CN102389584B - Preparation method of konjac sponge medical dressing - Google Patents
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Abstract
本发明公开了一种魔芋海绵医用敷料及其制备方法,属于医药技术领域。本发明的制备方法采用葡甘聚糖含量为50%~90%,分子量为100000~500000的魔芋精粉为原料,经魔芋水溶液的制备,魔芋海绵的成形,魔芋海绵的固化处理,魔芋海绵的切割、包装与灭菌处理得到吸液量为100~300g/g,透气率为80%~90%的魔芋海绵医用敷料。该魔芋海绵医用敷料表面平整无裂痕,而且具有优异的柔韧性、弹性、透气性、阻隔性、耐磨性、吸水性、生物相容性和可降解性和易去除性,可用于治疗手术伤口、烧烫伤创面等各种类型的皮肤创伤,防止细菌感染,促进组织修复,加速伤口愈合。The invention discloses a konjac sponge medical dressing and a preparation method thereof, belonging to the technical field of medicine. The preparation method of the present invention uses konjac fine powder with a glucomannan content of 50% to 90% and a molecular weight of 100,000 to 500,000 as a raw material, through the preparation of konjac aqueous solution, the forming of konjac sponge, the curing treatment of konjac sponge, and the preparation of konjac sponge. The konjac sponge medical dressing with a liquid absorption capacity of 100-300 g/g and an air permeability of 80%-90% is obtained through cutting, packing and sterilizing. The konjac sponge medical dressing has a smooth surface without cracks, and has excellent flexibility, elasticity, air permeability, barrier properties, abrasion resistance, water absorption, biocompatibility, degradability and easy removal, and can be used to treat surgical wounds Various types of skin wounds, such as burns and scalds, prevent bacterial infection, promote tissue repair, and accelerate wound healing.
Description
技术领域 technical field
本发明涉及一种魔芋海绵医用敷料及其制备方法,属于医药技术领域。 The invention relates to a konjac sponge medical dressing and a preparation method thereof, belonging to the technical field of medicine. the
背景技术 Background technique
皮肤具有抵抗体外病原细菌的入侵,排泄人体废物,防止人体水分蒸发散失,调节人体温度,感受压力、寒冷、温度的刺激等重要的功能。在因创伤、擦伤、烧伤以及溃烂等导致皮肤受损时,很容易感染细菌,或发生液体流失并引起各种并发症,因此治疗时需要使用医用敷料来保护创面和促进创面修复愈合。传统的医用敷料(纱布)仅起覆盖创面的作用,随着社会的发展和科技的进步,特别是现代医学、生物学和高分子材料科学的迅速发展,现代敷料的概念已经发生了根本的变化。现代医用敷料应当具备:(1)优异的覆盖性,能够阻止细菌入侵和限制细菌在伤口上的繁殖;(2)良好的吸湿性能和阻塞性能,能够吸收伤口渗出液,同时阻碍渗出液对健康组织的浸渍;(3)良好的弹性、柔韧性、透气性和止血功能;(4)生物相容性好,长期使用不会引起伤口部位皮肤敏感或过敏反应等不良症状;(5)提供潮湿的愈合环境,加速伤口的愈合;(6)在创面上稳定,易去除,应用与贮存方便;(7)生物可降解,其废弃物不会造成环境污染。采用天然高分子材料加工而成的海绵材料,具有优异的生物相容性和可降解性,而且海绵材料因具有特殊的多孔结构而有很强的吸水能力,当与潮湿的伤口接触时,脓血等伤口渗出液被毛细孔吸收入海绵之中,并由接触面向海绵的内部和后背面转移,从而起到了把脓血从伤口表面去除的作用。同时,吸附在海绵材料中的渗出液不易挥发,提供创面愈合需要的潮湿环境,加速创面肉芽组织的生长,因此非常适合用于制作医用敷料。 The skin has important functions such as resisting the invasion of pathogenic bacteria outside the body, excreting human waste, preventing the evaporation of water in the human body, regulating the temperature of the human body, and feeling the stimulation of pressure, cold and temperature. When the skin is damaged due to trauma, abrasions, burns, and ulcers, it is easy to be infected with bacteria, or fluid loss occurs and cause various complications. Therefore, medical dressings are required to protect the wound and promote wound healing during treatment. The traditional medical dressing (gauze) only plays the role of covering the wound surface. With the development of society and the advancement of science and technology, especially the rapid development of modern medicine, biology and polymer material science, the concept of modern dressing has undergone fundamental changes. . Modern medical dressings should have: (1) excellent coverage, which can prevent bacterial invasion and limit the reproduction of bacteria on the wound; (2) good hygroscopicity and blocking performance, can absorb wound exudate, and at the same time block the exudate Impregnation of healthy tissue; (3) Good elasticity, flexibility, air permeability and hemostatic function; (4) Good biocompatibility, long-term use will not cause adverse symptoms such as skin sensitivity or allergic reactions at the wound site; (5) Provide a moist healing environment to accelerate wound healing; (6) stable on the wound surface, easy to remove, convenient for application and storage; (7) biodegradable, and its waste will not cause environmental pollution. The sponge material processed from natural polymer materials has excellent biocompatibility and degradability, and the sponge material has a strong water absorption capacity due to its special porous structure. When in contact with a moist wound, pus Wound exudates such as blood are absorbed into the sponge by the capillary pores, and are transferred from the contact surface to the inside and back of the sponge, thereby removing pus and blood from the wound surface. At the same time, the exudate adsorbed in the sponge material is not easy to volatilize, provides a moist environment required for wound healing, and accelerates the growth of wound granulation tissue, so it is very suitable for making medical dressings. the
