CN107237005B - Alginic acid and chitosan double-component fiber and preparation method thereof - Google Patents
Alginic acid and chitosan double-component fiber and preparation method thereof Download PDFInfo
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- CN107237005B CN107237005B CN201710464271.6A CN201710464271A CN107237005B CN 107237005 B CN107237005 B CN 107237005B CN 201710464271 A CN201710464271 A CN 201710464271A CN 107237005 B CN107237005 B CN 107237005B
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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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- 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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/32—Side-by-side structure; Spinnerette packs therefor
Abstract
The invention relates to alginic acid and chitosan bicomponent fiber and a preparation method thereof, which solve the technical problem that the existing calcium alginate and chitosan composite medical dressing product can not be processed into yarns and woven fabrics, and in the cross section, the alginic acid fiber component and the chitosan fiber component divide the cross section into two parts with any composition proportion and shape; preferably, the alginic acid fiber component and the chitosan fiber component have a shape of a semicircle or a sector or an arch in a circular cross section thereof. The invention provides a preparation method of alginic acid and chitosan bicomponent fiber, which comprises the following steps: the preparation method comprises the steps of preparing the sodium alginate spinning solution, preparing the chitosan spinning solution and preparing the alginic acid and chitosan bicomponent fiber, and can be widely applied to the field of surgical medical dressings.
Description
Technical Field
The invention relates to the field of surgical medical dressings, in particular to alginic acid and chitosan bicomponent fiber and a preparation method thereof.
Background
Chitosan (Chitosan) is used as the only basic polysaccharide widely existing in the nature, has excellent bioactivity, biocompatibility, microbial degradability and low toxicity, and is suitable for controlled release of drugs, beauty treatment, food preservation, fertilizers and biodegradable packaging materials. Meanwhile, the metal ion adsorbent can absorb metal ions and hydrophobic organic compounds, and can be used in the field of wastewater treatment. The chitosan serving as a medical hemostatic material can resist bacteria, stop bleeding, repair and activate damaged cells, promote wound healing and prevent tissue and organ adhesion. Chitosan as an ideal hemostatic material has the following advantages: 1. and (4) a hemostatic function. In the environment without blood coagulation factors and blood platelets, chitosan with positive charges on the surface interacts with red blood cells with negative charges on the surface, and is coagulated and adhered on the surface of a wound, so that the aim of rapidly closing a bleeding part is fulfilled. 2. Promoting wound healing. Chitosan can activate complement C3 and C5, which in turn induces local macrophage proliferation and enhanced activity. Meanwhile, chitosan can also promote the secretion of type III collagen, accelerate the generation of granulation tissues and epithelial tissues and shorten the wound healing time. 3. It is safe and analgesic. The biocompatibility between chitosan and human cells is good, and the tissue of a wound part is not stimulated. Meanwhile, the medicine can adsorb protons released by acidic substances of wound inflammation to achieve the effect of analgesia. 4. The scar is weakened. The chitosan can relieve wound contraction and weaken scar by inhibiting the growth of I-type ossein and fibroblast at wound.
Alginic Acid (Alginic Acid) is a natural polymer material, has good biocompatibility and biodegradability, and can be used as a natural plant wound repair material to protect the wound surface and treat burns and scalds. Wherein, the calcium alginate fiber prepared by the wet spinning of the sodium alginate spinning solution is commonly used as surgical medical dressing. When the calcium alginate fiber contacts with the exudate of the wound part, calcium ions in the calcium alginate and sodium ions in the exudate are subjected to ion exchange, and the calcium alginate is converted into water-soluble sodium alginate. Meanwhile, the fiber is converted into gel after absorbing a large amount of moisture, and the surface of the wound can be kept moist. Modern medical research finds that the alginic acid fiber provides a relatively humid, slightly acidic and anaerobic or hypoxic environment, is beneficial to the release of growth factors at a wound part, stimulates cell proliferation, stimulates epidermal cell regeneration and movement, directly acts on macrophages, promotes wound healing and relieves wound pain. The alginic acid fiber has high hygroscopicity and moisture retention, and the hydrogel formed by the alginic acid fiber has the effects of stopping bleeding, coagulating, inhibiting bacteria and the like, is easy to remove after being used, and can avoid two wounds.
With the development of medical technology, single-component medical dressings prepared from calcium alginate fibers or chitosan fibers cannot meet the requirements of modern clinical care, and calcium alginate/chitosan composite medical dressings are regarded as ideal medical dressings due to excellent moisturizing, hemostasis, blood coagulation and antibacterial effects. Chinese patent publication No. CN 104069536 a discloses a preparation method of a sodium alginate/chitosan nano-grade medical dressing: and spinning the sodium alginate and the synthetic polymer ethanol solution by using the chitosan solution as a coagulating liquid, and adsorbing chitosan on the surface of the calcium alginate fiber through electrostatic interaction to obtain the sodium alginate/chitosan composite nanofiber. Chinese patent publication No. CN 104623716A prepares a medical calcium alginate fiber composite dressing by blending alginate fiber staple fibers and chitosan staple fibers. The disadvantage is that the products prepared by these methods cannot be processed into yarns and woven fabrics.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide alginic acid and chitosan bicomponent fiber with strong regulation and control performance and processability and a preparation method thereof on the basis of excellent moisturizing, hemostasis, blood coagulation and antibacterial effects.
