CN111548122B - 一种抗菌精雕石瓷砖及其制备方法 - Google Patents
一种抗菌精雕石瓷砖及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种抗菌精雕石瓷砖及其制备方法,属于瓷砖加工制造技术领域。本发明的抗菌精雕石瓷砖由高岭土、球土、钾长石、瓷土、叶蜡石、覆盖釉料、复合光催化抗菌剂和膨润土经球磨制浆、成型、一次性烧结、喷墨、添加复合光催化抗菌剂施釉、二次烧结、抛光修边制得。添加了利用溶胶‑凝胶法经高温煅烧制成的TiO2/Ag2O复合微球光催化抗菌剂,TiO2和Ag2O所产生的光生空穴和和电子可以互相迁移,降低了光生空穴和电子的复合率,提高了光催化活性,具有比表面积大、光催化反应活性高、抗菌效率高等优点,能长时间稳定发挥抗菌作用。还有良好的空气净化作用,能够有效去除空气中的TVOC等物质。工艺简单、操作简便,适合于规模化生产。
Description
技术领域
本发明属于瓷砖加工制造技术领域,具体涉及一种抗菌精雕石瓷砖及其制备方法。
背景技术
随着生活水平提高,人们对卫生环境的重视程度也越来越高,对抗菌功能的需求进一步扩展到居住环境。建筑陶瓷材料作为人们居住环境不可或缺的产品,其抗菌功能备受关注。在陶瓷抗菌产品中,卫浴占绝大多数,这方面的研究相对较多。随着人们对居住环境卫生的重视程度的提高,陶瓷砖领域在抗菌材料方面的研究成果也在不断增多,因此提高瓷砖的抗菌性能成为本技术领域的关键。
精雕石瓷砖是继瓷片、抛光砖、仿古砖、微晶石瓷砖之后的一种瓷砖新品类,在纹理、色彩、质感、手感以及视觉效果完全达到天然石材的逼真效果,装饰效果优于天然石材。凭借逼真的装饰效果和优越的实用性能赢得了消费者的青睐,精雕石瓷砖已发展成为瓷砖领域的主流产品之一。
目前瓷砖抗菌性能的实现,主要有离子掺杂型制备和光催化表面镀膜型制备两种方法。金属离子掺杂型制备方法是将银、锌等金属离子添加到陶瓷砖坯体或者釉料中经过800~1380℃烧成工序烧制而成。如中国专利CN103641439A公开了一种抗菌陶瓷砖及其制备方法,其组成为高岭土60~90份、陶瓷粘土30~40份、石英1~10份、钾长石1~10份、磷酸银0 .1~0 .5份、氧化铜1~5份,其制备方法是将所述物质按上述比例混合均匀,将粉料压制成型烧制,得抗菌陶瓷产品。由于抗菌材料是直接加入陶瓷砖坯体或者釉料中烧成,其抗菌有效成分被包覆在坯体或釉料中,其抗菌效果会大打折扣,烧制的抗菌陶瓷制品因为力学、热力学性能不匹配而出现裂纹、不光滑等。
光催化表面镀膜型制备方法是在已制好的陶瓷成品表面镀上一层 TiO2或TiO2掺金属离子溶胶凝胶薄膜,再经过低温烧结实现,其要点在于热处理后薄膜材料与陶瓷结合牢固且保持抗菌性能。如中国专利CN 109293338A公开了一种负离子抗菌瓷砖及其生产工艺,所述抗菌瓷砖包括胚体、底釉和面釉,胚体包括黏土、砂、瓷砖废料、碎陶土粉、硅藻土及功能纤维布,底釉和面釉均包括黏土、长石、石英、纳米银、纳米二氧化钛等,纳米银和纳米二氧化钛的使用,借助胚体孔洞中的水分和空气,激发抗菌功能,但该抗菌瓷砖得抗菌功能仍然难以维持长久。目前光催化剂的锐钛矿型 TiO2材料最大的缺点是在850℃左右容易失效。并且低温热处理抗菌层与釉面结合力较弱,实际应用时抗菌层容易脱落,抗菌持久性较差。