魔芋是南天星科魔芋属多年生草本植物,其中含有40%~60%葡甘聚糖(KGM),是迄今发现的自然界惟一可大量获得葡甘聚糖的植物。魔芋葡甘聚糖结构独特,由葡萄糖、甘露糖按1∶1.6的比例,主链通过1-4糖苷键相连,短支链以1-3糖苷键连接的相对分子量分布较窄的杂多糖。魔芋甘聚糖具有高粘性、高膨胀和高弹性和很好的发泡能力,而且生物相容性和可降解性优异,可用于制备海绵材料。中国专利公开号为CN 1184180 A,公开日为1998年6月10日,发明名称为魔芋泡棉的制作工艺,该申请案将魔芋精粉加入沸水中,膨胀后加入碱液得到混合料,然后注模、气蒸、冷冻、除碱、杀酶、脱色、护色、自然干燥、包装而得海绵状魔芋产品。中国专利公开号为CN 1197676 A,公开日为1998年11月4日,发明名称为用魔芋制成的 卫生敷料及其制法,该申请案将葡萄甘露聚糖的热水溶液用碱液调节pH值为8~12,然后剧烈搅拌形成大量泡沫,低温冷冻和高温烘干而得到海绵状魔芋产品。中国专利公开号为CN1249313 A,公开日为2000年4月5日,发明名称为魔芋美容保湿护肤海绵的制造方法,该申请案将魔芋精粉加入沸水中形成粘稠液体,加碱后注模并高温汽蒸得到胶质初坯,然后经冷冻、去碱、脱色、护色、保湿后装入包装袋,抽真空充氮气,密封后高温灭菌即得成品。中国专利公开号为CN 1583838 A,公开日为2005年2月3日,发明名称为一种大孔魔芋凝胶的制备方法,该申请案公开了以魔芋精粉为原料,无机碱为絮凝剂,通过高温反应形成凝胶,然后通过低温冷冻、室温融化、反复冻融,冻干得到大孔魔芋凝胶。中国专利公开号为CN 101011163A,公开日为2007年8月8日,发明名称为用魔芋、粮食制成的絮绒毛状可食性保健按摩毛巾,该申请案将魔芋粉加水糊化后与粮食粉混合,并加入发酵剂发酵和凝固剂凝固,然后将部分物料粉碎成末状,经混合、注模、熟化、冷冻、解冻、脱水、最终烘干而成。中国专利公开号为CN 101147658 A,公开日为2008年3月26日,发明名称为具有护肤功能的魔芋毛巾,该申请案将魔芋粉加水糊化后与粮食粉混合,并加入发酵剂发酵和凝固剂凝固,然后注模、熟化、冷冻、解冻、脱水、浸泡护肤植物浆液、真空干燥而成。中国专利公开号为CN 101423613 A,公开日为2009年5月6日,发明名称为葡甘露聚糖海绵环境友好制备方法,该申请案公开了以氢氧化钙为絮凝剂,生产工艺中不产生碱性无水和脱色污水的沐浴用葡甘露聚糖海绵的环境友好制备方法。中国专利公开号为CN 102178484 A,公开日为2011年9月14日,发明名称为具有洗浴和按摩功能的魔芋面巾及其制备方法,该申请案公开了将魔芋膳食纤维粉加水糊化后再添加絮凝剂制备混合料,然后注模、蒸煮、低温反复冷冻和解冻脱水、漂白、脱硫、杀菌和冷冻干燥制备魔芋海绵面巾的方法。 Konjac is a perennial herbaceous plant of Asteraceae Konjac, which contains 40% to 60% glucomannan (KGM), and is the only plant found so far that can obtain a large amount of glucomannan in nature. Konjac glucomannan has a unique structure. It consists of glucose and mannose in a ratio of 1:1.6. The main chain is connected by 1-4 glycosidic bonds, and the short branches are connected by 1-3 glycosidic bonds. It is a heteropolysaccharide with narrow relative molecular weight distribution. Konjac mannan has high viscosity, high expansion, high elasticity and good foaming ability, and has excellent biocompatibility and degradability, and can be used to prepare sponge materials. The Chinese patent publication number is CN 1184180 A, and the disclosure date is June 10, 1998. The invention name is the production process of konjac foam. In this application, konjac fine powder is added to boiling water, and after expansion, lye is added to obtain the mixture, and then Spongy konjac products are obtained by injection molding, steaming, freezing, alkali removal, enzyme killing, decolorization, color protection, natural drying, and packaging. The Chinese patent publication number is CN 1197676 A, and the publication date is November 4, 1998. The title of the invention is a sanitary dressing made of konjac and its preparation method. The application adjusts the pH of the hot water solution of glucomannan with lye The value is 8 to 12, then vigorously stirred to form a large amount of foam, frozen at low temperature and dried at high temperature to obtain a spongy konjac product. The Chinese patent publication number is CN1249313 A, and the disclosure date is April 5, 2000. The invention name is the manufacturing method of konjac beauty moisturizing skin care sponge. In this application, konjac fine powder is added into boiling water to form a viscous liquid, which is then injected into the mold after adding alkali. And high-temperature steaming to obtain the colloidal blank, and then put it into a packaging bag after freezing, alkali removal, decolorization, color protection, and moisture retention, vacuumize and fill with nitrogen, seal and then sterilize at high temperature to obtain the finished product. The Chinese patent publication number is CN 1583838 A, the publication date is February 3, 2005, and the title of the invention is a preparation method of macroporous konjac gel. The application discloses using konjac powder as raw material and inorganic alkali as flocculant , form a gel through high temperature reaction, then freeze at low temperature, thaw at room temperature, freeze-thaw repeatedly, and freeze-dry to obtain macroporous konjac gel. The Chinese patent publication number is CN 101011163A, and the disclosure date is August 8, 2007. The name of the invention is an edible health care massage towel made of konjac and grain. Mixing, adding starter to ferment and coagulant to coagulate, then crushing part of the material into powder, mixing, injection molding, ripening, freezing, thawing, dehydration, and finally drying. The Chinese patent publication number is CN 101147658 A, and the disclosure date is March 26, 2008. The invention name is called konjac towel with skin care function. In this application, the konjac powder is gelatinized with water and mixed with grain powder, and added starter fermentation and The coagulant is solidified, then injected, matured, frozen, thawed, dehydrated, soaked in skin care plant serum, and vacuum-dried. The Chinese patent publication number is CN 101423613 A, the publication date is May 6, 2009, and the invention name is an environmentally friendly preparation method of glucomannan sponge. The application discloses that calcium hydroxide is used as a flocculant, and no Environmentally friendly preparation of glucomannan sponge for bathing in alkaline anhydrous and decolorized sewage. The Chinese patent publication number is CN 102178484 A, and the disclosure date is September 14, 2011. The name of the invention is a konjac face towel with bathing and massage functions and its preparation method. Adding flocculant to prepare mixed material, followed by injection molding, boiling, repeated freezing and thawing at low temperature for dehydration, bleaching, desulfurization, sterilization and freeze drying to prepare konjac sponge face towel. the
