CN112521043B - 一种混凝土改性减水剂及其制备方法 - Google Patents
一种混凝土改性减水剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种混凝土改性减水剂及其制备方法,将改性底物载体、双酚A性环氧树脂、添加物进行共混反应,通过十二叔胺和温度的控制使得双酚A性环氧树脂上的两个环氧基开环,其中一个开环的环氧基与改性底物载体上的邻苯二酚基团反应,另一个开环的环氧基与添加物侧链上的氨基进行反应,使得添加物固定在改性底物载体上,制得改性减水剂,并将增强液与聚乙烯吡咯烷酮溶液混合,进而进行静电纺丝,得到底物载体,该底物载体能够使得混凝土的韧性增强,并能够改善混凝土的结构,使得总孔隙率减少,毛细孔径减小,进而增加了混凝土的抗渗性,防止了混凝土的开裂。
Description
技术领域
本发明涉及混凝土制备技术领域,具体涉及一种混凝土改性减水剂及其制备方法。
背景技术
混凝土是现代应用最广泛的建筑材料,其具有原料丰富、价格低廉、工艺简单、强度高、耐久性好等优点。预拌混凝土是混凝土的一种,是指由水泥、集料、水以及根据需要掺入的外加剂、矿物掺合料等组分按一定比例在搅拌站经计量、拌制后出售的、并采用运输车在规定时间内运至使用地点的混凝土拌合物。因为现场施工对环境影响较大,所以预拌混凝土受到越来越多的关注。
现有的混凝土改性减水剂,在使用过程中能够达到减水效果,但制备出的混凝土强度一般,长时间使用后,混凝土会出现开裂的现象,且受到外力作用时,易出现破损。
发明内容
本发明的目的在于提供一种混凝土改性减水剂及其制备方法。
本发明要解决的技术问题:
现有的混凝土改性减水剂,在使用过程中能够达到减水效果,但制备出的混凝土强度一般,长时间使用后,混凝土会出现开裂的现象,且受到外力作用时,易出现破损。
本发明的目的可以通过以下技术方案实现:
一种混凝土改性减水剂,由如下步骤制成:
步骤S1:将对硝基苯乙烯、铁粉、乙醇加入反应釜中,在温度为80-85℃的条件下,进行回流反应3-5h后,加入盐酸溶液,加入时间20min,继续反应5-8h后,调节反应液pH值为7-8,制得对氨基苯乙烯;
步骤S2:将烯丙基聚乙二醇和甲基丙烯磺酸钠加入反应釜中,在温度为60-65℃的条件下,进行溶解后加入丙烯酸、对氨基苯乙烯、过硫酸铵水溶液,在温度为80-90℃的条件下,进行反应2-3h后,降温至室温,过滤去除滤液,将滤饼烘干,制得添加物;
添加物结构式为:
步骤S3:将底物载体浸泡在多巴胺溶液中,在温度为25-30℃的条件下,浸泡20-24h后,过滤去除滤液,将滤饼烘干制得改性底物载体,将改性底物载体、双酚A性环氧树脂、2-辛酮加入反应釜中,在转速为150-200r/min的条件下,进行搅拌至均匀后,加入步骤S2制得的添加物和十二叔胺,在温度为120-150℃的条件下,进行反应5-8h后,过滤去除滤液,将滤饼进行烘干,制得改性减水剂。
进一步,步骤S1所述的对硝基苯乙烯、铁粉、乙醇、盐酸溶液的用量比为2.8g:4.53g:60mL:10mL,乙醇的体积分数为90%,盐酸溶液为质量分数为36%的浓盐酸和体积分数95%的乙醇以体积比1:9混合,步骤S2所述的烯丙基聚乙二醇、甲基丙烯磺酸钠、丙烯酸、对氨基苯乙烯、过硫酸铵水溶液的用量比为2g:3g:1g:2g:5mL,过硫酸铵水溶液的质量分数为15-20%,步骤A3所述的多巴胺溶液的浓度为0.5g/L,改性底物载体、双酚A性环氧树脂、添加物、十二叔胺的用量质量比为2:5:3:0.2。
