CN112679628B - Medical dressing based on alginate fibers and preparation method thereof - Google Patents
Medical dressing based on alginate fibers and preparation method thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 143
- 235000010443 alginic acid Nutrition 0.000 title claims abstract description 46
- 229920000615 alginic acid Polymers 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 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 abstract description 14
- 229940072056 alginate Drugs 0.000 title abstract description 14
- 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 claims abstract description 65
- JJMDCOVWQOJGCB-UHFFFAOYSA-N 5-aminopentanoic acid Chemical compound [NH3+]CCCCC([O-])=O JJMDCOVWQOJGCB-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000648 calcium alginate Substances 0.000 claims abstract description 36
- 235000010410 calcium alginate Nutrition 0.000 claims abstract description 36
- 229960002681 calcium alginate Drugs 0.000 claims abstract description 36
- 229960001126 alginic acid Drugs 0.000 claims abstract description 32
- 239000000783 alginic acid Substances 0.000 claims abstract description 32
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- 239000010410 layer Substances 0.000 claims abstract description 32
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- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 19
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 16
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- 239000000661 sodium alginate Substances 0.000 claims description 19
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- 239000000243 solution Substances 0.000 claims description 15
- BXRFQSNOROATLV-UHFFFAOYSA-N 4-nitrobenzaldehyde Chemical compound [O-][N+](=O)C1=CC=C(C=O)C=C1 BXRFQSNOROATLV-UHFFFAOYSA-N 0.000 claims description 14
- 238000009987 spinning Methods 0.000 claims description 14
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- 238000006243 chemical reaction Methods 0.000 claims description 13
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000001110 calcium chloride Substances 0.000 claims description 12
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- 238000001035 drying Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
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- 238000001914 filtration Methods 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 6
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- 238000005345 coagulation Methods 0.000 claims description 5
- 238000000643 oven drying Methods 0.000 claims description 4
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- 238000002715 modification method Methods 0.000 claims description 2
- 206010052428 Wound Diseases 0.000 abstract description 24
- 208000027418 Wounds and injury Diseases 0.000 abstract description 24
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- 239000002994 raw material Substances 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 description 38
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- 238000012360 testing method Methods 0.000 description 28
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- MCHZKGNHFPNZDP-UHFFFAOYSA-N 2-aminoethane-1,1,1-triol;hydrochloride Chemical compound Cl.NCC(O)(O)O MCHZKGNHFPNZDP-UHFFFAOYSA-N 0.000 description 6
- 230000035699 permeability Effects 0.000 description 6
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- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 3
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- 229910001424 calcium ion Inorganic materials 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
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- 238000002474 experimental method Methods 0.000 description 3
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
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- 238000012876 topography Methods 0.000 description 2
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- -1 5-aminovaleric acid modified sodium alginate Chemical class 0.000 description 1
- 241001474374 Blennius Species 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 208000032544 Cicatrix Diseases 0.000 description 1
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- 125000003368 amide group Chemical group 0.000 description 1
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Images
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- Materials For Medical Uses (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a medical dressing based on alginate fibers and a preparation method thereof, belonging to the technical field of medical dressings, the medical dressing comprises a surface layer, a middle layer and a wound contact layer, wherein the surface layer is polyester fiber non-woven fabric, the middle layer and the wound contact layer are both calcium alginate fibers and polyvinyl alcohol fiber mixed needle-punched non-woven fabric, and the calcium alginate fibers are prepared by taking modified alginic acid grafted with 5-aminopentanoic acid as a raw material and utilizing wet spinning. The medical dressing based on the alginate fibers and the preparation method thereof have the advantages of low preparation cost, convenience in rapid wound healing and good comfort.
Description
Technical Field
The invention belongs to the technical field of medical dressings, and particularly relates to a medical dressing based on alginate fibers and a preparation method thereof.
Background
Wound repair and regeneration is a complex dynamic process involving migration and proliferation of cells, deposition and reorganization of intercellular matrix, a process of tissue continuity and functional recovery. In the process, the occurrence of certain pathological physiological and metabolic diseases can change the normal wound repair process, so that the wound healing is delayed, and even chronic wounds which are difficult to heal are serious, thereby endangering the life safety of patients. Conventional medical dressings such as cotton gauze do not meet this wound treatment need. Modern medical theory development proves that the moist condition can shorten the healing period of the wound and reduce pain and scars.
