CN1687499A - Blended fiber of sodium alginate/water soluble chitin, preparation method and application thereof - Google Patents
Blended fiber of sodium alginate/water soluble chitin, preparation method and application thereof Download PDFInfo
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- 229920002101 Chitin Polymers 0.000 title claims abstract description 40
- 239000000835 fiber Substances 0.000 title claims abstract description 40
- 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 title claims abstract description 39
- 239000000661 sodium alginate Substances 0.000 title claims abstract description 39
- 235000010413 sodium alginate Nutrition 0.000 title claims abstract description 39
- 229940005550 sodium alginate Drugs 0.000 title claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 34
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 229920001661 Chitosan Polymers 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 238000009987 spinning Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000007711 solidification Methods 0.000 claims 3
- 230000008023 solidification Effects 0.000 claims 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 claims 2
- 238000010612 desalination reaction Methods 0.000 claims 2
- 238000001556 precipitation Methods 0.000 claims 2
- 238000004062 sedimentation Methods 0.000 claims 2
- 230000015271 coagulation Effects 0.000 abstract description 6
- 238000005345 coagulation Methods 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000001766 physiological effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- 239000002244 precipitate Substances 0.000 description 5
- 235000010443 alginic acid Nutrition 0.000 description 4
- 229920000615 alginic acid Polymers 0.000 description 4
- 230000029663 wound healing Effects 0.000 description 4
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 3
- 206010052428 Wound Diseases 0.000 description 3
- 208000027418 Wounds and injury Diseases 0.000 description 3
- 239000001110 calcium chloride Substances 0.000 description 3
- 229910001628 calcium chloride Inorganic materials 0.000 description 3
- 235000011148 calcium chloride Nutrition 0.000 description 3
- 238000007872 degassing Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 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 description 2
- 108010010803 Gelatin Proteins 0.000 description 2
- 229940072056 alginate Drugs 0.000 description 2
- 229960001126 alginic acid Drugs 0.000 description 2
- 239000000783 alginic acid Substances 0.000 description 2
- 150000004781 alginic acids Chemical class 0.000 description 2
- 239000008273 gelatin Substances 0.000 description 2
- 229920000159 gelatin Polymers 0.000 description 2
- 235000019322 gelatine Nutrition 0.000 description 2
- 235000011852 gelatine desserts Nutrition 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 206010048629 Wound secretion Diseases 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006196 deacetylation Effects 0.000 description 1
- 238000003381 deacetylation reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011240 wet gel Substances 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
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Abstract
本发明公开了一种海藻酸钠/水溶性甲壳素共混纤维及其制备方法和用途。这种海藻酸钠/水溶性甲壳素共混纤维采用如下方法制备：将制得的质量百分比为3～5％的海藻酸钠溶液与制得的质量百分比为3～5％的甲壳素溶液按水溶性甲壳素在产物(共混纤维)中所占的质量百分含量为10％～70％的比例充分混匀，经过滤、减压脱泡后，于室温在凝固液中以溶液纺丝法制备海藻酸钠/水溶性甲壳素共混纤维，纤维拉伸率为10～30％。该共混纤维具有较高的生理活性、优良的力学性能和吸水性能，又因其原料来源丰富，价格便宜，在医疗领域具有广泛的应用前景，尤其适合用于制造无纺布作伤口敷料用。The invention discloses a sodium alginate/water-soluble chitin blend fiber, a preparation method and application thereof. This sodium alginate/water-soluble chitin blended fiber is prepared by the following method: the prepared sodium alginate solution with a mass percentage of 3 to 5% and the prepared chitin solution with a mass percentage of 3 to 5% are The mass percentage of water-soluble chitin in the product (blend fiber) is 10% to 70% and mixed thoroughly, filtered, degassed under reduced pressure, and spun in a coagulation solution at room temperature Sodium alginate/water-soluble chitin blended fibers were prepared by the method, and the stretching rate of the fibers was 10-30%. The blended fiber has high physiological activity, excellent mechanical properties and water absorption properties, and because of its rich source of raw materials and low price, it has wide application prospects in the medical field, especially suitable for making non-woven fabrics for wound dressings .
Description
技术领域technical field
本发明涉及一种可用于制作无纺布的海藻酸钠/水溶性甲壳素共混纤维及其制备方法和用途，属高分子化学材料领域。The invention relates to a sodium alginate/water-soluble chitin blend fiber which can be used for making non-woven fabrics, a preparation method and application thereof, and belongs to the field of macromolecule chemical materials.
