyl methyl cellulose are 3:1, and configuration obtains the co-blended spinning liquid A that mass percent is 6%；
Second step, the Cellulose nanocrystal (relative to sodium alginate) for weighing 8wt%, and be dissolved in deionized water,
At 25 DEG C, ultrasonic wave disperses 2~3h under 800~1000w power, obtains Cellulose nanocrystal dispersion liquid；
Cellulose nanocrystal dispersion liquid obtained by co-blended spinning liquid A obtained by the first step and second step is sufficiently mixed by third step,
And the polysorbas20 that mass fraction is 0.05% is added thereto, co-blended spinning liquid B is obtained after successively agitated, deaeration；
Co-blended spinning liquid B obtained by third step is placed in coagulating bath by the 4th step, using wet spinning technology, through drawing-off, water
It washes, be immersed in after the alcoholic solution of 90wt%, drying up to alginic acid fibre；
15~40 DEG C of spinning solution temperature, 15~30 DEG C of coagulation bath temperature, three-stage draft process is taken in drawing-off, and every section is led
The multiple stretched is 1.2~1.5 times, washes 15~50 DEG C of temperature taken, dries 50~70 DEG C of temperature taken.
Embodiment 2:
Difference from Example 1 is: the quality proportioning of sodium alginate and hydroxypropyl methyl cellulose is 4:1.
Embodiment 3:
Difference from Example 1 is: the quality proportioning of sodium alginate and hydroxypropyl methyl cellulose is 5:1.
Embodiment 4:
Difference from Example 1 is: cellulose ether selects hydroxyethyl cellulose, sodium alginate and hydroxyethyl cellulose
Quality proportioning be 4:1, poly- polysaccharide nano-crystalline selects nanometer starch crystal.
Embodiment 5:
Difference from Example 1 is: cellulose ether selects hydroxypropyl cellulose, sodium alginate and hydroxypropyl cellulose
Quality proportioning be 4:1, poly- polysaccharide nano-crystalline selection chitosan nano is brilliant.
Embodiment 6:
Difference from Example 1 is:
Cellulose nanocrystal dispersion liquid obtained by co-blended spinning liquid A obtained by the first step and second step is sufficiently mixed by third step,
And the compound of polysorbas20 and monoglyceride that mass fraction is 0.5% is added thereto, spinning must be blended after successively agitated, deaeration
Silk liquid B.
Embodiment 7:
Difference from Example 1 is:
Cellulose nanocrystal dispersion liquid obtained by co-blended spinning liquid A obtained by the first step and second step is sufficiently mixed by third step,
And the monoglyceride that mass fraction is 0.5% is added thereto, co-blended spinning liquid B is obtained after successively agitated, deaeration.
Comparative example 1:
Raw material sodium alginate is dissolved in deionized water by the first step, and configuration obtains the alginic acid that mass percent is 6%
Spinning solution A；
Second step, the Cellulose nanocrystal (relative to sodium alginate) for weighing 8wt%, and be dissolved in deionized water,
At 25 DEG C, ultrasonic wave disperses 2~3h under 800~1000w power, obtains Cellulose nanocrystal dispersion liquid；
Cellulose nanocrystal dispersion liquid obtained by spinning solution A obtained by the first step and second step is sufficiently mixed by third step, and to
The polysorbas20 that mass fraction is 0.05% is wherein added, co-blended spinning liquid B is obtained after successively agitated, deaeration；
Co-blended spinning liquid B obtained by third step is placed in coagulating bath by the 4th step, using wet spinning technology, through drawing-off, water
It washes, be immersed in after the alcoholic solution of 90wt%, drying up to alginic acid fibre；
15~40 DEG C of spinning solution temperature, 15~30 DEG C of coagulation bath temperature, three-stage draft process is taken in drawing-off, and every section is led
The multiple stretched is 1.2~1.5 times, washes 15~50 DEG C of temperature taken, dries 50~70 DEG C of temperature taken.