目前文献报道的制备魔芋海绵材料的方法均为冻融法,这类魔芋海绵的结构致密,吸水倍数小,吸水速率慢,而且干燥状态时该产品发硬,表面粗糙,湿润时易滋生细菌,短时间就会降解,储存困难。因此,该类魔芋海绵仅能用于制作毛巾、面擦和粉扑等产品,无法满足医用敷料的使用要求。 The method for preparing the konjac sponge material reported in the literature at present is the freeze-thaw method. The structure of this type of konjac sponge is compact, the water absorption multiple is small, and the water absorption rate is slow, and the product is hard when dry, and the surface is rough. When wet, it is easy to breed bacteria. It degrades in a short time and is difficult to store. Therefore, this type of konjac sponge can only be used to make products such as towels, face wipes and powder puffs, and cannot meet the requirements for use of medical dressings. the
发明内容 Contents of the invention
针对上述存在的问题,本发明的目的在于提供一种以魔芋精粉为原料,生产工艺简单的魔芋海绵医用敷料及其制备方法,且该魔芋海绵医用敷料的吸湿性、透气性、柔软度、韧性、弹性和强度等综合性能优异,能够用于治疗手术伤口、烧烫伤创面等各种类型的皮肤创伤,为了实现上述目的,其技术解决方案为: For above-mentioned existing problem, the object of the present invention is to provide a kind of with konjac fine powder as raw material, simple konjac sponge medical dressing and preparation method thereof of production process, and the hygroscopicity, air permeability, softness, It has excellent comprehensive properties such as toughness, elasticity and strength, and can be used to treat various types of skin wounds such as surgical wounds and burn wounds. In order to achieve the above goals, its technical solutions are:
一种魔芋海绵医用敷料,魔芋海绵医用敷料以葡甘聚糖含量为50%~90%,分子量为 100000~500000的魔芋精粉为原料,蒸馏水为溶剂,采用高速搅拌和高温溶解制备溶液,通过低温预冻和真空干燥技术成形,然后采用氢氧化钠乙醇溶液固化处理,并经切割、分装、灭菌而成,其中所述魔芋海绵医用敷料的吸液量为100~300g/g,透气率为80%~90%。 A konjac sponge medical dressing. The konjac sponge medical dressing uses konjac fine powder with a glucomannan content of 50% to 90% and a molecular weight of 100,000 to 500,000 as a raw material, distilled water as a solvent, and a solution prepared by high-speed stirring and high-temperature dissolution. It is formed by low-temperature pre-freezing and vacuum drying technology, and then solidified by sodium hydroxide ethanol solution, cut, sub-packaged, and sterilized. The konjac sponge medical dressing has a liquid absorption of 100-300g/g and is breathable The rate is 80% to 90%. the
一种魔芋海绵医用敷料的制备方法,魔芋海绵医用敷料的制备方法包括如下步骤: A kind of preparation method of konjac sponge medical dressing, the preparation method of konjac sponge medical dressing comprises the steps:
a魔芋精粉水溶液的制备 a Preparation of konjac powder aqueous solution
将蒸馏水与魔芋精粉按照质量比为1∶0.01~0.05的比例混合,然后高速搅拌溶解,高速搅拌机的转速为5000~10000r/min,溶解温度为30~60℃,溶解时间为2~6h,得到溶解均匀的魔芋精粉水溶液,其中魔芋精粉中葡甘聚糖含量为50%~90%,分子量为100000~500000; Mix distilled water and konjac powder according to the mass ratio of 1:0.01-0.05, then stir and dissolve at a high speed, the speed of the high-speed mixer is 5000-10000r/min, the dissolution temperature is 30-60°C, and the dissolution time is 2-6h. Obtain a homogeneously dissolved konjac fine powder aqueous solution, wherein the glucomannan content in the konjac fine powder is 50% to 90%, and the molecular weight is 100000 to 500000;
b魔芋海绵的成形 b Forming of konjac sponge
将经步骤a制得的魔芋精粉水溶液分装到模具中进行预冻,预冻温度为-26~-16℃,预冻时间为5~12h,然后将模具置于真空烘箱中进行真空干燥,真空度≤100Pa,干燥温度为30~50℃,干燥时间为4~12h,干燥后脱模得到成形的魔芋海绵; Pack the konjac fine powder aqueous solution prepared in step a into molds for prefreezing, the prefreezing temperature is -26~-16°C, and the prefreezing time is 5~12h, and then the mold is placed in a vacuum oven for vacuum drying , the vacuum degree is ≤100Pa, the drying temperature is 30-50°C, the drying time is 4-12h, and the molded konjac sponge is obtained after drying;
c魔芋海绵的固化处理 c Curing treatment of konjac sponge
将乙醇与氢氧化钠按照质量比为1∶0.01~0.05的比例混合,然后搅拌至溶解均匀,得到魔芋海绵的凝固浴,将经步骤b得到的魔芋海绵浸泡在上述凝固浴中进行固化,固化温度为40~60℃,固化时间为2~8h,然后将固化后的魔芋海绵置于乙醇中进行漂洗,浴比为1∶100,洗涤时间为3~5min/次,洗涤2~5次,取出后自然晾干,得到固化魔芋海绵; Mix ethanol and sodium hydroxide according to the mass ratio of 1:0.01~0.05, and then stir until it dissolves evenly to obtain a coagulation bath of konjac sponge, soak the konjac sponge obtained through step b in the above coagulation bath for solidification, solidify The temperature is 40-60°C, the curing time is 2-8 hours, and then the cured konjac sponge is rinsed in ethanol, the bath ratio is 1:100, the washing time is 3-5min/time, and the washing time is 2-5 times. Take it out and dry it naturally to obtain solidified konjac sponge;
d魔芋海绵敷料的制备 d Preparation of konjac sponge dressing
将经步骤c得到的固化魔芋海绵切割、包装,然后经Co60辐照灭菌,得到吸液量为100~300g/g,透气率为80%~90%的魔芋海绵医用敷料。 The solidified konjac sponge obtained in step c is cut, packaged, and then sterilized by Co 60 radiation to obtain a konjac sponge medical dressing with a liquid absorption of 100-300 g/g and an air permeability of 80%-90%.
