CN109593393B - 内墙涂料用抗菌剂的制备方法 - Google Patents

内墙涂料用抗菌剂的制备方法 Download PDF

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CN109593393B
CN109593393B CN201811616695.0A CN201811616695A CN109593393B CN 109593393 B CN109593393 B CN 109593393B CN 201811616695 A CN201811616695 A CN 201811616695A CN 109593393 B CN109593393 B CN 109593393B
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杨仁宗
曾佳
赵秀秀
陆旭超
童仁可
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SHANXI YAXIN ENERGY GROUP Co.,Ltd.
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Abstract

本发明公开了一种内墙涂料用抗菌剂的制备方法,包括如下步骤:步骤1:将尿素、六偏磷酸钠加入水中,搅拌混合后加入聚氧丙烯氧化乙烯甘油醚,再加入氯化钠溶液和硝酸银溶液;步骤2:将硫酸氧钛水溶液加入,然后再加入硫酸锆溶液;步骤3:水浴恒温反应;步骤4:反应结束后,冷却至室温并加入磷酸氢二钠溶液;步骤5:抽滤,得到沉淀,洗涤沉淀,然后将沉淀进行恒温干燥,得到干燥的粉体;步骤6:将粉体进行煅烧,然后自然冷却至室温,研磨煅烧后的粉体。本发明的有益效果为:采用该抗菌剂制成的内墙涂料具有优异的抗菌性能。