The technical scheme adopted by the invention for solving the technical problem is as follows: the invention provides alginic acid and chitosan bicomponent fiber, in the cross section of which, the alginic acid fiber component and the chitosan fiber component divide the cross section into two parts with any proportion and shape, and the alginic acid fiber component and the chitosan fiber component are connected by Van der Waals force.
Preferably, the alginic acid fiber component and the chitosan fiber component have a shape of a semicircle or a sector or an arch in a circular cross section thereof.
The invention provides a preparation method of alginic acid and chitosan bicomponent fiber, which comprises the following steps:
(1) preparation of sodium alginate spinning solution
Dissolving alginic acid in a mixed solution consisting of water, sodium chloride and sodium hydroxide, wherein the mass fraction of the sodium chloride is 0.01-0.1%, and the mass fraction of the sodium hydroxide is 1-8%, and then filtering and defoaming to prepare a sodium alginate spinning solution with the mass fraction of 4-30%;
(2) preparation of chitosan spinning solution
Dissolving chitosan in glacial acetic acid water solution with the mass fraction of 0.8-10%, filtering, and defoaming to prepare chitosan spinning solution with the mass fraction of 0.5-8%;
(3) preparation of chitosan and alginic acid double-component fiber
And (3) simultaneously conveying the sodium alginate spinning solution prepared in the step (1) and the chitosan spinning solution prepared in the step (2) to a spinning part by using a metering pump, and then spinning the bicomponent fiber by a dry-jet wet spinning process: solidifying and forming the spinning solution by using a solidifying solution, wherein the solidifying solution consists of water, linear or dendritic lower alcohol and ketone, the mass fraction of the lower alcohol is 0-50%, the mass fraction of the ketone is 0-20%, and then carrying out conventional process treatment of drafting, washing, drying and filament collection to obtain the chitosan and alginic acid bicomponent fiber; distance of spinning member from liquid surface of coagulating liquid: 3-25 cm; conveying speed of spinning solution: 50-1000 mL/min; spinning temperature: 30-70 ℃; temperature of the coagulation bath: 20-50 ℃; draft ratio: 1 to 5.
Preferably, the alginic acid in the step (1) is one or more of pure alginic acid, alginate and derivatives thereof, and blends, compounds and modified substances using alginic acid or alginate as a matrix.
Preferably, the alginate and the derivative thereof are selected from one or more of sodium alginate, potassium alginate, ammonium alginate or propylene glycol alginate; the blend, compound or modifier with alginic acid or alginate as matrix is selected from one or more of chitosan and alginic acid, collagen and alginic acid, and silver and alginic acid.
Preferably, the chitosan in step (2) comprises pure chitosan, a chitosan blend, a chitosan composite, and water-soluble or water-swelling chitosan with chitosan as a matrix.
Preferably, the chitosan blend is a blend of chitosan and a spinnable polymer; the spinnable polymer is one or more of polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone or sodium carboxymethylcellulose; the chitosan compound is selected from one or more than one of a compound of silver and chitosan, a compound of collagen and chitosan, a compound of alginate and chitosan, and a compound of folic acid and chitosan; the water soluble or water swelling chitosan with chitosan as matrix is one or more of carboxymethyl chitosan, hydroxypropyl chitosan, hydroxyethyl chitosan or carboxybutyl chitosan.
Preferably, the lower alcohol in step (3) is a C1-C12 linear or dendritic alcohol which is one or more of methanol, ethanol, propanol, isopropanol, butanol, sec-butanol, isobutanol and tert-butanol.
Preferably, the step (3) ketone is acetone or methyl ethyl ketone.
Preferably, the spinning part in the step (3) mainly comprises a first distribution plate, a first spinneret plate, a second distribution plate and a second spinneret plate, wherein a plurality of first distribution holes are formed in the inner ring of the first distribution plate, and a plurality of spinning solution through holes are formed in the outer ring of the first distribution plate; the first spinneret plate is of a disc-shaped structure with high edge and low bottom, a plurality of first spinneret holes are formed in the bottom of the first spinneret plate and communicated with the first distribution holes, and the uppermost end of the edge of the first spinneret plate is fixedly connected with the inner ring of the first distribution plate; the second spinneret plate is of a basin-shaped structure with a high edge and a low bottom, a plurality of second spinneret holes are formed in the bottom of the basin-shaped structure, and the uppermost end of the edge of the basin-shaped structure is fixedly connected with the outer ring of the first distribution plate; the second distribution plate is fixedly arranged at the bottom of an inner cavity of the second spinneret plate and is arranged below the first spinneret plate, the second distribution plate is provided with a plurality of second distribution holes and a plurality of third spinneret holes, the second distribution holes are communicated with the second spinneret holes, the third spinneret holes are the same in number as the second spinneret holes and are communicated with the second spinneret holes in a one-to-one correspondence manner in position, the third spinneret holes are the same in size as the first spinneret holes and smaller than the second spinneret holes, and the third spinneret holes are hermetically connected with the first spinneret holes through spinneret tubes; the outer side wall of the first spinneret plate and the inner side wall of the second spinneret plate form a spinning solution channel, and the spinning solution channel is respectively communicated with the spinning solution through hole and the second distribution hole.
