CN105669172A - 环保型日用陶瓷及其制备方法 - Google Patents
环保型日用陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种环保型日用陶瓷,包括以下重量份的组分:水30~60份、SiO275~120份、Al2O35~12份、中药提取物0.1~0.96份、TiO24.1~6.8份、CaCO32~10份、B2O35~9份、Na2SiO35~10份、ZnO1~6份、CuO1~4份、MnO1~4份、CeO21~6份、Li2O1~3份、BaO4~12份、Fe2O30.5~5份、MgO1~3份、羧甲基纤维素钠0.5~1.2份、聚丙烯酰胺0.1~3份。本发明的陶瓷釉料能很快达到抗菌效果,起效快,且抗菌性能够较长时间保持。
Description
技术领域
本发明涉及一种陶瓷,具体涉及一种环保型日用陶瓷及其制备方法。属于陶瓷技术领域。
背景技术
陶瓷是以天然粘土以及各种天然矿物为主要原料经过粉碎混炼、成型和煅烧制得的材料的各种制品。随着经济社会的高速发展,人们的生活质量日益提高,且消费观念也不断转变,在陶瓷制品的选择上,不单单会关注其实用性、艺术性和观赏性,还对其功能性提出了更高的要求,特别是对抗菌性的需求更是越来越高。具有抗菌功能的陶瓷制品,它是在陶瓷制品生产过程中,加入无机抗菌剂,从而使陶瓷表面具有抗菌作用的一种新型功能陶瓷。抗菌陶瓷作为功能性陶瓷产品,能够有效避免各种传染疾病对人类的侵害,特别是公共场所的卫生预防。目前的抗菌陶瓷主要是通过添加氧化钛、银、稀土元素或者麦饭石和远红外材料抗菌剂来实现杀菌作用。但是现有的抗菌陶瓷要么生产成本高不利于大范围推广使用,要么对热和光敏感,容易变黑影响浅色陶瓷的外观,最重要的是,抗菌效果均不够理想。
植物野百合为一年生直立草本,高20~100厘米,被紧贴稍长的毛,毛略粗糙。单叶,线形或披针形,叶片大小变化很大,长2.5~8厘米,阔0.5~1厘米,两端狭尖,先端通常有束状毛,上面略被毛或几无毛,下面披丝光质毛;几无叶柄;托叶极细小,刚毛状。总状花序,顶生或腋生,有花2~20朵,花朵密集一起。苞片及小苞片极相似,线形;小苞片着生于花梗上部,均被略粗糙的长毛;花梗极短,结果时下垂:花萼长10~15毫米,密被棕黄色长毛,萼齿先端尖;花冠蝶形,紫蓝色或淡蓝色,约与花萼等长,旗瓣圆形,翼瓣较旗瓣短,倒卵状矩圆形,龙骨瓣与翼瓣等长,内弯,具喙;雄蕊10,单体,花药2型;子房无柄,花柱细长。荚果无毛,长圆形,约与花萼等长;种子10~15颗。花期9月。生于荒地杂草中。分布东北、华东、华南以及西南各地。
芩又名元芩、枯芩,首载于《神农本草经》,为唇形科植物ScutellariabaicalensisGeorgi的干燥根。黄芩味苦、性寒,有清热燥湿、泻火解毒、止血、安胎等功效。主治温热病、上呼吸道感染、肺热咳嗽、湿热黄胆、肺炎、痢疾、咳血、目赤、胎动不安、高血压、痈肿疖疮等症。黄芩是我国中医临床常用中药品种之一,具有悠久的用药历史,主产于河北、山西、内蒙古、辽宁等省区,俄罗斯东西伯利亚,蒙古,朝鲜,日本均有分布。黄芩主要含黄酮类化合物,目前从黄芩中分离的黄酮苷元及苷有40多种。此外黄芩中还含有大量的二萜类化合物和丰富的微量元素(其中铁、铜、锌、锰的含量均很高)
三棱是黑三棱科植物黑三棱SparganiumstoloniferumBuch.-Ham.的干燥块茎,自1977年起,被各版《中国药典》收载。其具有破血行气、消积止痛的功效,为常用破血药;主治癥瘕痞块、瘀血经闭、食积肿胀等证,多用于治疗月经不调、积聚结块。冬季至次年春采挖,洗净,削去外皮,晒干。分布于东北、黄河、流域、长江中下游及西藏。