由于采用了上述技术方案,本发明一种魔芋海绵医用敷料及其制备方法的有益技术效果是: Owing to having adopted above-mentioned technical scheme, the beneficial technical effect of a kind of konjac sponge medical dressing of the present invention and preparation method thereof is:
1本发明的魔芋海绵医用敷料的制备以葡甘聚糖含量为50%~90%,分子量为100000~500000的魔芋精粉为原料,通过魔芋精粉的纯度和分子量的控制以及魔芋精粉水溶液浓度的调节,得到溶解充分且粘度适中的溶液,从而获得空间结构合理,弹性、韧性和强度等综合性能优异,吸液量达到100~300g/g,透气率达到80%~90%的魔芋海绵医用敷料。 1. The preparation of konjac sponge medical dressing of the present invention is 50%~90% with glucomannan content, and the konjac fine powder that molecular weight is 100000~500000 is raw material, through the control of the purity of konjac fine powder and molecular weight and konjac fine powder aqueous solution Adjust the concentration to obtain a solution with sufficient dissolution and moderate viscosity, so as to obtain a konjac sponge with reasonable spatial structure, excellent comprehensive properties such as elasticity, toughness and strength, liquid absorption of 100-300g/g, and air permeability of 80%-90%. Medical dressing. the
2本发明魔芋海绵医用敷料的制备采用低温预冻和真空干燥技术成形,通过水的结晶和升华的方式得到吸湿性和透气性优异、生物相容和生物可降解、表面细腻平整且无裂痕以及易去除的魔芋海绵材料,该魔芋海绵材料可作为医用敷料用于治疗手术伤口、烧烫伤创面等各 种类型的皮肤创伤,弥补了现有的魔芋海绵仅能用于制作毛巾、面擦和粉扑等产品的缺陷,扩大了魔芋的应用范围,为农副产品的综合开发利用提供了一条有效途径。 2. The preparation of the konjac sponge medical dressing of the present invention adopts low-temperature pre-freezing and vacuum drying technology to form, and obtains excellent hygroscopicity and air permeability, biocompatibility and biodegradability, smooth surface and no cracks through the crystallization and sublimation of water. Easy to remove konjac sponge material, the konjac sponge material can be used as a medical dressing to treat various types of skin wounds such as surgical wounds and burn wounds, making up for the fact that the existing konjac sponge can only be used to make towels, face wipes and puffs The defects of such products expand the scope of application of konjac and provide an effective way for the comprehensive development and utilization of agricultural and sideline products. the
3本发明的魔芋海绵医用敷料的制备采用氢氧化钠的乙醇溶液进行固化,并以乙醇为洗涤液进行清洗,可以有效的防止海绵孔洞结构的塌陷、粘连和封闭以及海绵表面的粗糙和发硬,无需添加柔软剂,就可以得到柔软性优异,吸液量达到100~300g/g,透气率达到80%~90%的魔芋海绵医用敷料。 3. The preparation of the konjac sponge medical dressing of the present invention adopts the ethanol solution of sodium hydroxide to solidify, and cleans with ethanol as the washing liquid, which can effectively prevent the collapse, adhesion and sealing of the sponge pore structure and the roughness and hardening of the sponge surface , without adding softener, can obtain konjac sponge medical dressing with excellent softness, liquid absorption of 100-300g/g, air permeability of 80%-90%. the
4本发明魔芋海绵的制备方法采用普通冰箱预冻和真空干燥箱真空干燥,并采用自然风干的技术制备魔芋海绵医用敷料,生产设备和工艺简单且能耗低,降低了生产成本,储存方便,有利于魔芋海绵医用敷料的推广使用。 4. The preparation method of konjac sponge of the present invention adopts common refrigerator pre-freezing and vacuum drying in a vacuum oven, and adopts the technology of natural air-drying to prepare konjac sponge medical dressing. The production equipment and process are simple and energy consumption is low, which reduces production costs and is convenient for storage. It is beneficial to popularize and use of konjac sponge medical dressing. the
具体实施方式 Detailed ways
一种魔芋海绵医用敷料,魔芋海绵医用敷料以葡甘聚糖含量为50%~90%,分子量为100000~500000的魔芋精粉为原料,通过低温预冻和真空干燥技术成形,然后采用氢氧化钠乙醇溶液固化处理,并经切割、分装、灭菌而成,其中所述魔芋海绵医用敷料的吸液量为100~300g/g,透气率为80%~90%。 A konjac sponge medical dressing. The konjac sponge medical dressing uses konjac fine powder with a glucomannan content of 50% to 90% and a molecular weight of 100,000 to 500,000 as a raw material, which is formed by low-temperature pre-freezing and vacuum drying technology, and then hydrogenated. The sodium ethanol solution is solidified, cut, packaged and sterilized. The konjac sponge medical dressing has a liquid absorption capacity of 100-300 g/g and an air permeability of 80-90%. the
一种魔芋海绵医用敷料的制备方法,魔芋海绵医用敷料的制备方法包括如下步骤: A kind of preparation method of konjac sponge medical dressing, the preparation method of konjac sponge medical dressing comprises the steps:
a魔芋精粉水溶液的制备 a Preparation of konjac powder aqueous solution
将蒸馏水与魔芋精粉按照质量比为1∶0.01~0.05的比例混合,然后高速搅拌溶解,高速搅拌机的转速为5000~10000r/min,溶解温度为30~60℃,溶解时间为2~6h,得到溶解均匀的魔芋精粉水溶液,其中魔芋精粉中葡甘聚糖含量为50%~90%,分子量为100000~500000。 Mix distilled water and konjac powder according to the mass ratio of 1:0.01-0.05, then stir and dissolve at a high speed, the speed of the high-speed mixer is 5000-10000r/min, the dissolution temperature is 30-60°C, and the dissolution time is 2-6h. A homogeneously dissolved konjac powder aqueous solution is obtained, wherein the content of glucomannan in the konjac powder is 50%-90%, and the molecular weight is 100000-500000. the
