CN113667061B - 一种吸水树脂及其制备方法与应用 - Google Patents
一种吸水树脂及其制备方法与应用 Download PDFInfo
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Abstract
本发明提供一种吸水树脂及其制备方法与应用。所述吸水树脂的原料包括:火山灰活性材料,所述火山灰活性材料的火山灰活性指数为60~95%。将该吸水树脂用于高强度自养护混凝土中,在混凝土碱性条件下火山灰活性材料的凝胶活性被激发,发生水化反应,所得水化产物填补了吸水树脂失水后留下的孔隙,可以有效的减少混凝土强度的降低,提高混凝土的强度和耐久性。
Description
技术领域
本发明属于建筑材料技术领域,具体涉及一种吸水树脂及其制备方法与应用。
背景技术
随着建筑技术的发展,混凝土逐渐向轻质高强方向发展,呈现出低水胶比、水泥细度大等特点。混凝土早期强度发展较快,容易出现应力集中,从而导致混凝土开裂。在混凝土中加入超吸水树脂(SAP)可以缓慢释放水分,进一步促进水泥水化,增加混凝土的耐久性,但SAP释放水后所形成的孔隙会降低混凝土的强度。
通过有机-无机复合制备SAP,可以增加SAP的强度和耐盐性。目前已经有研究将高岭土、膨润土等无机材料在合成过程中加入到SAP中,制备有机-无机复合SAP。这种SAP比传统的吸水率和吸盐水率都有一定的提高,但加入到混凝土中仍然会降低混凝土的强度。
发明内容
本发明提供了一种吸水树脂及其制备方法与应用,该吸水树脂具有优异的保水性能,而且加入水泥基材料后,不影响水泥基材料的强度。
具体来说,本发明提供了如下技术方案:
一种吸水树脂,其原料包括:火山灰活性材料。
所述火山灰活性又称潜在水硬性,火山灰活性材料是以含活性二氧化硅和氧化铝为主要矿物的材料,其本身基本不具有水化活性或活性较弱,在外界激发条件下可与水发生反应生成胶凝材料。
本发明的吸水树脂加入到水泥基材料中后,在水泥基中的碱性条件下,火山灰活性材料的凝胶活性被激发,发生水化反应,水化产物填补了吸水树脂失水后留下的空隙,可以有效的减少混凝土强度的降低。
在优选的实施方案中,所述火山灰活性材料的火山灰活性指数为60~95%。发明人发现,如果火山灰活性材料的火山灰活性指数偏大,则制备得到的吸水树脂贮存稳定性差,在普通环境下火山灰活性材料既会发生水化反应,如果火山灰活性材料的火山灰活性指数果过低,则对水泥基材料的密实度增加幅度较小。
在优选的实施方案中,所述火山灰活性材料含有钒钛矿渣和/或表面改性剂改性的钒钛矿渣,所述表面改性剂选自3-氨丙基三乙氧基硅烷、γ-缩水甘油醚氧丙基三甲氧基硅烷和γ-巯丙基三乙氧基硅烷、十六烷基三甲氧基硅烷中的一种或多种。
以钒钛磁铁矿为原料在高炉炼铁时产生的废渣称为钒钛矿渣。钒钛矿渣的主要化学成分为CaO、Si02、Al2O3、MgO等。发明人发现,钒钛矿渣的火山灰活性最适宜用作本发明的火山灰活性材料,利用其制备的复合吸水树脂吸液率高,在吸水树脂制作过程中基本与水不反应,当吸水树脂加入到水泥基材料中后,在水泥基中的碱性条件下,钒钛矿渣被激发发生水化反应,形成水化硅酸钙,进而避免了混凝土强度的降低,兼顾了优异的贮存稳定性和提高混凝土耐久性能。
在优选的实施方案中,所述吸水树脂的原料包括聚合单体、中和剂、水溶性纤维素、引发剂、交联剂和所述火山灰活性材料;
在更优选的实施方案中,
所述聚合单体为丙烯酸和/或丙烯酰胺;
和/或,所述中和剂选自氢氧化钠、氢氧化钙、氢氧化钾中的一种或多种;