The calcium alginate fiber is a natural high molecular functional fiber which is prepared by using sodium alginate extracted from brown algae as a basic raw material, performing wet spinning, washing, drafting, shaping and the like, has good moisture absorption and gelling performance, can absorb moisture and expand when contacting wound exudate, forms hydrogel to cover the surface of a wound, and promotes the healing of the wound. And it has good overall easy removability, high oxygen permeability, biocompatibility, biodegradability and absorbability, and is widely used as a novel medical dressing raw material at home and abroad. However, the alginate fiber has the defects of poor elasticity, low strength, high price and the like, and the application and the development of the alginate fiber are limited. The polyvinyl alcohol fiber has good biocompatibility, biodegradability and environmental friendliness, is low in price, good in hygroscopicity, similar to cotton in performance, has a shielding effect, and has wide application in medical absorbable materials and protective materials.
In the prior art, for example, a Chinese patent with an authorization publication number of CN 101381356B discloses a composite medical dressing applying calcium alginate fibers, which comprises a surface layer, a middle layer and a wound contact layer, and is characterized in that the surface layer is polyester fiber non-woven fabric, the middle layer and the wound contact layer are both calcium alginate fibers and polyvinyl alcohol fibers mixed needle-punched non-woven fabric, the content of the calcium alginate fibers in the middle layer is 40-70%, the content of the polyvinyl alcohol fibers is 30-60%, and the gram weight of the middle layer is 30-80g/m2The content of calcium alginate fiber of the wound contact layer is 80-99%, the content of polyvinyl alcohol fiber is 1-20%, and the gram weight of the wound contact layer is 30-50g/m2. The invention can reduce the dosage of calcium alginate fiber and reduce the production cost on the premise of ensuring the wound healing effect, and has the outstanding advantages of simple processing technique and avoiding using chemical adhesives.
Disclosure of Invention
The invention aims to provide a medical dressing based on alginate fibers and a preparation method thereof, wherein the medical dressing is low in preparation cost, convenient for rapid wound healing and good in comfort.
The technical scheme adopted by the invention for realizing the purpose is as follows:
providing modified alginic acid, wherein the preparation method of the modified alginic acid comprises the following steps: dissolving sodium alginate in water, adjusting pH to 3-4 with hydrochloric acid, adding 4-nitrobenzaldehyde while stirring, standing for 5-8min, adding 5-aminovaleric acid, placing in a constant temperature water bath kettle at 55-60 deg.C, reacting for 3-5h, adding anhydrous ethanol into the reaction system after reaction, purifying at 40-50 deg.C, stirring for 20-30min, vacuum filtering the suspension, repeatedly washing with anhydrous ethanol, and oven drying in a drying oven to obtain the final product. 4-nitrobenzaldehyde can catalyze amido of 5-aminopentanoic acid and carboxylic acid groups on the alginic acid polymer skeleton to form amido bond connection, and the grafting rate of 5-aminopentanoic acid on alginic acid is improved.
Preferably, the mass ratio of the sodium alginate to the 5-aminovaleric acid is 1: 2.5-2.9.
Preferably, the mass ratio of the 4-nitrobenzaldehyde to the sodium alginate is 1: 3.3-3.7.
The preparation method of the modified calcium alginate fiber comprises the following steps:
s1, chemically modifying alginic acid;
s2, spinning modified calcium alginate fibers;
the modification method of alginic acid in the step S1 includes: dissolving sodium alginate in water, adjusting pH to 3-4 with hydrochloric acid, adding 4-nitrobenzaldehyde while stirring, standing for 5-8min, adding 5-aminovaleric acid, placing in a constant temperature water bath kettle at 55-60 deg.C, reacting for 3-5h, adding anhydrous ethanol into the reaction system after reaction, purifying at 40-50 deg.C, stirring for 20-30min, vacuum filtering the suspension, repeatedly washing with anhydrous ethanol, and oven drying in a drying oven to obtain the final product. 4-nitrobenzaldehyde can catalyze amino of 5-aminopentanoic acid and carboxylic acid groups on an alginic acid polymer skeleton to form amido bond connection, the grafting rate of 5-aminopentanoic acid on alginic acid is improved, the number of entanglement points among molecular chains is increased by introduced molecular chains, the interaction force among the molecular chains is enhanced, the mechanical strength of fibers is improved, and meanwhile, the modified calcium alginate fibers can keep better liquid absorption property by introduced hydrophilic group carboxyl, so that the comfort of the dressing can be improved when the dressing is prepared.
