CN112941667B - Alginate fiber and preparation method thereof - Google Patents
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- 239000000835 fiber Substances 0.000 title claims abstract description 91
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229940072056 alginate Drugs 0.000 title claims abstract description 52
- 235000010443 alginic acid Nutrition 0.000 title claims abstract description 52
- 229920000615 alginic acid Polymers 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 238000009987 spinning Methods 0.000 claims abstract description 52
- 239000000243 solution Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 36
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000661 sodium alginate Substances 0.000 claims abstract description 26
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 26
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 26
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- 230000015271 coagulation Effects 0.000 claims abstract description 20
- 238000005345 coagulation Methods 0.000 claims abstract description 20
- 230000001112 coagulating effect Effects 0.000 claims abstract description 17
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229920005862 polyol Polymers 0.000 claims description 2
- 150000003077 polyols Chemical class 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 9
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 5
- 238000013270 controlled release Methods 0.000 abstract description 3
- 238000012377 drug delivery Methods 0.000 abstract description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000004753 textile Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 14
- 238000003756 stirring Methods 0.000 description 6
- 238000007493 shaping process Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- AEMOLEFTQBMNLQ-AZLKCVHYSA-N (2r,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-AZLKCVHYSA-N 0.000 description 2
- LMDZBCPBFSXMTL-UHFFFAOYSA-N 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide Substances CCN=C=NCCCN(C)C LMDZBCPBFSXMTL-UHFFFAOYSA-N 0.000 description 2
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 239000000648 calcium alginate Substances 0.000 description 2
- 235000010410 calcium alginate Nutrition 0.000 description 2
- 229960002681 calcium alginate Drugs 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- OKHHGHGGPDJQHR-YMOPUZKJSA-L calcium;(2s,3s,4s,5s,6r)-6-[(2r,3s,4r,5s,6r)-2-carboxy-6-[(2r,3s,4r,5s,6r)-2-carboxylato-4,5,6-trihydroxyoxan-3-yl]oxy-4,5-dihydroxyoxan-3-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylate Chemical compound [Ca+2].O[C@@H]1[C@H](O)[C@H](O)O[C@@H](C([O-])=O)[C@H]1O[C@H]1[C@@H](O)[C@@H](O)[C@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@H](O2)C([O-])=O)O)[C@H](C(O)=O)O1 OKHHGHGGPDJQHR-YMOPUZKJSA-L 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- AEMOLEFTQBMNLQ-SYJWYVCOSA-N (2s,3s,4s,5s,6r)-3,4,5,6-tetrahydroxyoxane-2-carboxylic acid Chemical compound O[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@@H]1O AEMOLEFTQBMNLQ-SYJWYVCOSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 229920001222 biopolymer Polymers 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000007444 cell Immobilization Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001523 electrospinning Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000002163 immunogen Effects 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Images
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
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Molecular Biology (AREA)
- Textile Engineering (AREA)
- General Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides alginate fibers and a preparation method thereof. The method comprises the following steps: dissolving sodium alginate and polyalcohol in water to obtain a spinning solution; extruding the spinning solution into a coagulating bath for coagulation to obtain spinning fibers, and treating the spinning fibers to obtain alginate fibers; the coagulation bath is an aqueous solution with a pH value lower than 4. According to the invention, the hydroxyl on the polyalcohol is grafted on the carboxyl of the sodium alginate sugar chain, so that stable alginate fibers can be obtained, the preparation process of the spinning solution is simple, the coagulating bath can be recycled, the process is green and environment-friendly, and the production cost is reduced. The alginate fiber obtained by the invention has excellent mechanical property, hydrophobicity and acid resistance, has good application prospect in the fields of textile, drug delivery, controlled release and the like, and improves the effective utilization of ocean resources.
Description
Technical Field
The invention relates to the technical field of chemical fibers, and relates to an alginate fiber and a preparation method thereof.
Background
Sodium alginate is both a biopolymer and a polyelectrolyte that is considered biocompatible, non-toxic, non-immunogenic, and biodegradable. Alginate is characterized by a microstructure of a biocompatible unbranched copolymer, which has been widely used as an ideal biomaterial in many fields, such as cell immobilization, tissue engineering, drug delivery, controlled release, immobilized microorganisms, and food applications.
At present, the calcium alginate fiber is generally spun by a wet method, the most common coagulating bath used is 2 to 8 percent of calcium chloride water solution by weight, and Ga in the coagulating bath is passed through2+Cross-linking with carboxyl group on sodium alginate, consuming Ga2+Meanwhile, a large amount of water resources are consumed, and the obtained alginate calcium fiber has high hydrophilicity and poor acid resistance and hydrophobic property.