和/或,所述水溶性纤维素选自羧甲基纤维素、海藻酸钠、壳聚糖中的一种或多种;
和/或,所述引发剂为过硫酸钾和/或过硫酸铵;
和/或,所述交联剂为N,N′-亚甲基双丙烯酰胺。
在优选的实施方案中,所述吸水树脂的原料包括50~80重量份聚合单体、10~20重量份中和剂、1~5重量份水溶性纤维素、0.03~0.40重量份引发剂、0.01~0.06重量份交联剂、1~10重量份所述火山灰活性材料。
本发明还保护上述吸水树脂的制备方法,包括以下步骤:
将聚合单体、中和剂和水混合,得到部分中和的聚合单体溶液;
将所述部分中和的聚合单体溶液、水溶性纤维素、引发剂、交联剂和火山灰活性材料混合,得到待聚合料液;
将所述待聚合料液引发聚合反应,得到所述吸水树脂。
在优选的实施方案中,所述部分中和的聚合单体溶液中,聚合单体的中和度为70~90%。
在优选的实施方案中,通过加热引发所述聚合反应,加热温度为50~80℃,加热时间为2~4h。
本发明还保护上述的吸水树脂或上述制备方法制得的吸水树脂在混凝土添加剂领域中的应用。添加上述吸水树脂的混凝土,吸水树脂中有机组分缓慢释放水分,促进胶凝材料水化,减少混凝土收缩开裂;同时,在混凝土中碱性条件下火山灰活性材料激发出潜在的胶凝活性,水化产物填补有机组分失水后留下的孔隙,减少这些孔隙导致混凝土强度降低,有效降低混凝土的收缩,提高混凝土的耐久性,且不降低混凝土的强度。
本发明还保护一种自养护混凝土,其原料包括上述的吸水树脂或上述制备方法制得的吸水树脂;优选的,所述原料包括:水泥600~900重量份、砂子800~1000重量份、石子400~450重量份、水160~170重量份、减水剂20~25重量份、吸水树脂1~5重量份。
本发明所取得的有益效果:
本发明提供的吸水树脂中,火山灰活性材料提供骨架,有机组分吸收液体,进入到混凝土中后火山灰活性材料反应形成胶凝材料,填补失水后的空隙,有效阻止了混凝土强度的降低,为高强混凝土的发展提供了有力的技术支持。
具体实施方式
以下实施例用于说明本发明,但不用来限制本发明的范围。实施例中未注明具体技术或条件者,按照本领域内的文献所描述的技术或条件,或者按照产品说明书进行。
以下实施例中,所用仪器等未注明生产厂商者,均为可通过正规渠道商购买得到的常规产品。所述方法如无特别说明均为常规方法,所述原材料如无特别说明均能从公开商业途径而得。
以下实施例中,所述钒钛矿渣粉来源于河北省承德地区某厂,具体成分如下表:
钒钛矿渣的化学组成(wt%)
以下实施例中,所述改性钒钛矿渣粉通过以下方法制备得到:将5kg钒钛矿渣粉和50kg碳酸氢铵水溶液(浓度为10%)投入反应釜中,搅拌均匀后,在150℃下烘干得到羟基活化的钒钛矿渣粉;然后将9.5kg所述羟基活化的钒钛矿渣粉和9.5kgγ-巯丙基三乙氧基硅烷乙醇水溶液(浓度为10%)加入反应釜中,反应1h,在120℃下焙烧2h,得到改性钒钛矿渣粉。
实施例1
本实施例提供一种有机-无机复合吸水树脂SAF,制备方法包括以下步骤:
将60kg丙烯酸、13kg氢氧化钠和80kg水进行混合,释放大量的热,得到部分中和的小分子单体溶液;
将中和的小分子单体溶液和4kg海藻酸钠加入到反应釜中,快速搅拌5分钟,混合均匀,无大块团聚体出现;向反应釜中加入0.125kg过硫酸铵和0.06kg N,N′-亚甲基双丙烯酰胺,快速搅拌并加热;
加热到45℃后,向反应釜中加入2kg钒钛矿渣粉(火山灰活性指数为75),反应3小时后,停止加热,得到超吸水树脂。将所述吸水树脂剪成小块,105℃烘干后,粉磨得到吸水树脂。
实施例2