由于魔芋精粉其分子量较高,粘度较大且纯度较低,溶解比较困难,本发明采用高速搅拌和高温溶解的办法,实现了魔芋精粉在蒸馏水中的溶解,缩短了溶解时间。 Because konjac fine powder has high molecular weight, high viscosity and low purity, and is difficult to dissolve, the present invention adopts high-speed stirring and high-temperature dissolution to realize the dissolution of konjac fine powder in distilled water and shorten the dissolution time. the
b魔芋海绵的成形 b Forming of konjac sponge
将经步骤a制得的魔芋精粉水溶液分装到模具中,然后置于冰箱中进行预冻,预冻温度为-26~-16℃,预冻时间为5~12h,然后将模具置于真空烘箱中进行真空干燥,真空度≤100Pa,干燥温度为30~50℃,干燥时间为4~12h,干燥后脱模得到成形的魔芋海绵。 Pack the konjac fine powder aqueous solution prepared in step a into molds, and then place them in a refrigerator for prefreezing. The prefreezing temperature is -26 to -16°C, and the prefreezing time is 5 to 12 hours. Vacuum drying is carried out in a vacuum oven, the vacuum degree is ≤100 Pa, the drying temperature is 30-50° C., and the drying time is 4-12 hours. After drying, the konjac sponge is demolded to obtain a shape. the
现有工艺是采用冻融法制备魔芋海绵材料,通过针扎(刺)将魔芋凝胶中的融化水排出,从而得到多孔的海绵状魔芋材料。由于凝胶体的密度较大且融化水的体积较大,所以制得的海绵粗糙且干燥后发硬,无法满足医用敷料的使用要求。本发明的制备方法采用低温预冻和高温真空干燥技术成形,预冻过程中魔芋精粉水溶液发生冻结,内部形成细小的结晶水晶粒, 高温真空干燥时结晶水晶粒升华,留下细密孔洞,从而得到细腻柔软,弹性和韧性优异,且透气性和吸水性能突出的海绵状魔芋材料,满足医用敷料的使用要求。另外,现有的真空冷冻干燥技术需要采用冷冻干燥机,该设备成本高且能耗高,本发明借助家用冰箱(或冷库)和普通的真空烘箱实现了魔芋海绵的制备,降低了设备成本,且真空烘箱的干燥温度较高,缩短了干燥时间,节约了能源,降低了产品的成本,有利于该产品的推广使用。 The existing technology is to prepare the konjac sponge material by freeze-thawing method, and the melted water in the konjac gel is discharged by needle sticking (puncturing), thereby obtaining the porous spongy konjac material. Due to the high density of the gel and the large volume of melted water, the prepared sponge is rough and hard after drying, which cannot meet the requirements for use of medical dressings. The preparation method of the present invention adopts low-temperature pre-freezing and high-temperature vacuum drying technology to form. During the pre-freezing process, the aqueous solution of konjac fine powder freezes, forming fine crystal grains inside, and the crystal grains sublimate during high-temperature vacuum drying, leaving fine and dense holes, thereby A spongy konjac material that is fine and soft, excellent in elasticity and toughness, and outstanding in air permeability and water absorption is obtained, which meets the requirements for use of medical dressings. In addition, the existing vacuum freeze-drying technology needs to adopt a freeze-drying machine, which has high cost and high energy consumption. The present invention realizes the preparation of konjac sponge by means of a household refrigerator (or cold storage) and a common vacuum oven, which reduces the equipment cost. Moreover, the drying temperature of the vacuum oven is relatively high, which shortens the drying time, saves energy, reduces the cost of the product, and is beneficial to popularization and use of the product. the
c魔芋海绵的固化处理 c Curing treatment of konjac sponge
将乙醇与氢氧化钠按照质量比为1∶0.01~0.05的比例混合,然后搅拌至溶解均匀,得到魔芋海绵的凝固浴,将经步骤b得到的魔芋海绵浸泡在上述凝固浴中进行固化,固化温度为40~60℃,固化时间为2~8h,然后将固化后的魔芋海绵置于乙醇中进漂洗,浴比为1∶100,洗涤时间为3~5min/次,洗涤2~5次,为了节约洗涤时间和增强洗涤效果,本发明还可对魔芋海绵进行超声波洗涤,超声波的功率为1200W,温度为50℃,取出后自然晾干,得到固化魔芋海绵,所述的乙醇均为100%的分析纯。 Mix ethanol and sodium hydroxide according to the mass ratio of 1:0.01~0.05, and then stir until it dissolves evenly to obtain a coagulation bath of konjac sponge, soak the konjac sponge obtained through step b in the above coagulation bath for solidification, solidify The temperature is 40-60°C, the curing time is 2-8 hours, and then the cured konjac sponge is rinsed in ethanol, the bath ratio is 1:100, the washing time is 3-5min/time, and the washing time is 2-5 times. In order to save washing time and enhance the washing effect, the present invention can also carry out ultrasonic cleaning to the konjac sponge, the power of the ultrasonic wave is 1200W, the temperature is 50°C, and after taking it out, it is naturally dried to obtain a solidified konjac sponge, and the ethanol is 100% of analytical purity. the
冷冻干燥成形后的魔芋海绵溶于水,因此需要进行固化处理以提高其吸水性,满足医用敷料的使用要求。现有工艺中魔芋的絮凝浴采用氢氧化钠的水溶液,由于魔芋海绵溶于水,凝固过程中海绵的部分孔洞结构发生坍塌、粘连和封闭,使得海绵的结构致密、坚硬、发脆且缺乏弹性。本发明的制备方法以氢氧化钠的乙醇溶液做为魔芋海绵的凝固浴,并采用乙醇作为洗涤液,利用魔芋海绵不溶于乙醇的特性,有效地避免了上述问题,从而得到柔韧性和弹性俱佳的魔芋海绵。另外,由于乙醇易于挥发,不需要经过二次冷冻干燥成形和高温烘干处理,自然条件下风干就可以得到干燥的魔芋海绵,节约了能源,降低了成本。 The freeze-dried konjac sponge is soluble in water, so it needs to be solidified to improve its water absorption and meet the requirements of medical dressings. The flocculation bath of konjac in the existing technology adopts the aqueous solution of sodium hydroxide, because the konjac sponge is dissolved in water, some pore structures of the sponge collapse, stick and close during the solidification process, making the structure of the sponge compact, hard, brittle and lack of elasticity . The preparation method of the present invention uses the ethanol solution of sodium hydroxide as the coagulation bath of the konjac sponge, and adopts ethanol as the washing liquid, utilizes the characteristic that the konjac sponge is insoluble in ethanol, effectively avoids the above-mentioned problems, thereby obtains flexibility and elasticity The best konjac sponge. In addition, since ethanol is easy to volatilize, there is no need for secondary freeze-drying and high-temperature drying treatment, and the dry konjac sponge can be obtained by air-drying under natural conditions, which saves energy and reduces costs. the