The invention has the beneficial effects that: the invention provides alginic acid and chitosan bicomponent fiber and a preparation method thereof, on the basis of having excellent moisturizing, hemostasis, blood coagulation and antibacterial effects, a new preparation process is adopted, the controllability of the processing process is enhanced, the produced alginic acid and chitosan bicomponent fiber has strong processability, can be processed into yarn, woven fabric, knitted fabric and non-woven fabric medical dressing materials, has wide application range, and solves the problems of the prior art; in addition, the biocompatibility and the biodegradability are good. The detection shows that the prepared fiber has the strength of 1.0-2.6 g/d and the elongation at break of 12-24%, and meets the requirements of subsequent manufacturing of mechanical properties of yarns, woven fabrics, knitted fabrics and non-woven fabrics.
Drawings
FIG. 1 is a schematic structural diagram of an alginic acid and chitosan bicomponent fiber of the present invention;
FIG. 2 is a schematic view of the configuration of FIG. 1 in which the fiber component of circular cross-section is semi-circular;
FIG. 3 is a schematic view of the circular cross-section fiber component of FIG. 1 in fan-shaped configuration;
FIG. 4 is a schematic view of the configuration of FIG. 1 in which the circular cross-section fiber component is arcuate;
FIG. 5 is a schematic diagram of the structure of the main process of the present invention;
FIG. 6 is a schematic structural view of a spinning element of the present invention;
FIG. 7 is a top view of FIG. 6;
FIG. 8 is a bottom view of FIG. 6;
FIG. 9 is a sectional view A-A of FIG. 7;
FIG. 10 is a front view of a first distributor plate in the spinning pack of the present invention;
FIG. 11 is a cross-sectional view of the first distributor plate of FIG. 9;
fig. 12 is a front view of a first spinneret in a spinning member of the present invention;
FIG. 13 is a top view of FIG. 12;
fig. 14 is a cross-sectional view of a first spinneret in the spinning member of fig. 9;
FIG. 15 is a front view of a second distributor plate in the spinning section of the present invention;
FIG. 16 is a bottom view of FIG. 15;
fig. 17 is a cross-sectional view of the first spinneret and the second distribution plate in the spinning section of fig. 9;
fig. 18 is a front view of a second spinneret in a spinning member of the present invention;
fig. 19 is a cross-sectional view of the second spinneret of fig. 9;
fig. 20 is a schematic view of the structure in which the sodium alginate spinning solution and the chitosan spinning solution are separately passed through the spinning part.
Description of reference numerals: 1. the spinning process comprises the following steps of (1) alginic acid fiber, (2) chitosan fiber, (3) chitosan and alginic acid bicomponent fiber, (4) a first distribution plate, (5) a first spinneret plate, (6) a second distribution plate, (7) a second spinneret plate, (8) a first distribution hole, (9) a spinning solution through hole, (10) a first spinneret hole, (11) a third spinneret hole, (12) a second distribution hole, (13) a second spinneret hole, (14) a spinneret tube, (15) a spinning solution channel, (16) sodium alginate spinning solution, (17) chitosan spinning solution, (18) a first metering pump, (19) a second metering pump, (20) a spinning part, (21) a curing tank, (22) drafting, (23) water washing, (24) yarn collecting and (25) yarn guide rollers.
Detailed Description
The invention is further described below in conjunction with the drawings and the specific embodiments to assist in understanding the contents of the invention. The method used in the invention is a conventional method if no special provisions are made; the raw materials and the apparatus used are, unless otherwise specified, conventional commercially available products.
Example 1
The invention provides a preparation method of alginic acid and chitosan bicomponent fiber, which comprises the following steps:
(1) preparation of sodium alginate spinning solution
Dissolving pure alginic acid in a mixed solution consisting of water, sodium chloride and sodium hydroxide, wherein the mass fraction of the sodium chloride is 0.01%, and the mass fraction of the sodium hydroxide is 1%, and then filtering and defoaming to prepare a sodium alginate spinning solution with the mass fraction of 4%;
(2) preparation of chitosan spinning solution
Dissolving pure chitosan in glacial acetic acid water solution with the mass fraction of 0.8%, and filtering and defoaming to prepare chitosan spinning solution with the mass fraction of 0.5%;
(3) preparation of chitosan and alginic acid double-component fiber
And (3) simultaneously conveying the sodium alginate spinning solution prepared in the step (1) and the chitosan spinning solution prepared in the step (2) to a spinning part by using a metering pump, and then spinning the bicomponent fiber by a dry-jet wet spinning process: solidifying and forming the spinning solution by using a solidifying solution, wherein the solidifying solution consists of water and methyl ethyl ketone, the mass fraction of the methyl ethyl ketone is 2%, and then carrying out conventional process treatment of drafting, washing, drying and filament collection to obtain the chitosan and alginic acid bicomponent fiber; distance of spinning member from liquid surface of coagulating liquid: 3-25 cm; conveying speed of spinning solution: 50-1000 mL/min; spinning temperature: 30-70 ℃; temperature of the coagulation bath: 20-50 ℃; draft ratio: 1 to 5.
Tests prove that the prepared alginic acid and chitosan bicomponent fiber has the strength of 1.5-2.3 g/d and the elongation at break of 12-20%, and meets the requirements of subsequent manufacturing of mechanical properties of yarns, woven fabrics, knitted fabrics and non-woven fabrics medical dressing materials.
