CN109437855A - 一种环保软瓷的制备方法 - Google Patents
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Abstract
本发明涉及一种环保软瓷的制备方法,包括制备纳米银纤维、改性氮化硼纳米管、制备相变微胶囊、制备软瓷和表面处理,所述环保软瓷包括无机粉料30‑50份、水泥15‑35份、相变微胶囊10‑15份、丙烯酸类聚合物乳液10‑30份、颜料0‑2份、偶联剂0.5‑2份、蒙脱石0.5‑1.2份、硅藻土0.5‑1.2份、木纤维0.8‑1.5份,本申请制备的环保软瓷,具有良好的透气、防污自洁和调温控湿性能。
Description
技术领域
本发明涉及建筑及装饰材料领域,具体涉及一种环保软瓷的制备方法。
背景技术
改性无机粉材料,简称MCM装饰材料,俗称软瓷,是以天然原始土、城建废弃土、水泥弃块及瓷渣、石粉等无机物为原料,经分类混合、复合改性,在光化异构及曲线温度下成型,制成的墙体饰面板材,外观质感好,具有柔、薄、轻、安全,方便施工等特点。软瓷技术在节能减排的指标上符合环保节能的发展趋势,是建筑垃圾再利用的一种新型低碳环保装饰材料,具有广泛的推广价值。
尽管软瓷具有上述优点,但普遍存在物理性能指标单一的问题,其功能化产品种类稀少,综合性能指标相对不高,随着软瓷技术的不断发展,功能化、多元化的软瓷产品将成为行业发展方向,如保温隔热,抗污自洁,透气拒水等。
发明内容
针对上述问题,本发明提供一种环保软瓷的制备方法。
本发明的目的采用以下技术方案来实现:一种环保软瓷的制备方法,包括以下步骤:
(1)采用多元醇法制备纳米银纤维;
(2)氢氧化钠溶液对氮化硼纳米管进行羟基化改性,再交联纳米银纤维并用戊二醛进行醛基化改性;
(3)正十八烷在壳聚糖的乙酸水溶液中分散乳化,再与改性的氮化硼纳米管相互作用制备相变微胶囊;
(4)按原料质量比例为:经前处理的无机粉料30-50份、水泥15-35份、相变微胶囊10-15份、丙烯酸类聚合物乳液10-30份、颜料0-2份、蒙脱石0.5-1.2份、硅藻土0.5-1.2份、木纤维0.8-1.5份,混合后加入5-10%的水,搅拌均匀得到浆料,模具浇注,100-120℃压制成型,180-200℃固化,脱模得到产品;
所述前处理为无机粉料粉碎后加入0.5-2份偶联剂进行加热搅拌均匀后干燥,温度80-100℃;
优选的,所述纳米银纤维直径60-70nm,长度15-35μm;
优选的,所述氢氧化钠溶液浓度为5M,氮化硼纳米管添加量为5g/L,改性条件为100℃保温搅拌12h;
优选的,所述戊二醛溶液质量分数为50%,与羟基化改性的氮化硼纳米管的添加比例为2ml/g;
优选的,所述壳聚糖脱乙酰度为85-95%,质量浓度15%,正十八烷添加量为壳聚糖的10%;
优选的,所述无机粉料为废弃泥土、红黄黑白土、水泥弃块粉料、石粉、煤渣粉料之一或其组合;
优选的,所述木纤维为竹木纤维、杨木纤维、松木纤维、梨木纤维、澳亚木纤维之一或其组合,纤维直径0.01-0.1mm,纤维长度0.5-5mm;
优选的,脱模后对产品进行10-100kGy的辐射处理;
优选的,所述原料还含有0.5-1.5份的抗氧化剂和/或0.5-1.5份的紫外线吸收剂;