Preferably, the mass ratio of the sodium alginate to the 5-aminovaleric acid is 1: 2.5-2.9.
Preferably, the mass ratio of the 4-nitrobenzaldehyde to the sodium alginate is 1: 3.3-3.7.
Preferably, the spinning method of the modified calcium alginate fiber comprises the following steps: preparing 2-3.5% modified alginic acid solution, filtering, defoaming in vacuum for 8-12h to obtain spinning stock solution, preparing modified calcium alginate fibers by wet spinning, extruding the spinning solution through a spinneret orifice, feeding the extruded spinning solution into a coagulating bath, drafting, washing, drying and winding to obtain a modified calcium alginate fiber sample;
the coagulating bath contains CaCl2And a mixed solution of tris hydrochloride;
CaCl in the coagulation bath2The concentration of (a) is 2.8-3.5% (m/m), the above-mentioned tris hydrochloride and CaCl2The mass ratio of (A) to (B) is 1: 7.3-8.0. When the wet spinning is utilized to prepare the calcium alginate fiber, the trihydroxymethyl aminomethane hydrochloride is added, the steric hindrance of modified alginic acid can be increased, the ion exchange between calcium ions and sodium ions is prevented, a certain gelation degree is reduced, the grooves on the surface of the fiber are obvious, and when the added trihydroxymethyl aminomethane hydrochloride is added in the trihydroxymethyl aminomethane hydrochloride: CaCl2When the (m/m) is within the range of 1:7.3-8.0, the moisture absorption capacity of the alginate fiber can be improved under the condition of ensuring the mechanical property, and when the alginate fiber is used for preparing medical dressings, the moisture absorption capacity of the dressings can be improved and the diffusivity and permeability of liquid can be reduced while the comfort is ensured.
Provides a modified calcium alginate fiber, which is prepared by the preparation method of the modified calcium alginate fiber.
Providing a composite medical dressing based on calcium alginate fibers, wherein the composite medical dressing comprises a surface layer, a middle layer and a wound contact layer;
the surface layer is polyester fiber non-woven fabric;
the middle layer and the wound contact layer are both calcium alginate fiber and polyvinyl alcohol fiber mixed needle-punched non-woven fabrics.
Preferably, the calcium alginate fiber is prepared by the preparation method of the modified calcium alginate fiber.
More preferably, the content (m/m) of the calcium alginate fiber in the middle layer is 30-40%, the content (m/m) of the polyvinyl alcohol fiber is 60-70%, and the surface density is 30-60g/m2；
The content (m/m) of calcium alginate fiber in the wound contact layer is 60-70%, the content (m/m) of polyvinyl alcohol fiber is 30-40%, and the areal density is 30-60g/m2. The modified calcium alginate fiber prepared by the preparation method of the modified calcium alginate fiber has the advantages that the mechanical strength is increased, meanwhile, the liquid absorption of the modified calcium alginate fiber is enhanced, the use of the calcium alginate fiber can be reduced, the damage during needling can be reduced when the composite medical dressing is prepared, the entanglement effect of a fiber web is improved, the comfort and the moisture absorption capacity of the dressing can be improved, and the diffusivity and the permeability of liquid are reduced.
The invention adopts 4-nitrobenzaldehyde to catalyze 5-amino pentanoic acid to modify alginic acid, thereby having the following beneficial effects: the grafting rate of 5-aminovaleric acid on alginic acid can be improved, the introduced molecular chain increases the number of intertwining points among molecular chains, the interaction force among the molecular chains can be enhanced, the mechanical strength of fibers is improved, and the introduced hydrophilic group carboxyl enables the modified calcium alginate fibers to keep better liquid absorption property, so that the comfort of the dressing can be improved when the dressing is prepared, and meanwhile, the dressing has better hygroscopicity and can better prevent liquid diffusion and permeation.