Example 2
The invention provides a preparation method of alginic acid and chitosan bicomponent fiber, which comprises the following steps:
(1) preparation of sodium alginate spinning solution
Dissolving pure alginic acid in a mixed solution consisting of water, sodium chloride and sodium hydroxide, wherein the mass fraction of the sodium chloride is 0.05 percent, and the mass fraction of the sodium hydroxide is 5 percent, and then filtering and defoaming to prepare a sodium alginate spinning solution with the mass fraction of 15 percent;
(2) preparation of chitosan spinning solution
Dissolving pure chitosan in a glacial acetic acid aqueous solution with the mass fraction of 5%, and filtering and defoaming to prepare a chitosan spinning solution with the mass fraction of 4%;
(3) preparation of chitosan and alginic acid double-component fiber
And (3) simultaneously conveying the sodium alginate spinning solution prepared in the step (1) and the chitosan spinning solution prepared in the step (2) to a spinning part by using a metering pump, and then spinning the bicomponent fiber by a dry-jet wet spinning process: solidifying and forming the spinning solution by using a solidifying solution, wherein the solidifying solution consists of 5 mass percent of water, 2 mass percent of ethanol and 2 mass percent of acetone, and then carrying out conventional process treatment of drawing, washing, drying and filament collection to obtain the chitosan and alginic acid bicomponent fiber; distance of spinning member from liquid surface of coagulating liquid: 3-25 cm; conveying speed of spinning solution: 50-1000 mL/min; spinning temperature: 30-70 ℃; temperature of the coagulation bath: 20-50 ℃; draft ratio: 1 to 5.
Tests prove that the prepared alginic acid and chitosan bicomponent fiber has the strength of 1.2-2.4 g/d and the elongation at break of 15-20%, and meets the requirements of subsequent manufacturing of mechanical properties of yarns, woven fabrics, knitted fabrics and non-woven fabrics medical dressing materials.
Example 3
The invention provides a preparation method of alginic acid and chitosan bicomponent fiber, which comprises the following steps:
(1) preparation of sodium alginate spinning solution
Dissolving pure alginic acid in a mixed solution consisting of water, sodium chloride and sodium hydroxide, wherein the mass fraction of the sodium chloride is 0.1%, and the mass fraction of the sodium hydroxide is 8%, and then filtering and defoaming to prepare a sodium alginate spinning solution with the mass fraction of 30%;
(2) preparation of chitosan spinning solution
Dissolving pure chitosan into a glacial acetic acid aqueous solution with the mass fraction of 10%, and filtering and defoaming to prepare a chitosan spinning solution with the mass fraction of 8%;
(3) preparation of chitosan and alginic acid double-component fiber
And (3) simultaneously conveying the sodium alginate spinning solution prepared in the step (1) and the chitosan spinning solution prepared in the step (2) to a spinning part by using a metering pump, and then spinning the bicomponent fiber by a dry-jet wet spinning process: solidifying and forming the spinning solution by using a solidifying solution, wherein the solidifying solution consists of 10 mass percent of propanol and 4 mass percent of methyl ethyl ketone, and then carrying out conventional process treatment of drawing, washing, drying and filament collection to obtain the chitosan and alginic acid bicomponent fiber; distance of spinning member from liquid surface of coagulating liquid: 3-25 cm; conveying speed of spinning solution: 50-1000 mL/min; spinning temperature: 30-70 ℃; temperature of the coagulation bath: 20-50 ℃; draft ratio: 1 to 5.
Tests prove that the prepared alginic acid and chitosan bicomponent fiber has the strength of 1.0-1.8 g/d and the elongation at break of 12-17%, and meets the requirements of subsequent manufacturing of mechanical properties of yarns, woven fabrics, knitted fabrics and non-woven fabrics medical dressing materials.
Example 4
The invention provides a preparation method of alginic acid and chitosan bicomponent fiber, which comprises the following steps:
(1) preparation of sodium alginate spinning solution
Dissolving sodium alginate in a mixed solution consisting of water, sodium chloride and sodium hydroxide, wherein the mass fraction of the sodium chloride is 0.01 percent, and the mass fraction of the sodium hydroxide is 1 percent, and then filtering and defoaming to prepare a sodium alginate spinning solution with the mass fraction of 4 percent;
(2) preparation of chitosan spinning solution
Dissolving the blend of chitosan and polyvinyl alcohol in glacial acetic acid aqueous solution with the mass fraction of 0.8%, filtering and defoaming to prepare chitosan spinning solution with the mass fraction of 0.5%;
(3) preparation of chitosan and alginic acid double-component fiber
And (3) simultaneously conveying the sodium alginate spinning solution prepared in the step (1) and the chitosan spinning solution prepared in the step (2) to a spinning part by using a metering pump, and then spinning the bicomponent fiber by a dry-jet wet spinning process: solidifying and forming the spinning solution by using a solidification solution, wherein the solidification solution consists of water, isopropanol and acetone, the mass fraction of the isopropanol is 15%, the mass fraction of the acetone is 6%, and then carrying out conventional process treatment of drawing, washing, drying and filament collection to obtain the chitosan and alginic acid bicomponent fiber; distance of spinning member from liquid surface of coagulating liquid: 3-25 cm; conveying speed of spinning solution: 50-1000 mL/min; spinning temperature: 30-70 ℃; temperature of the coagulation bath: 20-50 ℃; draft ratio: 1 to 5.
Tests prove that the prepared alginic acid and chitosan bicomponent fiber has the strength of 1.1-2.2 g/d and the elongation at break of 16-24%, and meets the requirements of subsequent manufacturing of mechanical properties of yarns, woven fabrics, knitted fabrics and non-woven fabrics medical dressing materials.