优选的,脱模得到的产品进行介质阻挡放电等离子体处理,再喷淋雾化的硬脂酸。
本发明的有益效果为:
(1)环保,本申请中无机粉料可用城建废弃土,实现资源的综合利用,摒弃煤炭、重油等高污染原料,生产过程无污染,废料可循环利用。
(2)微孔透气,硅藻土具有天然的多孔性构造,增加软瓷的透气性能,蒙脱石为极细颗粒的含水铝硅酸盐构成的层状矿物,吸水易膨胀,在高温烘焙条件下,蒙脱石脱水,水蒸气溢出,体积收缩和水蒸气溢出为软瓷提供均匀的微孔结构,进一步增强软瓷透气性能;木纤维除提高柔韧性外,在高温烘焙条件下也发生部分碳化,为软瓷提供微孔结构。
(3)调温控湿,硅藻土、蒙脱石、碳化纤维以及软瓷都具有多微孔结构,能对环境湿度做出响应,改变其含水量,对环境具有一定的控湿作用;软瓷中添加的相变微胶囊,具有潜热高的特点,纳米银纤维与改性氮化硼纳米管形成交联网络,增强相变微胶囊壁材-芯材之间的导热效果,具有良好的调温作用。
(4)防污自洁,软瓷表面进行等离子体刻蚀,构造类荷叶表面的疏水微纳粗糙结构,与具有低表面能的蜡质晶体的共同作用,表现出良好的防污自清洁效果。
具体实施方式
结合以下实施例对本发明作进一步描述。
丙烯酸类聚合物乳液包括丙烯酸酯类聚合物乳液、丙烯酸酯类高分子共聚乳液、丙烯酸-2-乙基己酯聚合物乳液;颜料多为无机颜料,可根据实际需要施用;偶联剂为铝酸酯偶联剂或钛酸酯偶联剂;抗氧化剂包括抗氧剂1010、抗氧剂164;紫外吸收剂包括紫外吸收剂UV-0、紫外吸收剂UV-9。
实施例1
一种环保软瓷的制备方法,包括以下步骤:
(1)纳米银纤维制备
100ml热的丙三醇中加入3.0g PVP搅拌溶解,冷却后加入0.8g Ag(NO)3、5ml丙三醇、0.02g NaCl,0.3ml去离子水,边缓慢搅拌边加热至200℃,停止加热,继续搅拌至冷,8000rpm离心10min,100ml无水乙醇洗涤沉淀,重复三次离心和洗涤,得到纳米银纤维的乙醇分散液,记为溶液A;
(2)BNNT改性
氮化硼纳米管添加到5M的氢氧化钠溶液中,添加量为5g/L,加热至100℃保温搅拌12h,过滤并洗涤滤饼至滤液呈中性,真空干燥制得表面羟基化改性的氮化硼,记为产物B,取5g产物B,加入80ml无水乙醇,边摇晃边滴加入10ml的50%的戊二醛溶液,50℃保温24h,加入20ml溶液A,充分混匀后滤出沉淀,去离子水洗涤,沉淀用40ml去离子水分散,记为溶液C;
(3)相变微胶囊的制备
脱乙酰度90%的壳聚糖在4%的乙酸水溶液中溶解,溶解浓度15%(w/v),加热至40℃,逐滴滴加壳聚糖质量10%的正二十烷,1500r/min搅拌4h充分乳化,缓慢滴加壳聚糖溶液体积25%的溶液C,同时500r/min搅拌,滴加完毕后,保持搅拌8h,滤出沉淀,分别以稀碱溶液、去离子水洗涤,干燥,得到相变微胶囊;
(4)软瓷制备
废弃泥土30份粉碎后加入0.5份偶联剂进行加热搅拌,温度80℃,搅拌均匀后干燥,加入水泥15份、相变微胶囊10份、丙烯酸类聚合物乳液10份、蒙脱石0.5份、硅藻土0.5份、木纤维0.8份,原料混合后加入5%的水,搅拌均匀得到浆料,模具浇注,100-120℃压制成型,180-200℃固化,脱模得到软瓷,软瓷进行10kGy的辐射处理。
实施例2
一种环保软瓷的制备方法,包括以下步骤:
(1)纳米银纤维制备
