CN108751928A - 一种防污高强度抛光砖的制备方法 - Google Patents
一种防污高强度抛光砖的制备方法 Download PDFInfo
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Abstract
本发明涉及一种高防污高强度抛光砖的制备方法,属于环保材料制备技术领域。本发明将有机硅、有机氟双组分聚合物引入抛光砖中,有机硅聚合物中以Si‑O‑Si为主链,通过Si‑C键与有机基团生成侧链的半无机半有机高分子化合物,起提高防污性能的效果,本发明利用电弧法制备多孔碳纳米管,并制备纳米铜引入碳纳米管晶格中,碳纳米管本身具有很好的力学性能,也可以与有机硅烷结合形成Si‑C键,砖体内部结构空间更加紧密,引入铜,结合金属铜优异的强度,使碳纳米管的力学性能得到很大的提高,从而提高抛光砖的强度,有机硅、有机氟双组分聚合物也具有非常稳定致密的内部结构,Si‑O键、Si‑C键和C‑F键键能大,空间结构稳定,极大提高抛光砖的强度,具有广阔的应用前景。
Description
技术领域
本发明涉及一种防污高强度抛光砖的制备方法,属于环保材料制备技术领域。
背景技术
抛光砖称为地砖之王,是通体砖坯体的表面经过打磨而成的一种光亮的砖,属通体砖的一种。相对通体砖而言,抛光砖表面要光洁得多。抛光砖坚硬耐磨,适合在除洗手间、厨房以外的多数室内空间中使用比如用于阳台,外墙装饰等。在运用渗花技术的基础上,抛光砖可以做出各种仿石、仿木效果。
我国抛光砖随着生产技术水平的不断提高,品质走在世界前列,质量处于国际先进水平。国标高于欧标,表面平整度、边直度、直角度和耐磨性等参数都比欧标高2倍以上。工艺上的要求比国外小规格瓷砖更高,在无缝拼接上,对于瓷砖尺寸精确度要求也更高,品质也更优秀。抛光砖在出口上占很大份额。但超大规格瓷砖受环境、强度、破损率的影响,不会有更大的发展。为了求变,陶瓷企业在科技上大下力度,提高抛光砖性能,使抛光砖具有突破性的创新。但是说到瓷砖一般还是很难与艺术扯到一块,它只是铺到地上的一块块砖,其实正是这一块块砖,通过点点滴滴的艺术渗透彰显家居的品位与风格。
在低温快速烧成瓷质抛光砖的坯体中,玻璃相约占50%~60%,其它为石英、莫来石和气孔。由于石英和玻璃相的膨胀系数相差很大,如果石英颗粒过大,则冷却时玻璃相会受到大的张应力而产生裂纹,甚至使砖坯中的裂纹贯穿。所以,当砖坯中的粗颗粒石英含水量量过高时,砖坯中就存在许多的微裂纹。在抛光过程中,砖坯经过粗磨、细磨和抛光三个受力工序后,在磨头强大外力的作用下,使砖坯内的微裂纹都有不同程度的扩展(如果原来的微裂纹较大,就会发生砖坯断裂、破损的现象)。因此,抛光面是一个布满许多细小裂纹的被磨损的表面,当污染物落到抛光砖的抛光面后,一部分污染物就会渗透到许许多多的小裂纹内,造成抛光砖防污能力差。
因此,发明一种强度高且防污性能好的抛光砖对环保材料制备技术领域具有积极意义。
发明内容
本发明所要解决的技术问题:针对目前抛光砖针对目前抛光砖强度不够、防污性差的缺陷,提供了一种防污高强度抛光砖的制备方法。
为解决上述技术问题,本发明采用的技术方案是:
一种防污高强度抛光砖的制备方法,其特征在于具体制备步骤为:
(1)按重量份数计,称取7~9份甲基丙烯酸甲酯、15~18份苯二烯、10~12份甲基丙烯酸异冰片酯、25~28份丙烯酸丁酯、13~15份甲基丙烯酸羟乙酯和10~12份全氟辛酸混合搅拌得到混合液,将二甲苯和乙酸丁酯按质量比1:3搅拌混合得到反应溶剂,将反应溶剂投入反应釜中,在氮气保护下升温,恒温静置;