The invention adopts the method that when the wet spinning is used for preparing the calcium alginate fiber, the trihydroxymethyl aminomethane hydrochloride (the trihydroxymethyl aminomethane hydrochloride: CaCl) with a certain proportion is added2(m/m) ═ 1:7.3 to 8.0), and thus has the following advantageous effects: can increase the steric hindrance of the modified alginic acid and block calcium ions from reacting withThe sodium ions are subjected to ion exchange, a certain gelatinization degree is reduced, grooves on the surfaces of the fibers are obvious, the moisture absorption capacity of the alginate fibers can be improved under the condition of ensuring the mechanical property, and when the alginate fiber is used for preparing medical dressings, the moisture absorption capacity of the dressings can be improved while the comfort is ensured, and the diffusivity and the permeability of liquid are reduced.
Therefore, the medical dressing based on the alginate fibers and the preparation method thereof have the advantages of low preparation cost, convenience in rapid wound healing and better comfort.
Drawings
FIG. 1 is a graph showing an infrared spectrum in test example 1 of the present invention;
FIG. 2 is a graph showing the results of the measurement of the graft ratio in test example 1 of the present invention;
FIG. 3 is a surface topography of a fiber in test example 1 of the present invention;
FIG. 4 shows the results of testing the breaking strength, breaking elongation and initial modulus of the fiber in test example 1 of the present invention;
FIG. 5 shows the results of testing the water absorption of the fibers in test example 1 of the present invention;
FIG. 6 is a test result of the liquid absorptivity of the dressing in test example 2 of the present invention;
FIG. 7 is a graph showing the results of the test of the liquid absorption amount and the soaking time of the dressing in test example 2 of the present invention;
fig. 8 shows the results of the measurements of extensibility and permanent set of the dressing according to test example 2 of the present invention.
Detailed Description
The present invention is further described in detail with reference to the following examples:
example 1:
1. a preparation method of modified calcium alginate fibers comprises the following steps:
s1, chemical modification of alginic acid: dissolving 3g of sodium alginate in 200mL of water, adjusting the pH value to 3 by using 0.1mol/L hydrochloric acid, adding 0.85g of 4-nitrobenzaldehyde while stirring, standing for 6min, adding 8g of 5-aminovaleric acid while stirring, placing in a constant-temperature water bath kettle at 55 ℃, stirring for reacting for 4h, adding 200mL of absolute ethyl alcohol into a reaction system after the reaction is finished, purifying at 45 ℃, stirring for 20min, carrying out suction filtration on the suspension, repeatedly washing by using absolute ethyl alcohol, and drying in a drying oven to obtain the modified alginic acid.
S2, spinning of modified calcium alginate fibers: preparing 2.5% modified alginic acid solution, filtering, defoaming in vacuum for 10h to obtain spinning stock solution, preparing modified calcium alginate fiber by wet spinning, extruding the spinning solution through a spinneret orifice, entering a coagulating bath, drafting, washing, drying, and winding to obtain a modified calcium alginate fiber sample. The coagulation bath contained 3.2% (m/m) of CaCl2The solution was cooled in a coagulation bath at 40 ℃ and a draw ratio of 1.5.
2. A composite medical dressing based on calcium alginate fibers, comprising a surface layer, an intermediate layer and a wound contact layer, wherein:
raw materials: polyester nonwoven fabric available from Jinjiang Henlida nonwoven fabrics Co., Ltd, having an areal density of 50g/m2The prepared seaweed calcium fiber has the length of 41mm, the polyvinyl alcohol fiber is water-soluble fiber, the dissolving temperature in water is 90 ℃, and the length is about 36 mm.
The surface layer is polyester non-woven fabric;
the middle layer is 30/70(m/m) calcium alginate fiber/polyvinyl alcohol fiber composite non-woven fabric;
the wound contact layer is 70/30(m/m) calcium alginate fiber/polyvinyl alcohol fiber composite non-woven fabric.