Description

内墙涂料用抗菌剂的制备方法
技术领域
本发明涉及,特别涉及一种内墙涂料用抗菌剂的制备方法。
背景技术
墙面涂料是指用于建筑墙面起装饰和保护,使建筑墙面美观整洁,同时也能够起到保护建筑墙面,延长其使用寿命的作用。墙面涂料按建筑墙面分类包括内墙涂料和外墙涂料两大部分。其中,内墙涂料的主要功能是装饰和保护室内墙面,使其美观整洁,让人们处于愉悦的居住环境中。
公开号为CN105440830A的中国专利公开了一种低粘度高遮盖高耐擦洗的内墙涂料及其制备方法。该内墙涂料由以下组分配制而成:水35-40份、羟乙基纤维素0.2-0.3份、无机触变增稠剂0.1-0.3份、膨润土0.1-0.3份、水性多功能助剂0.1-0.2份、分散剂0.7-0.8份、润湿剂0.3-0.4份、硅藻土3-4份、钛白粉15-18份、800目重钙3-5份、滑石粉4-6份、煅烧高岭土9-10份、乳液16-19份、抗冻剂0.8-1.2份、成膜助剂0.6-0.7份、消泡剂0.6-0.8份、增稠剂1-1.2份、防腐防霉剂0.8-1.2份。
随着社会的发展,人们不再仅仅满足于内墙涂料只起到装饰和保护室内墙面的作用,人们开始希望内墙涂料能够具有优异的抗菌性能,从而降低室内细菌含量,保护人们身体健康。而该内墙涂料无法满足人们的需求,有待改进。
发明内容
本发明的目的是提供一种内墙涂料用抗菌剂的制备方法。采用该抗菌剂制成的内墙涂料具有优异的抗菌性能。
本发明的上述技术目的是通过以下技术方案得以实现的:
一种内墙涂料用抗菌剂的制备方法,包括如下步骤:
步骤1:将尿素、六偏磷酸钠加入水中,搅拌混合后加入聚氧丙烯氧化乙烯甘油醚,再加入氯化钠溶液和硝酸银溶液;
步骤2:将硫酸氧钛水溶液加入,然后再加入硫酸锆溶液;
步骤3:水浴恒温反应;
步骤4:反应结束后,冷却至室温并加入磷酸氢二钠溶液;
步骤5:抽滤,得到沉淀,洗涤沉淀,然后将沉淀进行恒温干燥,得到干燥的粉体;
步骤6:将粉体进行煅烧,然后自然冷却至室温,研磨煅烧后的粉体。
本发明进一步设置为:所述尿素和六偏磷酸钠的质量比385∶1;所述聚氧丙烯氧化乙烯甘油醚和六偏磷酸钠的质量比为1∶1;所述氯化钠和六偏磷酸钠的质量比为2∶1;所述硝酸银和六偏磷酸钠的质量比为5∶1;所述硫酸氧钛和六偏磷酸钠的质量比为50∶1;所述硫酸锆和六偏磷酸钠的质量比为50∶1;所述磷酸氢二钠和六偏磷酸钠的质量比为130∶1。
本发明进一步设置为:所述尿素、六偏磷酸钠和水的搅拌速度为300-350rad/min。
本发明进一步设置为:所述水浴加热温度为90-100℃,反应时间为0.5-1h。
本发明进一步设置为:所述恒温干燥温度为90-100℃,干燥时间为1-3h。
本发明进一步设置为:所述粉体煅烧温度为800-900℃,所述煅烧时间为3-5h。
本发明进一步设置为:所述抗菌剂的制备方法还包括如下步骤:
步骤7:将沸石粉加入水中,搅拌均匀后加入硝酸锌,静置22-24h后,超声分散0.5-1h后取出过滤烘干,研磨成粉体;
步骤8:将步骤6得到的粉体研磨后加入水中,搅拌均匀后再加入硝酸铈,然后超声分散0.5-1h,得到基体;
步骤9:将步骤7得到的粉体加入到步骤8得到的基体中,调节溶液pH至3-4,在60-70℃恒温条件下搅拌,取出抽滤,干燥1-2h,然后焙烧1-2h,研磨即可。
综上所述,本发明具有以下有益效果:
1、该抗菌剂既综合银离子的抗菌作用,又综合纳米二氧化钛为空结构对细菌的吸附作用。银离子引入到二氧化钛晶格结构内部,从而在其晶格中引入新电荷、形成缺陷或改变晶格类型,降低二氧化钛光生电子跃迁的禁带宽度,产生并强化电子-空穴对陷阱,促进二氧化钛的光催化活性;
2、锌元素具有一定的抗菌作用,抗菌强度相比于银离子较弱,但也能够促进二氧化钛的光催化活性;铈元素存在多化合价,能够使二氧化钛成为光生电子-空穴对的浅势捕获陷阱,延长电子与空穴的复合时间,从而提高二氧化钛的光催化活性。同时,铈元素的电子能级比一般元素更多,可以吸收或发射从紫外光区、可见光区到红外光区的各种波长的电磁波辐射;
3、利用沸石负载银离子、锌元素和铈元素,从而实现对二氧化钛进行共掺杂改性,相互补充,共同作用,避免单独使用银离子、锌元素或者铈元素时,既成为捕获中心又称为复合中心,导致电子和空穴分离效率低进而影响二氧化钛光催化活性的问题。抗菌剂不仅在紫外光照射时,具有较强的光催化抗菌性能,而且在日光灯、室内自然光、甚至黑暗时也具有较明显的光催化抗菌效果。
具体实施方式
实施例1-5用于说明内墙涂料用抗菌剂的制备方法。
一种抗菌剂的制备方法,包括如下步骤:
步骤1:将尿素、六偏磷酸钠加入水中,搅拌混合后加入聚氧丙烯氧化乙烯甘油醚,再加入氯化钠溶液和硝酸银溶液;
步骤2:将硫酸氧钛水溶液加入,然后再加入硫酸锆溶液;
步骤3:水浴恒温反应;
步骤4:反应结束后,冷却至室温并加入磷酸氢二钠溶液;
步骤5:抽滤,得到沉淀,洗涤沉淀,然后将沉淀进行恒温干燥,得到干燥的粉体;
步骤6:将粉体进行煅烧,然后自然冷却至室温,研磨煅烧后的粉体;
步骤7:将沸石粉加入水中,搅拌均匀后加入硝酸锌,静置后超声分散,再取出过滤烘干,研磨成粉体;
步骤8:将步骤6得到的粉体研磨后加入水中,搅拌均匀后再加入硝酸铈,然后超声分散,得到基体;
步骤9:将步骤7得到的粉体加入到步骤8得到的基体中,调节溶液pH,恒温搅拌,取出抽滤,干燥,然后焙烧,研磨即可。
其中,尿素和六偏磷酸钠的质量比385∶1;聚氧丙烯氧化乙烯甘油醚和六偏磷酸钠的质量比为1∶1;氯化钠和六偏磷酸钠的质量比为2∶1;硝酸银和六偏磷酸钠的质量比为5∶1;硫酸氧钛和六偏磷酸钠的质量比为50:1;硫酸锆和六偏磷酸钠的质量比为50∶1;磷酸氢二钠和六偏磷酸钠的质量比为130∶1;
硝酸锌和沸石粉的质量比为1∶100;步骤6的粉体(以二氧化钛计)和硝酸铈的物质的量比为40∶1;硝酸锌和硝酸铈的物质的量比为1∶1。
氯化钠溶液、硝酸银溶液、硫酸氧钛溶液、硫酸锆溶液、磷酸氢二钠溶液的浓度均为1mol/L。
表1、实施例1-5抗菌剂的制备方法参数表
Figure BDA0001925357730000041
实施例6-10用于说明内墙涂料组分。实施例6-10内墙涂料组分见表2。
表2、实施例6-10内墙涂料组分表
Figure BDA0001925357730000042
Figure BDA0001925357730000051
注:单位“份”指重量份;颜料为氧化锌。
结合表2,以下详细说明内墙涂料的制备方法。
一种内墙涂料的制备方法,包括如下步骤:
步骤1:按照重量份,称取苯丙乳液、聚丙烯酸钠、六偏磷酸钠、聚氧丙烯氧化乙烯甘油醚、十二碳醇酯、羟乙基纤维素、AMP-95、蒙脱石粉、抗菌剂、水、颜料;
步骤2:在400-500rad/min转速下往水中依次加入羟乙基纤维素、蒙脱石粉,搅拌3-5min;
步骤3:在800-1000rad/min转速下,依次加入聚丙烯酸钠、六偏磷酸钠、聚氧丙烯氧化乙烯甘油醚、颜料,然后提高转速至1800-2000rad/min,搅拌15-20min;步骤4:检测细度,当细度≤60μm,降低转速至1000-1200rad/min,依次加入苯丙乳液、十二碳醇酯、AMP-95、抗菌剂,搅拌15-20min至混合液体均匀。
表3、实施例6-10内墙涂料的制备方法参数表
Figure BDA0001925357730000052
对比例1
选取公开号为CN105440830A的中国专利的实施例1作为对比例1。
抗菌试验
参照GB/T 21866-2008《抗菌涂料(漆膜)抗菌性测定法和抗菌效果》对实施例6-10和对比例1进行测试。
表4、实施例6-10和对比例1抗菌试验记录表
Figure BDA0001925357730000061
从表4可知,采用本发明制成的抗菌剂而制成的内墙涂料具有优异的抗菌性能。
本实施例仅仅是对本发明的解释,其并不是对本发明的限制,本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改,但只要在本发明的权利要求范围内都受到专利法的保护。

