CN107163866B - Medical ultraviolet-curing water-based conductive pressure-sensitive adhesive - Google Patents
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
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- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/314—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive layer and/or the carrier being conductive
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Abstract
Description
技术领域technical field
本发明属于高分子材料技术领域,具体为一种医用紫外光固化水性导电压敏胶。The invention belongs to the technical field of polymer materials, in particular to a medical UV-curable water-based conductive voltage-sensitive adhesive.
背景技术Background technique
近年来,电子医学装置如高阻抗的肌电图仪、心电图仪、胃电图仪、电刺激仪和高频电刀等广泛用于诊断和治疗疾病,它们用电极和人体表皮接触,在仪器上反映人体的生物电信号,因此就需要电极具有导电性并能和人体表皮紧密接触。导电压敏胶既是压敏型的,又具有导电性,是在无溶剂存在下通过指压而活化的始终保持粘性的黏弹性材料。在用力较轻的指压条件下,胶面即可瞬间与人体皮肤表面相粘,与医疗专用设备组合后,能很好地传递电流信号。由于其具有良好的内聚力和不干性,使用结束可方便地与皮肤剥离,且在皮肤表面不留下残留物,因此具有广阔的应用前景。In recent years, electronic medical devices such as high-impedance electromyography, electrocardiograph, gastroenterograph, electrical stimulator, and high-frequency electrosurgery have been widely used in the diagnosis and treatment of diseases. It reflects the bioelectrical signals of the human body, so the electrodes are required to be conductive and to be in close contact with the human epidermis. Conductive pressure-sensitive adhesives are both pressure-sensitive and conductive, and are viscoelastic materials that are activated by finger pressure in the absence of solvents and remain viscous. Under the condition of light acupressure, the adhesive surface can be instantly adhered to the surface of human skin, and when combined with special medical equipment, it can transmit current signals well. Due to its good cohesion and non-drying properties, it can be easily peeled off from the skin at the end of use and leaves no residue on the skin surface, so it has broad application prospects.
但是现有的导电压敏胶制作过程不够环保,成品具有一定的细胞毒性和致敏性环保,从而一定程度上限制了导电压敏胶的应用。However, the existing conductive voltage-sensitive adhesive manufacturing process is not environmentally friendly enough, and the finished product has certain cytotoxicity and sensitization environmental protection, which limits the application of the conductive voltage-sensitive adhesive to a certain extent.
发明内容SUMMARY OF THE INVENTION
为解决现有技术存在的导电压敏胶制作过程不环保,成品具有一定的细胞毒性和致敏性环保,从而一定程度上限制了导电压敏胶的应用的缺陷,本发明提供一种医用紫外光固化水性导电压敏胶。In order to solve the problems in the prior art that the production process of the conductive voltage-sensitive adhesive is not environmentally friendly, and the finished product has certain cytotoxicity and sensitization environmental protection, thus limiting the application of the conductive voltage-sensitive adhesive to a certain extent, the present invention provides a medical ultraviolet Light-curing water-based conductive voltage-sensitive adhesive.
一种医用紫外光固化水性导电压敏胶,采用以下步骤制备:A medical UV-curable water-based conductive voltage-sensitive adhesive is prepared by the following steps:
1)、将水溶性高分子材料如羧甲基纤维素钠或羟乙基纤维素等隔夜充分溶解在水里或将壳聚糖溶解在体积比为1%的醋酸溶液中,获得质量浓度为1-10%的水溶液;1), fully dissolve water-soluble polymer materials such as sodium carboxymethyl cellulose or hydroxyethyl cellulose in water overnight or dissolve chitosan in an acetic acid solution with a volume ratio of 1% to obtain a mass concentration of 1-10% aqueous solution;
2)、取上述溶液10-50mL加入丙烯酸5-30g、丙烯酸羟丙酯1-20g、交联剂0.1-1、光引发剂0.1-2.0、丙三醇5-30g和氢氧化钠0.1-1.0g,搅拌均匀至全部溶解;2), get the above solution 10-50mL and add acrylic acid 5-30g, hydroxypropyl acrylate 1-20g, crosslinking agent 0.1-1, photoinitiator 0.1-2.0, glycerol 5-30g and sodium hydroxide 0.1-1.0 g, stir until all dissolved;
3)、采用漆膜涂布器进行涂布,获得厚度为1.0-2.0mm的湿膜;3), use a paint film applicator to coat to obtain a wet film with a thickness of 1.0-2.0 mm;
4)、将上述湿膜放置于紫外线固化机灯管下方10-40cm处,辐照5-120秒后取出得到所述水性导电性压敏胶。4), place the above wet film at 10-40 cm below the lamp tube of the ultraviolet curing machine, and take it out after irradiating for 5-120 seconds to obtain the water-based conductive pressure-sensitive adhesive.