The preparation route is as follows: fiber mix open → carding → needling. When the fibers are mixed and opened, the calcium alginate fibers and the polyvinyl alcohol fibers in different proportions are firstly subjected to preliminary manual opening and mixing, and then the opening and the opening are carried out twice by adopting a wool blending machine so as to uniformly mix the calcium alginate fibers and the polyvinyl alcohol fibers; then carding by a carding machine, after the web is carded, needling the calcium alginate fiber and the polyvinyl alcohol fiber web by a pre-needling machine, wherein the parameters of the carding machine during carding are as follows: the feeding speed is 0.51r/min, the rotating speed of the licker-in roll is 520.83r/min, the rotating speed of the cylinder is 500r/min, the rotating speed of the doffer is 8.33r/min, the net outlet speed is 4.4m/min, and the needling parameters of the needling machine are as follows: the density of the implanted needle is 2000 pieces/m, and the rotating speed is 200 r/min. Preparing middle layer calcium alginate fiberThe ratio of calcium alginate fiber to polyvinyl alcohol fiber is 30/70(m/m) when polyvinyl alcohol fiber non-woven fabric is used, and the surface density is 60g/m2(ii) a When the wound contact layer calcium alginate fiber/polyvinyl alcohol fiber non-woven fabric is prepared, the ratio of the calcium alginate fiber to the polyvinyl alcohol fiber is 70/30(m/m), and the surface density is 40g/m2. After the non-woven fabrics of the intermediate layer and the wound contact layer are processed, the non-woven fabrics of the wound contact layer, the intermediate layer and the surface layer are superposed in sequence, and then are bonded together by an ultrasonic lace sewing machine, the parameters of the ultrasonic adhesive are set to be the rotating speed of a compression roller of 2.5r/s, the output power of 3.2w and the pressure of the compression roller of 15MPa, and the finished dressing is obtained.
Example 2:
in the modification process of alginic acid, 4-nitrobenzaldehyde was not used, and the rest was completely the same as in example 1.
Example 3:
in the modification of alginic acid, 5-aminopentanoic acid was not used, and the remainder was identical to that of example 1.
Example 4:
alginic acid was not modified, and the rest was completely the same as in example 1.
Example 5:
when the modified calcium alginate fiber is spun, the coagulating bath contains 3.2 percent (m/m) of CaCl2And 0.42% (m/m) of tris hydrochloride, the remainder being identical to example 1.
Example 6:
when the modified calcium alginate fiber is spun, the coagulating bath contains 3.2 percent (m/m) of CaCl2And 0.42% (m/m) of tris hydrochloride, and the remainder was completely the same as in example 4.
Example 7:
when the modified calcium alginate fiber is spun, the coagulating bath contains 3.2 percent (m/m) of CaCl2And 0.39% (m/m) of tris hydrochloride, the remainder being identical to example 1.
Example 8:
modified calcium alginateWhen spinning the fiber, the coagulation bath contained 3.2% (m/m) of CaCl2And 0.44% (m/m) of tris hydrochloride, the remainder being identical to example 1.
Test example 1:
1.1 determination of infrared spectrum: the molecular structures of the modified alginic acid prepared in example 1 and the unmodified alginic acid prepared in example 4 were characterized by a fourier infrared spectrometer, and the infrared spectrum was measured by a potassium bromide tabletting method. The infrared spectrum is shown in FIG. 1.
1.2 determination of the graft ratio: weighing the mass to be 3g (i.e. m)1) Dissolving sodium alginate in 200mL of water, adjusting pH to 3 with 0.1mol/L hydrochloric acid, standing for 6min, placing in a 55 ℃ constant temperature water bath kettle, stirring for reaction for 4h, adding 200mL of absolute ethanol into a reaction system after the reaction is finished, purifying at 45 ℃, stirring for 20min, carrying out suction filtration on the suspension, repeatedly washing with absolute ethanol, drying in a drying oven, and weighing m3. The graft ratio (G) is calculated by the following formula:
(G) { [ (m) graft ratio2-m1)-(m3-m1)]/m1}×100％
In the formula, m1The mass (g), m, of sodium alginate before modification in the above examples2The mass (g) of the modified sodium alginate in the above examples. The results of the graft ratio measurement are shown in FIG. 2.
As can be seen from FIG. 1, 3433cm of alginic acid of example 4-1Corresponding to stretching vibration of the O-H group, 1773cm-1Corresponding to the stretching vibration of carboxylic acid C ═ O, the modified alginic acid of example 1 was found to be 1713cm-1、1634cm-1、1527cm-1The obvious absorption peaks at the positions respectively correspond to the stretching vibration of C ═ O, the in-plane deformation vibration of N-H and the stretching vibration of C-N bonds of amido bonds, and the result proves that the 5-aminovaleric acid is successfully grafted on the alginic acid in a mode of forming the amido bonds with the alginic acid.
