CN111944168A - A hydrogel patch material fixed on the edge of a mask or medical goggles and its preparation method and application - Google Patents
A hydrogel patch material fixed on the edge of a mask or medical goggles and its preparation method and applicationDownload PDFInfo
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Abstract
Translated fromChinese
Description
Translated fromChinese技术领域technical field
本发明涉及一种网络水凝胶，尤其是涉及一种固定于口罩或医用护目镜边缘的水凝胶贴片材料及其制备方法和应用。The invention relates to a network hydrogel, in particular to a hydrogel patch material fixed on the edge of a mask or medical goggles, and a preparation method and application thereof.
背景技术Background technique
口罩是一种卫生用品，将其戴在口鼻部位用于过滤进入口鼻的空气，以达到阻挡有害的气体、气味、飞沫进出佩戴者口鼻的效果，对进入肺部的空气有一定的过滤作用。在呼吸道传染病流行时，在粉尘等污染的环境中作业时，戴口罩具有非常好的作用。A mask is a sanitary product that is worn on the mouth and nose to filter the air entering the mouth and nose to achieve the effect of blocking harmful gases, odors, and droplets from entering and leaving the wearer's mouth and nose, and has a certain effect on the air entering the lungs. filtering effect. When respiratory infectious diseases are prevalent, wearing a mask has a very good effect when working in a polluted environment such as dust.
口罩和护目镜一般都是依靠耳带或者弹力带的拉扯作用产生对面部的挤压来实现密封效果。Masks and goggles generally rely on the pulling effect of ear straps or elastic straps to squeeze the face to achieve the sealing effect.
口罩和护目镜一般都是依靠耳带或者弹力带的拉扯作用产生对面部的挤压来实现密封效果，加之护目镜下端与口罩上部重叠，因此长期佩戴口罩和护目镜会对鼻部和面部的皮肤产生一定的压力性损伤。因人体鼻部高度有差异，目前绝大多数口罩都是采取钢丝夹、铝片等硬性材料与人脸及鼻部进行贴合，因此并不能完全起到密封的效果，很容易导致细菌的进入。同时加上这些硬性材料会在鼻部与面部之间产生摩擦，使皮肤受损加重，间接地增大感染风险；由于口罩、护目镜与人脸之间会形成相对封闭的环境，口罩和护目镜不具有良好的吸湿功能，人体呼吸的水分以及分泌的汗液无法很好地排出，因此导致护具内部环境较为潮湿，影响佩戴的舒适性。急需解决佩戴口罩和护目镜所产生的压力性损伤。提高口罩的密封效果，改善口罩和护目镜内部潮湿环境，提高佩戴的舒适性。Masks and goggles generally rely on the pulling action of the ear strap or elastic band to squeeze the face to achieve the sealing effect. In addition, the lower end of the goggles overlaps with the upper part of the mask, so wearing masks and goggles for a long time will affect the nose and face. The skin produces a certain pressure injury. Due to the difference in the height of the human nose, most masks currently use hard materials such as wire clips and aluminum sheets to fit the face and nose, so they cannot fully seal and easily lead to the entry of bacteria. . At the same time, these hard materials will cause friction between the nose and the face, aggravate the skin damage, and indirectly increase the risk of infection; due to the relatively closed environment between masks, goggles and the face, masks and protective gear The eyepiece does not have a good moisture absorption function, and the water breathed by the human body and the sweat secreted cannot be discharged well, so the internal environment of the protective gear is relatively humid, which affects the comfort of wearing. There is an urgent need to address pressure injuries from wearing masks and goggles. Improve the sealing effect of the mask, improve the humid environment inside the mask and goggles, and improve the wearing comfort.
水凝胶是一种具有独特三维空间网络结构的功能高分子材料，其内部含有亲水基团能够吸收水分形成高粘度凝胶。水凝胶优良的生物相容性使其在药物缓释载体、创面敷料、组织工程具有广泛的应用。通过设计双网络结构可使水凝胶具有良好的回弹性、韧性和快速恢复能力。Hydrogel is a functional polymer material with a unique three-dimensional network structure, and its interior contains hydrophilic groups that can absorb water to form a high-viscosity gel. The excellent biocompatibility of hydrogels makes it widely used in drug sustained-release carriers, wound dressings, and tissue engineering. By designing the double network structure, the hydrogel can have good resilience, toughness and rapid recovery ability.
发明内容SUMMARY OF THE INVENTION
为解决现有技术中，本发明的目提供一种固定于口罩或医用护目镜边缘的水凝胶贴片材料，该材料可用于预防口罩或医用护目镜压力性损伤。In order to solve the problem in the prior art, the object of the present invention is to provide a hydrogel patch material fixed on the edge of a mask or medical goggles, which can be used to prevent pressure injury of the mask or medical goggles.
本发明还提供了一种固定于口罩或医用护目镜边缘的水凝胶贴片材料的制备方法，该方法操作简单。The invention also provides a preparation method of a hydrogel patch material fixed on the edge of a mask or medical goggles, and the method is simple to operate.
本发明还提供了一种固定于口罩或医用护目镜边缘的水凝胶贴片材料的应用。The invention also provides the application of a hydrogel patch material fixed on the edge of a mask or medical goggles.