d魔芋海绵敷料的制备 d Preparation of konjac sponge dressing
将经步骤c得到的固化魔芋海绵切割、包装,然后经Co60辐照灭菌,得到吸液量为100~300g/g,透气率为80%~90%的魔芋海绵医用敷料。 The solidified konjac sponge obtained in step c is cut, packaged, and then sterilized by Co 60 radiation to obtain a konjac sponge medical dressing with a liquid absorption of 100-300 g/g and an air permeability of 80%-90%.
本发明的制备方法通过魔芋精粉原料的纯度和分子量控制,以及魔芋精粉水溶液浓度的调节,并通过高速搅拌和高温溶解,得到溶解充分且粘度适中的溶液,采用低温预冻和高温真空干燥技术得到柔性海绵状魔芋材料,并以氢氧化钠的乙醇溶液做为魔芋海绵的凝固浴以及乙醇作为洗涤液,提高了魔芋海绵的吸水性,同时有效的避免魔芋海绵的孔洞结构发生坍塌、粘连和封闭,从而得到空间结构合理,表面细腻平整且无裂痕,以及柔软度、弹性、韧性和强度等综合性能优异,吸液量达到100~300g/g,透气率达到80%~90%,生物相容和生物可降解的魔芋海绵医用敷料,该魔芋海绵材料可作为医用敷料用于治疗手术伤口、烧烫伤创面等各种类型的皮肤创伤,弥补了现有的魔芋海绵仅能用于制作毛巾、面擦和粉扑等产品 的缺陷,扩大了魔芋的应用范围,为农副产品的综合开发利用提供了一条有效途径。 The preparation method of the present invention controls the purity and molecular weight of the konjac fine powder raw material, adjusts the concentration of the konjac fine powder aqueous solution, and obtains a fully dissolved and moderately viscous solution through high-speed stirring and high-temperature dissolution, and adopts low-temperature pre-freezing and high-temperature vacuum drying Technology obtains flexible sponge-like konjac material, and uses ethanol solution of sodium hydroxide as the coagulation bath of the konjac sponge and ethanol as the washing liquid, which improves the water absorption of the konjac sponge and effectively prevents the pore structure of the konjac sponge from collapsing and sticking And closed, so as to obtain reasonable space structure, fine and smooth surface without cracks, and excellent comprehensive properties such as softness, elasticity, toughness and strength, liquid absorption reaches 100-300g/g, air permeability reaches 80%-90%, biological Compatible and biodegradable konjac sponge medical dressing, the konjac sponge material can be used as a medical dressing to treat various types of skin wounds such as surgical wounds, burn wounds, etc., making up for the fact that the existing konjac sponge can only be used to make towels The defects of products such as konjac, noodle rub and powder puff have expanded the application range of konjac and provided an effective way for the comprehensive development and utilization of agricultural and sideline products. the
下面结合具体实施例对本发明的一种魔芋海绵医用敷料及其制备方法作进一步详细描述: A kind of konjac sponge medical dressing of the present invention and preparation method thereof are described in further detail below in conjunction with specific examples:
具体实施例 specific embodiment
实施例1 Example 1
依次称取100克蒸馏水、5克葡甘聚糖含量为50%且分子量为100000的魔芋精粉,边搅拌边将称取的魔芋精粉添加到60℃的蒸馏水中,高速搅拌溶解,高速搅拌机的转速为5000r/min,溶解时间为6h,得到溶解均匀的魔芋精粉水溶液;将魔芋精粉水溶液分装到模具中,将模具置于-26℃的冰箱中进行预冻,预冻时间为5h,然后置于50℃的真空干燥箱中进行真空干燥,真空度为60Pa,干燥时间为4h,然后脱模得到成形的魔芋海绵;依次称取100克的乙醇、5克的氢氧化钠,将氢氧化钠添加到乙醇中并搅拌均匀,得到魔芋海绵的凝固浴,将成形的魔芋海绵浸泡在上述凝固浴中进行固化,固化温度为60℃,固化时间为2h,然后将魔芋海绵置于乙醇中漂洗,洗涤时间为3min/次,洗涤5次,洗涤完成后自然晾干,得到固化魔芋海绵;将固化后的魔芋海绵切割、包装,然后经Co60辐照灭菌得到吸液量为100g/g,透气率为90%的魔芋海绵医用敷料。 Take by weighing 100 grams of distilled water, 5 grams of konjac powder with a glucomannan content of 50% and a molecular weight of 100,000, add the konjac powder to 60°C distilled water while stirring, stir and dissolve at a high speed, and use a high-speed mixer The rotating speed is 5000r/min, and the dissolving time is 6h to obtain a homogeneously dissolved konjac powder aqueous solution; the konjac powder aqueous solution is divided into molds, and the mold is placed in a refrigerator at -26°C for pre-freezing. The pre-freezing time is 5h, then be placed in the vacuum oven of 50 ℃ and carry out vacuum drying, and vacuum tightness is 60Pa, and drying time is 4h, then demoulding obtains the konjac sponge of forming; Take by successively the sodium hydroxide of 100 grams of ethanol, 5 grams, Add sodium hydroxide to ethanol and stir evenly to obtain a coagulation bath of konjac sponge. Soak the formed konjac sponge in the above coagulation bath for curing. The curing temperature is 60°C and the curing time is 2h. Then put the konjac sponge in Rinse in ethanol, the washing time is 3min/time, wash 5 times, dry naturally after washing, obtain solidified konjac sponge; the konjac sponge after solidification is cut, packaged, then through Co 60 irradiation sterilization to obtain liquid absorption: 100g/g, konjac sponge medical dressing with air permeability of 90%.