进一步,所述底物载体由如下步骤制成:
步骤A1:将高岭土粉加入马弗炉中,在升温速率为10-15℃/min的条件下,进行升温至600℃,煅烧1-1.5h后,继续升温至800℃,煅烧2-3h后,在降温速率为5-10℃/min的条件下,进行降温至温度到达室温,停止加热,制得活化高岭土粉;
步骤A2:将碳纳米管分散在浓硫酸溶液中,加入浓硝酸溶液,在转速为150-200r/min,温度为110℃的条件下,进行搅拌5-8h后,加入去离子水继续搅拌10-15min后,过滤去除滤液,制得羧基化碳纳米管,将羧基化碳纳米管分散在去离子水中,加入步骤A1制得的活性高岭土粉,在频率为8-10MHz的条件下,进行超声处理1-1.5h后,过滤去除滤液,将滤饼进行烘干,制得改性碳纳米管;
步骤A3:将步骤A2制得的改性碳纳米管分散在N,N-二甲基甲酰胺中,加入4,4-二氨基二苯醚,通入氮气进行保护,在温度为160-170℃的条件下,进行搅拌回流10-15h后,加入3,3’,4,4’-联苯四甲酸二酐,在转速为200-300r/min,温度为零下5-3℃的条件下,进行搅拌10-15h,制得增强碳纳米管;
步骤A4:将钛酸四丁酯和无水乙醇加入反应釜中,在转速为120-130r/min,温度为50-55℃的条件下,进行搅拌并滴加冰醋酸溶液,滴加速度为0.05mL/s,滴加完毕后,加入聚乙二醇并调节反应液pH至为2-3,进行反应15-20min后,加入步骤A3制得的增强碳纳米管,在频率为5-8MHz的条件下,进行超声处理1-1.5h,制得增强液;
步骤A5:将聚乙烯吡咯烷酮和无水乙醇加入反应釜中,在转速为200-300r/min的条件下,进行搅拌至聚乙烯吡咯烷酮完全溶解后,加入步骤A4制得的增强液,在转速为500-800r/min的条件下,进行搅拌30-40min后,在电压为25KV,喷丝针尖与接收距离为20厘米,流速为0.5mL/h的条件下,进行静电纺丝,纺丝完毕后,在温度为60-70℃的条件下,进行烘干,制得底物载体。
进一步,步骤A2所述的碳纳米管、浓硫酸溶液、浓硝酸溶液的用量比为0.5g:45mL:15mL,浓硫酸溶液的质量分数为70%,浓硝酸的质量分数为68%,羧基化碳纳米管和活性高岭土粉的用量比质量比为5:1.8-2.3。
进一步,步骤A3所述的改性碳纳米管、4,4-二氨基二苯醚、3,3’,4,4’-联苯四甲酸二酐的用量质量比为8:3:3。
进一步,步骤A4所述的钛酸四丁酯、无水乙醇、冰醋酸溶液、聚乙二醇的用量比为10mL:20mL:25mL:1g,冰醋酸溶液为无水乙醇和冰醋酸以体积比2.5:2混合,增强碳纳米管的用量为钛酸四丁酯、无水乙醇、冰醋酸溶液、聚乙二醇总质量的50-60%。
进一步,步骤A5所述的聚乙烯吡咯烷酮、增强液的用量体积比为5:4。
一种混凝土改性减水剂的制备方法,具体包括如下步骤:
步骤S1:将对硝基苯乙烯、铁粉、乙醇加入反应釜中,在温度为80-85℃的条件下,进行回流反应3-5h后,加入盐酸溶液,加入时间20min,继续反应5-8h后,调节反应液pH值为7-8,制得对氨基苯乙烯;
步骤S2:将烯丙基聚乙二醇和甲基丙烯磺酸钠加入反应釜中,在温度为60-65℃的条件下,进行溶解后加入丙烯酸、对氨基苯乙烯、过硫酸铵水溶液,在温度为80-90℃的条件下,进行反应2-3h后,降温至室温,过滤去除滤液,将滤饼烘干,制得添加物;