发明内容
本发明的目的是为克服上述现有技术的不足,提供一种含中草药提取物的抗菌陶瓷。
本发明还提供了该陶瓷的制备方法。
为实现上述目的,本发明采用下述技术方案:
环保型日用陶瓷,包括以下重量份的组分:水30~60份、SiO275~120份、Al2O35~12份、中药提取物0.1~0.96份、TiO24.1~6.8份、CaCO32~10份、B2O35~9份、Na2SiO35~10份、ZnO1~6份、CuO1~4份、MnO1~4份、CeO21~6份、Li2O1~3份、BaO4~12份、Fe2O30.5~5份、MgO1~3份、羧甲基纤维素钠0.5~1.2份、聚丙烯酰胺0.1~3份。
所述中药提取物的制备方法包含以下操作步骤:(a)将黑三棱、野百合、黄芩、的干燥块粉碎,用85~95%乙醇热回流提取,合并提取液,浓缩至无醇味,依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取,分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物;(b)步骤(a)中乙酸乙酯萃取物用大孔树脂除杂,先用10%乙醇洗脱8个柱体积,再用80%乙醇洗脱10个柱体积,收集80%乙醇洗脱液,减压浓缩得80%乙醇洗脱物浸膏;(c)步骤(b)中80%乙醇洗脱浸膏用正相硅胶分离,依次用体积比为75:1、45:1、25:1、15:1和1:1的二氯甲烷-甲醇梯度洗脱得到5个组分;(d)步骤(c)中组分4用正相硅胶进一步分离,依次用体积比为20:1、15:1和8:1的二氯甲烷-甲醇梯度洗脱得到3个组分;(e)步骤(d)中组分2用十八烷基硅烷键合的反相硅胶分离,用体积百分浓度为70%的甲醇水溶液等度洗脱,收集10~12个柱体积洗脱液,洗脱液减压浓缩得到中药提取物,所述黑三棱、野百合、黄芩的重量比为1:2:2~8;所述黑三棱、野百合、黄芩的重量与所述85~95%乙醇的质量体积比为1g:50~200ml。
所述的环保型日用陶瓷的制备方法,其特征在于:包括如下步骤:
(1)将羧甲基纤维素钠、聚丙烯酰胺依据重量份加入到容器中,加入蒸馏水,常温下,充分溶解后,再加入中药提取物,以50-80rpm转速机械搅拌0.5~2h,然后将其倒入球磨罐中;
(2)按配方比依次例加入剩余组份,以80-120rpm转速,球磨3-4h,入模成型制备陶瓷生坯;
(3)将生坯在40-60℃真空干燥0.5-1.5h,将生坯在氮气体保护下于400~650℃下熔炼2~4.5小时,接着在800~1200℃下,熔炼1~2小时,后分别在1000℃和1200℃下交替烧制2~次,每次烧制时间为20分钟,随炉冷却后,得到抗菌陶瓷。
本发明的有益效果:
本发明提供的产品经测试,产品达到国家防静电陶瓷砖标准GB26539-2011要求、《抗菌陶瓷制品抗菌性能》JC/T897-2002的要求。
本发明的抗菌陶瓷以SiO2为基料,添加高岭土、钠基膨润土、珍珠岩粉等辅料,再添加中草药提取物作为抗菌剂,以聚丙烯酰胺粉为粘结剂,调整各组分的含量,意外发现通过本发明配方的协同作用达到明显优于现有技术的抗菌效果。舍弃了含铁或含银的杀菌材料,有效避免了现有抗菌陶瓷对热和光敏感的问题。
本发明的陶瓷能很快达到抗菌效果,起效快,且抗菌性能够较长时间保持。通过本发明的陶瓷釉料制备的陶瓷样品盛放牛奶的最长耐变质时间也是远远优于市场上的普通陶瓷釉料产品(20小时以下)。
具体实施方式
下面结合实施例对本发明进行进一步的阐述,应该说明的是,下述说明仅是为了解释本发明,并不对其内容进行限定。
实施例1:
环保型日用陶瓷,包括以下重量份的组分:水30份、SiO275份、Al2O35份、中药提取物0.1份、TiO24.1份、CaCO32份、B2O35份、Na2SiO35份、ZnO1份、CuO1份、MnO1份、CeO21份、Li2O1份、BaO4份、Fe2O30.5份、MgO1份、羧甲基纤维素钠0.5份、聚丙烯酰胺0.1份。
所述中药提取物的制备方法包含以下操作步骤:(a)将黑三棱、野百合、黄芩、的干燥块粉碎,用85%乙醇热回流提取,合并提取液,浓缩至无醇味,依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取,分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物;(b)步骤(a)中乙酸乙酯萃取物用大孔树脂除杂,先用10%乙醇洗脱8个柱体积,再用80%乙醇洗脱10个柱体积,收集80%乙醇洗脱液,减压浓缩得80%乙醇洗脱物浸膏;(c)步骤(b)中80%乙醇洗脱浸膏用正相硅胶分离,依次用体积比为75:1、45:1、25:1、15:1和1:1的二氯甲烷-甲醇梯度洗脱得到5个组分;(d)步骤(c)中组分4用正相硅胶进一步分离,依次用体积比为20:1、15:1和8:1的二氯甲烷-甲醇梯度洗脱得到3个组分;(e)步骤(d)中组分2用十八烷基硅烷键合的反相硅胶分离,用体积百分浓度为70%的甲醇水溶液等度洗脱,收集10个柱体积洗脱液,洗脱液减压浓缩得到中药提取物,所述黑三棱、野百合、黄芩的重量比为1:2:2;所述黑三棱、野百合、黄芩的重量与所述85~95%乙醇的质量体积比为1g:50ml。
所述的环保型日用陶瓷的制备方法,其特征在于:包括如下步骤:
(1)将羧甲基纤维素钠、聚丙烯酰胺依据重量份加入到容器中,加入蒸馏水,常温下,充分溶解后,再加入中药提取物,以50rpm转速机械搅拌0.5h,然后将其倒入球磨罐中;
(2)按配方比依次例加入剩余组份,以80rpm转速,球磨3h,入模成型制备陶瓷生坯;
(3)将生坯在40℃真空干燥0.5h,将生坯在氮气体保护下于400℃下熔炼2小时,接着在800℃下,熔炼1小时,后分别在1000℃和1200℃下交替烧制2次,每次烧制时间为20分钟,随炉冷却后,得到抗菌陶瓷。
实施例2:
环保型日用陶瓷,包括以下重量份的组分:水60份、SiO2120份、Al2O312份、中药提取物0.96份、TiO26.8份、CaCO310份、B2O39份、Na2SiO310份、ZnO6份、CuO4份、MnO4份、CeO26份、Li2O3份、BaO12份、Fe2O35份、MgO3份、羧甲基纤维素钠1.2份、聚丙烯酰胺3份。
所述中药提取物的制备方法包含以下操作步骤:(a)将黑三棱、野百合、黄芩、的干燥块粉碎,用95%乙醇热回流提取,合并提取液,浓缩至无醇味,依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取,分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物;(b)步骤(a)中乙酸乙酯萃取物用大孔树脂除杂,先用10%乙醇洗脱8个柱体积,再用80%乙醇洗脱10个柱体积,收集80%乙醇洗脱液,减压浓缩得80%乙醇洗脱物浸膏;(c)步骤(b)中80%乙醇洗脱浸膏用正相硅胶分离,依次用体积比为75:1、45:1、25:1、15:1和1:1的二氯甲烷-甲醇梯度洗脱得到5个组分;(d)步骤(c)中组分4用正相硅胶进一步分离,依次用体积比为20:1、15:1和8:1的二氯甲烷-甲醇梯度洗脱得到3个组分;(e)步骤(d)中组分2用十八烷基硅烷键合的反相硅胶分离,用体积百分浓度为70%的甲醇水溶液等度洗脱,收集12个柱体积洗脱液,洗脱液减压浓缩得到中药提取物,所述黑三棱、野百合、黄芩的重量比为1:2:8;所述黑三棱、野百合、黄芩的重量与所述85~95%乙醇的质量体积比为1g:200ml。