本实施例提供一种有机-无机复合吸水树脂SAFG,该制备方法包括以下步骤:
将50kg丙烯酸、10kg丙烯酰胺、11kg氢氧化钠和80kg水进行混合,释放大量的热,得到部分中和的小分子单体溶液;
将中和的小分子单体溶液和4kg海藻酸钠加入到反应釜中,快速搅拌5分钟,混合均匀,无大块团聚体出现;向反应釜中加入0.125kg过硫酸铵和0.06kgN,N′-亚甲基双丙烯酰胺,快速搅拌并加热;
加热到45℃后,向反应釜中加入5kg改性钒钛矿渣粉(火山灰活性指数为77),反应3.5小时后,停止加热,得到超吸水树脂。将所述吸水树脂剪成小块,105℃烘干后,粉磨得到吸水树脂。
实施例3
本实施例提供一种有机-无机复合吸水树脂CMFG,该制备方法包括以下步骤:
将50kg丙烯酸、15kg丙烯酰胺、11kg氢氧化钠和80kg水进行混合,释放大量的热,得到部分中和的小分子单体溶液;
将中和的小分子单体溶液和3.5kg羧甲基纤维素加入到反应釜中,快速搅拌5分钟,混合均匀,无大块团聚体出现;向反应釜中加入0.20kg过硫酸钾和0.025kg N,N′-亚甲基双丙烯酰胺,快速搅拌并加热;
加热到45℃后,向反应釜中加入5kg改性钒钛矿渣粉,反应4小时后,停止加热,得到超吸水树脂。将所述吸水树脂剪成小块,105℃烘干后,粉磨得到吸水树脂。
实施例4
本实施例提供一种有机-无机复合吸水树脂CTFG,该制备方法包括以下步骤:
将50kg丙烯酸、10kg丙烯酰胺、11kg氢氧化钠和80kg水进行混合,释放大量的热,得到部分中和的小分子单体溶液;
将中和的小分子单体溶液和3.5kg壳聚糖加入到反应釜中,快速搅拌5分钟,混合均匀,无大块团聚体出现;向反应釜中加入0.40kg过硫酸钾和0.05kgN,N′-亚甲基双丙烯酰胺,快速搅拌并加热;
加热到45℃后,向反应釜中加入5kg改性钒钛矿渣粉,反应3小时后,停止加热,得到超吸水树脂。将所述吸水树脂剪成小块,105℃烘干后,粉磨得到吸水树脂。
实施例5
本实施例提供一种有机-无机复合吸水树脂SAMG,该制备方法包括以下步骤:
将50kg丙烯酸、10kg丙烯酰胺、11kg氢氧化钠和80kg水进行混合,释放大量的热,得到部分中和的小分子单体溶液;
将中和的小分子单体溶液和3.5kg海藻酸钠加入到反应釜中,快速搅拌5分钟,混合均匀,无大块团聚体出现;向反应釜中加入0.40kg过硫酸钾和0.05kgN,N′-亚甲基双丙烯酰胺,快速搅拌并加热;
加热到45℃后,向反应釜中加入5kg火山灰活性指数105%的S105矿粉,反应3小时后,停止加热,得到超吸水树脂。将所述吸水树脂剪成小块,105℃烘干后,粉磨得到吸水树脂。
实施例6
本实施例提供一种有机-无机复合吸水树脂SAFA,该制备方法包括以下步骤:
将50kg丙烯酸、10kg丙烯酰胺、11kg氢氧化钠和80kg水进行混合,释放大量的热,得到部分中和的小分子单体溶液;
将中和的小分子单体溶液和3.5kg海藻酸钠加入到反应釜中,快速搅拌5分钟,混合均匀,无大块团聚体出现;向反应釜中加入0.40kg过硫酸钾和0.05kgN,N′-亚甲基双丙烯酰胺,快速搅拌并加热;
加热到45℃后,向反应釜中加入5kg二级粉煤灰(火山灰活性指数为70),反应3小时间后,停止加热,得到超吸水树脂。将所述吸水树脂剪成小块,105℃烘干后,粉磨得到吸水树脂。
对比例1
本实施例提供一种纯有机吸水树脂SAPP,该制备方法包括以下步骤:
将50kg丙烯酸、10kg丙烯酰胺、11kg氢氧化钠和80kg水进行混合,释放大量的热,得到部分中和的小分子单体溶液;