进一步的,所述的交联剂为三羟甲基丙烷三甲基丙烯酸酯等水溶性的交联剂。Further, the cross-linking agent is a water-soluble cross-linking agent such as trimethylolpropane trimethacrylate.
进一步的,所述的光引发剂为Irgacure系列水溶性的引发剂。Further, the photoinitiator is an Irgacure series water-soluble initiator.
进一步的,所述紫外线固化机为功率为500-2000W的冷光型紫外线固化机。所述紫外线固化机灯管为高压汞灯。Further, the ultraviolet curing machine is a cold light type ultraviolet curing machine with a power of 500-2000W. The lamp tube of the ultraviolet curing machine is a high pressure mercury lamp.
有益效果:本发明全部原料均为水溶性,以水为溶剂,减少了环境污染及产品的体外细胞毒性和致敏性;以纤维素基质或壳聚糖基质,天然环保,并且有利于调节压敏胶的涂布粘度;采用水性光引发剂,有利于避免油溶性引发剂分解后产生的恶臭气味;利用UV光辐照快速固化,固化速度极快,产品生产效率极高。Beneficial effects: all the raw materials of the present invention are water-soluble, and water is used as the solvent, which reduces environmental pollution and the in vitro cytotoxicity and sensitization of the product; the cellulose matrix or the chitosan matrix is natural and environmentally friendly, and is conducive to regulating pressure. The coating viscosity of the sensitive adhesive; the use of water-based photoinitiator is beneficial to avoid the bad smell generated by the decomposition of the oil-soluble initiator; the use of UV light irradiation to quickly cure, the curing speed is extremely fast, and the product production efficiency is extremely high.
具体实施方式Detailed ways
实施例1Example 1
将将壳聚糖溶解在体积比为1%的醋酸溶液中,获得质量浓度为2%的水溶液。(2)取上述溶液40mL加入丙烯酸30g,丙烯酸羟丙酯15g,交联剂0.7g,光引发剂0.8g,丙三醇30g,氢氧化钠0.8g,搅拌均匀直至固体全部溶解。(3)采用漆膜涂布器进行涂布,获得厚度为2.0mm的湿膜。(4)将湿膜放置于功率为2000W的冷光型紫外线固化机灯管下方30cm处,辐照50秒后取出得到具有导电性的压敏胶。Chitosan was dissolved in an acetic acid solution with a volume ratio of 1% to obtain an aqueous solution with a mass concentration of 2%. (2) Take 40 mL of the above solution, add 30 g of acrylic acid, 15 g of hydroxypropyl acrylate, 0.7 g of crosslinking agent, 0.8 g of photoinitiator, 30 g of glycerol, and 0.8 g of sodium hydroxide, and stir until all solids are dissolved. (3) Coating with a paint film coater to obtain a wet film with a thickness of 2.0 mm. (4) Place the wet film at 30 cm below the lamp tube of a cold light type ultraviolet curing machine with a power of 2000W, and take it out after irradiating for 50 seconds to obtain a conductive pressure-sensitive adhesive.