Example 5
The invention provides a preparation method of alginic acid and chitosan bicomponent fiber, which comprises the following steps:
(1) preparation of sodium alginate spinning solution
Dissolving potassium alginate in a mixed solution composed of water, sodium chloride and sodium hydroxide, wherein the mass fraction of the sodium chloride is 0.03%, and the mass fraction of the sodium hydroxide is 2%, and then filtering and defoaming to prepare a sodium alginate spinning solution with the mass fraction of 8%;
(2) preparation of chitosan spinning solution
Dissolving the blend of chitosan and polyethylene glycol in 2% glacial acetic acid water solution by mass fraction, filtering and defoaming to prepare 1% chitosan spinning solution by mass fraction;
(3) preparation of chitosan and alginic acid double-component fiber
And (3) simultaneously conveying the sodium alginate spinning solution prepared in the step (1) and the chitosan spinning solution prepared in the step (2) to a spinning part by using a metering pump, and then spinning the bicomponent fiber by a dry-jet wet spinning process: solidifying and forming the spinning solution by using a solidifying solution, wherein the solidifying solution consists of 20 mass percent of butanol and 8 mass percent of methyl ethyl ketone, and then carrying out conventional process treatment of drawing, washing, drying and filament collection to obtain the chitosan and alginic acid bicomponent fiber; distance of spinning member from liquid surface of coagulating liquid: 3-25 cm; conveying speed of spinning solution: 50-1000 mL/min; spinning temperature: 30-70 ℃; temperature of the coagulation bath: 20-50 ℃; draft ratio: 1 to 5.
Tests prove that the prepared alginic acid and chitosan bicomponent fiber has the strength of 1.0-2.0 g/d and the elongation at break of 14-22%, and meets the requirements of subsequent manufacturing of mechanical properties of yarns, woven fabrics, knitted fabrics and non-woven fabrics medical dressing materials.
Example 6
The invention provides a preparation method of alginic acid and chitosan bicomponent fiber, which comprises the following steps:
(1) preparation of sodium alginate spinning solution
Dissolving a blend of silver and alginic acid in a mixed solution consisting of water, sodium chloride and sodium hydroxide, wherein the mass fraction of the sodium chloride is 0.04%, and the mass fraction of the sodium hydroxide is 4%, and then filtering and defoaming to prepare a 10% mass fraction sodium alginate spinning solution;
(2) preparation of chitosan spinning solution
Dissolving a compound of collagen and chitosan in a glacial acetic acid aqueous solution with the mass fraction of 4%, filtering and defoaming to prepare a chitosan spinning solution with the mass fraction of 2%;
(3) preparation of chitosan and alginic acid double-component fiber
And (3) simultaneously conveying the sodium alginate spinning solution prepared in the step (1) and the chitosan spinning solution prepared in the step (2) to a spinning part by using a metering pump, and then spinning the bicomponent fiber by a dry-jet wet spinning process: solidifying and forming the spinning solution by using a solidification solution, wherein the solidification solution consists of water, sec-butyl alcohol and acetone, the mass fraction of the sec-butyl alcohol is 25%, the mass fraction of the acetone is 10%, and then carrying out conventional process treatment of drawing, washing, drying and filament collection to obtain the chitosan and alginic acid bicomponent fiber; distance of spinning member from liquid surface of coagulating liquid: 3-25 cm; conveying speed of spinning solution: 50-1000 mL/min; spinning temperature: 30-70 ℃; temperature of the coagulation bath: 20-50 ℃; draft ratio: 1 to 5.
Tests prove that the prepared alginic acid and chitosan bicomponent fiber has the strength of 1.8-2.6 g/d and the elongation at break of 13-19%, and meets the requirements of subsequent manufacturing of mechanical properties of yarns, woven fabrics, knitted fabrics and non-woven fabrics medical dressing materials.
Example 7
The invention provides a preparation method of alginic acid and chitosan bicomponent fiber, which comprises the following steps:
(1) preparation of sodium alginate spinning solution
Dissolving a compound of collagen and alginic acid in a mixed solution consisting of water, sodium chloride and sodium hydroxide, wherein the mass fraction of the sodium chloride is 0.06%, and the mass fraction of the sodium hydroxide is 5%, and then filtering and defoaming to prepare a sodium alginate spinning solution with the mass fraction of 15%;
(2) preparation of chitosan spinning solution
Dissolving hydroxyethyl chitosan in a glacial acetic acid aqueous solution with the mass fraction of 6%, filtering and defoaming to prepare a chitosan spinning solution with the mass fraction of 4%;
(3) preparation of chitosan and alginic acid double-component fiber
And (3) simultaneously conveying the sodium alginate spinning solution prepared in the step (1) and the chitosan spinning solution prepared in the step (2) to a spinning part by using a metering pump, and then spinning the bicomponent fiber by a dry-jet wet spinning process: solidifying and molding the spinning solution by using a solidification solution, wherein the solidification solution consists of water, isobutanol and methyl ethyl ketone, the mass fraction of the isobutanol is 30%, the mass fraction of the methyl ethyl ketone is 12%, and then performing conventional process treatment of drawing, washing, drying and filament collection to obtain the chitosan and alginic acid bicomponent fiber; distance of spinning member from liquid surface of coagulating liquid: 3-25 cm; conveying speed of spinning solution: 50-1000 mL/min; spinning temperature: 30-70 ℃; temperature of the coagulation bath: 20-50 ℃; draft ratio: 1 to 5.