背景技术Background technique
海藻酸是由β-1，4-D-甘露糖醛酸和α-1，4-L-葡糖醛酸组成的杂多糖。以Ca2+溶液为凝固液，海藻酸钠可以通过湿态纺丝法制成纤维。纤维中的Ca2+可以与人体伤口分泌物中的Na+进行离子交换而在患口处形成湿态凝胶。由于具有可以形成湿态伤口愈合环境以及高度的人体可吸收性这两个优点，海藻酸敷料在今天已得到越来越广泛的应用。但海藻酸纤维的弹性、强度都不够理想，其经济成本也较高。壳聚糖可以促进伤口愈合，但壳聚糖的刚性结构使它们不溶于水，这就阻碍了与伤口的相互作用，而脱乙酰度50％左右的甲壳素可溶于水，故被称为水溶性甲壳素，由于它的水溶性而使它可以与伤口充分作用，研究表明它在促进伤口愈合方面更有效。Alginic acid is a heteropolysaccharide composed of β-1,4-D-mannuronic acid and α-1,4-L-glucuronic acid. Using Ca 2+ solution as coagulation solution, sodium alginate can be made into fiber by wet spinning method. The Ca 2+ in the fiber can ion-exchange with the Na + in the human wound secretion to form a wet gel at the affected mouth. Due to the two advantages of forming a moist wound healing environment and high body absorbability, alginic acid dressings have been more and more widely used today. However, the elasticity and strength of alginate fiber are not ideal, and its economic cost is also relatively high. Chitosan can promote wound healing, but the rigid structure of chitosan makes them insoluble in water, which hinders the interaction with the wound, while chitin with a deacetylation degree of about 50% is soluble in water, so it is called Water-soluble chitin, due to its water solubility allows it to fully interact with the wound, studies have shown that it is more effective in promoting wound healing.
发明内容Contents of the invention
本发明针对海藻酸纤维的弹性、强度都不够理想的缺点，通过共混改性这一提高高分子材料性能的简便有效的方法，将海藻酸钠与有促进伤口愈合功能的水溶性甲壳素共混，提供一种综合性能较为理想的海藻酸钠/水溶性甲壳素共混纤维，该共混纤维具有良好的生理活性、力学性能和吸水性能，而且本发明还提供了制备海藻酸钠/明胶共混纤维的方法，该方法简单可行、成本较低。The present invention aims at the shortcomings that the elasticity and strength of the alginate fiber are not ideal enough, and through blending and modification, which is a simple and effective method for improving the performance of polymer materials, sodium alginate is co-mixed with water-soluble chitin that has the function of promoting wound healing. It provides a kind of sodium alginate/water-soluble chitin blended fiber with ideal comprehensive performance. The blended fiber has good physiological activity, mechanical properties and water absorption performance, and the present invention also provides a method for preparing sodium alginate/gelatin The method of blending fibers is simple, feasible and low in cost.
本发明提供的技术方案是采用如下方法制备海藻酸钠/明胶共混纤维：The technical scheme provided by the invention is to adopt the following method to prepare sodium alginate/gelatin blended fiber:
(1)将适量海藻酸钠溶于水得到质量百分比为3～5％的海藻酸钠溶液。(1) Dissolving an appropriate amount of sodium alginate in water to obtain a sodium alginate solution with a mass percentage of 3-5%.
(2)将适量壳聚糖溶解于40-60％(体积百分比)甲醇、3-5％(体积百分比)乙酸混合水溶液中，加入与壳聚糖的质量比为0.37∶1-0.45∶1的乙酸酐，室温下搅拌反应3-6小时，加入足量丙酮产生沉淀，将沉淀过滤、除盐、干燥得水溶性甲壳素。(2) Dissolve an appropriate amount of chitosan in a mixed aqueous solution of 40-60% (volume percent) methanol and 3-5% (volume percent) acetic acid, and add chitosan with a mass ratio of 0.37:1-0.45:1 Acetic anhydride, stirring and reacting at room temperature for 3-6 hours, adding a sufficient amount of acetone to produce a precipitate, filtering the precipitate, removing salt, and drying to obtain water-soluble chitin.
(3)将水溶性甲壳素溶于水中得到质量百分比为3～5％的甲壳素溶液。(3) dissolving the water-soluble chitin in water to obtain a chitin solution with a mass percentage of 3-5%.
(4)将上述两种溶液按水溶性甲壳素在产物(共混纤维)中所占的质量百分含量为10％～70％的比例充分混匀，经过滤、减压脱泡后，于室温在足量凝固液中以溶液纺丝法制备海藻酸钠/水溶性甲壳素共混纤维，纤维拉伸率为10～30％。(4) The above two solutions are fully mixed according to the ratio of 10% to 70% of the mass percentage of water-soluble chitin in the product (blend fiber), filtered, and degassed under reduced pressure. Sodium alginate/water-soluble chitin blended fibers are prepared by solution spinning in sufficient coagulating liquid at room temperature, and the stretching ratio of the fibers is 10-30%.