综上所述,目前的抗菌瓷砖存在抗菌性能不稳定、抗菌层容易脱落、难以持久、烧制的抗菌陶瓷制品因为力学、热力学性能不匹配而出现裂纹、不光滑等问题,因此急需开发一种性能稳定的抗菌精雕石瓷砖。
发明内容
为解决现有技术中的不足,本发明目的在于提供一种抗菌精雕石瓷砖及其制备方法。该抗菌精雕石瓷砖抗菌效果良好、持续时间长、产品性能优异,制备方法操作简便、易于规模化生产。
本发明具体技术方案如下:
一种抗菌精雕石瓷砖,是以下原料经球磨制浆、成型、一次性烧结、喷墨、添加复合光催化抗菌剂施釉、二次烧结、抛光修边而成,所述份数均为重量份:
高岭土 5~25份;
球土 5~26份;
钾长石 25~50份;
瓷土 25~40份;
叶蜡石 5~10份;
覆盖釉料 2~10份;
复合光催化抗菌剂 2~10份;
膨润土 2~5份。
本发明的原料优选如下:
其中所述高岭土优选苏州阳山高岭土,Al2O3含量35~45%,颜色洁白;其中所述的球土优选国产超白球土;
其中所述釉料包括下述重量份的原料:钠长石25~30份,高岭土13~15份,白云石8~15份,氧化铝2~8份,氧化锌5~10份,烧滑石6~10份;
其中所述的复合光催化抗菌剂为TiO2/Ag2O复合微球。
所述的TiO2/Ag2O复合微球的制备方法为:
S1:碳微球制备:取6kg葡萄糖和1kg尿素溶于去离子水中,充分搅拌混匀后,倒入50 mL 聚四氟乙烯衬里的水热反应釜中,130~140℃下反应3h,然后140~160℃下反应3h,冷却至室温,得到黑色沉淀,将黑色沉淀物过滤,用去离子水充分洗涤,70~80℃下干燥5h,得到碳微球;
S2:Ag2O微球的制备:取1.15kg硝酸银和步骤1制备的碳微球依次加入去离子水中,磁力搅拌10min,缓慢滴加浓度为0.1mol/L的NaOH溶液,PH=13时停止滴加,用去离子水洗涤,恒温干燥(干燥温度70~80℃,干燥时间1.5~3h)制得Ag2O微球;
S3:TiO2/Ag2O复合微球的制备:取0.15kg步骤2制备的Ag2O微球加入10L无水乙醇中,加1L去离子水,匀速滴加1L钛酸四丁酯,高速搅拌,溶液呈溶胶凝胶状后倒入水热反应釜中,120~160℃下反应2~3h,冷却至室温,得到的黑色沉淀充分洗涤干燥后,得到TiO2/Ag2O复合微球备用。
所述抗菌精雕石瓷砖加工方法,步骤如下:
1)以高岭土、球土、钾长石、瓷土、叶蜡石、膨润土为原料,过筛除杂,细度250~300目,压泥、练泥,制备浆料;
2)上述步骤制得的浆料通过球磨混合后,过300目筛,水分控制在35%左右,制备出具有良好流动性和悬浮稳定性的水基陶瓷料浆;
3)成型,陶瓷料浆经真空搅拌除气后注入陶瓷流延机的盛浆料斗,并从料斗下部均匀地流至成型模具得到合格的瓷坯;
4)将步骤3)制备的瓷坯干燥,在850~1300℃下素烧6~10 h,冷却至室温;
5)在在烧结瓷坯上喷墨,形成墨水层,喷墨采用的是功能墨水;
6)制备TiO2/Ag2O复合微球;
7)将步骤6)制备的TiO2/Ag2O复合微球按照质量比1:1加入釉料中,然后将制备的釉料均匀施于步骤5)喷墨后的瓷坯上二次烧结,烧成温度为450~550℃;时间为3~6 h;
8)抛光修边,得到本发明所述的抗菌精雕石瓷砖。
本发明的有益效果:
(1)本发明领用溶胶-凝胶法经高温煅烧后制成TiO2/Ag2O复合微球得到复合光催化抗菌剂,TiO2/Ag2O复合微球由于TiO2和Ag2O所产生的光生空穴和和电子可以互相迁移,降低了光生空穴和电子的复合率,提高了光催化活性,具有比表面积大、光催化反应活性高、抗菌效率高等优点,能长时间稳定发挥抗菌作用。
(2)本发明的抗菌精雕石瓷砖还有良好的空气净化作用,能够有效去除空气中的TVOC等物质,安全环保。
(3)本发明的抗菌精雕石瓷砖覆盖釉的添加TiO2/Ag2O复合微球,提高了TiO2/Ag2O复合微球的粘结度,釉面不易脱落;瓷砖表面为哑光,墨水同釉料共同烧成形成了类天然材料的特征纹理,产品美观耐用。
(4)本发明的抗菌精雕石瓷砖工艺简单、操作简便,适合于规模化工业生产。
具体实施方式
为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例,实施例不应视作对本发明保护范围的限定。
实施例1
一种抗菌精雕石瓷砖,是以下原料经球磨制浆、成型、一次性烧结、喷墨、添加复合光催化抗菌剂施釉、二次烧结、抛光修边而成,所述份数均为重量份:
高岭土 5份;
球土 5份;
钾长石 25份;
瓷土 25份;
叶蜡石 5份;
覆盖釉料 2份;
TiO2/Ag2O复合微球 2份;
膨润土 2~5份。
其中所述釉料包括下述重量份的原料:钠长石25份,高岭土13份,白云石8份,氧化铝2份,氧化锌5份,烧滑石6份。
其中所述高岭土优选苏州阳山高岭土,Al2O3含量35~45%,颜色洁白;其中所述的球土优选国产超白球土。
一种制备上述抗菌精雕石瓷砖的方法,包括以下步骤:
1)以高岭土、球土、钾长石、瓷土、叶蜡石、膨润土为原料,过筛除杂,细度250~300目,压泥、练泥,制备浆料。
2)上述步骤制得的浆料通过球磨混合后,过300目筛,水分控制在35%左右,制备出具有良好流动性和悬浮稳定性的水基陶瓷料浆;
3)成型,陶瓷料浆经真空搅拌除气后注入陶瓷流延机的盛浆料斗,并从料斗下部均匀地流至成型模具得到合格的瓷坯;
4)将步骤3)制备的瓷坯干燥,在850~1300℃下素烧6~10 h,冷却至室温;
5)在在烧结瓷坯上喷墨,形成墨水层,喷墨采用的是功能墨水;
6)制备TiO2/Ag2O复合微球碳微球制备:取6kg葡萄糖和1kg尿素溶于去离子水中,充分搅拌混匀后,倒入50 mL 聚四氟乙烯衬里的水热反应釜中,130~140℃下反应3h,140~160℃下反应3 h,冷却至室温,得到黑色沉淀,将黑色沉淀物过滤,用去离子水充分洗涤,70~80℃下干燥5 h,得到碳微球;取1.15kg硝酸银和碳微球依次加入去离子水中,磁力搅拌10min,缓慢滴加浓度为0.1mol/L的NaOH溶液,PH=13时停止滴加,用去离子水洗涤,恒温干燥(干燥温度70~80℃,干燥时间1.5~3h)制得Ag2O微球;取0.15kgAg2O微球加入10L无水乙醇中,加1L去离子水,匀速滴加1L钛酸四丁酯,高速搅拌,溶液呈溶胶凝胶状后倒入水热反应釜中,120~160℃下反应2~3 h, 冷却至室温,得到的黑色沉淀充分洗涤干燥后,得到TiO2/Ag2O复合微球;
7)将步骤6)制备的TiO2/Ag2O复合微球按照质量比1:1加入釉料中,然后将制备的釉料均匀施于步骤5)喷墨后的瓷坯上二次烧结,烧成温度为450~550℃;时间为3~6 h;
8)抛光修边,得到本发明所述的抗菌精雕石瓷砖。
实施例2
一种抗菌精雕石瓷砖,是以下原料经球磨制浆、成型、一次性烧结、喷墨、添加复合光催化抗菌剂施釉、二次烧结、抛光修边而成,所述份数均为重量份:
高岭土 20份;
球土 16份;
钾长石 45份;
瓷土 36份;
叶蜡石 8份;
覆盖釉料 6份;
TiO2/Ag2O复合微球 6份;
膨润土 3份。
其中所述釉料包括下述重量份的原料:钠长石26份,高岭土14份,白云石11份,氧化铝5份,氧化锌7份,烧滑石8份。
其中所述高岭土优选苏州阳山高岭土,Al2O3含量35~45%,颜色洁白;其中所述的球土优选国产超白球土。
制备方法同实施例1。
实施例3
一种抗菌精雕石瓷砖,是以下原料经球磨制浆、成型、一次性烧结、喷墨、添加复合光催化抗菌剂施釉、二次烧结、抛光修边而成,所述份数均为重量份:
高岭土 25份;
球土 26份;
钾长石 50份;
瓷土 40份;
叶蜡石 10份;
覆盖釉料 10份;
TiO2/Ag2O复合微球 10份;
膨润土 5份。
其中所述釉料包括下述重量份的原料:钠长石30份,高岭15份,白云石15份,氧化铝8份,氧化锌10份,烧滑石10份。
其中所述高岭土优选苏州阳山高岭土,Al2O3含量35~45%,颜色洁白;其中所述的球土优选国产超白球土。制备方法同实施例1。
对比例1
仅不用覆盖釉料,其他同实施例1。
对比例2
仅不用TiO2/Ag2O复合微球,其他同实施例1。
对比例3
仅用银羟基磷灰石抗菌剂替代TiO2/Ag2O复合微球,其他同实施例1。
结果对照:
分别对上述实施例1~3和对比例1~3制备的抗菌瓷砖的抗菌效果和持久性按照JC/T 897-2014《抗菌陶瓷制品抗菌性能》标准,以大肠杆菌和金黄色葡萄球菌为测试菌种进行测试,测试性能指标如下表。
检测结果表明:在初始菌数基本相同的情况下,经过168h,实施例1~3中的抗菌性能和持久性99.90以上,抗菌效果优异且持久,TVOC去除率 87%以上。对比例1中由于未使用覆盖釉料,复合光催化抗菌剂与瓷胚的结合作用减弱,抗菌性能、持久性和TVOC去除率稍差;对比例2中未使用抗菌剂作为光催化剂,无法提供充足的自由电子形成杀菌性强的负价银离子,也无法形成羟基自由基等抗菌基团,造成其抗菌效果较差,并且不能去除TVOC。对比例3所用抗菌剂不同,其抗菌效果和TVOC去除率虽然稍差,但与实施例1相差不大。
综上所述,本发明的抗菌精雕石瓷砖具有优异的抗菌性能以及稳定持久性,能部分去除TVOC。
Claims (8)
1.一种抗菌精雕石瓷砖,其特征在于由以下原料经球磨制浆、成型、一次性烧结、喷墨、添加复合光催化抗菌剂施釉、二次烧结、抛光修边而成,份数均为重量份:
高岭土 5~25份;
球土 5~26份;
钾长石 25~50份;
瓷土 25~40份;
叶蜡石 5~10份;
覆盖釉料 2~10份;
复合光催化抗菌剂 2~10份;
膨润土 2~5份;
所述的复合光催化抗菌剂为TiO2/Ag2O复合微球;
所述的TiO2/Ag2O复合微球的制备包括以下步骤:
S1:碳微球制备:取6kg葡萄糖和1kg尿素溶于去离子水中,充分搅拌混匀后,倒入50 mL聚四氟乙烯衬里的水热反应釜中,连续升温反应6h,冷却至室温,得到黑色沉淀,将黑色沉淀物过滤,用去离子水充分洗涤,70~80℃下干燥5 h,得到碳微球;
S2:Ag2O微球的制备:取1.15kg硝酸银和步骤1制备的碳微球依次加入去离子水中,磁力搅拌10min,缓慢滴加浓度为0.1mol/L的NaOH溶液,pH =13时停止滴加,用去离子水洗涤,恒温干燥制得Ag2O微球;