As can be seen from FIG. 2, the grafting rate of 5-aminopentanoic acid in examples 1, 5, 7 and 8 is significantly higher than that in examples 2, 3, 4 and 6, which shows that 4-nitrobenzaldehyde can catalyze amide bond connection between amino of 5-aminopentanoic acid and carboxylic acid groups on a sodium alginate polymer skeleton, and the grafting rate of 5-aminopentanoic acid on sodium alginate is improved.
1.3 surface morphology observation: the modified calcium alginate fiber prepared by wet spinning in the above embodiment is pasted on a conductive adhesive on a copper platform, and after gold spraying coating treatment (10mA 30s), the surface morphology of the fiber is observed by adopting a JSM-5610LV scanning electron microscope of JEOL company of Japan, and the voltage is 10 kV. The surface topography of the fibers is shown in FIG. 3.
As can be seen from fig. 3, the grooves on the surface of the fiber prepared in example 1 are not obvious, smooth and uniform in appearance, and the grooves on the surface of the fiber prepared in example 5 are obvious and uniform in appearance. This shows that when the wet spinning is used to prepare calcium alginate fibers, the trihydroxymethyl aminomethane hydrochloride is added to increase the steric hindrance of the modified alginic acid, prevent the ion exchange between calcium ions and sodium ions, and reduce a certain degree of gelation, so that the grooves on the fiber surface are significant.
1.4 mechanical property test: the breaking strength was measured by a single fiber strength tester manufactured by electronics of Laizhou, Inc. and having a model number of LLY-06E. The test conditions were 20 ℃ temperature, 65% humidity, 20mm/min stretching speed, 10mm nip distance, and 0.05cN pre-tension. The results of the tests for breaking strength, breaking elongation and initial modulus of the fibers are shown in FIG. 4.
1.5 liquid absorption Performance test: according to standard "contact wound dressing test method: section 1 liquid absorbency (YY/T0471.1-2004) 3.2 preparation of test A solution (composition simulating wound exudate from human, 8.3g NaCl and 0.277g anhydrous CaCl)2Diluted to 1L) for testing.
Weighing W0The calcium alginate fibers prepared in the examples are respectively soaked in 20mL of A solution for 180min, the fibers are clamped by forceps, the alginate fibers are dehydrated for 10min at the rotating speed of 1000r/min, and the weight is recorded as W1The water absorption of the fiber is calculated by the following formula:
water absorption (g/g) ((W))1-W0)/W0
The results of the fiber water absorption are shown in FIG. 5.
As can be seen from fig. 4 and 5, the breaking strength, breaking elongation and initial modulus of the fiber prepared in example 1 are significantly higher than those of the fibers prepared in examples 2, 3 and 4, and the breaking strength, breaking elongation and initial modulus of the fiber prepared in example 5 are significantly higher than those of the fiber prepared in example 6; compared with the fibers prepared in the examples 2, 3 and 4, the fibers prepared in the example 1 have no obvious difference in water absorption, and compared with the fibers prepared in the example 6, the fibers prepared in the example 5 have no obvious difference in water absorption, which shows that 5-aminovaleric acid is grafted on sodium alginate by amido bonds, the number of entanglement points among molecular chains is increased by the introduced molecular chains, the interaction force among the molecular chains can be enhanced, the mechanical strength of the fibers is improved, and simultaneously, the modified calcium alginate fibers can keep good liquid absorption performance by the introduced hydrophilic group carboxyl.
As can be seen from fig. 4 and 5, the breaking strength, breaking elongation and initial modulus of the fiber prepared in example 8 are significantly lower than those of example 1, the breaking strength, breaking elongation and initial modulus of the fiber prepared in example 5 and example 7 are not significantly different from those of example 1, and the breaking strength, breaking elongation and initial modulus of the fiber prepared in example 6 are not significantly different from those of example 4; the water absorption of the fibers prepared in examples 5 and 8 is significantly higher than that of the fibers prepared in example 1, the water absorption of the fibers prepared in example 7 is not significantly different from that of the fibers prepared in example 1, and the water absorption of the fibers prepared in example 6 is significantly higher than that of the fibers prepared in example 4, which shows that when the calcium alginate fibers are prepared by wet spinning, when the amount of the added tris hydrochloride is in the range of tris hydrochloride: CaCl2When the (m/m) is within the range of 1:7.3-8.0, the moisture absorption capacity of the calcium alginate fiber can be improved under the condition of ensuring the mechanical property.