所述的环保型日用陶瓷的制备方法,其特征在于:包括如下步骤:
(1)将羧甲基纤维素钠、聚丙烯酰胺依据重量份加入到容器中,加入蒸馏水,常温下,充分溶解后,再加入中药提取物,以80rpm转速机械搅拌2h,然后将其倒入球磨罐中;
(2)按配方比依次例加入剩余组份,以120rpm转速,球磨4h,入模成型制备陶瓷生坯;
(3)将生坯在60℃真空干燥1.5h,将生坯在氮气体保护下于650℃下熔炼4.5小时,接着在1200℃下,熔炼2小时,后分别在1000℃和1200℃下交替烧制3次,每次烧制时间为20分钟,随炉冷却后,得到抗菌陶瓷。
实施例3:
环保型日用陶瓷,包括以下重量份的组分:水:40份、SiO280份、Al2O36份、中药提取物0.2份、TiO24.5份、CaCO33份、B2O36份、Na2SiO36份、ZnO2份、CuO2份、MnO2份、CeO22份、Li2O1.5份、BaO5份、Fe2O31.5份、MgO1.5份、羧甲基纤维素钠0.6份、聚丙烯酰胺0.5份。
所述中药提取物的制备方法包含以下操作步骤:(a)将黑三棱、野百合、黄芩、的干燥块粉碎,用86%乙醇热回流提取,合并提取液,浓缩至无醇味,依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取,分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物;(b)步骤(a)中乙酸乙酯萃取物用大孔树脂除杂,先用10%乙醇洗脱8个柱体积,再用80%乙醇洗脱10个柱体积,收集80%乙醇洗脱液,减压浓缩得80%乙醇洗脱物浸膏;(c)步骤(b)中80%乙醇洗脱浸膏用正相硅胶分离,依次用体积比为75:1、45:1、25:1、15:1和1:1的二氯甲烷-甲醇梯度洗脱得到5个组分;(d)步骤(c)中组分4用正相硅胶进一步分离,依次用体积比为20:1、15:1和8:1的二氯甲烷-甲醇梯度洗脱得到3个组分;(e)步骤(d)中组分2用十八烷基硅烷键合的反相硅胶分离,用体积百分浓度为70%的甲醇水溶液等度洗脱,收集11个柱体积洗脱液,洗脱液减压浓缩得到中药提取物,所述黑三棱、野百合、黄芩的重量比为1:2:3;所述黑三棱、野百合、黄芩的重量与所述85~95%乙醇的质量体积比为1g:100ml。
所述的环保型日用陶瓷的制备方法,其特征在于:包括如下步骤:
(1)将羧甲基纤维素钠、聚丙烯酰胺依据重量份加入到容器中,加入蒸馏水,常温下,充分溶解后,再加入中药提取物,以550rpm转速机械搅拌1.0h,然后将其倒入球磨罐中;
(2)按配方比依次例加入剩余组份,以90rpm转速,球磨3.5h,入模成型制备陶瓷生坯;
(3)将生坯在45℃真空干燥1.0h,将生坯在氮气体保护下于450℃下熔炼2.2小时,接着在900℃下,熔炼1.5小时,后分别在1000℃和1200℃下交替烧制3次,每次烧制时间为20分钟,随炉冷却后,得到抗菌陶瓷。
实施例4:
环保型日用陶瓷,包括以下重量份的组分:水55份、SiO280份、Al2O37份、中药提取物0.55份、TiO25.5份、CaCO36份、B2O37份、Na2SiO38份、ZnO4份、CuO3.5份、MnO3.5份、CeO24.5份、Li2O1.5份、BaO9份、Fe2O34.5份、MgO2.5份、羧甲基纤维素钠0.9份、聚丙烯酰胺2.5份。