Tests prove that the prepared alginic acid and chitosan bicomponent fiber has the strength of 1.6-2.3 g/d and the elongation at break of 17-23%, and meets the requirements of subsequent manufacturing of mechanical properties of yarns, woven fabrics, knitted fabrics and non-woven fabrics medical dressing materials.
Example 8
The invention provides a preparation method of alginic acid and chitosan bicomponent fiber, which comprises the following steps:
(1) preparation of sodium alginate spinning solution
Dissolving a modified substance of alginic acid and chitosan in a mixed solution consisting of water, sodium chloride and sodium hydroxide, wherein the mass fraction of the sodium chloride is 0.08%, and the mass fraction of the sodium hydroxide is 6%, and then filtering and defoaming to prepare a sodium alginate spinning solution with the mass fraction of 25%;
(2) preparation of chitosan spinning solution
Dissolving a mixture of carboxymethyl chitosan and hydroxypropyl chitosan in a glacial acetic acid aqueous solution with the mass fraction of 8%, filtering, and defoaming to prepare a chitosan spinning solution with the mass fraction of 6%;
(3) preparation of chitosan and alginic acid double-component fiber
And (3) simultaneously conveying the sodium alginate spinning solution prepared in the step (1) and the chitosan spinning solution prepared in the step (2) to a spinning part by using a metering pump, and then spinning the bicomponent fiber by a dry-jet wet spinning process: solidifying and molding the spinning solution by using a solidification solution, wherein the solidification solution consists of water, tert-butyl alcohol and acetone, the mass fraction of the tert-butyl alcohol is 40%, the mass fraction of the acetone is 15%, and then carrying out conventional process treatment of drawing, washing, drying and filament collection to obtain the chitosan and alginic acid bicomponent fiber; distance of spinning member from liquid surface of coagulating liquid: 3-25 cm; conveying speed of spinning solution: 50-1000 mL/min; spinning temperature: 30-70 ℃; temperature of the coagulation bath: 20-50 ℃; draft ratio: 1 to 5.
Tests prove that the prepared alginic acid and chitosan bicomponent fiber has the strength of 1.2-2.1 g/d and the elongation at break of 15-22%, and meets the requirements of subsequent manufacturing of mechanical properties of yarns, woven fabrics, knitted fabrics and non-woven fabrics medical dressing materials.
Example 9
The invention provides a preparation method of alginic acid and chitosan bicomponent fiber, which comprises the following steps:
(1) preparation of sodium alginate spinning solution
Dissolving a mixture of sodium alginate and alginic acid in a mixed solution consisting of water, sodium chloride and sodium hydroxide, wherein the mass fraction of the sodium chloride is 0.1%, and the mass fraction of the sodium hydroxide is 8%, and then filtering and defoaming the solution to prepare a sodium alginate spinning solution with the mass fraction of 30%;
(2) preparation of chitosan spinning solution
Dissolving a compound of folic acid and chitosan in a glacial acetic acid aqueous solution with the mass fraction of 10%, and filtering and defoaming to prepare a chitosan spinning solution with the mass fraction of 8%;
(3) preparation of chitosan and alginic acid double-component fiber
And (3) simultaneously conveying the sodium alginate spinning solution prepared in the step (1) and the chitosan spinning solution prepared in the step (2) to a spinning part by using a metering pump, and then spinning the bicomponent fiber by a dry-jet wet spinning process: solidifying and forming the spinning solution by using a solidifying solution, wherein the solidifying solution consists of water, linear or dendritic lower alcohol and methyl ethyl ketone, the lower alcohol is a mixture of methanol and ethanol, the mass fraction of the lower alcohol is 50%, the mass fraction of the methyl ethyl ketone is 20%, and then carrying out conventional process treatment of drawing, water washing, drying and filament collection to obtain the chitosan and alginic acid bicomponent fiber; distance of spinning member from liquid surface of coagulating liquid: 3-25 cm; conveying speed of spinning solution: 50-1000 mL/min; spinning temperature: 30-70 ℃; temperature of the coagulation bath: 20-50 ℃; draft ratio: 1 to 5.
Tests prove that the prepared alginic acid and chitosan bicomponent fiber has the strength of 1.5-2.3 g/d and the elongation at break of 13-21%, and meets the requirements of subsequent manufacturing of mechanical properties of yarns, woven fabrics, knitted fabrics and non-woven fabrics medical dressing materials.
As shown in fig. 1-4, the prepared alginic acid and chitosan bicomponent fiber consists of alginic acid fiber 1 and chitosan fiber 2, in the cross section of the fiber, the alginic acid fiber component and the chitosan fiber component divide the cross section into two parts with any proportion and shape, and the alginic acid fiber component and the chitosan fiber component are connected by van der waals force; the spinneret orifice shape of the spinning part determines the composition ratio and the shape of the two components in the cross section of the invention, for example, the spinneret orifice shape of the spinning part can be set to be circular, and in the circular cross section of the bicomponent fiber, the shapes of the alginic acid fiber component and the chitosan fiber component are 3 common shapes of a semicircle or a sector or an arch. Tests prove that the prepared alginic acid and chitosan bicomponent fiber has the strength of 1.0-2.6 g/d and the elongation at break of 12-24%, meets the requirements of the processing mechanical properties of yarns, woven fabrics, knitted fabrics and non-woven fabrics medical dressing materials, and solves the problems in the prior art. In addition, the invention has good biocompatibility and biodegradability, meets the functional requirements of human bodies and protects the environment.