步骤S3:将底物载体浸泡在多巴胺溶液中,在温度为25-30℃的条件下,浸泡20-24h后,过滤去除滤液,将滤饼烘干制得改性底物载体,将改性底物载体、双酚A性环氧树脂、2-辛酮加入反应釜中,在转速为150-200r/min的条件下,进行搅拌至均匀后,加入步骤S2制得的添加物和十二叔胺,在温度为120-150℃的条件下,进行反应5-8h后,过滤去除滤液,将滤饼进行烘干,制得改性减水剂。
本发明的有益效果:本发明在制备一种混凝土改性减水剂时,以对硝基苯乙烯为原料,将对硝基苯乙烯用铁粉进行还原,使得苯环对位上硝基转变为氨基,制得对氨基苯乙烯,将对氨基苯乙烯、烯丙基聚乙二烯、甲基丙烯磺酸钠、丙烯酸、对氨基苯乙烯进行聚合,制得添加物,再将底物载体浸泡在多巴胺溶液中,多巴胺在底物载体表面形成一层聚多巴胺层,制得改性底物载体,将改性底物载体、双酚A性环氧树脂、添加物进行共混反应,通过十二叔胺和温度的控制使得双酚A性环氧树脂上的两个环氧基开环,其中一个开环的环氧基与改性底物载体上的邻苯二酚基团反应,另一个开环的环氧基与添加物侧链上的氨基进行反应,使得添加物固定在改性底物载体上,制得改性减水剂,该改性减水剂中的羧基和磺酸基提供了吸附点和静电斥力,在水泥颗粒表面定向吸附,部分极性基团指向液相,亲水基团的电离作用使得水泥颗粒表面带上相同的正电荷或负电荷,进而形成双电层,使得水泥颗粒之间形成静电斥力,破坏水泥颗粒的絮凝结构,使颗粒相互分散,释放出絮团中的自由水,从而增大拌合物流动性,底物载体以高岭土粉为原料通过煅烧将结晶水的数量减少,制得活化高岭土粉,在将碳纳米管用浓硫酸和浓硝酸进行氧化,使得碳纳米管羧基化,将羧基化碳纳米管分散在去离子水中,在与活性高岭土粉进行超声处理,使得活性高岭土粉嵌与羧基化碳纳米管表面间隙中,制得改性碳纳米管,将4,4-二氨基二苯醚和3,3’,4,4’-联苯四甲酸二酐进行聚合并与改性碳纳米管表面的羧基进行反应,使得碳纳米管表面接枝有聚酰亚胺,进而将钛酸四丁酯进行反应制得二氧化钛胶溶并与增强碳纳米管共混,的到增强液,并将增强液与聚乙烯吡咯烷酮溶液混合,进而进行静电纺丝,得到底物载体,该底物载体能够使得混凝土的韧性增强,并能够改善混凝土的结构,使得总孔隙率减少,毛细孔径减小,进而增加了混凝土的抗渗性,防止了混凝土的开裂。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1
一种混凝土改性减水剂,由如下步骤制成:
步骤S1:将对硝基苯乙烯、铁粉、乙醇加入反应釜中,在温度为80℃的条件下,进行回流反应3h后,加入盐酸溶液,加入时间20min,继续反应5h后,调节反应液pH值为7,制得对氨基苯乙烯;
步骤S2:将烯丙基聚乙二醇和甲基丙烯磺酸钠加入反应釜中,在温度为60℃的条件下,进行溶解后加入丙烯酸、对氨基苯乙烯、过硫酸铵水溶液,在温度为80℃的条件下,进行反应2h后,降温至室温,过滤去除滤液,将滤饼烘干,制得添加物;
步骤S3:将底物载体浸泡在多巴胺溶液中,在温度为25℃的条件下,浸泡20h后,过滤去除滤液,将滤饼烘干制得改性底物载体,将改性底物载体、双酚A性环氧树脂、2-辛酮加入反应釜中,在转速为150r/min的条件下,进行搅拌至均匀后,加入步骤S2制得的添加物和十二叔胺,在温度为120℃的条件下,进行反应5h后,过滤去除滤液,将滤饼进行烘干,制得改性减水剂。