其中所用凝固液为含有5％～10％(质量百分比)CaCl2的水溶液与30～50％(体积百分比)无水乙醇的混和液。制备海藻酸钠溶液、甲壳素溶液所用的水最好为蒸馏水。Wherein the coagulation liquid used is a mixed liquid containing 5%-10% (mass percentage) CaCl 2 aqueous solution and 30-50% (volume percentage) absolute ethanol. The water used for preparing sodium alginate solution and chitin solution is preferably distilled water.
由于海藻酸钠/水溶性甲壳素共混纤维不仅具有海藻酸钠纤维和水溶性甲壳素的优点，而且力学性能也很好，又因其原料来源丰富、价格便宜，所以在医疗领域具有广泛的应用前景，尤其适合用于制造无纺布作伤口敷料用。Because the sodium alginate/water-soluble chitin blend fiber not only has the advantages of sodium alginate fiber and water-soluble chitin, but also has good mechanical properties, and because of its rich source of raw materials and low price, it has a wide range of applications in the medical field. Application prospects, especially suitable for making non-woven fabrics for wound dressings.
具体实施方式Detailed ways
实施例1：取45g海藻酸钠溶于855ml蒸馏水得到5％(质量百分比)的海藻酸钠溶液；40g壳聚糖溶解于600ml40％(体积百分比)甲醇、3％(体积百分比)乙酸混合水溶液中，加入15g乙酸酐，室温下搅拌反应6小时，加入足量丙酮，沉淀被过滤、除盐、干燥得水溶性甲壳素。取5g水溶性甲壳素溶于蒸馏水中得到5％(质量百分比)的水溶性甲壳素溶液。将上述两种溶液充分混匀，过滤，减压脱泡后，于室温在组成为5％(质量百分比)CaCl2的水溶液与30％(体积百分比)无水乙醇的混和液的凝固液中通过溶液纺丝法制备海藻酸钠/水溶性甲壳索纤维，纤维拉伸率为30％。Embodiment 1: get 45g sodium alginate and be dissolved in 855ml distilled water and obtain the sodium alginate solution of 5% (mass percentage); 40g chitosan is dissolved in 600ml40% (volume percentage) methyl alcohol, 3% (volume percentage) in the mixed aqueous solution of acetic acid , add 15g of acetic anhydride, stir and react at room temperature for 6 hours, add enough acetone, the precipitate is filtered, desalinated, and dried to obtain water-soluble chitin. 5 g of water-soluble chitin was dissolved in distilled water to obtain a 5% (mass percent) water-soluble chitin solution. The above two solutions are fully mixed, filtered, and after degassing under reduced pressure, pass through the coagulation solution of the mixed solution of 5% (mass percentage) CaCl2 solution and 30% (volume percentage) absolute ethanol at room temperature Sodium alginate/water-soluble chitosan fibers were prepared by solution spinning, and the stretching rate of the fibers was 30%.
实施例2：取35g海藻酸钠溶于840ml蒸馏水得到4％(质量百分比)的海藻酸钠溶液；40g壳聚糖溶解于600ml50％(体积百分比)甲醇、4％(体积百分比)乙酸混合水溶液中，加入17g乙酸酐，室温下搅拌反应5小时，加入足量丙酮，沉淀被过滤、除盐、干燥得水溶性甲壳素。取15g水溶性甲壳素溶于蒸馏水中得到4％(质量百分比)的水溶性甲壳素溶液。将上述两种溶液充分混匀，过滤，减压脱泡后，于室温在组成为7％(质量百分比)CaCl2的水溶液与40％(体积百分比)无水乙醇的混和液的凝固液中通过溶液纺丝法制备海藻酸钠/水溶性甲壳索纤维，纤维拉伸率为20％。Embodiment 2: get 35g sodium alginate and be dissolved in 840ml distilled water and obtain 4% (mass percentage) sodium alginate solution; 40g chitosan is dissolved in 600ml50% (volume percentage) methanol, 4% (volume percentage) in the mixed aqueous solution of acetic acid , add 17g of acetic anhydride, stir and react at room temperature for 5 hours, add enough acetone, the precipitate is filtered, desalinated, and dried to obtain water-soluble chitin. 15 g of water-soluble chitin was dissolved in distilled water to obtain a 4% (mass percentage) water-soluble chitin solution. The above two solutions are fully mixed, filtered, and after degassing under reduced pressure, pass through the coagulation solution of the mixed solution of 7% (mass percentage) CaCl2 solution and 40% (volume percentage) absolute ethanol at room temperature Sodium alginate/water-soluble chitosan fibers were prepared by solution spinning, and the stretching ratio of the fibers was 20%.