The alginic acid fibre that above-described embodiment 1- embodiment 7, comparative example 1 are prepared carries out following Mechanics Performance Testing,
Wherein, the test method of major parameter are as follows: use single fiber tester, fiber is fixed in fixture, the stretching of fiber is tested
Breaking strength and fracture elongation.Gauge: 10mm, tensile speed: 8mm/min.The mechanical property of fiber takes the flat of 50 samples
Mean value.Test result is as shown in table 1.
The physical mechanical property of the modified alginic acid fibre of table 1
The hydrogen bond that above-mentioned table 1 further demonstrates between poly- polysaccharide nano-crystalline and alginic acid also enhances to a certain extent
Active force between the two.As depicted in figs. 1 and 2, the cross section surface of pure alginic acid fibre is smooth, some regions are in mirror surface,
Belong to typical brittle fracture, and fiber cross sections mirror sections completely disappear in embodiment 3, occur rough tough
Nest illustrates that embodiment toughness enhances.As shown in figure 3, the purer alginic acid fibre enhancing of 3 crystallinity of embodiment, elaborates its strength
One of the reason of increase.
It uses for reference the prior art and can be realized in the part that do not addressed in the present invention.
It should be noted that any equivalent way that those skilled in the art are made under the introduction of this specification, or
Obvious variant should all be within the scope of the present invention.
Claims (8)
1. a kind of preparation method of biodegradable alginic acid fibre, which is characterized in that successively the following steps are included:
Raw material sodium alginate and cellulose ether are dissolved in deionized water by a, the quality of the sodium alginate and cellulose ether
Than for 3~5:1, configuration obtains the co-blended spinning liquid A that mass percent is 6~12%；
B weighs a certain amount of poly- polysaccharide nano-crystalline, and is dissolved in deionized water, at 25 DEG C, under 800~1000w power
Ultrasonic wave disperses 2~3h, obtains poly- polysaccharide nano dispersion fluid；
Co-blended spinning liquid A obtained by step a and poly- polysaccharide nano dispersion fluid obtained by step b are sufficiently mixed by c, and matter is added thereto
The substance D that score is 0.05~0.5% is measured, co-blended spinning liquid B is obtained after successively agitated, deaeration；
Co-blended spinning liquid B described in step c is placed in coagulating bath by d, using wet spinning technology, through drawing-off, washing, immersion,
Up to alginic acid fibre after drying；
The cellulose ether is water soluble anionic or non-ionic, and the substance D is polysorbas20, monoglyceride or both
Compound.
2. the preparation method of the biodegradable alginic acid fibre of one kind according to claim 1, it is characterised in that: water-soluble
Property anionic cellulose ether be carboxymethyl cellulose, non-ionic cellulose ether be methylcellulose, hydroxy ethyl fiber
Element, hydroxypropyl cellulose or hydroxypropyl methyl cellulose.
3. the preparation method of the biodegradable alginic acid fibre of one kind according to claim 2, it is characterised in that: described
Cellulose ether be hydroxypropyl methyl cellulose.
4. the preparation method of the biodegradable alginic acid fibre of one kind according to claim 1, it is characterised in that: step
In a, the mass ratio of the sodium alginate and cellulose ether is 4:1.
5. the preparation method of the biodegradable alginic acid fibre of one kind according to claim 1, it is characterised in that: step
In b, it is brilliant that the poly- polysaccharide nano-crystalline is selected from Cellulose nanocrystal, nanometer starch crystal or chitosan nano.
6. the preparation method of the biodegradable alginic acid fibre of one kind according to claim 5, it is characterised in that: described
Poly- polysaccharide nano-crystalline be Cellulose nanocrystal.
7. the preparation method of the biodegradable alginic acid fibre of one kind according to claim 1, which is characterized in that step
The preparation step of coagulating bath described in d are as follows: a certain amount of calcium chloride is dissolved in distilled water, produces to obtain mass percent to be 4
~6% calcium chloride water, coagulation bath temperature are 15~30 DEG C.
8. the preparation method of the biodegradable alginic acid fibre of one kind according to claim 1, it is characterised in that: step
In d, three-stage draft process is taken, the multiple of every segment process drawing-off is 1.2~1.5 times, 15~50 DEG C of temperature taken are washed,
Dry 50~70 DEG C of temperature taken.
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