所述底物载体由如下步骤制成:
步骤A1:将高岭土粉加入马弗炉中,在升温速率为10℃/min的条件下,进行升温至600℃,煅烧1h后,继续升温至800℃,煅烧2h后,在降温速率为5℃/min的条件下,进行降温至温度到达室温,停止加热,制得活化高岭土粉;
步骤A2:将碳纳米管分散在浓硫酸溶液中,加入浓硝酸溶液,在转速为150r/min,温度为110℃的条件下,进行搅拌5h后,加入去离子水继续搅拌10min后,过滤去除滤液,制得羧基化碳纳米管,将羧基化碳纳米管分散在去离子水中,加入步骤A1制得的活性高岭土粉,在频率为8MHz的条件下,进行超声处理1h后,过滤去除滤液,将滤饼进行烘干,制得改性碳纳米管;
步骤A3:将步骤A2制得的改性碳纳米管分散在N,N-二甲基甲酰胺中,加入4,4-二氨基二苯醚,通入氮气进行保护,在温度为160℃的条件下,进行搅拌回流10h后,加入3,3’,4,4’-联苯四甲酸二酐,在转速为200r/min,温度为零下5℃的条件下,进行搅拌10h,制得增强碳纳米管;
步骤A4:将钛酸四丁酯和无水乙醇加入反应釜中,在转速为120r/min,温度为50℃的条件下,进行搅拌并滴加冰醋酸溶液,滴加速度为0.05mL/s,滴加完毕后,加入聚乙二醇并调节反应液pH至为2,进行反应15min后,加入步骤A3制得的增强碳纳米管,在频率为5MHz的条件下,进行超声处理1h,制得增强液;
步骤A5:将聚乙烯吡咯烷酮和无水乙醇加入反应釜中,在转速为200r/min的条件下,进行搅拌至聚乙烯吡咯烷酮完全溶解后,加入步骤A4制得的增强液,在转速为500r/min的条件下,进行搅拌30min后,在电压为25KV,喷丝针尖与接收距离为20厘米,流速为0.5mL/h的条件下,进行静电纺丝,纺丝完毕后,在温度为60℃的条件下,进行烘干,制得底物载体。
实施例2
一种混凝土改性减水剂,由如下步骤制成:
步骤S1:将对硝基苯乙烯、铁粉、乙醇加入反应釜中,在温度为80℃的条件下,进行回流反应5h后,加入盐酸溶液,加入时间20min,继续反应5h后,调节反应液pH值为8,制得对氨基苯乙烯;
步骤S2:将烯丙基聚乙二醇和甲基丙烯磺酸钠加入反应釜中,在温度为60℃的条件下,进行溶解后加入丙烯酸、对氨基苯乙烯、过硫酸铵水溶液,在温度为90℃的条件下,进行反应2h后,降温至室温,过滤去除滤液,将滤饼烘干,制得添加物;
步骤S3:将底物载体浸泡在多巴胺溶液中,在温度为30℃的条件下,浸泡20h后,过滤去除滤液,将滤饼烘干制得改性底物载体,将改性底物载体、双酚A性环氧树脂、2-辛酮加入反应釜中,在转速为200r/min的条件下,进行搅拌至均匀后,加入步骤S2制得的添加物和十二叔胺,在温度为120℃的条件下,进行反应8h后,过滤去除滤液,将滤饼进行烘干,制得改性减水剂。
所述底物载体由如下步骤制成:
步骤A1:将高岭土粉加入马弗炉中,在升温速率为10℃/min的条件下,进行升温至600℃,煅烧1.5h后,继续升温至800℃,煅烧2h后,在降温速率为10℃/min的条件下,进行降温至温度到达室温,停止加热,制得活化高岭土粉;
步骤A2:将碳纳米管分散在浓硫酸溶液中,加入浓硝酸溶液,在转速为150r/min,温度为110℃的条件下,进行搅拌8h后,加入去离子水继续搅拌10min后,过滤去除滤液,制得羧基化碳纳米管,将羧基化碳纳米管分散在去离子水中,加入步骤A1制得的活性高岭土粉,在频率为10MHz的条件下,进行超声处理1h后,过滤去除滤液,将滤饼进行烘干,制得改性碳纳米管;