Test example 2:
2.1 testing of the liquid hygroscopicity of the dressing: weighing a sample of 5cm multiplied by 5cm, putting the sample into a culture dish after weighing the sample, adding a preheated solution A at the temperature of 37 ℃, wherein the adding amount is 40 times of the weight of the sample, then moving the sample into a drying oven, and keeping the sample at the temperature of 37 ℃ for 30 min; then clamping one corner or one end of the sample, weighing the sample after the sample is suspended for 30s, repeating the steps for other samples, and calculating a test result according to the following formula:
B＝[(M2-M1)/M1]×100％
b is liquid absorption,%; m1Mass of the sample before absorption of the liquid, g; m2The mass of the sample after absorption of the liquid, g. The results of the dressing liquid uptake rate test are shown in figure 6.
2.2 testing of liquid diffusion and permeability: a sample of 5cm by 5cm was taken and tested according to standard YY/T0471.1-2004, method for contact wound dressing test: part 1: in liquid absorbency ", a solution a for experiments was prepared, and a small amount of ink was added thereto and sufficiently stirred to dissolve, so that a small amount of red pen ink was easily observed for experiments and sufficiently stirred to dissolve. The solution A is slowly dropped onto the sample during the test, and the amount of liquid required for the liquid to penetrate the sample and the shortest time for the liquid to penetrate the sample are taken as performance indexes of the sample for preventing the liquid from diffusing and permeating. The results of the dressing liquid uptake and soak times are shown in figure 7.
2.3 testing of comfort: the extensibility and permanent set of the dressing was used to assess the comfort of the dressing. The test adopts the standard YY/T0471.4 Experimental method for contact wound dressing, fourth part: comfort, test temperature 21 ℃ and relative humidity 65%. The specific test method comprises the following steps: cutting 3 samples with length of 150mm and width of 25mm, bonding two ends of the sample with ultrasonic lace sewing machine, making two parallel marks at positions 25mm away from two ends of the sample, clamping the sample except the marks in two stretching chucks of instron3369, stretching the sample at a stretching speed of 300mm/min for 20mm, recording Maximum Load (ML), holding the sample at the position for 60s, taking off the sample, relaxing for 300s, and measuring distance between the two marks (L)2). The extensibility (E) and Permanent Set (PS) of the sample can be calculated according to the Maximum Load (ML) and the length after stretching of the measured sample, and the calculation formula is as follows:
E＝ML/2.5；
PS＝[(L2-100)/100]×100％。
the results of the measurements of the extensibility and permanent deformation of the dressing are shown in figure 8.
As can be seen from fig. 6, fig. 7 and fig. 8, the extensibility of the dressing prepared in example 1 is significantly greater than that of examples 2, 3 and 4, the permanent deformation is significantly lower than that of examples 2, 3 and 4, the liquid absorption rate, the liquid absorption amount and the soaking time of the dressing prepared in example 1 are not significantly different from those of examples 2, 3 and 4, the extensibility of the dressing prepared in example 5 is significantly greater than that of example 6, the permanent deformation is significantly lower than that of example 6, and the liquid absorption rate, the liquid absorption amount and the soaking time of the dressing prepared in example 5 are not significantly different from those of example 6, which shows that, when the calcium alginate fiber prepared from the 5-aminovaleric acid modified sodium alginate is used for preparing the dressing, the comfort of the dressing can be improved, and meanwhile, the calcium alginate fiber has better hygroscopicity and can better prevent liquid from diffusing and soaking.