本发明是通过下述技术方案实现的：The present invention is achieved through the following technical solutions:
一种固定于口罩或医用护目镜边缘的水凝胶贴片材料，所述水凝胶是PAA/CMCS双网络水凝胶，其包括以Fe3+为交联剂，过硫酸铵或过硫酸钾为引发剂，丙烯酸和羧甲基壳聚糖为基材制备得到的。A hydrogel patch material fixed on the edge of a mask or medical goggles, the hydrogel is a PAA/CMCS double network hydrogel, which comprises Fe3+ as a cross-linking agent, ammonium persulfate or persulfuric acid Potassium is used as initiator, and acrylic acid and carboxymethyl chitosan are used as substrates.
本发明所述的一种固定于口罩或医用护目镜边缘的水凝胶贴片材料，所述PAA/CMCS双网络水凝胶与氧化葡聚糖发生席夫碱反应来形成高粘附双网络水凝胶。A hydrogel patch material fixed on the edge of a mask or medical goggles according to the present invention, the PAA/CMCS double network hydrogel undergoes Schiff base reaction with oxidized dextran to form a high adhesion double network Hydrogels.
本发明的水凝胶是通过Fe3+化合物与聚丙烯酸分子(PAA)和羧甲基壳聚糖(CMCS)中的-COOH发生金属络合作用形成PAA/CMCS双网络水凝胶，PAA/CMCS双网络水凝胶的-NH2与氧化葡聚糖发生席夫碱反应来形成高粘附双网络水凝胶。The hydrogel of the present invention forms a PAA/CMCS double network hydrogel through metal complexation between Fe3+ compounds and polyacrylic acid molecules (PAA) and -COOH in carboxymethyl chitosan (CMCS). The -NH of the CMCSdouble network hydrogel undergoes Schiff base reaction with oxidized dextran to form a highly adhesive double network hydrogel.
上述本发明中所述丙烯酸的质量为羧甲基壳聚糖质量的4～8倍，所述交联剂的质量为基材质量的0.1％-0.5％，所述引发剂为基材质量的0.004％-0.025％。The quality of the acrylic acid in the above-mentioned invention is 4 to 8 times the quality of the carboxymethyl chitosan, the quality of the crosslinking agent is 0.1%-0.5% of the quality of the base material, and the initiator is 0.1% to 0.5% of the quality of the base material. 0.004%-0.025%.
进一步地，本发明中所述丙烯酸的质量为羧甲基壳聚糖质量的4～5倍。Further, the quality of the acrylic acid in the present invention is 4-5 times that of the carboxymethyl chitosan.
进一步地，本发明所述交联剂的质量过多样品变硬，脆性增加；过少样品强度不足，弹性减弱。Further, if the mass of the crosslinking agent in the present invention is too large, the sample will become hard and brittle; if the mass of the crosslinking agent is too small, the strength will be insufficient and the elasticity will be weakened.
进一步地，本发明所述引发剂质量过多则反应速度太快，难以控制；过少则不易引发，反应不能正常进行。Further, if the quality of the initiator in the present invention is too high, the reaction speed is too fast and difficult to control; if the quality of the initiator is too small, it is difficult to initiate and the reaction cannot proceed normally.
本发明所述的Fe3+为交联剂为氯化铁。The Fe3+ of the present invention is the cross-linking agent, which is ferric chloride.
上述本发明中所述氧化葡聚糖的质量是羧甲基壳聚糖质量的2～8倍。优选2-5倍。The quality of the oxidized glucan in the present invention is 2 to 8 times that of the carboxymethyl chitosan. Preferably 2-5 times.
为了增强抗菌性，优选在PAA/CMCS双网络水凝胶中填加纳米银。所述纳米银的质量为基材质量的0.01％-0.5％。优选0.01-0.1％。In order to enhance the antibacterial properties, it is preferable to add nano-silver into the PAA/CMCS double network hydrogel. The mass of the nano-silver is 0.01%-0.5% of the mass of the base material. Preferably 0.01-0.1%.
进一步优选，本发明一种固定于口罩或医用护目镜边缘的水凝胶贴片材料，所述水凝胶是PAA/CMCS双网络水凝胶，其包括以羧甲基壳聚糖、丙烯酸、Fe3+为交联剂，引发剂、纳米银和氧化葡聚糖按照2:10:0.06:0.003：0.012：10制备得到的。Further preferably, a hydrogel patch material of the present invention is fixed on the edge of a mask or medical goggles, and the hydrogel is a PAA/CMCS double network hydrogel, which includes carboxymethyl chitosan, acrylic acid, Fe3+ is a cross-linking agent, and the initiator, nano-silver and oxidized dextran are prepared according to 2:10:0.06:0.003:0.012:10.
本发明还包括一种固定于口罩或医用护目镜边缘的水凝胶贴片材料的制备方法，具体步骤为：The present invention also includes a preparation method of the hydrogel patch material fixed on the edge of the mask or medical goggles, the specific steps are:
(1)将羧甲基壳聚糖加入去离子水溶解,形成羧甲基壳聚糖溶液；(1) adding carboxymethyl chitosan into deionized water to dissolve, forming a carboxymethyl chitosan solution;
(2)将纳米银加入去离子水溶解，形成纳米银溶液；(2) adding nano-silver into deionized water to dissolve, forming nano-silver solution;
(3)将丙烯酸加入去离子水中溶解，形成丙烯酸溶液；(3) adding acrylic acid into deionized water and dissolving to form acrylic acid solution;
(4)然后将步骤(3)所得丙烯酸溶液与步骤(1)所得羧甲基壳聚糖溶液和步骤(2)所得纳米银溶液混合，向所得混合溶液中加入交联剂氯化铁与引发剂，搅拌均匀，反应，溶液变成弹性的水凝胶，形成PAA/CMCS双网络水凝胶；(4) then the acrylic acid solution obtained in step (3) is mixed with the carboxymethyl chitosan solution obtained in step (1) and the nano-silver solution obtained in step (2), and the crosslinking agent ferric chloride and the initiator are added to the obtained mixed solution. agent, stir evenly, react, the solution becomes an elastic hydrogel, forming a PAA/CMCS double network hydrogel;
(5)将氧化葡聚糖加入去离子水溶解，形成氧化葡聚糖溶液；(5) adding the oxidized glucan into deionized water to dissolve to form an oxidized glucan solution;
(6)将步骤(4)所得的PAA/CMCS双网络水凝胶置于步骤(5)所得的氧化葡聚糖溶液中，反应，得到高粘附性双网络水凝胶。(6) placing the PAA/CMCS double network hydrogel obtained in step (4) in the oxidized dextran solution obtained in step (5), and reacting to obtain a high adhesive double network hydrogel.