将中和的小分子单体溶液和3.5kg海藻酸钠加入到反应釜中,快速搅拌5分钟,混合均匀,无大块团聚体出现;向反应釜中加入0.40kg过硫酸钾和0.05kgN,N′-亚甲基双丙烯酰胺,快速搅拌并加热到45℃进行反应;
反应3小时后,停止加热,得到超吸水树脂。将所述吸水树脂剪成小块,105℃烘干后,粉磨得到吸水树脂。
实验例1(吸水率实验)
称取0.50g吸水树脂放入到100目的尼龙网袋中,称取吸液前尼龙网袋和吸水树脂的总质量m1,将网袋浸泡在自来水和饱和氢氧化钙溶液中,浸泡2h后取出尼龙网袋,悬挂15分钟至网袋不再滴水后,称取吸液后尼龙网袋质量和超吸水树脂总质量m2。
吸液率=(m2-m1)/0.5;测试结果如表1。
表1吸水树脂的吸水率
实验例2(自养护混凝土性能测试)
测试所用的自养护混凝土的原材料如下所示:
原材料采用:P.I 42.5水泥,河砂细度模数2.8小砂子,石英石(1~0.5mm和0.5~0.08mm两级级配)大砂子,二级粉煤灰,S95矿粉,聚羧酸减水剂,实施例1-6制备的吸水树脂SAF、SAFG、CMFG、CTFG、SAMG、SAFA中的一种或对比例1制备的吸水树脂SAPP。
所述的自养护混凝土的配方如下表2所示。
表2自养护混凝土配合比(kg/m3)
按照GB50080、GB50081和GB50082测试混凝土的流动性、28天抗压强度和28天混凝土收缩,结果如表3所示:
表3自养护混凝土的性能
试验组 | 坍落度/mm | 28d抗压强度/MPa | 28d干燥收缩/×10-6 |
1 | 220 | 99.05 | 634 |
2 | 225 | 83.73 | 378 |
3 | 210 | 85.61 | 329 |
4 | 215 | 98.70 | 333 |
5 | 210 | 96.53 | 356 |
6 | 210 | 89.10 | 325 |
7 | 215 | 109.75 | 320 |
8 | 210 | 110.80 | 264 |
9 | 215 | 102.90 | 306 |
10 | 210 | 101.65 | 243 |
由表3可见,试验组1为基准组,试验组2将粉煤灰、有机吸水树脂加入到混凝土中,实验组3将矿渣粉、吸水树脂加入到混凝土中,试验组4将粉煤灰与有机吸水树脂复合后加入到混凝土,试验组5将矿粉与有机吸水树脂复合后加入到混凝土,实验组6为只加有机吸水树脂。试验发现无论以何种形式加入到混凝土中,粉煤灰、矿粉和有机吸水树脂都可以降低混凝土的干燥收缩,试验组2~6,分别降低收缩40%,48%,48%,44%和49%,但是将粉煤灰或矿粉与有机组分分开加入到混凝土中会降低混凝土的强度。实验组2~6,分别降低强度15%,14%,3%、0%和1%。
试验组7~10组为加入不同类型的有机-矾钛矿渣粉进行试验。试验发现,7~10组的干燥收缩分别降低了50%、58%、52%和60%,显著降低了混凝土的干燥收缩。而且其分别增加混凝土的强度11%、12%、4%和3%。
掺加吸水树脂SAMG的试验组5,混凝土的强度略有降低;掺加有机-粉煤灰复合吸水树脂SAFA的试验组4,混凝土的强度基本不变。这两组都没能像7~10组那样增加混凝土28天的强度,主要是因为SAMG和SAFA吸收饱和氢氧化钙溶液量较小(表1),对混凝土后期的养护作用没有有机-矾钛矿渣好。同时,SAMG中所用S105矿粉的火山灰活性较高,在制备吸水树脂过程中可能有部分已经发生水化,也影响了后期的补强作用。