As can be seen from fig. 6, fig. 7 and fig. 8, the liquid absorption rate, the liquid absorption amount and the soaking time of the dressings prepared in examples 5 and 8 are significantly greater than those of example 1, the liquid absorption rate, the liquid absorption amount, the soaking time, the extensibility and the permanent deformation of the dressing prepared in example 7 are not significantly different from those of example 1, the extensibility and the permanent deformation of example 5 are not significantly different from those of example 1, and the extensibility and the permanent deformation of the dressing prepared in example 8 are significantly lower than those of example 1 and significantly higher than those of example 1; the dressing prepared in example 6 has a significantly higher liquid absorption rate, liquid absorption amount, and soaking time than those of example 4, and the extensibility and permanent set are not significantly different from those of example 4. This shows that when calcium alginate fibers are prepared by wet spinning, the amount of tris hydrochloride added is in the range of tris hydrochloride: CaCl2When the (m/m) is within the range of 1:7.3-8.0, the moisture absorption capacity of the calcium alginate fiber can be improved under the condition of ensuring the mechanical property, and when the calcium alginate fiber is used for preparing medical dressings, the moisture absorption capacity of the dressings can be improved while the comfort is ensured, and the diffusivity and the permeability of liquid are reduced.
Conventional techniques in the above embodiments are known to those skilled in the art, and therefore, will not be described in detail herein.
The above embodiments are merely illustrative, and not restrictive, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention, and the protection scope of the present invention should be defined by the claims.
Claims (5)
1. A modified alginic acid is characterized in that: the preparation method of the modified alginic acid comprises the following steps: dissolving sodium alginate in water, adjusting pH to 3-4 with hydrochloric acid, adding 4-nitrobenzaldehyde while stirring, standing for 5-8min, adding 5-aminovaleric acid, placing in a constant temperature water bath kettle at 55-60 deg.C, reacting for 3-5h, adding anhydrous ethanol into the reaction system after reaction is finished, purifying at 40-50 deg.C, stirring for 20-30min, vacuum filtering the suspension, repeatedly washing with anhydrous ethanol, and oven drying in a drying oven to obtain the product;
the mass ratio of the sodium alginate to the 5-aminovaleric acid is 1: 2.5-2.9;
the mass ratio of the 4-nitrobenzaldehyde to the sodium alginate is 1: 3.3-3.7.
2. The preparation method of the modified calcium alginate fiber is characterized by comprising the following steps:
s1, chemically modifying alginic acid;
s2, spinning modified calcium alginate fibers;
the modification method of alginic acid in the step S1 comprises: dissolving sodium alginate in water, adjusting pH to 3-4 with hydrochloric acid, adding 4-nitrobenzaldehyde while stirring, standing for 5-8min, adding 5-aminovaleric acid, placing in a constant temperature water bath kettle at 55-60 deg.C, reacting for 3-5h, adding anhydrous ethanol into the reaction system after reaction is finished, purifying at 40-50 deg.C, stirring for 20-30min, vacuum filtering the suspension, repeatedly washing with anhydrous ethanol, and oven drying in a drying oven to obtain the product;
the mass ratio of the sodium alginate to the 5-aminovaleric acid is 1: 2.5-2.9;
the mass ratio of the 4-nitrobenzaldehyde to the sodium alginate is 1: 3.3-3.7.
3. The method of claim 2, wherein: the spinning method of the modified calcium alginate fiber comprises the following steps: preparing 2-3.5% modified alginic acid solution, filtering, defoaming in vacuum for 8-12h to obtain spinning stock solution, preparing modified calcium alginate fibers by wet spinning, extruding the spinning solution through a spinneret orifice, feeding the extruded spinning solution into a coagulating bath, drafting, washing, drying and winding to obtain a modified calcium alginate fiber sample;
the coagulating bath contains CaCl2And tris hydrochloride;
CaCl in the coagulation bath2Is 2.8-3.5% (m/m), said tris hydrochloride salt is reacted with CaCl2The mass ratio of (A) to (B) is 1: 7.3-8.0.
4. A modified calcium alginate fiber is characterized in that: the preparation method of claim 2 or 3.
5. A composite medical dressing based on calcium alginate fibers is characterized in that: the composite medical dressing comprises a surface layer, a middle layer and a wound contact layer;
the surface layer is polyester fiber non-woven fabric;
the middle layer and the wound contact layer are both the modified calcium alginate fiber and polyvinyl alcohol fiber mixed needle-punched non-woven fabric of claim 4.
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