Claims (6)

1.一种内墙涂料用抗菌剂的制备方法,其特征是:包括如下步骤:
步骤1:将尿素、六偏磷酸钠加入水中,搅拌混合后加入聚氧丙烯氧化乙烯甘油醚,再加入氯化钠溶液和硝酸银溶液;
步骤2:将硫酸氧钛水溶液加入,然后再加入硫酸锆溶液;
步骤3:水浴恒温反应;
步骤4:反应结束后,冷却至室温并加入磷酸氢二钠溶液;
步骤5:抽滤,得到沉淀,洗涤沉淀,然后将沉淀进行恒温干燥,得到干燥的粉体;
步骤6:将粉体进行煅烧,然后自然冷却至室温,研磨煅烧后的粉体;
步骤7:将沸石粉加入水中,搅拌均匀后加入硝酸锌,静置22-24h后,超声分散0.5-1h后取出过滤烘干,研磨成粉体;
步骤8:将步骤6得到的粉体研磨后加入水中,搅拌均匀后再加入硝酸铈,然后超声分散0.5-1h,得到基体;
步骤9:将步骤7得到的粉体加入到步骤8得到的基体中,调节溶液pH至3-4,在60-70℃恒温条件下搅拌,取出抽滤,干燥1-2h,然后焙烧1-2h,研磨即可。
2.根据权利要求1所述的内墙涂料用抗菌剂的制备方法,其特征是:所述尿素和六偏磷酸钠的质量比385:1;所述聚氧丙烯氧化乙烯甘油醚和六偏磷酸钠的质量比为1:1;所述氯化钠和六偏磷酸钠的质量比为2:1;所述硝酸银和六偏磷酸钠的质量比为5:1;所述硫酸氧钛和六偏磷酸钠的质量比为50:1;所述硫酸锆和六偏磷酸钠的质量比为50:1;所述磷酸氢二钠和六偏磷酸钠的质量比为130:1。
3.根据权利要求1所述的内墙涂料用抗菌剂的制备方法,其特征是:所述尿素、六偏磷酸钠和水的搅拌速度为300-350rad/min。
4.根据权利要求1所述的内墙涂料用抗菌剂的制备方法,其特征是:所述水浴加热温度为90-100℃,反应时间为0.5-1h。
5.根据权利要求1所述的内墙涂料用抗菌剂的制备方法,其特征是:所述恒温干燥温度为90-100℃,干燥时间为1-3h。
6.根据权利要求1所述的内墙涂料用抗菌剂的制备方法,其特征是:所述粉体煅烧温度为800-900℃,所述煅烧时间为3-5h。
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