S3:TiO2/Ag2O复合微球的制备:取0.15kg步骤2制备的Ag2O微球加入10L无水乙醇中,加1L去离子水,匀速滴加1L钛酸四丁酯,高速搅拌,溶液呈溶胶凝胶状后倒入水热反应釜中反应2~3h,冷却至室温,得到黑色沉淀,充分洗涤干燥后,得到TiO2/Ag2O复合微球备用。
2.如权利要求1所述的抗菌精雕石瓷砖,其特征在于所述覆盖釉料包括下述重量份的原料:
钠长石 25~30份;
高岭土 13~15份;
白云石 8~15份;
氧化铝 2~8份;
氧化锌 5~10份;
烧滑石 6~10份。
3.如权利要求1所述的抗菌精雕石瓷砖,其特征在于:其中所述高岭土为苏州阳山高岭土,Al2O3含量35~45%,颜色洁白。
4.一种制备如权利要求1、2或3任一所述的抗菌精雕石瓷砖的方法,其特征在于包括以下步骤:
1)以高岭土、球土、钾长石、瓷土、叶蜡石、膨润土为原料,过筛除杂,细度250~300目,压泥、练泥,制备浆料;
2)上述步骤制得的浆料通过球磨混合后,过300目筛,水分控制在35%左右,制备出水基陶瓷料浆;
3)成型,陶瓷料浆经真空搅拌除气后注入陶瓷流延机的盛浆料斗,并从料斗下部均匀地流至成型模具得到合格的瓷坯;
4)将步骤3)制备的瓷坯干燥,在850~1300℃下素烧6~10 h,冷却至室温;
5)在烧结瓷坯上喷墨,形成墨水层,喷墨采用的是功能墨水;
6)制备TiO2/Ag2O复合微球;
7)将步骤6)制备的TiO2/Ag2O复合微球加入釉料中,然后将制备的釉料均匀施布于步骤5)喷墨后的瓷坯上二次烧结,烧成温度为450~550℃;时间为3~6 h;
8)抛光修边,得到所述的抗菌精雕石瓷砖。
5.如权利要求4所述的一种抗菌精雕石瓷砖的制备方法,其特征在于:所述步骤7)中添加的TiO2/Ag2O复合微球和覆盖釉料的质量比为1:1。
6.如权利要求1所述的一种抗菌精雕石瓷砖的制备方法,其特征在于:步骤S1中所述的连续升温反应6h为130~140℃下反应3h后140~160℃下反应3 h。
7.如权利要求1所述的一种抗菌精雕石瓷砖的制备方法,其特征在于:步骤S2中所述的恒温干燥干燥温度70~80℃,干燥时间1.5~3h。
8.如权利要求1所述的一种抗菌精雕石瓷砖的制备方法,其特征在于:步骤S3中所述的水热反应釜的反应温度为120~160℃。
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CN107721174A (zh) * | 2017-09-28 | 2018-02-23 | 禹州市正玉钧窑有限公司 | 一种具有保健作用的钧瓷釉料的施釉工艺 |
CN108569889A (zh) * | 2018-07-09 | 2018-09-25 | 福建省德化臻南陶瓷有限公司 | 一种耐高温抗菌陶瓷及其制备方法 |
CN109851396B (zh) * | 2019-04-24 | 2022-07-12 | 同曦集团有限公司 | 一种抗菌瓷砖及其制备方法 |
CN111072284B (zh) * | 2020-03-23 | 2020-08-18 | 广东欧文莱陶瓷有限公司 | 一种精雕陶瓷砖及其生产工艺 |
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