实施例2Example 2
(1)将水溶性高分子材料如羧甲基纤维素钠隔夜充分溶解在水里获得质量浓度为3%的水溶液。(2)取上述溶液20mL加入丙烯酸10g,丙烯酸羟丙酯10g,交联剂0.5g,光引发剂0.4g,丙三醇20g,氢氧化钠0.2g,搅拌均匀直至固体全部溶解。(3)采用漆膜涂布器进行涂布,获得厚度为1.0mm的湿膜。(4)将湿膜放置于功率为1000W的冷光型紫外线固化机灯管下方20cm处,辐照80秒后取出得到具有导电性的压敏胶。(1) A water-soluble polymer material such as sodium carboxymethyl cellulose is fully dissolved in water overnight to obtain an aqueous solution with a mass concentration of 3%. (2) Take 20 mL of the above solution, add 10 g of acrylic acid, 10 g of hydroxypropyl acrylate, 0.5 g of crosslinking agent, 0.4 g of photoinitiator, 20 g of glycerol, and 0.2 g of sodium hydroxide, and stir until all solids are dissolved. (3) Coating with a paint film applicator to obtain a wet film with a thickness of 1.0 mm. (4) The wet film is placed 20 cm below the lamp tube of a cold light type ultraviolet curing machine with a power of 1000W, and after irradiating for 80 seconds, it is taken out to obtain a conductive pressure-sensitive adhesive.
实施例3Example 3
(1)将水溶性高分子材料羟乙基纤维素隔夜充分溶解在水里,获得质量浓度为5%的水溶液。(2)取上述溶液30mL加入丙烯酸15g,丙烯酸羟丙酯20g,交联剂0.7g,光引发剂0.6g,丙三醇25g,氢氧化钠0.4g,搅拌均匀直至固体全部溶解。(3)采用漆膜涂布器进行涂布,获得厚度为1.5mm的湿膜。(4)将湿膜放置于功率为1500W的冷光型紫外线固化机灯管下方25cm处,辐照60秒后取出得到具有导电性的压敏胶。(1) The water-soluble polymer material hydroxyethyl cellulose is fully dissolved in water overnight to obtain an aqueous solution with a mass concentration of 5%. (2) Take 30 mL of the above solution, add 15 g of acrylic acid, 20 g of hydroxypropyl acrylate, 0.7 g of crosslinking agent, 0.6 g of photoinitiator, 25 g of glycerol, and 0.4 g of sodium hydroxide, and stir until all solids are dissolved. (3) Coating with a paint film applicator to obtain a wet film with a thickness of 1.5 mm. (4) Place the wet film at 25 cm below the lamp tube of a cold light type ultraviolet curing machine with a power of 1500W, and take it out after irradiating for 60 seconds to obtain a conductive pressure-sensitive adhesive.
实施例4Example 4
(1)将将壳聚糖溶解在体积比为1%的醋酸溶液中,获得质量浓度为1%的水溶液。(2)取上述溶液10mL加入丙烯酸5g,丙烯酸羟丙酯1g,交联剂0.1g,光引发剂0.1g,丙三醇5g,氢氧化钠0.1g,搅拌均匀直至固体全部溶解。(3)采用漆膜涂布器进行涂布,获得厚度为1.0mm的湿膜。(4)将湿膜放置于功率为500W的冷光型紫外线固化机灯管下方10cm处,辐照5秒后取出得到具有导电性的压敏胶。(1) Dissolving chitosan in an acetic acid solution with a volume ratio of 1% to obtain an aqueous solution with a mass concentration of 1%. (2) Take 10 mL of the above solution, add 5 g of acrylic acid, 1 g of hydroxypropyl acrylate, 0.1 g of crosslinking agent, 0.1 g of photoinitiator, 5 g of glycerol, and 0.1 g of sodium hydroxide, and stir until all the solids are dissolved. (3) Coating with a paint film applicator to obtain a wet film with a thickness of 1.0 mm. (4) The wet film is placed 10 cm below the lamp tube of a cold light type ultraviolet curing machine with a power of 500 W, and after irradiating for 5 seconds, the pressure-sensitive adhesive with conductivity is taken out.