100ml热的丙三醇中加入3.0g PVP搅拌溶解,冷却后加入0.8g Ag(NO)3、5ml丙三醇、0.02g NaCl,0.3ml去离子水,边缓慢搅拌边加热至200℃,停止加热,继续搅拌至冷,8000rpm离心10min,100ml无水乙醇洗涤沉淀,重复三次离心和洗涤,得到纳米银纤维的乙醇分散液,记为溶液A;
(2)BNNT改性
氮化硼纳米管添加到5M的氢氧化钠溶液中,添加量为5g/L,加热至100℃保温搅拌12h,过滤并洗涤滤饼至滤液呈中性,真空干燥制得表面羟基化改性的氮化硼,记为产物B,取5g产物B,加入80ml无水乙醇,边摇晃边滴加入10ml的50%的戊二醛溶液,50℃保温24h,加入20ml溶液A,充分混匀后滤出沉淀,去离子水洗涤,沉淀用40ml去离子水分散,记为溶液C;
(3)相变微胶囊的制备
脱乙酰度85%的壳聚糖在4%的乙酸水溶液中溶解,溶解浓度15%(w/v),加热至40℃,逐滴滴加壳聚糖质量10%的正二十烷,1500r/min搅拌4h充分乳化,缓慢滴加壳聚糖溶液体积25%的溶液C,同时500r/min搅拌,滴加完毕后,保持搅拌8h,滤出沉淀,分别以稀碱溶液、去离子水洗涤,干燥,得到相变微胶囊;
(4)软瓷制备
废弃泥土、水泥弃块粉料、红***40份粉碎后加入1份偶联剂进行加热搅拌,温度100℃,搅拌均匀后干燥,加入水泥25份、相变微胶囊13份、丙烯酸类聚合物乳液20份、蒙脱石1份、硅藻土1份、木纤维1份、抗氧化剂0.5份、紫外吸收剂1.5份,原料混合后加入10%的水,搅拌均匀得到浆料,模具浇注,100-120℃压制成型,180-200℃固化,脱模得到软瓷,软瓷进行50kGy的辐射处理。
实施例3
一种环保软瓷的制备方法,包括以下步骤:
(1)纳米银纤维制备
100ml热的丙三醇中加入3.0g PVP搅拌溶解,冷却后加入0.8g Ag(NO)3、5ml丙三醇、0.02g NaCl,0.3ml去离子水,边缓慢搅拌边加热至200℃,停止加热,继续搅拌至冷,8000rpm离心10min,100ml无水乙醇洗涤沉淀,重复三次离心和洗涤,得到纳米银纤维的乙醇分散液,记为溶液A;
(2)BNNT改性
氮化硼纳米管添加到5M的氢氧化钠溶液中,添加量为5g/L,加热至100℃保温搅拌12h,过滤并洗涤滤饼至滤液呈中性,真空干燥制得表面羟基化改性的氮化硼,记为产物B,取5g产物B,加入80ml无水乙醇,边摇晃边滴加入10ml的50%的戊二醛溶液,50℃保温24h,加入20ml溶液A,充分混匀后滤出沉淀,去离子水洗涤,沉淀用40ml去离子水分散,记为溶液C;
(3)相变微胶囊的制备
脱乙酰度95%的壳聚糖在4%的乙酸水溶液中溶解,溶解浓度15%(w/v),加热至40℃,逐滴滴加壳聚糖质量10%的正二十烷,1500r/min搅拌4h充分乳化,缓慢滴加壳聚糖溶液体积25%的溶液C,同时500r/min搅拌,滴加完毕后,保持搅拌8h,滤出沉淀,分别以稀碱溶液、去离子水洗涤,干燥,得到相变微胶囊;
(4)软瓷制备
水泥弃块粉料、石粉共50份粉碎后加入2份偶联剂进行加热搅拌,温度100℃,搅拌均匀后干燥,加入水泥35份、相变微胶囊15份、丙烯酸类聚合物乳液25份、蒙脱石1.2份、硅藻土0.8份、木纤维1.5份、抗氧化剂1份、紫外吸收剂1份,原料混合后加入10%的水,搅拌均匀得到浆料,模具浇注,100-120℃压制成型,180-200℃固化,脱模得到软瓷,软瓷进行100kGy的辐射处理;