(2)向上述反应釜中滴加反应溶剂质量30~40%的混合液和5~8%的偶氮二异丁酯,氮气环境条件下滴加3~4h,滴加结束后,恒温静置40~60min得到反应浆液,降温并向反应釜中滴加反应浆液质量40~45%的端烃羟基聚硅氧烷,恒温反应4~5h后过滤得到滤液,备用;
(3)将石墨棒放于电弧室中分别作为阴极和阳极,在氩气条件下通电反应50~70min得到黑色粉末,按重量份数计,称取1~3份黑色粉末、20~22份硫酸和硝酸溶液放入三口烧瓶中,将三口烧瓶放入水浴锅中,搅拌60~80min后得到悬浊液;
(4)将悬浊液过滤得到滤渣,用蒸馏水清洗滤渣3~5次后用硫酸铜浸泡滤渣后过滤得到改性滤渣,用蒸馏水浸泡改性滤渣并以80mL/min的速率向蒸馏水中通入氢气,反应后过滤去除溶剂,得到改性粉末;
(5)将20~22份高岭土、10~12份膨润土、5~8份钾长石、5~8份高铝石、15~18份石英砂、10~15份备用的滤液、5~8份上述改性粉末和11~13份水加入球磨机中研磨得到研磨产物,将研磨产物放入模具中,压制得到砖坯,将砖坯放入烧成窑中煅烧,得到半成砖,将半成砖抛光制得防污高强度抛光砖。
步骤(1)中所述的反应釜温度升温至120~125℃,恒温静置时间为30~40min。
步骤(2)中所述的搅拌转速为300~400r/min,温度为120~125℃,反应釜降低温度至35~40℃。
步骤(3)中所述的电弧室中电压为60~70V,电流为50~60A,硫酸的质量分数为90~95%,硝酸的质量分数为30~40%,水浴温度为80~85℃。
步骤(4)中所述的浸泡时间为2~3h,通氢气的反应时间为4~5h。
步骤(5)中所述的压制模具的压强为320~340MPa,烧成窑中温度为1150~1200℃。
本发明的有益技术效果是:
(1)本发明首先制得有机氟聚合物,再将有机氟聚合物中结合有机硅烷成分制得有机氟和有机硅双组份聚合物,然后利用电弧放电法制得多孔碳纳米管,并对碳纳米管进行改性,向碳纳米管晶格中嵌入纳米铜单质,最后将砖的原料与改性碳纳米管和有机硅、有机氟双组分聚合物混合,烧制制得防污高强度抛光砖,本发明将有机硅、有机氟双组分聚合物引入抛光砖中,有机硅聚合物中以Si-O-Si为主链,通过Si-C键与有机基团生成侧链的半无机半有机高分子化合物,Si-O键的键能很高,不易分解,结构十分稳定,这种化合物分子间作用力低,从而使分子柔顺性好,降低表面能,使油污附着力下降,起提防污性能的效果,同时具有C-F键,C-F键键能大,聚合物分子的分子间作用力也很低,因此使有机氟聚合物也有很低的表面能,并且有机硅、有机氟双组份聚合物的内部结构致密稳定,不会轻易被污染物腐蚀或者渗透,因此使抛光砖具有优异的防污能力;
(2)本发明利用电弧法制备多孔碳纳米管,并制备纳米铜引入碳纳米管晶格中,碳纳米管本身具有很好的力学性能,也可以与有机硅烷结合形成Si-C键,使砖体内部结构空间更加紧密,同时引入铜,结合金属铜优异的强度,使碳纳米管的力学性能得到很大的提高,从而提高抛光砖的强度,有机硅、有机氟双组分聚合物也具有非常稳定致密的内部结构,Si-O键、Si-C键和C-F键键能大,空间结构稳定,极大提高抛光砖的强度,具有广阔的应用前景。
具体实施方式