所述中药提取物的制备方法包含以下操作步骤:(a)将黑三棱、野百合、黄芩、的干燥块粉碎,用90%乙醇热回流提取,合并提取液,浓缩至无醇味,依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取,分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物;(b)步骤(a)中乙酸乙酯萃取物用大孔树脂除杂,先用10%乙醇洗脱8个柱体积,再用80%乙醇洗脱10个柱体积,收集80%乙醇洗脱液,减压浓缩得80%乙醇洗脱物浸膏;(c)步骤(b)中80%乙醇洗脱浸膏用正相硅胶分离,依次用体积比为75:1、45:1、25:1、15:1和1:1的二氯甲烷-甲醇梯度洗脱得到5个组分;(d)步骤(c)中组分4用正相硅胶进一步分离,依次用体积比为20:1、15:1和8:1的二氯甲烷-甲醇梯度洗脱得到3个组分;(e)步骤(d)中组分2用十八烷基硅烷键合的反相硅胶分离,用体积百分浓度为70%的甲醇水溶液等度洗脱,收集12个柱体积洗脱液,洗脱液减压浓缩得到中药提取物,所述黑三棱、野百合、黄芩的重量比为1:2:6;所述黑三棱、野百合、黄芩的重量与所述85~95%乙醇的质量体积比为1g:150ml。
所述的环保型日用陶瓷的制备方法,其特征在于:包括如下步骤:
(1)将羧甲基纤维素钠、聚丙烯酰胺依据重量份加入到容器中,加入蒸馏水,常温下,充分溶解后,再加入中药提取物,以75rpm转速机械搅拌1.8h,然后将其倒入球磨罐中;
(2)按配方比依次例加入剩余组份,以98rpm转速,球磨4h,入模成型制备陶瓷生坯;
(3)将生坯在40-60℃真空干燥0.5-1.5h,将生坯在氮气体保护下于600℃下熔炼3.2小时,接着在1000℃下,熔炼1.5小时,后分别在1000℃和1200℃下交替烧制2~次,每次烧制时间为20分钟,随炉冷却后,得到抗菌陶瓷。
实施例5:
环保型日用陶瓷,包括以下重量份的组分:水50份、SiO2118份、Al2O39份、中药提取物0.95份、TiO26.5份、CaCO39.8份、B2O35.9份、Na2SiO36.8份、ZnO4.2份、CuO3.8份、MnO3.4份、CeO25.2份、Li2O1.9份、BaO11份、Fe2O34.5份、MgO2.8份、羧甲基纤维素钠1.5份、聚丙烯酰胺0.9份。
中药提取物的制备方法,同实例3。
环保型日用陶瓷的制备方法,同实例3。
实施例6:
环保型日用陶瓷,包括以下重量份的组分:水32份、SiO2148份、Al2O311份、中药提取物0.68份、TiO24.85份、CaCO38.60份、B2O36.3份、Na2SiO35.9份、ZnO4.9份、CuO2.6份、MnO3.9份、CeO21.96份、Li2O2.5份、BaO4.9份、Fe2O34.5份、MgO2.96份、羧甲基纤维素钠1.1份、聚丙烯酰胺1.96份。
中药提取物的制备方法,同实例1。
环保型日用陶瓷的制备方法,同实例1。
试验例1:
采用实施例1~6制备的陶瓷釉料,对陶瓷进行施釉、干燥、烧结。取尺寸大小为5mm×5mm的陶瓷片作为陶瓷试品。产品完成后,再对产品的抗菌性能做抗菌性能检测。抗菌性能检测采用日本JISZ2801:2006标准,具体检测结果见表1。
表1.2小时、24小时、5天后抗菌性能检测结果
从表1可以看出,利用本发明的陶瓷釉料制备的陶瓷试品,在2小时后对大肠杆菌和金黄色葡萄球菌的抗菌率均达到95%以上,24小时后有所下降,5天后抗菌率仍然保持在较高水平,说明本发明的陶瓷釉料能很快达到抗菌效果,起效快,且抗菌性能够较长时间保持。
试验例2:
采用实施例1~6制备的陶瓷釉料制作用于盛放牛奶的陶瓷样品,并将牛奶置于30℃恒温箱中观察乳制品变质情况,分别检测大肠杆菌(检测方法参见国家标准GB/T4789.3)、沙门氏菌(GB/T4789.4)、志贺氏菌(GB/T4789.5)、金黄色葡萄球菌(GB/T4789.10)和霉菌和酵母计数(GB/T4789.15),超出国家标准即为变质。检测结果见表2。
表2.牛奶变质情况
从表2可以看出,本发明的陶瓷釉料制备的陶瓷样品盛放牛奶的最长耐变质时间达到164小时,所有实施例的耐变质时间均在120小时以上,远远优于市场上的普通陶瓷釉料产品(20小时以下)。
表3.抗折强度情况
实施例 | 1 | 2 | 3 | 4 | 5 | 6 |
抗折强度Mpa | 18 | 10 | 16 | 14 | 15 | 20 |
上述虽然对本发明的具体实施方式进行了描述,但并非对本发明保护范围的限制,在本发明的技术方案的基础上,本领域技术人员不需要付出创造性劳动即可做出的各种修改或变形仍在本发明的保护范围以内。
Claims (3)
1.一种环保型日用陶瓷,其特征在于:包括以下重量份的组分:水30~60份、SiO275~120份、Al2O35~12份、中药提取物0.1~0.96份、TiO24.1~6.8份、CaCO32~10份、B2O35~9份、Na2SiO35~10份、ZnO1~6份、CuO1~4份、MnO1~4份、CeO21~6份、Li2O1~3份、BaO4~12份、Fe2O30.5~5份、MgO1~3份、羧甲基纤维素钠0.5~1.2份、聚丙烯酰胺0.1~3份。
2.权利要求1所述的环保型日用陶瓷,其特征在:所述中药提取物的制备方法包含以下操作步骤:(a)将黑三棱、野百合、黄芩、的干燥块粉碎,用85~95%乙醇热回流提取,合并提取液,浓缩至无醇味,依次用石油醚、乙酸乙酯和水饱和的正丁醇萃取,分别得到石油醚萃取物、乙酸乙酯萃取物和正丁醇萃取物;(b)步骤(a)中乙酸乙酯萃取物用大孔树脂除杂,先用10%乙醇洗脱8个柱体积,再用80%乙醇洗脱10个柱体积,收集80%乙醇洗脱液,减压浓缩得80%乙醇洗脱物浸膏;(c)步骤(b)中80%乙醇洗脱浸膏用正相硅胶分离,依次用体积比为75:1、45:1、25:1、15:1和1:1的二氯甲烷-甲醇梯度洗脱得到5个组分;(d)步骤(c)中组分4用正相硅胶进一步分离,依次用体积比为20:1、15:1和8:1的二氯甲烷-甲醇梯度洗脱得到3个组分;(e)步骤(d)中组分2用十八烷基硅烷键合的反相硅胶分离,用体积百分浓度为70%的甲醇水溶液等度洗脱,收集10~12个柱体积洗脱液,洗脱液减压浓缩得到中药提取物,所述黑三棱、野百合、黄芩的重量比为1:2:2~8;所述黑三棱、野百合、黄芩的重量与所述85~95%乙醇的质量体积比为1g:50~200ml。
3.权利要求1所述的环保型日用陶瓷的制备方法,其特征在于:包括如下步骤:
(1)将羧甲基纤维素钠、聚丙烯酰胺依据重量份加入到容器中,加入蒸馏水,常温下,充分溶解后,再加入中药提取物,以50-80rpm转速机械搅拌0.5~2h,然后将其倒入球磨罐中;
(2)按配方比依次例加入剩余组份,以80-120rpm转速,球磨3-4h,入模成型制备陶瓷生坯;
(3)将生坯在40-60℃真空干燥0.5-1.5h,将生坯在氮气体保护下于400~650℃下熔炼2~4.5小时,接着在800~1200℃下,熔炼1~2小时,后分别在1000℃和1200℃下交替烧制2~次,每次烧制时间为20分钟,随炉冷却后,得到抗菌陶瓷。
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