实施例2 Example 2
依次称取100克蒸馏水、1克葡甘聚糖含量为90%且分子量为500000的魔芋精粉,边搅拌边将称取的魔芋精粉添加到30℃的蒸馏水中,高速搅拌溶解,高速搅拌机的转速为10000r/min,溶解时间为2h,得到溶解均匀的魔芋精粉水溶液;将魔芋精粉水溶液分装到模具中,将模具置于-16℃的冰箱中进行预冻,预冻时间为12h,然后置于30℃的真空干燥箱中进行真空干燥,真空度为100Pa,干燥时间为12h,然后脱模得到成形的魔芋海绵;依次称取100克的乙醇、1克的氢氧化钠,将氢氧化钠添加到乙醇中并搅拌均匀,得到魔芋海绵的凝固浴,将成形的魔芋海绵浸泡在上述凝固浴中进行固化,固化温度为40℃,固化时间为8h,然后将魔芋海绵置于乙醇中漂洗,洗涤时间为5min/次,洗涤2次,洗涤完成后自然晾干,得到固化魔芋海绵;将固化后的魔芋海绵切割、包装,然后经Co60辐照灭菌得到吸液量为300g/g,透气率为80%的魔芋海绵医用敷料。 Take by weighing 100 grams of distilled water and 1 gram of konjac powder with a glucomannan content of 90% and a molecular weight of 500,000 in turn, add the konjac powder to 30°C distilled water while stirring, stir and dissolve at a high speed, and use a high-speed mixer The rotation speed of the konjac powder is 10000r/min, and the dissolution time is 2h to obtain a homogeneously dissolved konjac powder aqueous solution; the konjac powder aqueous solution is divided into molds, and the mold is placed in a refrigerator at -16°C for pre-freezing. The pre-freezing time is 12h, then be placed in the vacuum oven of 30 ℃ and carry out vacuum drying, and vacuum tightness is 100Pa, and drying time is 12h, then demoulding obtains the konjac sponge of forming; Take by successively the sodium hydroxide of 100 grams of ethanol, 1 gram, Add sodium hydroxide to ethanol and stir evenly to obtain a coagulation bath of konjac sponge. Soak the formed konjac sponge in the above coagulation bath for curing. The curing temperature is 40°C and the curing time is 8h. Then put the konjac sponge in Rinse in ethanol, the washing time is 5min/time, wash 2 times, dry naturally after washing, obtain solidified konjac sponge; the konjac sponge after solidification is cut, packaged, then through Co 60 radiation sterilization to obtain the liquid absorption capacity of 300g/g, konjac sponge medical dressing with an air permeability of 80%.
实施例3 Example 3
依次称取100克蒸馏水、4克葡甘聚糖含量为60%且分子量为180000的魔芋精粉,边搅拌边将称取的魔芋精粉添加到50℃的蒸馏水中,高速搅拌溶解,高速搅拌机的转速为6000r/min,溶解时间为5h,得到溶解均匀的魔芋精粉水溶液;将魔芋精粉水溶液分装到模具中, 将模具置于-18℃的冰箱中进行预冻,预冻时间为8h,然后置于35℃的真空干燥箱中进行真空干燥,真空度为90Pa,干燥时间为10h,然后脱模得到成形的魔芋海绵;依次称取100克的乙醇、4克的氢氧化钠,将氢氧化钠添加到乙醇中并搅拌均匀,得到魔芋海绵的凝固浴,将成形的魔芋海绵浸泡在上述凝固浴中进行固化,固化温度为50℃,固化时间为4h,然后将魔芋海绵置于乙醇中进行超声清洗,超声波超声波的功率为1200W,温度为50℃,洗涤时间为3min/次,洗涤3次,洗涤完成后自然晾干,得到固化魔芋海绵;将固化后的魔芋海绵切割、包装,然后经Co60辐照灭菌得到吸液量为250g/g,透气率为85%的魔芋海绵医用敷料。 Take by weighing 100 grams of distilled water, 4 grams of konjac powder with a glucomannan content of 60% and a molecular weight of 180,000, add the konjac powder to 50°C distilled water while stirring, stir and dissolve at a high speed, and use a high-speed mixer The rotating speed is 6000r/min, and the dissolving time is 5h to obtain a homogeneously dissolved konjac fine powder aqueous solution; the konjac fine powder aqueous solution is divided into molds, and the mold is placed in a refrigerator at -18°C for pre-freezing. The pre-freezing time is 8h, then be placed in the vacuum oven of 35 ℃ and carry out vacuum drying, and vacuum tightness is 90Pa, and drying time is 10h, then demoulding obtains the konjac sponge of forming; Take by weighing the ethanol of 100 grams, the sodium hydroxide of 4 grams successively, Add sodium hydroxide to ethanol and stir evenly to obtain a coagulation bath of konjac sponge. Soak the formed konjac sponge in the above coagulation bath for curing. The curing temperature is 50°C and the curing time is 4h. Then put the konjac sponge in Carry out ultrasonic cleaning in ethanol, the power of ultrasonic ultrasonic is 1200W, temperature is 50 ℃, washing time is 3min/time, wash 3 times, after washing, dry naturally, obtain cured konjac sponge; cut and pack the konjac sponge after curing , and obtain the konjac sponge medical dressing with a liquid absorption capacity of 250g/g and an air permeability of 85% through Co 60 irradiation sterilization.