实施例3：取25g海藻酸钠溶于808ml蒸馏水得到3％(质量百分比)的海藻酸钠溶液；40g壳聚糖溶解于600ml60％(体积百分比)甲醇、5％(体积百分比)乙酸混合水溶液中，加入18g乙酸酐，室温下搅拌反应3小时，加入足量丙酮，沉淀被过滤、除盐、干燥得水溶性甲壳素。取25g水溶性甲壳素溶于蒸馏水中得到3％(质量百分比)的水溶性甲壳素溶液。将上述两种溶液充分混匀，过滤，减压脱泡后，于室温在组成为10％(质量百分比)CaCl2的水溶液与50％(体积百分比)无水乙醇的混和液的凝固液中通过溶液纺丝法制备海藻酸钠/水溶性甲壳素纤维，纤维拉伸率为10％。Embodiment 3: get 25g sodium alginate and be dissolved in 808ml distilled water and obtain 3% (mass percentage) sodium alginate solution; 40g chitosan is dissolved in 600ml60% (volume percentage) methanol, 5% (volume percentage) in the mixed aqueous solution of acetic acid , add 18g of acetic anhydride, stir and react at room temperature for 3 hours, add a sufficient amount of acetone, the precipitate is filtered, desalinated, and dried to obtain water-soluble chitin. 25 g of water-soluble chitin was dissolved in distilled water to obtain a 3% (mass percent) water-soluble chitin solution. The above two solutions are fully mixed, filtered, and after degassing under reduced pressure, pass through the coagulation solution of the mixed solution of 10% (mass percentage) CaCl2 solution and 50% (volume percentage) absolute ethanol at room temperature Sodium alginate/water-soluble chitin fibers were prepared by solution spinning, and the stretching rate of the fibers was 10%.
因溶液纺丝法是制备纤维的常规方法，这里不再对其进行详细说明。Since the solution spinning method is a conventional method for preparing fibers, it will not be described in detail here.
将实施例1、2、3所得产物进行力学性能及吸水率测试，测试结果见下表。The products obtained in Examples 1, 2, and 3 were tested for mechanical properties and water absorption, and the test results are shown in the table below.
由表中数据可知，海藻酸钠/水溶性甲壳素共混纤维具有优异的力学性能和吸水性。It can be seen from the data in the table that the sodium alginate/water-soluble chitin blend fiber has excellent mechanical properties and water absorption.
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| WO2007093805A1 (en) * | 2006-02-16 | 2007-08-23 | The University Of Bolton Education Corporation | Composite fibre of alginate and chitosan |
| CN100457990C (en) * | 2007-04-16 | 2009-02-04 | 青岛大学 | Producing method and use for common and functional calcium alginate fiber |
| CN101049515B (en) * | 2007-05-15 | 2010-10-13 | 浙江理工大学 | Preparation method of chitin and silk fiber blended wet-laid non-woven medical dressing |
| CN102031590A (en) * | 2011-01-12 | 2011-04-27 | 武汉理工大学 | Novel method for preparing sodium alginate/hydroxypropyl chitosan antibacterial blended fiber |
| CN102552966A (en) * | 2012-01-31 | 2012-07-11 | 青岛明药堂医药科技开发有限公司 | Alginate antibacterial dressing and its preparation method |
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| CN103469365A (en) * | 2013-09-22 | 2013-12-25 | 山东颐诺生物科技有限公司 | Alginic acid-chitosan composite fiber for tranma repairing and preparation method thereof |
| CN104069536A (en) * | 2014-07-11 | 2014-10-01 | 江苏开源康达医疗器械有限公司 | Method for preparing sodium alginate-chitosan nano-grade medical dressing |
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| CN1080784C (en) * | 1996-12-29 | 2002-03-13 | 冯鸿城 | Active wound dressing, zinc-calcium alginate fiber nonwoven fabric and its preparing technology |
| CN1297957A (en) * | 1999-12-01 | 2001-06-06 | 武汉大学 | Preparation and use of intermingled film or fiber of carboxymethyl chitosan and alginic acid |
| CN1228371C (en) * | 2003-12-02 | 2005-11-23 | 武汉大学 | Preparation method and uses of carboxymethyl chitosan and sodium alginate blend microcapsule |
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