通过以上对比可以发现,掺加纯有机吸水树脂会降低混凝土的强度,掺加有机-无机复合吸水树脂可以增加混凝土的强度,但要求复合吸水树脂有较好的吸收饱和氢氧化钙溶液的能力,且复合吸水树脂中的无机组分的火山灰活性不能太高。
虽然,上文中已经用一般性说明、具体实施方式及试验,对本发明作了详尽的描述,但在本发明基础上,可以对其作一些修改或改进,这对本领域技术人员而言是显而易见的。因此,在不偏离本发明精神的基础上所做的这些修改或改进,均属于本发明要求保护的范围。
Claims (7)
1.一种吸水树脂,其特征在于,其原料包括:火山灰活性材料;所述火山灰活性材料的火山灰活性指数为60~95%,所述火山灰活性材料为钒钛矿渣和/或表面改性剂改性的钒钛矿渣;
所述钒钛矿渣包括如下质量百分比的组分:CaO 38.73%、SiO224.74%、Al2O311.88%、MgO 10.00%、TiO2 9.04%、SO3 1.71%、Fe2O31.44%、Na2O 0.81%、K2O 0.55%、MnO 0.35%、Cl 0.28%;
所述原料包括50~80重量份聚合单体、10~20重量份中和剂、1~5重量份水溶性纤维素、0.03~0.40重量份引发剂、0.01~0.06重量份交联剂和1~10重量份所述火山灰活性材料;
所述表面改性剂改性的钒钛矿渣通过以下方法制备得到:将5kg钒钛矿渣粉和50kg浓度为10%的碳酸氢铵水溶液投入反应釜中,搅拌均匀后,在150℃下烘干得到羟基活化的钒钛矿渣粉;然后将9.5kg所述羟基活化的钒钛矿渣粉和9.5kg浓度为10%的γ-巯丙基三乙氧基硅烷乙醇水溶液加入反应釜中,反应1h,在120℃下焙烧2h,得到改性钒钛矿渣粉;
所述吸水树脂的制备方法,包括以下步骤:
将聚合单体、中和剂和水混合,得到部分中和的聚合单体溶液;所述部分中和的聚合单体溶液中,聚合单体的中和度为70~90%;
将所述部分中和的聚合单体溶液、水溶性纤维素、引发剂、交联剂和火山灰活性材料混合,得到待聚合料液;
将所述待聚合料液引发聚合反应,得到所述吸水树脂。
2.根据权利要求1所述的吸水树脂,其特征在于,所述聚合单体为丙烯酸和/或丙烯酰胺;
和/或,所述中和剂选自氢氧化钠、氢氧化钙、氢氧化钾中的一种或多种;
和/或,所述水溶性纤维素选自羧甲基纤维素、海藻酸钠、壳聚糖中的一种或多种;
和/或,所述引发剂为过硫酸钾和/或过硫酸铵;
和/或,所述交联剂为N,N′-亚甲基双丙烯酰胺。
3.权利要求1或2所述的吸水树脂的制备方法,其特征在于,包括以下步骤:
将聚合单体、中和剂和水混合,得到部分中和的聚合单体溶液;
将所述部分中和的聚合单体溶液、水溶性纤维素、引发剂、交联剂和火山灰活性材料混合,得到待聚合料液;
将所述待聚合料液引发聚合反应,得到所述吸水树脂。
4.根据权利要求3所述的制备方法,其特征在于,所述部分中和的聚合单体溶液中,聚合单体的中和度为70~90%。
5.根据权利要求3或4所述的制备方法,其特征在于,通过加热引发所述聚合反应,加热温度为50~80℃,加热时间为2~4h。
6.权利要求1或2所述的吸水树脂或权利要求3-5任一项制备方法制得的吸水树脂在混凝土添加剂领域中的应用。
7.一种自养护混凝土,其特征在于,其原料包括权利要求1或2所述的吸水树脂或权利要求3-5任一项制备方法制备得到吸水树脂;所述原料包括:水泥600~900重量份、砂子800~1000重量份、石子400~450重量份、水160~170重量份、减水剂20~25重量份、吸水树脂1~5重量份。
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