进一步地，本发明一种固定于口罩或医用护目镜边缘的水凝胶贴片材料的制备方法，具体步骤为：Further, a preparation method of a hydrogel patch material fixed on the edge of a mask or medical goggles of the present invention, the specific steps are:
(1)将羧甲基壳聚糖加入去离子水溶解,形成羧甲基壳聚糖溶液，其浓度为0.08-10.00g/ml；(1) adding carboxymethyl chitosan to deionized water to dissolve, forming carboxymethyl chitosan solution, and its concentration is 0.08-10.00g/ml;
(2)将纳米银加入去离子水溶解，形成纳米银溶液，浓度为0.01-1.00g/ml；(2) adding nano-silver into deionized water to dissolve, forming nano-silver solution, the concentration is 0.01-1.00g/ml;
(3)将丙烯酸加入去离子水中溶解，形成丙烯酸溶液，其浓度为0.10-15.0g/ml；(3) adding acrylic acid to deionized water and dissolving to form acrylic acid solution, and its concentration is 0.10-15.0g/ml;
(4)将步骤(3)丙烯酸溶液1-100ml与步骤(1)所得羧甲基壳聚糖溶液1ml-100ml和步骤(2)所得纳米银溶液0.01-10ml混合，向所得混合溶液中加入基材量0.1％-0.5％的交联剂氯化铁与基材量0.004％-0.025％的引发剂，搅拌均匀，在25-65℃下反应10-16h，溶液变成弹性的水凝胶，形成PAA/CMCS双网络水凝胶；(4) Mix 1-100 ml of acrylic acid solution in step (3) with 1 ml-100 ml of carboxymethyl chitosan solution obtained in step (1) and 0.01-10 ml of nano-silver solution obtained in step (2), and add base 0.1%-0.5% of the cross-linking agent ferric chloride and 0.004%-0.025% of the substrate initiator, stir evenly, and react at 25-65 ° C for 10-16 hours, the solution becomes an elastic hydrogel, Formation of PAA/CMCS double network hydrogel;
(5)将氧化葡聚糖加入去离子水溶解，形成氧化葡聚糖溶液，其浓度为1-20g/ml；(5) adding the oxidized dextran into deionized water to dissolve, forming the oxidized dextran solution, and its concentration is 1-20g/ml;
(6)将步骤(4)所得的PAA/CMCS双网络水凝胶置于步骤(5)所得的氧化葡聚糖溶液0.1-150ml中，在25-65℃下反应30min-2h，得到高粘附性双网络水凝胶。(6) placing the PAA/CMCS double network hydrogel obtained in step (4) in 0.1-150 ml of the oxidized dextran solution obtained in step (5), and reacting at 25-65° C. for 30min-2h to obtain a high viscosity Adhesive dual network hydrogels.
进一步地，上述技术方案中，步骤(1)羧甲基壳聚糖溶液，其浓度为1.0-2.50g/ml。Further, in the above technical solution, the concentration of the carboxymethyl chitosan solution in step (1) is 1.0-2.50 g/ml.
进一步地，上述技术方案中，步骤(2)纳米银溶液，浓度为0.01-1.00/ml；Further, in the above technical scheme, step (2) nano silver solution, the concentration is 0.01-1.00/ml;
进一步地，上述技术方案中，步骤(3)丙烯酸溶液，其浓度为2.00-4.60g/ml；Further, in the above-mentioned technical scheme, step (3) acrylic acid solution, its concentration is 2.00-4.60g/ml;
进一步地，上述技术方案中，步骤(5)氧化葡聚糖溶液，其浓度为10.00-18.00g/ml；Further, in the above technical solution, in step (5), the oxidized glucan solution has a concentration of 10.00-18.00 g/ml;
进一步地，上述技术方案中，步骤(4)在40-50℃下反应10-12h；步骤(5)在25-40℃下反应1-2h。Further, in the above technical solution, step (4) is reacted at 40-50° C. for 10-12 hours; and step (5) is reacted at 25-40° C. for 1-2 hours.
本发明另一技术方案，本发明提供了一种固定于口罩或医用护目镜边缘的水凝胶贴片材料的应用。所述应用包括将水凝胶贴片材料固定于口罩或护目镜的边缘处的，利用凝胶的自粘附性和缓冲作用来降低长期佩戴口罩和护目镜所产生的局部挤压，解决面部所产生的勒痕和局部密封问题，并利用凝胶材料的吸湿性能来改善口罩内部因汗液所形成的潮湿环境，提高佩戴舒适性。利用抗菌性能，减少面部过敏、皮肤溃烂。Another technical solution of the present invention provides the application of a hydrogel patch material fixed on the edge of a mask or medical goggles. The application includes fixing the hydrogel patch material at the edge of the mask or goggles, using the self-adhesion and buffering effect of the gel to reduce the local extrusion caused by wearing masks and goggles for a long time, and solve the problem of facial mask and goggles. The resulting streaks and local sealing problems, and the hygroscopic properties of the gel material are used to improve the moist environment formed by sweat inside the mask and improve wearing comfort. Utilize antibacterial properties to reduce facial allergies and skin ulcers.