实施例5Example 5
将将羟乙基纤维素溶解隔夜充分溶解在水里,获得质量浓度为10%的水溶液。(2)取上述溶液50mL加入丙烯酸30g,丙烯酸羟丙酯20g,交联剂1g,光引发剂2.0g,丙三醇30g,氢氧化钠1g,搅拌均匀直至固体全部溶解。(3)采用漆膜涂布器进行涂布,获得厚度为2.0mm的湿膜。(4)将湿膜放置于功率为2000W的冷光型紫外线固化机灯管下方40cm处,辐照120秒后取出得到具有导电性的压敏胶。The hydroxyethyl cellulose was fully dissolved in water overnight to obtain an aqueous solution with a mass concentration of 10%. (2) Take 50 mL of the above solution and add 30 g of acrylic acid, 20 g of hydroxypropyl acrylate, 1 g of crosslinking agent, 2.0 g of photoinitiator, 30 g of glycerol, and 1 g of sodium hydroxide, and stir until all solids are dissolved. (3) Coating with a paint film coater to obtain a wet film with a thickness of 2.0 mm. (4) The wet film is placed 40 cm below the lamp tube of a cold light type ultraviolet curing machine with a power of 2000W, and after irradiating for 120 seconds, it is taken out to obtain a conductive pressure-sensitive adhesive.
为验证本发明的医用紫外光固化水性导电压敏胶的性能,做以下测试:In order to verify the performance of the medical UV-curable water-based conductive voltage-sensitive adhesive of the present invention, the following tests were done:
1、电接触性能的测定1. Determination of electrical contact performance
将实施例1-5制得的医用紫外光固化水性导电压敏胶涂覆在铝箔上形成极板,然后将极板全部面积稳固的置于20cm×30cm的金属平板上,采用精密LCR测量仪测定频率为1000kHz下的交流阻抗。结果见表1。The medical UV-curable water-based conductive voltage-sensitive adhesive prepared in Examples 1-5 was coated on aluminum foil to form a pole plate, and then the entire area of the pole plate was firmly placed on a 20cm×30cm metal plate, and a precision LCR measuring instrument was used. AC impedance was measured at a frequency of 1000 kHz. The results are shown in Table 1.
2、持粘力测试2. Adhesion test
将实施例1-5制得的医用紫外光固化水性导电压敏胶涂覆在铝箔上形成极板,然后按照GB/T4851-2014进行测试,将事先裁剪好的25mm×60mm的样品贴在试验板表面,并进行滚压贴合。在1min内,先将整个试验样件轻轻放在试验架上,使试样的自由端垂直,再将砝码轻轻施加到夹具上。记录试样从试验板上完全分离所需的时间。结果见表1。The medical UV-curable water-based conductive voltage-sensitive adhesive prepared in Examples 1-5 was coated on aluminum foil to form a polar plate, and then tested according to GB/T4851-2014, and the pre-cut 25mm × 60mm sample was attached to the test. The surface of the board is rolled and bonded. Within 1min, first place the entire test specimen lightly on the test stand, so that the free end of the specimen is vertical, and then lightly apply the weight to the fixture. Record the time required for the specimen to completely separate from the test plate. The results are shown in Table 1.
3、180°剥离强度测试3. 180° peel strength test
将实施例1-5制得的医用紫外光固化水性导电压敏胶涂覆在铝箔上形成极板,然后按照GB/T2792-2014进行测试,剥离速度为300mm/min,记录下平均剥离力。结果见表1:The medical UV-curable water-based conductive voltage-sensitive adhesive prepared in Examples 1-5 was coated on aluminum foil to form a polar plate, and then tested according to GB/T2792-2014, the peeling speed was 300mm/min, and the average peeling force was recorded. The results are shown in Table 1:
表1实施例1-5的性能测试结果Table 1 Performance test results of Examples 1-5
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Application publication date: 20170915 Assignee: CHANGZHOU HOK SEAL MATERIAL Co.,Ltd. Assignor: JIANGSU University OF TECHNOLOGY Contract record no.: X2024980017576 Denomination of invention: A medical UV curable water-based conductive pressure-sensitive adhesive Granted publication date: 20200915 License type: Common License Record date: 20241009 |
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