按重量份数计,称取7~9份甲基丙烯酸甲酯、15~18份苯二烯、10~12份甲基丙烯酸异冰片酯、25~28份丙烯酸丁酯、13~15份甲基丙烯酸羟乙酯和10~12份全氟辛酸混合搅拌得到混合液,将二甲苯和乙酸丁酯按质量比1:3搅拌混合得到反应溶剂,将反应溶剂投入反应釜中,在氮气保护下升高温度至120~125℃,恒温静置30~40min;向上述反应釜中滴加反应溶剂质量30~40%的混合液和5~8%的偶氮二异丁酯,在转速为300~400r/min、温度为120~125℃的氮气环境条件下滴加3~4h,滴加结束后,恒温静置40~60min得到反应浆液,降温至35~40℃,向反应釜中滴加反应浆液质量40~45%的端烃羟基聚硅氧烷,恒温反应4~5h后过滤得到滤液,备用;将石墨棒放于电弧室中分别作为阴极和阳极,设置电压为60~70V,电流为50~60A,在氩气条件下通电反应50~70min得到黑色粉末,按重量份数计,称取1~3份黑色粉末、20~22份质量分数为90~95%的硫酸和30~40%的硝酸溶液放入三口烧瓶中,将三口烧瓶放入水浴温度为80~85℃的水浴锅中,搅拌60~80min后得到悬浊液;将悬浊液过滤得到滤渣,用蒸馏水清洗滤渣3~5次后用硫酸铜浸泡滤渣2~3h后过滤得到改性滤渣,用蒸馏水浸泡改性滤渣并以80mL/min的速率向蒸馏水中通入氢气,反应4~5h后过滤去除溶剂,得到改性粉末;将20~22份高岭土、10~12份膨润土、5~8份钾长石、5~8份高铝石、15~18份石英砂、10~15份备用的滤液、5~8份上述改性粉末和11~13份水加入球磨机中研磨得到研磨产物,将研磨产物放入模具中,以320~340MPa的压力压制得到砖坯,将砖坯放入温度为1150~1200℃的烧成窑中煅烧,得到半成砖,将半成砖抛光制得防污高强度抛光砖。
按重量份数计,称取7份甲基丙烯酸甲酯、15份苯二烯、10份甲基丙烯酸异冰片酯、25份丙烯酸丁酯、13份甲基丙烯酸羟乙酯和10份全氟辛酸混合搅拌得到混合液,将二甲苯和乙酸丁酯按质量比1:3搅拌混合得到反应溶剂,将反应溶剂投入反应釜中,在氮气保护下升高温度至120℃,恒温静置30min;向上述反应釜中滴加反应溶剂质量30%的混合液和5%的偶氮二异丁酯,在转速为300r/min、温度为120℃的氮气环境条件下滴加3h,滴加结束后,恒温静置40min得到反应浆液,降温至35℃,向反应釜中滴加反应浆液质量40%的端烃羟基聚硅氧烷,恒温反应4h后过滤得到滤液,备用;将石墨棒放于电弧室中分别作为阴极和阳极,设置电压为60V,电流为50A,在氩气条件下通电反应50min得到黑色粉末,按重量份数计,称取1份黑色粉末、20份质量分数为90%的硫酸和30%的硝酸溶液放入三口烧瓶中,将三口烧瓶放入水浴温度为80℃的水浴锅中,搅拌60min后得到悬浊液;将悬浊液过滤得到滤渣,用蒸馏水清洗滤渣3次后用硫酸铜浸泡滤渣2h后过滤得到改性滤渣,用蒸馏水浸泡改性滤渣并以80mL/min的速率向蒸馏水中通入氢气,反应4h后过滤去除溶剂,得到改性粉末;将20份高岭土、10份膨润土、5份钾长石、5份高铝石、15份石英砂、10份备用的滤液、5份上述改性粉末和11份水加入球磨机中研磨得到研磨产物,将研磨产物放入模具中,以320MPa的压力压制得到砖坯,将砖坯放入温度为1150℃的烧成窑中煅烧,得到半成砖,将半成砖抛光制得防污高强度抛光砖。