(5)表面处理
软瓷进行介质阻挡放电等离子体处理,处理条件为,高压电极与地电极间距8mm,材料置于地电极板上,电极间通有超纯水蒸汽,高压交流电源频率200Hz,电压15kV,水蒸汽流量0.5L/min,放电时间5min;硬脂酸加热至70-80℃,雾化,喷淋等离子体处理的软瓷表面,得到产品。
实施例4
一种环保软瓷的制备方法,包括以下步骤:
(1)纳米银纤维制备
100ml热的丙三醇中加入3.0g PVP搅拌溶解,冷却后加入0.8g Ag(NO)3、5ml丙三醇、0.02g NaCl,0.3ml去离子水,边缓慢搅拌边加热至200℃,停止加热,继续搅拌至冷,8000rpm离心10min,100ml无水乙醇洗涤沉淀,重复三次离心和洗涤,得到纳米银纤维的乙醇分散液,记为溶液A;
(2)BNNT改性
氮化硼纳米管添加到5M的氢氧化钠溶液中,添加量为5g/L,加热至100℃保温搅拌12h,过滤并洗涤滤饼至滤液呈中性,真空干燥制得表面羟基化改性的氮化硼,记为产物B,取5g产物B,加入80ml无水乙醇,边摇晃边滴加入10ml的50%的戊二醛溶液,50℃保温24h,加入20ml溶液A,充分混匀后滤出沉淀,去离子水洗涤,沉淀用40ml去离子水分散,记为溶液C;
(3)相变微胶囊的制备
脱乙酰度90%的壳聚糖在4%的乙酸水溶液中溶解,溶解浓度15%(w/v),加热至40℃,逐滴滴加壳聚糖质量10%的正二十烷,1500r/min搅拌4h充分乳化,缓慢滴加壳聚糖溶液体积25%的溶液C,同时500r/min搅拌,滴加完毕后,保持搅拌8h,滤出沉淀,分别以稀碱溶液、去离子水洗涤,干燥,得到相变微胶囊;
(4)软瓷制备
废弃泥土、煤渣粉料共38份粉碎后加入1.5份偶联剂进行加热搅拌,温度90℃,搅拌均匀后干燥,加入水泥25份、相变微胶囊13份、丙烯酸类聚合物乳液30份、蒙脱石1.2份、硅藻土0.8份、木纤维1份、颜料2份、抗氧化剂1.5份、紫外吸收剂0.5份,原料混合后加入8%的水,搅拌均匀得到浆料,模具浇注,100-120℃压制成型,180-200℃固化,脱模得到软瓷;
(5)表面处理
软瓷进行介质阻挡放电等离子体处理,处理条件为,高压电极与地电极间距8mm,材料置于地电极板上,电极间通有超纯水蒸汽,高压交流电源频率200Hz,电压15kV,水蒸汽流量0.5L/min,放电时间5min;硬脂酸加热至70-80℃,雾化,喷淋等离子体处理的软瓷表面,得到产品。
对比例:软瓷制备中不添加硅藻土、蒙脱石以及木纤维,其它条件同实施例3。
测试实验:
(1)将4μl去离子水滴于实施例制备的软瓷表面,通过分析仪实时记录水滴在软瓷表面的形状变化,经模拟测得接触角,测试结果见表1。
表1接触角测试结果
实施例1 | 实施例2 | 实施例3 | 实施例4 | |
接触角/° | 103 | 102 | 121 | 119 |
(2)测定实施例3与对比例所制备产品的密度,计算孔隙率测得孔隙率p为18.9%。
(3)各实施例制备的软瓷基本性能测试结果见表2。
表2基本性能测试结果
项目 | 方法 | 结果 |