步骤A3:将步骤A2制得的改性碳纳米管分散在N,N-二甲基甲酰胺中,加入4,4-二氨基二苯醚,通入氮气进行保护,在温度为170℃的条件下,进行搅拌回流10h后,加入3,3’,4,4’-联苯四甲酸二酐,在转速为300r/min,温度为零下5℃的条件下,进行搅拌15h,制得增强碳纳米管;
步骤A4:将钛酸四丁酯和无水乙醇加入反应釜中,在转速为120r/min,温度为55℃的条件下,进行搅拌并滴加冰醋酸溶液,滴加速度为0.05mL/s,滴加完毕后,加入聚乙二醇并调节反应液pH至为2,进行反应20min后,加入步骤A3制得的增强碳纳米管,在频率为5MHz的条件下,进行超声处理1.5h,制得增强液;
步骤A5:将聚乙烯吡咯烷酮和无水乙醇加入反应釜中,在转速为200r/min的条件下,进行搅拌至聚乙烯吡咯烷酮完全溶解后,加入步骤A4制得的增强液,在转速为800r/min的条件下,进行搅拌30min后,在电压为25KV,喷丝针尖与接收距离为20厘米,流速为0.5mL/h的条件下,进行静电纺丝,纺丝完毕后,在温度为70℃的条件下,进行烘干,制得底物载体。
实施例3
一种混凝土改性减水剂,由如下步骤制成:
步骤S1:将对硝基苯乙烯、铁粉、乙醇加入反应釜中,在温度为85℃的条件下,进行回流反应3h后,加入盐酸溶液,加入时间20min,继续反应8h后,调节反应液pH值为7,制得对氨基苯乙烯;
步骤S2:将烯丙基聚乙二醇和甲基丙烯磺酸钠加入反应釜中,在温度为65℃的条件下,进行溶解后加入丙烯酸、对氨基苯乙烯、过硫酸铵水溶液,在温度为80℃的条件下,进行反应3h后,降温至室温,过滤去除滤液,将滤饼烘干,制得添加物;
步骤S3:将底物载体浸泡在多巴胺溶液中,在温度为25℃的条件下,浸泡24h后,过滤去除滤液,将滤饼烘干制得改性底物载体,将改性底物载体、双酚A性环氧树脂、2-辛酮加入反应釜中,在转速为150r/min的条件下,进行搅拌至均匀后,加入步骤S2制得的添加物和十二叔胺,在温度为150℃的条件下,进行反应5h后,过滤去除滤液,将滤饼进行烘干,制得改性减水剂。
所述底物载体由如下步骤制成:
步骤A1:将高岭土粉加入马弗炉中,在升温速率为15℃/min的条件下,进行升温至600℃,煅烧1h后,继续升温至800℃,煅烧3h后,在降温速率为5℃/min的条件下,进行降温至温度到达室温,停止加热,制得活化高岭土粉;
步骤A2:将碳纳米管分散在浓硫酸溶液中,加入浓硝酸溶液,在转速为200r/min,温度为110℃的条件下,进行搅拌5h后,加入去离子水继续搅拌15min后,过滤去除滤液,制得羧基化碳纳米管,将羧基化碳纳米管分散在去离子水中,加入步骤A1制得的活性高岭土粉,在频率为8MHz的条件下,进行超声处理1.5h后,过滤去除滤液,将滤饼进行烘干,制得改性碳纳米管;
步骤A3:将步骤A2制得的改性碳纳米管分散在N,N-二甲基甲酰胺中,加入4,4-二氨基二苯醚,通入氮气进行保护,在温度为160℃的条件下,进行搅拌回流15h后,加入3,3’,4,4’-联苯四甲酸二酐,在转速为200r/min,温度为零下3℃的条件下,进行搅拌10h,制得增强碳纳米管;