按重量份数计,称取8份甲基丙烯酸甲酯、17份苯二烯、11份甲基丙烯酸异冰片酯、27份丙烯酸丁酯、14份甲基丙烯酸羟乙酯和11份全氟辛酸混合搅拌得到混合液,将二甲苯和乙酸丁酯按质量比1:3搅拌混合得到反应溶剂,将反应溶剂投入反应釜中,在氮气保护下升高温度至122℃,恒温静置35min;向上述反应釜中滴加反应溶剂质量35%的混合液和7%的偶氮二异丁酯,在转速为350r/min、温度为122℃的氮气环境条件下滴加3.5h,滴加结束后,恒温静置50min得到反应浆液,降温至37℃,向反应釜中滴加反应浆液质量42%的端烃羟基聚硅氧烷,恒温反应4.5h后过滤得到滤液,备用;将石墨棒放于电弧室中分别作为阴极和阳极,设置电压为65V,电流为55A,在氩气条件下通电反应60min得到黑色粉末,按重量份数计,称取2份黑色粉末、21份质量分数为92%的硫酸和35%的硝酸溶液放入三口烧瓶中,将三口烧瓶放入水浴温度为82℃的水浴锅中,搅拌70min后得到悬浊液;将悬浊液过滤得到滤渣,用蒸馏水清洗滤渣4次后用硫酸铜浸泡滤渣2.5h后过滤得到改性滤渣,用蒸馏水浸泡改性滤渣并以80mL/min的速率向蒸馏水中通入氢气,反应4.5h后过滤去除溶剂,得到改性粉末;将21份高岭土、11份膨润土、7份钾长石、7份高铝石、17份石英砂、12份备用的滤液、7份上述改性粉末和12份水加入球磨机中研磨得到研磨产物,将研磨产物放入模具中,以330MPa的压力压制得到砖坯,将砖坯放入温度为1170℃的烧成窑中煅烧,得到半成砖,将半成砖抛光制得防污高强度抛光砖。
按重量份数计,称取9份甲基丙烯酸甲酯、18份苯二烯、12份甲基丙烯酸异冰片酯、28份丙烯酸丁酯、15份甲基丙烯酸羟乙酯和12份全氟辛酸混合搅拌得到混合液,将二甲苯和乙酸丁酯按质量比1:3搅拌混合得到反应溶剂,将反应溶剂投入反应釜中,在氮气保护下升高温度至125℃,恒温静置40min;向上述反应釜中滴加反应溶剂质量40%的混合液和8%的偶氮二异丁酯,在转速为400r/min、温度为125℃的氮气环境条件下滴加4h,滴加结束后,恒温静置60min得到反应浆液,降温至40℃,向反应釜中滴加反应浆液质量45%的端烃羟基聚硅氧烷,恒温反应5h后过滤得到滤液,备用;将石墨棒放于电弧室中分别作为阴极和阳极,设置电压为70V,电流为60A,在氩气条件下通电反应70min得到黑色粉末,按重量份数计,称取3份黑色粉末、22份质量分数为95%的硫酸和40%的硝酸溶液放入三口烧瓶中,将三口烧瓶放入水浴温度为85℃的水浴锅中,搅拌80min后得到悬浊液;将悬浊液过滤得到滤渣,用蒸馏水清洗滤渣5次后用硫酸铜浸泡滤渣3h后过滤得到改性滤渣,用蒸馏水浸泡改性滤渣并以80mL/min的速率向蒸馏水中通入氢气,反应5h后过滤去除溶剂,得到改性粉末;将22份高岭土、12份膨润土、8份钾长石、8份高铝石、18份石英砂、15份备用的滤液、8份上述改性粉末和13份水加入球磨机中研磨得到研磨产物,将研磨产物放入模具中,以340MPa的压力压制得到砖坯,将砖坯放入温度为1200℃的烧成窑中煅烧,得到半成砖,将半成砖抛光制得防污高强度抛光砖。
对比例以佛山市某公司生产的防污高强度抛光砖作为对比例 对本发明制得的防污高强度抛光砖和对比例中的防污高强度抛光砖进行性能检测,检测结果如表1所示:
测试方法:
防污性测试:在实例1~3和对比例中的抛光砖表面涂抹墨水,15min后用抹布抹去,并用水冲洗,然后比较残留污渍颜色色调的深浅,来判断防污性能的好坏。
破坏强度和断裂模数测试按GB/T 3810.4-2016测试标准进行检测。
耐磨性测试按GB/T 3810.8试验方法进行检测。
无侧限抗压强度测试采用抗压试验机进行检测。
抗压回弹模量测试采用万能试验机进行检测。
表1抛光砖性能测定结果
测试项目 | 实例1 | 实例2 | 实例3 | 对比例 |
防污性 | 残留颜色浅 | 残留颜色浅 | 基本无残留颜色 | 残留颜色深 |