本发明提供一种口罩，其包括口罩，口罩上的耳带，所述口罩边缘上固定有水凝胶贴片材料。The invention provides a mask, which comprises a mask, ear straps on the mask, and a hydrogel patch material is fixed on the edge of the mask.
本发明提供一种医用护目镜，所述医用护目镜边缘上固定有水凝胶贴片材料。The invention provides medical goggles, wherein a hydrogel patch material is fixed on the edge of the medical goggles.
有益效果beneficial effect
1.本发明提供的PAA/CMCS双网络水凝胶结构稳定，具有优良的力学性能。本发明羧甲基壳聚糖分子链上的羧基与Fe3+离子形成离子键交联的同时，利用其本身稳定的性质和抗菌抗感染能力，加入后银纳米粒子使水凝胶产生协同的抗菌性能。通过席夫碱反应在凝胶表面引入氧化葡聚糖，增加了粘附性得到具有高粘附性的双网络水凝胶。1. The PAA/CMCS double network hydrogel provided by the present invention has a stable structure and excellent mechanical properties. The carboxyl groups on the molecular chain of the carboxymethyl chitosan of the present invention and Fe3+ ions form ionic bond cross-linking, and at the same time, use its own stable properties and antibacterial and anti-infective capabilities, and the silver nanoparticles are added to make the hydrogel produce synergistic effects. Antibacterial properties. The introduction of oxidized dextran on the surface of the gel through Schiff base reaction increases the adhesion to obtain a double network hydrogel with high adhesion.
2.本发明所以羧甲基壳聚糖，丙烯酸，氧化壳聚糖，纳米银为原料，原料具有良好的生物相容性和生物降解性，制备得到的水凝胶对人体皮肤无害，且可用于生物组织工程领域。可将该水凝胶材料贴附于口罩、护目镜内部的边缘，利用水凝胶的粘附性和缓冲作用来降低长期佩戴防护用具所产生的局部挤压，解决勒痕和局部密封的问题。通过凝胶材料的抗菌性能，减少面部过敏、皮肤溃烂等问题。同时利用凝胶材料的吸湿性能来改善口罩内部因汗液等原因形成的潮湿环境，从而提高佩戴舒适度。2. The present invention uses carboxymethyl chitosan, acrylic acid, oxidized chitosan and nano silver as raw materials, the raw materials have good biocompatibility and biodegradability, the prepared hydrogel is harmless to human skin, and Can be used in the field of biological tissue engineering. The hydrogel material can be attached to the inner edge of the mask and goggles, and the adhesion and buffering effect of the hydrogel can be used to reduce the local extrusion caused by wearing protective equipment for a long time, and solve the problems of streak marks and local sealing. . Through the antibacterial properties of the gel material, problems such as facial allergies and skin ulcers are reduced. At the same time, the hygroscopic properties of the gel material are used to improve the humid environment inside the mask due to sweat and other reasons, thereby improving wearing comfort.
附图说明Description of drawings
图1为一种固定于口罩或医用护目镜边缘的水凝胶贴片材料在口罩上应用的侧视图。Figure 1 is a side view of the application of a hydrogel patch material fixed to the edge of a mask or medical goggles on a mask.
图2为一种固定于口罩或医用护目镜边缘的水凝胶贴片材料在口罩上应用的主视图。Figure 2 is a front view of the application of a hydrogel patch material fixed to the edge of a mask or medical goggles on a mask.
其中1为水凝胶贴片材料，2为口罩，3为口罩上的耳带。Among them, 1 is the hydrogel patch material, 2 is the mask, and 3 is the ear strap on the mask.
具体实施方式Detailed ways
下面通过具体实施例来对本发明做进一步的阐述，但实施例不限制本发明的保护范围。The present invention is further described below through specific examples, but the examples do not limit the protection scope of the present invention.
实施例1Example 1
制备具有吸湿、抗压和抗菌性能的水凝胶，具体步骤为：To prepare a hydrogel with hygroscopic, anti-pressure and antibacterial properties, the specific steps are:
1)将羧甲基壳聚糖加入去离子水溶解,形成1.00g/ml的羧甲基壳聚糖溶液。1) Dissolve carboxymethyl chitosan in deionized water to form a 1.00g/ml carboxymethyl chitosan solution.
2)将纳米银加入去离子水溶解，形成0.04g/ml纳米银溶液。2) The nano-silver was added into deionized water to dissolve to form a 0.04g/ml nano-silver solution.
3)将丙烯酸加入去离子水中溶解，形成2.00g/ml丙烯酸溶液；3) adding acrylic acid to deionized water and dissolving to form 2.00g/ml acrylic acid solution;
4)将步骤(3)丙烯酸溶液20.00ml与步骤(1)所得羧甲基壳聚糖溶液10.00ml和步骤(2)所得纳米银溶液0.625ml混合，向所得混合溶液中加入氯化铁0.25g与引发剂过硫酸铵0.0025g，搅拌均匀，在40℃下反应10h，溶液变成弹性的水凝胶，形成PAA/CMCS双网络水凝胶。4) Mix 20.00 ml of acrylic acid solution in step (3) with 10.00 ml of carboxymethyl chitosan solution obtained in step (1) and 0.625 ml of nano-silver solution obtained in step (2), and add 0.25 g of ferric chloride to the obtained mixed solution With the initiator ammonium persulfate 0.0025g, stirred evenly, and reacted at 40 °C for 10 h, the solution became an elastic hydrogel, forming a PAA/CMCS double network hydrogel.