实施例4 Example 4
依次称取100克蒸馏水、3克葡甘聚糖含量为70%且分子量为220000的魔芋精粉,边搅拌边将称取的魔芋精粉添加到40℃的蒸馏水中,高速搅拌溶解,高速搅拌机的转速为7000r/min,溶解时间为4h,得到溶解均匀的魔芋精粉水溶液;将魔芋精粉水溶液分装到模具中,将模具置于-20℃的冰箱中进行预冻,预冻时间为10h,然后置于30℃的真空干燥箱中进行真空干燥,真空度为80Pa,干燥时间为8h,然后脱模得到成形的魔芋海绵;依次称取100克的乙醇、3克的氢氧化钠,将氢氧化钠添加到乙醇中并搅拌均匀,得到魔芋海绵的凝固浴,将成形的魔芋海绵浸泡在上述凝固浴中进行固化,固化温度为40℃,固化时间为5h,然后将魔芋海绵置于乙醇中超声清洗,超声波超声波的功率为1200W,温度为50℃,洗涤时间为5min,洗涤1次,洗涤完成后自然晾干,得到固化魔芋海绵;将固化后的魔芋海绵切割、包装,然后经Co60辐照灭菌得到吸液量为200g/g,透气率为90%的魔芋海绵医用敷料。 Take by weighing 100 grams of distilled water, 3 grams of konjac powder with a glucomannan content of 70% and a molecular weight of 220,000, add the konjac powder to 40°C distilled water while stirring, stir and dissolve at a high speed, and use a high-speed mixer The rotating speed is 7000r/min, and the dissolving time is 4h, and the aqueous solution of konjac fine powder that dissolves uniformly is obtained; 10h, then be placed in the vacuum oven of 30 ℃ and carry out vacuum drying, and vacuum tightness is 80Pa, and drying time is 8h, then demoulding obtains the konjac sponge of forming; Take by successively the ethanol of 100 grams, the sodium hydroxide of 3 grams, Add sodium hydroxide to ethanol and stir evenly to obtain a coagulation bath of konjac sponge. Soak the formed konjac sponge in the above coagulation bath for curing. The curing temperature is 40°C and the curing time is 5h. Then put the konjac sponge in Ultrasonic cleaning in ethanol, the power of the ultrasonic wave is 1200W, the temperature is 50°C, the washing time is 5min, and the washing time is 1 time. Co 60 irradiation sterilization obtains the konjac sponge medical dressing with a liquid absorption capacity of 200g/g and an air permeability of 90%.
实施例5 Example 5
依次称取100克蒸馏水、2克葡甘聚糖含量为80%且分子量为310000的魔芋精粉,边搅拌边将称取的魔芋精粉添加到60℃的蒸馏水中,高速搅拌溶解,高速搅拌机的转速为6000r/min,溶解时间为3h,得到溶解均匀的魔芋精粉水溶液;将魔芋精粉水溶液分装到模具中,将模具置于-22℃的冰箱中进行预冻,预冻时间为12h,然后置于30℃的真空干燥箱中进行真空干燥,真空度为80Pa,干燥时间为6h,然后脱模得到成形的魔芋海绵;依次称取100克的乙醇、2克的氢氧化钠,将氢氧化钠添加到乙醇中并搅拌均匀,得到魔芋海绵的凝固浴,将成形的魔芋海绵浸泡在上述凝固浴中进行固化,固化温度为50℃,固化时间为6h,然后将魔芋海绵置于乙醇中漂洗,洗涤时间为5min/次,洗涤2次,洗涤完成后自然晾干,得到固化魔芋海绵;将固化后的魔芋海绵切割、包装,然后经Co60辐照灭菌得到吸液量为180g/g,透气率为85%的魔芋海绵医用敷料。 Take by weighing 100 grams of distilled water, 2 grams of konjac fine powder with a glucomannan content of 80% and a molecular weight of 310,000 in turn, add the konjac fine powder taken into distilled water at 60°C while stirring, stir and dissolve at a high speed, and use a high-speed mixer The rotating speed is 6000r/min, and the dissolving time is 3h, and the konjac fine powder aqueous solution that dissolves uniformly is obtained; the konjac fine powder aqueous solution is divided into molds, and the mold is placed in a refrigerator at -22°C for pre-freezing, and the pre-freezing time is 12h, then be placed in the vacuum oven of 30 ℃ and carry out vacuum drying, and vacuum tightness is 80Pa, and drying time is 6h, then demoulding obtains the konjac sponge of forming; Take by successively the sodium hydroxide of 100 grams of ethanol, 2 grams, Add sodium hydroxide to ethanol and stir evenly to obtain a coagulation bath of konjac sponge. Soak the formed konjac sponge in the above coagulation bath for curing. The curing temperature is 50°C and the curing time is 6h. Then put the konjac sponge in Rinse in ethanol, the washing time is 5min/time, wash 2 times, dry naturally after washing, obtain solidified konjac sponge; the konjac sponge after solidification is cut, packaged, then through Co 60 radiation sterilization to obtain the liquid absorption capacity of 180g/g, konjac sponge medical dressing with an air permeability of 85%.
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