Disclosure of Invention
In view of the above-mentioned problems in the prior art, the present invention provides a alginate fiber and a method for preparing the same. The invention adopts the esterification reaction of the polyhydric alcohol and the sodium alginate to obtain the acid-resistant hydrophobic alginate fiber, and meanwhile, the coagulating bath is used as the catalyst, does not participate in the reaction, can be recycled, and is a green and environment-friendly spinning method.
The technical scheme of the invention is as follows:
a method for preparing alginate fibers comprises the following steps:
(1) dissolving sodium alginate and polyalcohol in water to obtain a spinning solution;
(2) extruding the spinning solution obtained in the step (1) into a coagulating bath for coagulation to obtain spinning fibers, and treating the spinning fibers to obtain alginate fibers;
wherein the coagulation bath is an aqueous solution with a pH value lower than 4.
In the above technical solution, the polyol is one or a mixture of more of ethylene glycol, propylene glycol, glycerol or pentaerythritol, and glycerol is preferred.
In the above technical solution, in the step (1), the concentration of the sodium alginate in the spinning solution is 1-10% by weight, preferably 2-7% by weight, and more preferably 3% by weight.
In the above technical solution, in the step (1), the weight percentage concentration of the polyhydric alcohol in the spinning solution is 0.4% to 15%, preferably 0.8% to 3%.
In the technical scheme, in the step (1), the polyhydric alcohol is added into the deionized water, stirred and mixed uniformly, then the sodium alginate is added, stirred uniformly, and subjected to vacuum centrifugal defoaming to obtain the spinning solution.
In the above technical scheme, the pH value of the coagulation bath is adjusted to be less than or equal to 4 by using acetic acid, citric acid, hydrochloric acid, sulfuric acid or phosphoric acid.
In the technical scheme, in the step (2), the spinning solution is extruded into a coagulating bath under the pressure of 0.2-0.6Mpa for coagulation to obtain spinning fibers, and the spinning fibers are washed, drafted and dried for shaping until the water content is less than 4% to obtain the alginate fibers, wherein the coagulation time of the extruded spinning fibers in the coagulating bath is 2-20min, and the temperature of the coagulating bath is 20-60 ℃.
In the above technical scheme, in the water washing step, the water washing temperature of the spun fiber is 20-60 ℃.
In the above technical scheme, in the drafting step, the drawing temperature of the spun fiber is 45-60 ℃, and the drawing multiple is 1-3 times.
In the above technical scheme, in the drying and setting step, the drying temperature of the spun fiber is 80-120 ℃.
The fiber obtained by spinning the spinning solution obtained by the method has good acid resistance, is solidified in an aqueous solution with the pH value less than or equal to 4, and has good mechanical property and acid resistance. The used coagulating bath is aqueous solution with pH value adjusted to be less than or equal to 4 by organic acid or inorganic acid, does not contain inorganic salt such as calcium chloride and the like, has no loss of components in the coagulating process, can be repeatedly recycled, and can greatly reduce the cost. In the present invention, an appropriate amount of an activator, such as 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride (EDC), may be added to the coagulation bath.HCl) and N-hydroxysuccinimide (NHS), etc., to accelerate fiber setting and suitably shorten setting time.
In the present invention, sodium alginate can be used in industrial or food grade, and preferably has a molecular weight of 3-5 × 106g/mol, preferably 3X 106g/mol。
The sodium alginate molecule is formed by connecting beta-D-mannuronic acid (beta-D-mannuronic, M) and alpha-L-guluronic acid (alpha-L-guluronic acid, G) according to a (1 → 4) bond, is a natural polysaccharide, and has a large number of carboxyl groups in the molecular structure.
The invention has the beneficial effects that:
the invention provides alginate fibers and a preparation method thereof for the first time. Dissolving sodium alginate in water solution containing polyalcohol to obtain spinning solution, and extruding the spinning solution into acidic coagulating bath through spinning to make hydroxyl on polyalcohol and carboxyl of sodium alginate sugar chain undergo esterification reaction and condensation to form alginate, i.e. the hydroxyl on polyalcohol is grafted on the carboxyl of sodium alginate sugar chain to obtain stable alginate fiber; the preparation process of the spinning solution is simple, the coagulating bath can be recycled, and the method is an environment-friendly process and reduces the production cost.
The alginate fibers prepared by the method have excellent mechanical property, hydrophobicity and acid resistance, have good application prospects in the fields of spinning, drug delivery, controlled release and the like, and improve the effective utilization of ocean resources.
Drawings
FIG. 1 shows a reaction scheme of the present invention (ethylene glycol is taken as an example).