5)将氧化葡聚糖加入去离子水溶解，形成10g/ml氧化葡聚糖溶液。5) The oxidized dextran was dissolved in deionized water to form a 10 g/ml oxidized dextran solution.
6)将步骤4)所得的PAA/CMCS双网络水凝胶置于步骤5)所得的氧化葡聚糖溶液8ml中，在25℃下反应1h，得到具有吸湿、抗压和抗菌性能的水凝胶。6) The PAA/CMCS double network hydrogel obtained in step 4) was placed in 8 ml of the oxidized dextran solution obtained in step 5), and reacted at 25° C. for 1 h to obtain a hydrogel with moisture absorption, pressure resistance and antibacterial properties. glue.
将本实施例所得到的水凝胶进行剥离力和压缩回弹测试，通过万能拉力机试验机测得剥离强度为28g·cm-1，压缩强度为85.41KPa(压缩形变为60％)。The hydrogel obtained in this example was tested for peel force and compression rebound, and the peel strength was 28 g·cm-1 and the compressive strength was 85.41 KPa (compression deformation was 60%) measured by a universal tensile tester.
将本实施例所得到的水凝胶进行生物相容性测试，细胞存活率为130.0％。The hydrogel obtained in this example was tested for biocompatibility, and the cell survival rate was 130.0%.
将本实施例所得到的水凝胶进行溶胀吸湿性能测试，温度控制在36℃进行溶胀实验，时间40min，溶胀率为120％。The hydrogel obtained in this example was subjected to a swelling and moisture absorption performance test, the temperature was controlled at 36° C. to carry out a swelling test, the time was 40 minutes, and the swelling rate was 120%.
实施例2Example 2
制备具有吸湿、抗压和抗菌性能的水凝胶的制备方法，具体步骤为：A preparation method for preparing a hydrogel with moisture absorption, compression resistance and antibacterial properties, the specific steps are:
1)将羧甲基壳聚糖加入去离子水溶解,形成1.50g/ml的羧甲基壳聚糖溶液；1) Dissolving carboxymethyl chitosan in deionized water to form a carboxymethyl chitosan solution of 1.50 g/ml;
2)将纳米银加入去离子水溶解，形成0.05g/ml纳米银溶液；2) adding the nano-silver into deionized water to dissolve to form a 0.05g/ml nano-silver solution;
3)将丙烯酸加入去离子水中溶解，形成4.00g/ml丙烯酸溶液；3) adding acrylic acid to deionized water to dissolve, forming 4.00g/ml acrylic acid solution;
4)将步骤(3)丙烯酸溶液15.0ml与步骤1)所得羧甲基壳聚糖溶液10.0ml和步骤2)所得纳米银溶液0.9ml混合，向所得混合溶液中加入氯化铁0.375g与引发剂过硫酸铵0.00375g，搅拌均匀，在40℃下反应10h，溶液变成弹性的水凝胶，形成PAA/CMCS双网络水凝胶；4) Mix 15.0 ml of acrylic acid solution in step (3) with 10.0 ml of carboxymethyl chitosan solution obtained in step 1) and 0.9 ml of nano-silver solution obtained in step 2), and add 0.375 g of ferric chloride to the resulting mixed solution and trigger the solution. Add 0.00375 g of ammonium persulfate as the agent, stir evenly, and react at 40 °C for 10 h, the solution becomes an elastic hydrogel, forming a PAA/CMCS double network hydrogel;
5)将氧化葡聚糖加入去离子水溶解，形成15.0g/ml氧化葡聚糖溶液。5) The oxidized dextran was dissolved in deionized water to form a 15.0 g/ml oxidized dextran solution.
6)将步骤4)所得的PAA/CMCS双网络水凝胶置于步骤5)所得的氧化葡聚糖溶液4.0ml中，在25℃下反应1h，得到具有吸湿、抗压和抗菌性能的水凝胶。6) Place the PAA/CMCS double network hydrogel obtained in step 4) in 4.0 ml of the oxidized dextran solution obtained in step 5), and react at 25° C. for 1 h to obtain water with moisture absorption, pressure resistance and antibacterial properties. gel.
将本实施例所得到的水凝胶进行剥离力和压缩回弹测试，通过万能拉力机试验机测得剥离强度为25.6g·cm-1，压缩强度为95.44KPa(压缩形变为60％)。The hydrogel obtained in this example was tested for peel force and compression rebound, and the peel strength was 25.6 g·cm-1 and the compressive strength was 95.44KPa (compression deformation was 60%) measured by a universal tensile tester.
将本实施例所得到的水凝胶进行生物相容性测试，细胞存活率为135.0％。The hydrogel obtained in this example was tested for biocompatibility, and the cell survival rate was 135.0%.
将本实施例所得到的水凝胶进行溶胀吸湿性能测试，温度控制在36℃进行溶胀实验，时间40min，溶胀率为121％。The hydrogel obtained in this example was subjected to a swelling and moisture absorption performance test, the temperature was controlled at 36° C. to carry out a swelling test, the time was 40 minutes, and the swelling rate was 121%.