抗化学腐蚀性 | GB/T 3810.13-2006 | 800h,无气泡、剥落现象 |
不透水性 | GB/T 18173.1-2006 | 30min,无渗透 |
阻燃性 | GB 8624-2006 | B级 |
抗冻性 | GB/T 3810.12-2006 | 100次循环后,无裂纹、剥落现象 |
耐老化性 | GB 1865-1997 | 1200h,外观无裂纹 |
撕裂强度 | GB/T 529-1999 | ≧20kN/m |
柔韧性 | JC/T 864-2000 | 无裂纹、断裂 |
最后应当说明的是,以上实施例仅用以说明本发明的技术方案,而非对本发明保护范围的限制,尽管参照较佳实施例对本发明作了详细地说明,本领域的普通技术人员应当理解,可以对本发明的技术方案进行修改或者等同替换,而不脱离本发明技术方案的实质和范围。
Claims (10)
1.一种环保软瓷的制备方法,其特征是,包括以下步骤:
(1)采用多元醇法制备纳米银纤维;
(2)氢氧化钠溶液对氮化硼纳米管进行羟基化改性,再交联纳米银纤维并用戊二醛进行醛基化改性;
(3)正十八烷在壳聚糖的乙酸水溶液中分散乳化,再与改性的氮化硼纳米管相互作用制备相变微胶囊;
(4)按原料质量比例为:经前处理的无机粉料30-50份、水泥15-35份、相变微胶囊10-15份、丙烯酸类聚合物乳液10-30份、颜料0-2份、蒙脱石0.5-1.2份、硅藻土0.5-1.2份、木纤维0.8-1.5份,混合后加入5-10%的水,搅拌均匀得到浆料,模具浇注,100-120℃压制成型,180-200℃固化,脱模得到产品;
所述前处理为无机粉料粉碎后加入0.5-2份偶联剂进行加热搅拌均匀后干燥,温度80-100℃。
2.根据权利要求1所述的一种环保软瓷的制备方法,其特征是,所述纳米银纤维直径60-70nm,长度15-35μm。
3.根据权利要求1所述的一种环保软瓷的制备方法,其特征是,所述氢氧化钠溶液浓度为5M,氮化硼纳米管添加量为5g/L,改性条件为100℃保温搅拌12h。
4.根据权利要求1所述的一种环保软瓷的制备方法,其特征是,所述戊二醛溶液质量分数为50%,与羟基化改性的氮化硼纳米管的添加比例为2ml/g。
5.根据权利要求1所述的一种环保软瓷的制备方法,其特征是,所述壳聚糖脱乙酰度为85-95%,质量浓度15%,正十八烷添加量为壳聚糖的10%。
6.根据权利要求1所述的一种环保软瓷的制备方法,其特征是,所述无机粉料为废弃泥土、红黄黑白土、水泥弃块粉料、石粉、煤渣粉料之一或其组合。
7.根据权利要求1所述的一种环保软瓷的制备方法,其特征是,所述木纤维为竹木纤维、杨木纤维、松木纤维、梨木纤维、澳亚木纤维之一或其组合,纤维直径0.01-0.1mm,纤维长度0.5-5mm。
8.根据权利要求1所述的一种环保软瓷的制备方法,其特征是,脱模后对产品进行10-100kGy的辐射处理。
9.根据权利要求1所述的一种环保软瓷的制备方法,其特征是,所述原料还含有0.5-1.5份的抗氧化剂和/或0.5-1.5份的紫外线吸收剂。
10.根据权利要求1所述的一种环保软瓷的制备方法,其特征是,脱模得到的产品进行介质阻挡放电等离子体处理,再喷淋雾化的硬脂酸。
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