FIG. 2 shows the infrared spectra of sodium alginate and the alginate fibers prepared in examples 1-3.
Fig. 3A shows a contact angle test chart of the alginate fiber prepared in example 1.
Fig. 3B shows a contact angle test chart of the alginate fiber prepared in example 2.
Fig. 3C shows a contact angle test chart of the alginate fiber prepared in example 3.
Detailed Description
In order to make the objects, schemes, procedures and advantages of the present invention more clear, the spinning process of the present invention will be further described in detail with reference to the accompanying drawings and examples, it should be noted that the specific examples herein are only for illustrating the present invention and are not to be construed as limiting the present invention. In the following examples, unless otherwise specified, the experimental methods used were all conventional methods, and the experimental instruments, materials, reagents and the like used were all available from chemical companies. The following are the starting materials used in the examples:
sodium alginate: purchased from Qingdao Mingyue algae group Ltd, molecular weight 3X 106g/mol。
Example 1
A method for preparing alginate fiber comprises:
(1) adding ethylene glycol into deionized water, fully stirring to uniformly mix, then adding sodium alginate, uniformly stirring, and carrying out vacuum centrifugal defoaming to obtain a spinning solution;
(2) uniformly pressing the spinning solution into a metering pump under the compressed air with the pressure of 0.2-0.6Mpa, metering by the metering pump, then feeding into a filter, spinning, extruding into a coagulating bath at 25 ℃, curing for 10min to form fibers, washing the fibers in a water bath at 40 ℃, drafting for 1.3 times under the water bath at 55 ℃, drying and shaping at 80 ℃ until the water content is less than 4%, and obtaining the alginate fibers.
In the step (1), the concentration of sodium alginate in the spinning solution was 3 wt%, and the concentration of ethylene glycol was 0.94 wt%.
In the step (2), the coagulation bath was an aqueous solution containing 0.72% hydrochloric acid, and the pH of the coagulation bath was 0.83.
Example 2
A method for preparing alginate fiber comprises:
(1) adding glycerol into deionized water, fully stirring to uniformly mix, then adding sodium alginate, uniformly stirring, and carrying out vacuum centrifugal deaeration to obtain a spinning solution;
(2) uniformly pressing the spinning solution into a metering pump under the compressed air with the pressure of 0.2-0.6Mpa, metering by the metering pump, feeding into a filter, spinning, extruding into a coagulating bath at 25 ℃, solidifying for 10min to form fibers, washing the fibers in a water bath at 40 ℃, drafting by 1.3 times in the water bath at 55 ℃, drying and shaping at 80 ℃ until the water content is less than 4%, and obtaining the alginate fibers.
In the step (1), the concentration of sodium alginate in the spinning solution was 3 wt%, and the concentration of glycerol was 1.4 wt%.
In step (2), the coagulation bath is an aqueous solution containing 0.72% hydrochloric acid.
Example 3
A method for preparing alginate fiber comprises:
(1) adding pentaerythritol into deionized water, fully stirring to uniformly mix, then adding sodium alginate, uniformly stirring, and carrying out vacuum centrifugal deaeration to obtain a spinning solution;
(2) uniformly pressing the spinning solution into a metering pump under the compressed air with the pressure of 0.2-0.6Mpa, metering by the metering pump, feeding into a filter, spinning, feeding the extruded spinning fiber into a coagulating bath at 25 ℃, solidifying for 10min to form fiber, washing the fiber in a water bath at 40 ℃, drafting for 1.3 times under the water bath at 55 ℃, and drying and shaping at 80 ℃ until the water content is less than 4% to obtain the alginate fiber.
In the step (1), the concentration of sodium alginate in the spinning solution was 3 wt%, and the concentration of pentaerythritol was 2.06 wt%.
In step (2), the coagulation bath is an aqueous solution containing 0.72% hydrochloric acid.
Example 4
Taking the alginate fibers and sodium alginate prepared in the examples 1-3, detecting by an infrared spectrometer (DZG-6021, platinum Elmer, USA), and tabletting the fibers by a KBr tabletting method; the test range is 500-4000cm-1。
The detection result is shown in FIG. 2, and it can be seen that the alginate fiber prepared by the method of the present invention is 1745cm-1And the ester group (COOR) stretching vibration peak of sodium alginate which is obviously distinguished exists on the left and the right, which proves that the fiber prepared by the method is the alginate.
Example 5
The alginate fibers prepared in examples 1 to 3 were used to test the breaking strength and the like of the composite fibers using a single fiber strength tester (LLY-06ED, Laizhou electric power instruments Co., Ltd.), and the test results are shown in Table 1 below:
taking composite fiber with standard length of 20mm, wherein the drawing speed is 10 mm/min; the test was performed at 20 ℃, 65% r.h; the results are shown in Table 1, with the results being averaged over 10 tests.