实施例3Example 3
制备具有吸湿、抗压和抗菌性能的水凝胶的制备方法，具体步骤为：A preparation method for preparing a hydrogel with moisture absorption, compression resistance and antibacterial properties, the specific steps are:
1)将羧甲基壳聚糖加入去离子水溶解,形成2.50g/ml的羧甲基壳聚糖溶液；1) Dissolving carboxymethyl chitosan in deionized water to form a carboxymethyl chitosan solution of 2.50 g/ml;
2)将纳米银加入去离子水溶解，形成0.10g/ml纳米银溶液；2) adding the nano-silver into deionized water to dissolve to form a 0.10g/ml nano-silver solution;
3)将丙烯酸加入去离子水中溶解，形成4.60g/ml丙烯酸溶液；3) adding acrylic acid to deionized water and dissolving to form 4.60g/ml acrylic acid solution;
4)将步骤(3)丙烯酸溶液22.0ml与步骤1)所得羧甲基壳聚糖溶液10.0ml和步骤2)所得纳米银溶液0.625ml混合，向所得混合溶液中加入氯化铁0.631g与引发剂过硫酸铵0.00631g，搅拌均匀，在40℃下反应10h，溶液变成弹性的水凝胶，形成PAA/CMCS双网络水凝胶；4) Mix 22.0 ml of acrylic acid solution in step (3) with 10.0 ml of carboxymethyl chitosan solution obtained in step 1) and 0.625 ml of nano-silver solution obtained in step 2), add 0.631 g of ferric chloride to the obtained mixed solution and trigger the solution. Add 0.00631 g of ammonium persulfate as the agent, stir evenly, and react at 40 °C for 10 h, the solution becomes an elastic hydrogel, forming a PAA/CMCS double network hydrogel;
5)将氧化葡聚糖加入去离子水溶解，形成18g/ml氧化葡聚糖溶液；5) adding the oxidized glucan into deionized water to dissolve to form a 18g/ml oxidized glucan solution;
6)将步骤4)所得的PAA/CMCS双网络水凝胶置于步骤5)所得的氧化葡聚糖溶液6.9ml中，在25℃下反应1h，得到具有吸湿、抗压和抗菌性能的水凝胶。6) The PAA/CMCS double network hydrogel obtained in step 4) was placed in 6.9 ml of the oxidized dextran solution obtained in step 5), and reacted at 25° C. for 1 h to obtain water with moisture absorption, pressure resistance and antibacterial properties. gel.
将本实施例所得到的水凝胶进行剥离力和压缩回弹测试，通过万能拉力机试验机测得剥离强度为27.8g·cm-1，压缩强度为92.56KPa(压缩形变为60％)。The hydrogel obtained in this example was tested for peel force and compression rebound, and the peel strength was 27.8 g·cm-1 and the compressive strength was 92.56 KPa (compression deformation was 60%) measured by a universal tensile tester.
将本实施例所得到的水凝胶进行生物相容性测试，细胞存活率为130.0％。The hydrogel obtained in this example was tested for biocompatibility, and the cell survival rate was 130.0%.
将本实施例所得到的水凝胶进行溶胀吸湿性能测试，温度控制在36℃进行溶胀实验，时间40min，溶胀率为119％。The hydrogel obtained in this example was subjected to the swelling and moisture absorption performance test, the temperature was controlled at 36° C. to carry out the swelling test, the time was 40 minutes, and the swelling rate was 119%.
实施例4Example 4
制备具有吸湿、抗压和抗菌性能的水凝胶的制备方法，具体步骤为：A preparation method for preparing a hydrogel with moisture absorption, compression resistance and antibacterial properties, the specific steps are:
1)将羧甲基壳聚糖加入去离子水溶解,形成0.08g/ml的羧甲基壳聚糖溶液；1) Add carboxymethyl chitosan to deionized water to dissolve to form 0.08g/ml carboxymethyl chitosan solution;
2)将纳米银加入去离子水溶解，形成0.10g/ml纳米银溶液；2) adding the nano-silver into deionized water to dissolve to form a 0.10g/ml nano-silver solution;
3)将丙烯酸加入去离子水中溶解，形成0.10g/ml丙烯酸溶液；3) adding acrylic acid to deionized water to dissolve, forming 0.10g/ml acrylic acid solution;
4)将步骤(3)丙烯酸溶液64ml与步骤1)所得羧甲基壳聚糖溶液20ml和步骤2)所得纳米银溶液0.32ml混合，向所得混合溶液中加入氯化铁0.04g与引发剂过硫酸铵0.0004g，搅拌均匀，在50℃下反应12h，溶液变成弹性的水凝胶，形成PAA/CMCS双网络水凝胶；4) 64ml of acrylic acid solution in step (3) is mixed with 20ml of carboxymethyl chitosan solution obtained in step 1) and 0.32ml of nano-silver solution obtained in step 2), and 0.04g of ferric chloride and an initiator are added to the obtained mixed solution. Ammonium sulfate 0.0004g, stirred evenly, reacted at 50°C for 12h, the solution became an elastic hydrogel, forming a PAA/CMCS double network hydrogel;
5)将氧化葡聚糖加入去离子水溶解，形成4.0g/ml氧化葡聚糖溶液；5) adding the oxidized glucan into deionized water to dissolve to form a 4.0g/ml oxidized glucan solution;
6)将步骤4)所得的PAA/CMCS双网络水凝胶置于步骤5)所得的氧化葡聚糖溶液0.8ml中，在40℃下反应2h，得到具有吸湿、抗压和抗菌性能的水凝胶。6) The PAA/CMCS double network hydrogel obtained in step 4) was placed in 0.8 ml of the oxidized dextran solution obtained in step 5), and reacted at 40° C. for 2 h to obtain water with moisture absorption, pressure resistance and antibacterial properties. gel.