步骤A4:将钛酸四丁酯和无水乙醇加入反应釜中,在转速为130r/min,温度为50℃的条件下,进行搅拌并滴加冰醋酸溶液,滴加速度为0.05mL/s,滴加完毕后,加入聚乙二醇并调节反应液pH至为3,进行反应15min后,加入步骤A3制得的增强碳纳米管,在频率为8MHz的条件下,进行超声处理1h,制得增强液;
步骤A5:将聚乙烯吡咯烷酮和无水乙醇加入反应釜中,在转速为300r/min的条件下,进行搅拌至聚乙烯吡咯烷酮完全溶解后,加入步骤A4制得的增强液,在转速为500r/min的条件下,进行搅拌40min后,在电压为25KV,喷丝针尖与接收距离为20厘米,流速为0.5mL/h的条件下,进行静电纺丝,纺丝完毕后,在温度为60℃的条件下,进行烘干,制得底物载体。
实施例4
一种混凝土改性减水剂,由如下步骤制成:
步骤S1:将对硝基苯乙烯、铁粉、乙醇加入反应釜中,在温度为85℃的条件下,进行回流反应5h后,加入盐酸溶液,加入时间20min,继续反应8h后,调节反应液pH值为8,制得对氨基苯乙烯;
步骤S2:将烯丙基聚乙二醇和甲基丙烯磺酸钠加入反应釜中,在温度为65℃的条件下,进行溶解后加入丙烯酸、对氨基苯乙烯、过硫酸铵水溶液,在温度为90℃的条件下,进行反应3h后,降温至室温,过滤去除滤液,将滤饼烘干,制得添加物;
步骤S3:将底物载体浸泡在多巴胺溶液中,在温度为30℃的条件下,浸泡24h后,过滤去除滤液,将滤饼烘干制得改性底物载体,将改性底物载体、双酚A性环氧树脂、2-辛酮加入反应釜中,在转速为200r/min的条件下,进行搅拌至均匀后,加入步骤S2制得的添加物和十二叔胺,在温度为150℃的条件下,进行反应8h后,过滤去除滤液,将滤饼进行烘干,制得改性减水剂。
所述底物载体由如下步骤制成:
步骤A1:将高岭土粉加入马弗炉中,在升温速率为15℃/min的条件下,进行升温至600℃,煅烧1.5h后,继续升温至800℃,煅烧3h后,在降温速率为10℃/min的条件下,进行降温至温度到达室温,停止加热,制得活化高岭土粉;
步骤A2:将碳纳米管分散在浓硫酸溶液中,加入浓硝酸溶液,在转速为200r/min,温度为110℃的条件下,进行搅拌8h后,加入去离子水继续搅拌15min后,过滤去除滤液,制得羧基化碳纳米管,将羧基化碳纳米管分散在去离子水中,加入步骤A1制得的活性高岭土粉,在频率为10MHz的条件下,进行超声处理1.5h后,过滤去除滤液,将滤饼进行烘干,制得改性碳纳米管;
步骤A3:将步骤A2制得的改性碳纳米管分散在N,N-二甲基甲酰胺中,加入4,4-二氨基二苯醚,通入氮气进行保护,在温度为170℃的条件下,进行搅拌回流15h后,加入3,3’,4,4’-联苯四甲酸二酐,在转速为300r/min,温度为零下3℃的条件下,进行搅拌15h,制得增强碳纳米管;
步骤A4:将钛酸四丁酯和无水乙醇加入反应釜中,在转速为130r/min,温度为55℃的条件下,进行搅拌并滴加冰醋酸溶液,滴加速度为0.05mL/s,滴加完毕后,加入聚乙二醇并调节反应液pH至为3,进行反应20min后,加入步骤A3制得的增强碳纳米管,在频率为8MHz的条件下,进行超声处理1.5h,制得增强液;
步骤A5:将聚乙烯吡咯烷酮和无水乙醇加入反应釜中,在转速为300r/min的条件下,进行搅拌至聚乙烯吡咯烷酮完全溶解后,加入步骤A4制得的增强液,在转速为800r/min的条件下,进行搅拌40min后,在电压为25KV,喷丝针尖与接收距离为20厘米,流速为0.5mL/h的条件下,进行静电纺丝,纺丝完毕后,在温度为70℃的条件下,进行烘干,制得底物载体。