In the above embodiments 1 to 9, as shown in fig. 6 to 20, the spinning part in step (3) mainly includes the first distribution plate 4, the first spinneret plate 5, the second distribution plate 6, and the second spinneret plate 7, the inner ring of the first distribution plate 4 is provided with a plurality of first distribution holes 8, the outer ring of the first distribution plate 4 is provided with a plurality of spinning solution through holes 9, and the inner ring is lower than the outer ring, so that the sodium alginate spinning solution is uniformly distributed in the flow channel cavity to prepare for subsequent spinning; the first spinneret plate 5 is of a disc-shaped structure with high edge and low bottom, a plurality of first spinneret holes 10 are formed in the bottom of the first spinneret plate 5 and communicated with the first distribution holes 8, and the uppermost end of the edge of the first spinneret plate 5 is fixedly connected with the inner ring of the first distribution plate 4; the second spinneret plate 7 is of a basin-shaped structure with a high edge and a low bottom, a plurality of second spinneret holes 13 are formed in the bottom of the basin-shaped structure, and the uppermost end of the edge of the basin-shaped structure is fixedly connected with the outer ring of the first distribution plate 4; the second distribution plate 6 is fixedly arranged at the bottom of the inner cavity of the second spinneret plate 7 and below the first spinneret plate 5, and the second distribution plate 6 is provided with a plurality of second distribution holes 12 and a plurality of third spinneret holes 11, so that the chitosan spinning solution is uniformly distributed in the flow channel cavity to prepare for subsequent spinning; the second distribution holes 12 are communicated with the second spinneret holes 13, the third spinneret holes 11 are the same in number as the second spinneret holes 13 and are communicated in a one-to-one correspondence manner in position, the third spinneret holes 11 are the same in pore size as the first spinneret holes 10 and smaller than the pore size of the second spinneret holes 13, and the third spinneret holes 11 are hermetically connected with the first spinneret holes 10 through spinneret tubes 14; the outer side wall of the first spinneret plate 5 and the inner side wall of the second spinneret plate 7 form a spinning solution channel 15, and the spinning solution channel 15 is respectively communicated with the spinning solution through hole 9 and the second distribution hole 12. Number of second orifices 13: 50-1000 parts; diameter of the second spinneret hole 13: 0.05-0.1 mm.
The main contents of the present invention will be described in detail below with reference to fig. 5 and 20 for a further understanding of the present invention: the prepared sodium alginate spinning solution 16 is fed to a spinning section 20 through a first metering pump 18, and the prepared chitosan spinning solution 17 is fed to the spinning section 20 through a second metering pump 19. The sodium alginate spinning solution 16 enters the first distribution holes 8 in the inner ring of the first distribution plate 4, passes through the first spinneret holes 10 of the first spinneret plate 5, passes through the spinneret tube 14, enters the third spinneret holes 11 of the second distribution plate 6, and enters the second spinneret holes 13 of the second spinneret plate 7 from the third spinneret holes 11 under the action of high-speed inertia; meanwhile, the chitosan spinning solution 17 enters the spinning solution through hole 9 on the outer ring of the first distribution plate 4, passes through the second distribution hole 12 of the second distribution plate 6 through the spinning solution channel 15, enters the second spinneret hole 13 of the second spinneret plate 7, is combined with the sodium alginate spinning solution 16 and is output. And then spinning the bicomponent fiber by a dry-jet wet spinning process: the combined and output spinning solution is solidified and formed through a curing tank 21, and then is processed through conventional processes of drawing 22, washing 23, drying and filament collecting 24 to obtain the chitosan and alginic acid bicomponent fiber 3. The whole preparation process is finished by guiding through a godet roller 25.
It should be noted that: the blend, compound or modifier with alginic acid or alginate as matrix is selected from one or more of chitosan and alginic acid, collagen and alginic acid, and silver and alginic acid, and refers to the blend with alginic acid or alginate as matrix is selected from one or more of chitosan and alginic acid, collagen and alginic acid, and silver and alginic acid, the complex or modifier with alginic acid or alginate as matrix is selected from one or more of chitosan and alginic acid, collagen and alginic acid, and silver and alginic acid, and the modifier with alginic acid or alginate as matrix is selected from one or more of chitosan and alginic acid, collagen and alginic acid, and silver and alginic acid.
However, the above description is only an embodiment of the present invention, and the scope of the present invention should not be limited by this, and all equivalent changes and modifications made in the claims of the present invention should be covered by the present invention.