将本实施例所得到的水凝胶进行剥离力和压缩回弹测试，通过万能拉力机试验机测得剥离强度为19.8g·cm-1，压缩强度为89.51KPa(压缩形变为60％)。The hydrogel obtained in this example was tested for peel force and compression rebound, and the peel strength was 19.8 g·cm-1 and the compressive strength was 89.51 KPa (compression deformation was 60%) measured by a universal tensile tester.
将本实施例所得到的水凝胶进行生物相容性测试，细胞存活率为124.0％。The hydrogel obtained in this example was tested for biocompatibility, and the cell survival rate was 124.0%.
将本实施例所得到的水凝胶进行溶胀吸湿性能测试，温度控制在36℃进行溶胀实验，时间40min，溶胀率为118％。The hydrogel obtained in this example was subjected to a swelling and moisture absorption performance test, the temperature was controlled at 36° C. to carry out a swelling test, the time was 40 minutes, and the swelling rate was 118%.
实施例5Example 5
制备具有吸湿、抗压和抗菌性能的水凝胶，具体步骤为：To prepare a hydrogel with hygroscopic, anti-pressure and antibacterial properties, the specific steps are:
1)将羧甲基壳聚糖加入去离子水溶解,形成3.00g/ml的羧甲基壳聚糖溶液。1) Dissolve carboxymethyl chitosan in deionized water to form a 3.00 g/ml carboxymethyl chitosan solution.
2)将纳米银加入去离子水溶解，形成0.05g/ml纳米银溶液。2) The nano-silver is added into deionized water to dissolve to form a 0.05g/ml nano-silver solution.
3)将丙烯酸加入去离子水中溶解，形成4.00g/ml丙烯酸溶液；3) adding acrylic acid to deionized water to dissolve, forming 4.00g/ml acrylic acid solution;
4)将步骤(3)丙烯酸溶液6.00ml与步骤(1)所得羧甲基壳聚糖溶液2.00ml和步骤(2)所得纳米银溶液0.0625ml混合，向所得混合溶液中加入氯化铁0.15g与引发剂过硫酸铵0.0015g，搅拌均匀，在50℃下反应12h，溶液变成弹性的水凝胶，形成PAA/CMCS双网络水凝胶。4) Mix 6.00 ml of acrylic acid solution in step (3) with 2.00 ml of carboxymethyl chitosan solution obtained in step (1) and 0.0625 ml of nano-silver solution obtained in step (2), and add 0.15 g of ferric chloride to the resulting mixed solution Add 0.0015 g of ammonium persulfate as an initiator, stir evenly, and react at 50 °C for 12 h. The solution turns into an elastic hydrogel to form a PAA/CMCS double network hydrogel.
5)将氧化葡聚糖加入去离子水溶解，形成5g/ml氧化葡聚糖溶液。5) The oxidized dextran was added to deionized water to dissolve to form a 5g/ml oxidized dextran solution.
6)将步骤4)所得的PAA/CMCS双网络水凝胶置于步骤5)所得的氧化葡聚糖溶液2.4ml中，在25℃下反应1h，得到具有吸湿、抗压和抗菌性能的水凝胶。6) Place the PAA/CMCS double network hydrogel obtained in step 4) in 2.4 ml of the oxidized dextran solution obtained in step 5), and react at 25° C. for 1 h to obtain water with moisture absorption, pressure resistance and antibacterial properties. gel.
实施例6Example 6
制备具有吸湿、抗压和抗菌性能的水凝胶，具体步骤为：To prepare a hydrogel with hygroscopic, anti-pressure and antibacterial properties, the specific steps are:
1)将羧甲基壳聚糖加入去离子水溶解,形成1.00g/ml的羧甲基壳聚糖溶液。1) Dissolve carboxymethyl chitosan in deionized water to form a 1.00g/ml carboxymethyl chitosan solution.
2)将纳米银加入去离子水溶解，形成0.04g/ml纳米银溶液。2) The nano-silver was added into deionized water to dissolve to form a 0.04g/ml nano-silver solution.
3)将丙烯酸加入去离子水中溶解，形成4.00g/ml丙烯酸溶液；3) adding acrylic acid to deionized water to dissolve, forming 4.00g/ml acrylic acid solution;
4)将步骤(3)丙烯酸溶液2.00ml与步骤(1)所得羧甲基壳聚糖溶液1.00ml和步骤(2)所得纳米银溶液0.2ml混合，向所得混合溶液中加入氯化铁0.045g与引发剂过硫酸钾0.00225g，搅拌均匀，在40℃下反应10h，溶液变成弹性的水凝胶，形成PAA/CMCS双网络水凝胶。4) Mix 2.00ml of acrylic acid solution in step (3) with 1.00ml of carboxymethyl chitosan solution obtained in step (1) and 0.2ml of nano-silver solution obtained in step (2), and add 0.045g of ferric chloride to the resulting mixed solution Add 0.00225 g of potassium persulfate as an initiator, stir evenly, and react at 40 °C for 10 h, the solution becomes an elastic hydrogel, forming a PAA/CMCS double network hydrogel.
5)将氧化葡聚糖加入去离子水溶解，形成8g/ml氧化葡聚糖溶液。5) The oxidized dextran was dissolved in deionized water to form an 8 g/ml oxidized dextran solution.