对比例
本对比例为市场上一种常见的混泥土减水剂。
将实施例1-4和对比例制得的减水剂用于混泥土制备,并对制备出的混凝土进行系能测试,测试结果如下表1所示;
表1
由上表1可知实施例1-4制得的减水剂制备出的水泥的最大抗渗压力为9.8-10.2MPa,抗压强度为165-172MPa,单向拉伸初裂强度为18-20MPa,而对比例制得的减水剂制备出的水泥的最大抗渗压力为6.5MPa,抗压强度为115MPa,单向拉伸初裂强度为8MPa,表明本发明能够让混凝土的强度提升。
以上内容仅仅是对本发明的构思所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明的构思或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (7)
1.一种混凝土改性减水剂,其特征在于:由如下步骤制成:
步骤S1:将对硝基苯乙烯、铁粉、乙醇加入反应釜中,在温度为80-85℃的条件下,进行回流反应3-5h后,加入盐酸溶液,加入时间20min,继续反应5-8h后,调节反应液pH值为7-8,制得对氨基苯乙烯;
步骤S2:将烯丙基聚乙二醇和甲基丙烯磺酸钠加入反应釜中,在温度为60-65℃的条件下,进行溶解后加入丙烯酸、对氨基苯乙烯、过硫酸铵水溶液,在温度为80-90℃的条件下,进行反应2-3h后,降温至室温,过滤去除滤液,将滤饼烘干,制得添加物;
步骤S3:将底物载体浸泡在多巴胺溶液中,在温度为25-30℃的条件下,浸泡20-24h后,过滤去除滤液,将滤饼烘干制得改性底物载体,将改性底物载体、双酚A性环氧树脂、2-辛酮加入反应釜中,在转速为150-200r/min的条件下,进行搅拌至均匀后,加入步骤S2制得的添加物和十二叔胺,在温度为120-150℃的条件下,进行反应5-8h后,过滤去除滤液,将滤饼进行烘干,制得改性减水剂;
所述底物载体由如下步骤制成:
步骤A1:将高岭土粉加入马弗炉中,在升温速率为10-15℃/min的条件下,进行升温至600℃,煅烧1-1.5h后,继续升温至800℃,煅烧2-3h后,在降温速率为5-10℃/min的条件下,进行降温至温度到达室温,停止加热,制得活化高岭土粉;
步骤A2:将碳纳米管分散在浓硫酸溶液中,加入浓硝酸溶液,在转速为150-200r/min,温度为110℃的条件下,进行搅拌5-8h后,加入去离子水继续搅拌10-15min后,过滤去除滤液,制得羧基化碳纳米管,将羧基化碳纳米管分散在去离子水中,加入步骤A1制得的活性高岭土粉,在频率为8-10MHz的条件下,进行超声处理1-1.5h后,过滤去除滤液,将滤饼进行烘干,制得改性碳纳米管;
步骤A3:将步骤A2制得的改性碳纳米管分散在N,N-二甲基甲酰胺中,加入4,4-二氨基二苯醚,通入氮气进行保护,在温度为160-170℃的条件下,进行搅拌回流10-15h后,加入3,3’,4,4’-联苯四甲酸二酐,在转速为200-300r/min,温度为零下5-3℃的条件下,进行搅拌10-15h,制得增强碳纳米管;
步骤A4:将钛酸四丁酯和无水乙醇加入反应釜中,在转速为120-130r/min,温度为50-55℃的条件下,进行搅拌并滴加冰醋酸溶液,滴加速度为0.05mL/s,滴加完毕后,加入聚乙二醇并调节反应液pH至为2-3,进行反应15-20min后,加入步骤A3制得的增强碳纳米管,在频率为5-8MHz的条件下,进行超声处理1-1.5h,制得增强液;