Claims (7)
1. The alginic acid and chitosan bicomponent fiber is characterized in that in the circular cross section, the alginic acid fiber component and the chitosan fiber component are in the shape of a semicircle, a sector or an arch, and are connected by Van der Waals force;
the preparation method comprises the following steps:
(1) preparation of sodium alginate spinning solution
Dissolving alginic acid in a mixed solution consisting of water, sodium chloride and sodium hydroxide, wherein the mass fraction of the sodium chloride is 0.01-0.1%, and the mass fraction of the sodium hydroxide is 1-8%, and then filtering and defoaming to prepare a sodium alginate spinning solution with the mass fraction of 4-30%;
(2) preparation of chitosan spinning solution
Dissolving chitosan in glacial acetic acid water solution with the mass fraction of 0.8-10%, filtering, and defoaming to prepare chitosan spinning solution with the mass fraction of 0.5-8%;
(3) preparation of chitosan and alginic acid double-component fiber
And (3) simultaneously conveying the sodium alginate spinning solution prepared in the step (1) and the chitosan spinning solution prepared in the step (2) to a spinning part by using a metering pump, and then spinning the bicomponent fiber by a dry-jet wet spinning process: solidifying and forming the spinning solution by using a solidifying solution, wherein the solidifying solution consists of water, linear or dendritic lower alcohol and ketone, the mass fraction of the lower alcohol is 0-50%, the mass fraction of the ketone is 0-20%, and then carrying out conventional process treatment of drafting, washing, drying and filament collection to obtain the chitosan and alginic acid bicomponent fiber; distance of spinning member from liquid surface of coagulating liquid: 3-25 cm; conveying speed of spinning solution: 50-1000 mL/min; spinning temperature: 30-70 ℃; temperature of the coagulation bath: 20-50 ℃; draft ratio: 1-5;
the spinning part in the step (3) mainly comprises a first distribution plate, a first spinneret plate, a second distribution plate and a second spinneret plate, wherein a plurality of first distribution holes are formed in the inner ring of the first distribution plate, and a plurality of spinning solution through holes are formed in the outer ring of the first distribution plate; the first spinneret plate is of a disc-shaped structure with high edge and low bottom, a plurality of first spinneret holes are formed in the bottom of the first spinneret plate and communicated with the first distribution holes, and the uppermost end of the edge of the first spinneret plate is fixedly connected with the inner ring of the first distribution plate; the second spinneret plate is of a basin-shaped structure with a high edge and a low bottom, a plurality of second spinneret holes are formed in the bottom of the basin-shaped structure, and the uppermost end of the edge of the basin-shaped structure is fixedly connected with the outer ring of the first distribution plate; the second distribution plate is fixedly arranged at the bottom of an inner cavity of the second spinneret plate and is arranged below the first spinneret plate, the second distribution plate is provided with a plurality of second distribution holes and a plurality of third spinneret holes, the second distribution holes are communicated with the second spinneret holes, the third spinneret holes are the same in number as the second spinneret holes and are communicated with the second spinneret holes in a one-to-one correspondence manner in position, the third spinneret holes are the same in size as the first spinneret holes and smaller than the second spinneret holes, and the third spinneret holes are hermetically connected with the first spinneret holes through spinneret tubes; and the outer side wall of the first spinneret plate and the inner side wall of the second spinneret plate form a spinning solution channel, and the spinning solution channel is respectively communicated with the spinning solution through hole and the second distribution hole.
2. The alginic acid and chitosan bicomponent fiber as claimed in claim 1, wherein the alginic acid in step (1) is one or more of pure alginic acid, alginate and its derivatives, and blend, composite and modified substance using alginic acid or alginate as matrix.
3. The alginic acid and chitosan bicomponent fiber of claim 2, wherein the alginate and the derivative thereof are selected from one or more of sodium alginate, potassium alginate, amine alginate or propylene glycol alginate; the blend, compound or modifier taking alginic acid or alginate as matrix is selected from one or more of chitosan and alginic acid, collagen and alginic acid, and silver and alginic acid.
4. The alginic acid and chitosan bicomponent fiber of claim 1, wherein the chitosan of step (2) comprises pure chitosan, chitosan blend, chitosan composite, water-soluble chitosan with chitosan as matrix or water-swelling chitosan.
5. The alginic acid and chitosan bicomponent fiber as claimed in claim 4, wherein the chitosan blend is a blend of chitosan and a spinnable polymer, and the spinnable polymer is one or more of polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone or sodium carboxymethylcellulose; the chitosan compound is selected from one or more than one of a compound of silver and chitosan, a compound of collagen and chitosan, a compound of alginate and chitosan, and a compound of folic acid and chitosan; the water-soluble or water-swelling chitosan with chitosan as matrix is one or more of carboxymethyl chitosan, hydroxypropyl chitosan, hydroxyethyl chitosan or carboxybutyl chitosan.
6. The alginic acid and chitosan bicomponent fiber of claim 1, wherein the lower alcohol of step (3) is a C1-C12 linear or dendritic alcohol, which is one or more of methanol, ethanol, propanol, isopropanol, butanol, sec-butanol, isobutanol and tert-butanol.
7. The alginic acid and chitosan bicomponent fiber of claim 1, wherein the ketone in step (3) is acetone or methyl ethyl ketone.
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| CN109972233A (en) * | 2019-02-19 | 2019-07-05 | 青岛大学 | The preparation method of the biodegradable alginic acid fibre with high-intensity and high-tenacity |
| CN109943979B (en) * | 2019-03-11 | 2021-06-29 | 浙江谷泓生物技术有限公司 | Natural-component nonwoven fabric base film substrate and preparation method thereof |
| WO2021006813A1 (en) * | 2019-07-09 | 2021-01-14 | Agency For Science, Technology And Research | An apparatus and a method of drawing a fibre |
| CN110804773B (en) * | 2019-10-22 | 2021-04-02 | 东华大学 | Anionic-cationic polyelectrolyte composite material and salt inhibition preparation process thereof |
| CN113244442B (en) * | 2021-06-01 | 2022-11-15 | 北京化工大学 | Application of polyamino cationic compound in preparation of surface procoagulant enhanced hemostatic material |
| CN114588307B (en) * | 2022-04-08 | 2022-12-23 | 山东万容生物科技有限公司 | Alginate dressing and preparation method thereof |
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