TABLE 1 Strength test results for alginate fibers
The results in table 1 show that: the alginate fibers prepared by the method have better breaking strength and breaking elongation rate, and are higher than those of common calcium alginate fibers.
Example 6
The alginate fibers prepared in the embodiments 1 to 3 are taken, the fibers are respectively put into 10.8 percent HCl aqueous solution (pH value is-0.5), soaked for 12 hours at 20 ℃, then washed by deionized water until the pH value of the fiber attachment solution is about 6 to 7, and then naturally dried for standby.
The treated fibers were tested for breaking strength and the like of the composite fibers according to the test method in example 6, and the test results are shown in table 2 below:
TABLE 2 Strength test results for alginate fibers
The results in table 1 show that: the alginate fibers prepared by the method have the strength of more than 2.9cN/dtex after being soaked in acid solution for 12 hours, and the strength loss rate of the alginate fibers is lower than 30 percent compared with the original fibers before being soaked in the acid solution; the alginate fibers prepared by the method have good acid resistance.
Example 7
The alginate fibers prepared in examples 1 to 3 were used and the samples were tested using a standard contact angle measuring instrument (model DSA25, kluss scientific instruments ltd) according to the following method:
the fiber was fixed on a glass slide, the sample was tested by sitting drop method, and the reading was taken after the drop was stable for 10 s. And (3) testing temperature: 20 ℃, test liquid: and (3) water.
Fig. 3A to 3C respectively show the measurement results of the alginate fibers prepared in examples 1 to 3, and it can be seen that the contact angle test results of the alginate fibers prepared by the method of the present invention by the sitting drop method are all greater than 90 °, which proves that the fibers prepared by the method of the present invention have good hydrophobicity.
In the above examples, a conventional wet spinning method of extruding the spinning solution through a spinneret of an appropriate diameter under a certain pressure to a coagulation bath to obtain a fiber was used, but the spinning solution of the present invention may also be applied to other various spinning methods such as electrospinning and the like. The fineness of the alginate fibers obtained in examples 1 to 3 was 30 to 84dtex, but alginate fibers of various fineness could be obtained depending on the drop of the spinneret or the spinning method.
The embodiments described above are intended to facilitate one of ordinary skill in the art in understanding and using the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (7)
1. A method for preparing alginate fibers comprises the following steps:
(1) dissolving sodium alginate and polyalcohol in water to obtain a spinning solution;
(2) extruding the spinning solution obtained in the step (1) into a coagulating bath for coagulation to obtain spinning fibers, and treating the spinning fibers to obtain alginate fibers;
wherein the coagulation bath is an aqueous solution with a pH value lower than 4;
the polyalcohol is one or a mixture of more of ethylene glycol, propylene glycol, glycerol or pentaerythritol;
in the step (1), the weight percentage concentration of the sodium alginate in the spinning solution is 1-10%, and the weight percentage concentration of the polyalcohol is 0.4-15%.
2. The method for preparing alginate fibers according to claim 1, wherein in the step (1), the polyol is added into the deionized water, stirred and mixed uniformly, then the sodium alginate is added, stirred uniformly, and subjected to vacuum centrifugal deaeration to obtain a spinning solution.
3. The method of claim 1, wherein the pH of the coagulation bath is adjusted to pH 4 or less with acetic acid, citric acid, hydrochloric acid, sulfuric acid or phosphoric acid.
4. The method for preparing alginate fibers according to claim 1, wherein in the step (2), the spinning solution is extruded into the coagulation bath under the pressure of 0.2-0.6Mpa to be coagulated, thereby obtaining the spinning fibers, and the spinning fibers are washed, drafted and dried to be formed to have the water content of less than 4%, thereby obtaining the alginate fibers, wherein the coagulation time of the extruded spinning fibers in the coagulation bath is 2-20min, and the temperature of the coagulation bath is 20-60 ℃.
5. The method for preparing alginate fibers according to claim 4, wherein the washing temperature of the spun fibers in the washing step is 20-60 ℃.
6. The method for preparing alginate fibers according to claim 4, wherein in the drawing step, the drawing temperature of the spun fibers is 45-60 ℃ and the drawing ratio is 1-3.
7. The method for preparing alginate fibers according to claim 4, wherein the drying and setting step is carried out at a temperature of 80-120 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110163959.7A CN112941667B (en) | 2021-02-05 | 2021-02-05 | Alginate fiber and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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