步骤A5:将聚乙烯吡咯烷酮和无水乙醇加入反应釜中,在转速为200-300r/min的条件下,进行搅拌至聚乙烯吡咯烷酮完全溶解后,加入步骤A4制得的增强液,在转速为500-800r/min的条件下,进行搅拌30-40min后,在电压为25KV,喷丝针尖与接收距离为20厘米,流速为0.5mL/h的条件下,进行静电纺丝,纺丝完毕后,在温度为60-70℃的条件下,进行烘干,制得底物载体。
2.根据权利要求1所述的一种混凝土改性减水剂,其特征在于:步骤S1所述的对硝基苯乙烯、铁粉、乙醇、盐酸溶液的用量比为2.8g:4.53g:60mL:10mL,乙醇的体积分数为90%,盐酸溶液为质量分数为36%的浓盐酸和体积分数95%的乙醇以体积比1:9混合,步骤S2所述的烯丙基聚乙二醇、甲基丙烯磺酸钠、丙烯酸、对氨基苯乙烯、过硫酸铵水溶液的用量比为2g:3g:1g:2g:5mL,过硫酸铵水溶液的质量分数为15-20%,步骤A3所述的多巴胺溶液的浓度为0.5g/L,改性底物载体、双酚A性环氧树脂、添加物、十二叔胺的用量质量比为2:5:3:0.2。
3.根据权利要求2所述的一种混凝土改性减水剂,其特征在于:步骤A2所述的碳纳米管、浓硫酸溶液、浓硝酸溶液的用量比为0.5g:45mL:15mL,浓硫酸溶液的质量分数为70%,浓硝酸的质量分数为68%,羧基化碳纳米管和活性高岭土粉的用量比质量比为5:1.8-2.3。
4.根据权利要求2所述的一种混凝土改性减水剂,其特征在于:步骤A3所述的改性碳纳米管、4,4-二氨基二苯醚、 3,3’,4,4’-联苯四甲酸二酐的用量质量比为8:3:3。
5.根据权利要求2所述的一种混凝土改性减水剂,其特征在于:步骤A4所述的钛酸四丁酯、无水乙醇、冰醋酸溶液、聚乙二醇的用量比为10mL:20mL:25mL:1g,冰醋酸溶液为无水乙醇和冰醋酸以体积比2.5:2混合,增强碳纳米管的用量为钛酸四丁酯、无水乙醇、冰醋酸溶液、聚乙二醇总质量的50-60%。
6.根据权利要求2所述的一种混凝土改性减水剂,其特征在于:步骤A5所述的聚乙烯吡咯烷酮、增强液的用量体积比为5:4。
7.根据权利要求1所述的一种混凝土改性减水剂的制备方法,其特征在于:具体包括如下步骤:
步骤S1:将对硝基苯乙烯、铁粉、乙醇加入反应釜中,在温度为80-85℃的条件下,进行回流反应3-5h后,加入盐酸溶液,加入时间20min,继续反应5-8h后,调节反应液pH值为7-8,制得对氨基苯乙烯;
步骤S2:将烯丙基聚乙二醇和甲基丙烯磺酸钠加入反应釜中,在温度为60-65℃的条件下,进行溶解后加入丙烯酸、对氨基苯乙烯、过硫酸铵水溶液,在温度为80-90℃的条件下,进行反应2-3h后,降温至室温,过滤去除滤液,将滤饼烘干,制得添加物;
步骤S3:将底物载体浸泡在多巴胺溶液中,在温度为25-30℃的条件下,浸泡20-24h后,过滤去除滤液,将滤饼烘干制得改性底物载体,将改性底物载体、双酚A性环氧树脂、2-辛酮加入反应釜中,在转速为150-200r/min的条件下,进行搅拌至均匀后,加入步骤S2制得的添加物和十二叔胺,在温度为120-150℃的条件下,进行反应5-8h后,过滤去除滤液,将滤饼进行烘干,制得改性减水剂。
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