破坏强度(N) | 2045 | 2050 | 2055 | 1850 |
断裂模数(MPa) | 40.1 | 40.4 | 40.6 | 25.7 |
耐磨性(mm3) | 96.5 | 96.6 | 96.7 | 78.5 |
7天无侧限抗压强度(MPa) | 8.0 | 8.2 | 8.4 | 6.5 |
28天无侧限抗压强度(MPa) | 9.3 | 9.4 | 9.6 | 7.1 |
90天抗压回弹模量(MPa) | 1960 | 1962 | 1965 | 1452 |
根据上述中数据可知本发明制得的防污高强度抛光砖防污性好,残留颜色浅,对比例中抛光砖残留颜色深,防污性差,强度高,破坏强度达到2055N,抗压强度高,抗压回弹模量高,具有广阔的应用前景。
Claims (6)
1.一种防污高强度抛光砖的制备方法,其特征在于具体制备步骤为:
(1)按重量份数计,称取7~9份甲基丙烯酸甲酯、15~18份苯二烯、10~12份甲基丙烯酸异冰片酯、25~28份丙烯酸丁酯、13~15份甲基丙烯酸羟乙酯和10~12份全氟辛酸混合搅拌得到混合液,将二甲苯和乙酸丁酯按质量比1:3搅拌混合得到反应溶剂,将反应溶剂投入反应釜中,在氮气保护下升高,恒温静置;
(2)向上述反应釜中滴加反应溶剂质量30~40%的混合液和5~8%的偶氮二异丁酯,氮气环境条件下滴加3~4h,滴加结束后,恒温静置40~60min得到反应浆液,降温并向反应釜中滴加反应浆液质量40~45%的端烃羟基聚硅氧烷,恒温反应4~5h后过滤得到滤液,备用;
(3)将石墨棒放于电弧室中分别作为阴极和阳极,在氩气条件下通电反应50~70min得到黑色粉末,按重量份数计,称取1~3份黑色粉末、20~22份硫酸和硝酸溶液放入三口烧瓶中,将三口烧瓶放入水浴锅中,搅拌60~80min后得到悬浊液;
(4)将悬浊液过滤得到滤渣,用蒸馏水清洗滤渣3~5次后用硫酸铜浸泡滤渣后过滤得到改性滤渣,用蒸馏水浸泡改性滤渣并以80mL/min的速率向蒸馏水中通入氢气,反应后过滤去除溶剂,得到改性粉末;
(5)将20~22份高岭土、10~12份膨润土、5~8份钾长石、5~8份高铝石、15~18份石英砂、10~15份备用的滤液、5~8份上述改性粉末和11~13份水加入球磨机中研磨得到研磨产物,将研磨产物放入模具中,压制得到砖坯,将砖坯放入烧成窑中煅烧,得到半成砖,将半成砖抛光制得防污高强度抛光砖。
2.根据权利要求1所述的一种防污高强度抛光砖的制备方法,其特征在于:步骤(1)中所述的反应釜温度升温至120~125℃,恒温静置时间为30~40min。
3.根据权利要求1所述的一种防污高强度抛光砖的制备方法,其特征在于:步骤(2)中所述的搅拌转速为300~400r/min,温度为120~125℃,反应釜降低温度至35~40℃。
4.根据权利要求1所述的一种防污高强度抛光砖的制备方法,其特征在于:步骤(3)中所述的电弧室中电压为60~70V,电流为50~60A,硫酸的质量分数为90~95%,硝酸的质量分数为30~40%,水浴温度为80~85℃。
5.根据权利要求1所述的一种防污高强度抛光砖的制备方法,其特征在于:步骤(4)中所述的浸泡时间为2~3h,通氢气的反应时间为4~5h。
6.根据权利要求1所述的一种防污高强度抛光砖的制备方法,其特征在于:步骤(5)中所述的压制模具的压强为320~340MPa,烧成窑中温度为1150~1200℃。
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