6)将步骤4)所得的PAA/CMCS双网络水凝胶置于步骤5)所得的氧化葡聚糖溶液1ml中，在25℃下反应1h，得到具有吸湿、抗压和抗菌性能的水凝胶。6) Place the PAA/CMCS double network hydrogel obtained in step 4) in 1 ml of the oxidized dextran solution obtained in step 5), and react at 25° C. for 1 h to obtain a hydrogel with moisture absorption, pressure resistance and antibacterial properties. glue.
实施例7Example 7
如图1,2所示一种口罩，其包括口罩1，口罩上的耳带2，口罩边缘上固定有水凝胶贴片材料3。As shown in Figures 1 and 2, a mask includes a
实施例8Example 8
一种医用护目镜，医用护目镜边缘上固定有水凝胶贴片材料。The utility model relates to medical goggles, wherein a hydrogel patch material is fixed on the edge of the medical goggles.
试验例Test example
本发明通过调控基材、交联剂的配比进而制备出具有吸湿性、弹性以及长效粘附性的功能性水凝胶贴片，按照表1配料进行制备。The present invention prepares a functional hydrogel patch with hygroscopicity, elasticity and long-term adhesion by adjusting the ratio of the base material and the cross-linking agent, and prepares according to the ingredients in Table 1.
表1Table 1
本发明羧甲基壳聚糖和丙烯酸比例对水凝胶影响较大，按照羧甲基壳聚糖：丙烯酸按照1:3-1:6配比使用，其1:4-5的效果好，尤其是1:5的效果最优。(序号1-5)。The ratio of carboxymethyl chitosan and acrylic acid in the present invention has a great influence on the hydrogel. According to the ratio of carboxymethyl chitosan and acrylic acid to 1:3-1:6, the effect of 1:4-5 is good. Especially the 1:5 effect is the best. (No. 1-5).
本发明的交联剂按照0.3-0.5％的基材量进行配比，最佳0.5％，交联后的水凝胶弹性和粘附性效果好。(序号4)。The cross-linking agent of the present invention is proportioned according to the amount of the base material in the range of 0.3-0.5%, and the optimum amount is 0.5%, and the cross-linked hydrogel has good elasticity and adhesion. (No. 4).
本发明为了增强抗菌性，在水凝胶中增加纳米银，抗菌性增强，与PAA/CMCS双网络水凝胶产生协同抗菌的效果。尤其是纳米银0.01％-0.1％内抗菌性最好，超过0.1％，其抗菌性降低。(序号8)In order to enhance the antibacterial property of the invention, nano silver is added in the hydrogel, the antibacterial property is enhanced, and the synergistic antibacterial effect is produced with the PAA/CMCS double network hydrogel. In particular, nano-silver has the best antibacterial property within 0.01%-0.1%, and if it exceeds 0.1%, its antibacterial property decreases. (No. 8)
本发明在与PAA/CMCS双网络水凝胶配合氧化葡聚糖增加粘性，产生协同作用。可见，本发明的氧化葡聚糖添加量是羧甲基壳聚糖的4-5倍时，粘性最好(序号11,12)。The invention cooperates with PAA/CMCS double network hydrogel with oxidized glucan to increase viscosity and produce synergistic effect. It can be seen that when the added amount of oxidized glucan of the present invention is 4-5 times that of carboxymethyl chitosan, the viscosity is the best (Nos. 11, 12).
通过表1可见，本发明的PAA/CMCS双网络水凝胶增加了纳米银和氧化葡聚糖，其无论是抗菌性和吸湿性及粘性有有大幅度的增加。本发明的最佳的配比组合为羧甲基壳聚糖：丙烯酸氯化铁为1:4-5，交联剂为基材量的0.5％，纳米银0.01％-0.1％，氧化葡聚糖添加量是羧甲基壳聚糖的4-5倍制备得到的PAA/CMCS双网络水凝胶的抗菌性、吸湿性、粘性、弹性是最好的。最佳PAA/CMCS双网络水凝胶是由羧甲基壳聚糖、丙烯酸、Fe3+为交联剂，引发剂、纳米银和氧化葡聚糖按照2:10:0.06:0.003：0.012：10制备得到的。It can be seen from Table 1 that the PAA/CMCS double network hydrogel of the present invention has increased nano-silver and oxidized dextran, and its antibacterial property, hygroscopicity and viscosity are greatly increased. The best combination of the present invention is carboxymethyl chitosan: ferric chloride of acrylic acid is 1:4-5, the crosslinking agent is 0.5% of the amount of the base material, the nano-silver is 0.01%-0.1%, the oxidized dextran The antibacterial, hygroscopic, viscous and elastic properties of the PAA/CMCS double network hydrogel prepared with the sugar addition amount being 4-5 times that of carboxymethyl chitosan were the best. The optimal PAA/CMCS double network hydrogel is composed of carboxymethyl chitosan, acrylic acid, Fe3+ as cross-linking agent, initiator, nano-silver and oxidized dextran according to 2:10:0.06:0.003:0.012: 10 were prepared.
最后应说明的是：以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, but not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that it can still be The technical solutions described in the foregoing embodiments are modified, or some technical features thereof are equivalently replaced; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
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| US5013769A (en)* | 1988-08-22 | 1991-05-07 | Medipro Sciences Limited | Method of making a hydrogel-forming wound dressing or skin coating material |
| CN109054051A (en)* | 2018-06-25 | 2018-12-21 | 浙江大学 | A kind of tough selfreparing physical hydrogel of height and preparation method thereof based on dual ion coordination |
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