CN115677249B - 一种水热合成粉煤灰硅酸盐骨料的制备方法 - Google Patents
一种水热合成粉煤灰硅酸盐骨料的制备方法 Download PDFInfo
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Abstract
本发明涉及硅酸盐骨料水热合成技术领域,且公开了一种水热合成粉煤灰硅酸盐骨料的制备方法,包括:以九水硅酸钠、氢氧化钾、无机‑有机杂化激发单体为原料复配得到无机‑有机复合型激发剂;配制硅酸盐骨料的原料,把计量好的粉煤灰、电石渣、生石灰、玻化微珠搅拌,加入无机‑有机复合型激发剂继续搅拌,制成混合料;成型方式采用成球盘,把成球核膨胀珍珠岩喷水润湿,加入制备好的混合料,边加入边喷水,静置养护,进入蒸压釜熟化活化处理,发生硅钙反应进行水热合成反应,得到水热合成硅酸盐骨料。本发明通过加快粉煤灰早期内部活性,并且全程激发粉煤灰的活性,制备得到了性能优异的硅酸盐骨料。
Description
技术领域
本发明涉及硅酸盐骨料水热合成技术领域,具体为一种水热合成粉煤灰硅酸盐骨料的制备方法。
背景技术
人工合成骨料具有密度小、筒压强度高、吸水率低、抗冻性能好等优点,其制品广泛应用于建筑结构、桥梁、隔热保温、吸音隔音等工程。传统的人造轻骨料以烧结陶粒为主,按堆积密度和筒压强度分为超轻陶粒﹑普通陶粒和高强陶粒等。随着装备水平的提高、工艺水平的进步以及国家环保政策的影响,非烧结类人造轻骨料的研究开发及应用将迎来新的快速发展阶段。
水热合成硅酸盐骨料是基于蒸压养护硬化方式提出的一种人工合成骨料,具体研究成果如下:一方面在湿基电石渣掺量为37.5%~43.4%,温度为180℃、压力为1MPa的养护条件下研制出了筒压强度高于市售陶粒4-6MPa、堆积密度低于900kg/m3、表观密度低于1800kg/m3的人造轻骨料;另一方面基于温度为180℃、压力为1.0MPa的饱和蒸汽蒸压养护工艺,研究了复掺不同矿物类型硅质材料和粉煤灰对环氧丙烷渣壳层陶粒及混凝土性能的影响,利用研制出的粗骨料配制出了立方体抗压强度最高达81.5MPa的次轻集料混凝土;并且方面研究表明,在基体相同的情况下,利用人造硅酸盐骨料等体积替换普通碎石,可配制出28d抗压强度与普通混凝土相当的人造硅酸盐骨料混凝土,但其表观密度比普通混凝土低约20.5%。
目前粉煤灰等工业固体废料一直可以用作混凝土掺合料使用,但是由于粉煤灰存在早期活性强度低的缺点,因此本发明提供一种加快粉煤灰早期内部活性,并且可以全程激发粉煤灰活性的水热合成粉煤灰硅酸盐骨料的制备方法。
发明内容
为了全程激发粉煤灰的活性,本发明提供一种水热合成粉煤灰硅酸盐骨料的制备方法,首先制备无机-有机复合型激发剂,该无机-有机复合型激发剂可以实现全程激发粉煤灰活性的作用,以氢氧化钾和九水硅酸钠为无机组分主要在早龄期激发粉煤灰的活性,促使粉煤灰颗粒表面的Si-O键和Al-O键断裂形成不饱和键,以无机-有机杂化激发单体(八羟基封端的POSS)为无机-有机杂化组分通过缓慢释放OH-在水化后期进一步激发粉煤灰的活性。
本发明提供一种水热合成粉煤灰硅酸盐骨料的制备方法,包括如下步骤:
步骤一,制备无机-有机复合型激发剂,其制备方法如下:
步骤Step1,制备无机-有机杂化激发单体,该无机-有机杂化激发单体是通过八巯基丙基笼状聚倍硅氧烷(POSS-SH8)的巯基官能团与丁烯醇单体的烯基官能团发生巯基-烯点击化学反应制备而成的,具体制备如下:将八巯基丙基笼状聚倍硅氧烷(POSS-SH8)、丁烯醇单体和四氢呋喃加入反应器中,待搅拌溶解后加入光引发剂,在波长365nm的UV灯照射下搅拌反应,反应过程中在暗室内进行,将反应液浓缩、沉淀、真空干燥至恒重,得到无机-有机杂化激发单体;
其中,丁烯醇单体为2-甲基-3-丁烯-2-醇、2,3-二甲基-3-丁烯-2-醇、3-甲基-3-丁烯-2-醇、3-丁烯-2-醇中的一种或几种组合;
光引发剂为光引发剂DMPA、光引发剂1173、光引发剂I907、光引发剂369、光引发剂2959中的一种;
步骤Step2,称取1-2重量份的九水硅酸钠、2-10重量份的氢氧化钾、0.3-1.5重量份的无机-有机杂化激发单体复配得到无机-有机复合型激发剂;
步骤二,配制硅酸盐骨料的原料,该原料包括:粉煤灰55%-75%,电石渣15%-25%,生石灰10%-20%,膨胀珍珠岩3%-5%,玻化微珠0.55%-1.50%,无机-有机复合型激发剂0.05-0.2%;
其中,膨胀珍珠岩的粒径为0.5-1mm;
步骤三,把计量好的粉煤灰、电石渣、生石灰、玻化微珠搅拌1-10min,加入无机-有机复合型激发剂继续搅拌1-5min,制成混合料;
步骤四,成型方式采用成球盘,把成球核膨胀珍珠岩喷水润湿,加入制备好的混合料,边加入边喷水,成型直径5mm-10mm,静置养护1-3h,进入蒸压釜,在温度为160-200℃、压力为1-1.3MPa的蒸压养护条件下进行熟化活化处理,发生硅钙反应进行水热合成反应,得到水热合成硅酸盐骨料;
其中,蒸压养护条件优选工艺参数为:温度为180℃、压力为1.15MPa。
本发明提供一种水热合成粉煤灰硅酸盐骨料,包括:粉煤灰55%-75%,电石渣15%-25%,生石灰10%-20%,膨胀珍珠岩3%-5%,玻化微珠0.55%-1.50%,无机-有机复合型激发剂0.05-0.2%,其吸水率为5.4%-7.8%、堆积密度为690-730kg/m3、筒压强度为10.7-18.3MPa。
与现有技术相比,本发明具备以下有益的技术效果:
本发明通过复配得到无机-有机复合型激发剂,其中的氢氧化钾和九水硅酸钠主要在早龄期激发粉煤灰的活性,促使粉煤灰颗粒表面的Si-O键和Al-O键断裂形成不饱和键,Na+较强的水化能力易于形成Si(OH)4单体,K+可加速Si(OH)4和AI(OH)-四面体之间的缩聚和重组,形成更多的三维骨架结构中的Q4 4结构单元,并且与电石渣中形成的活性Ca(OH)2反应生成水化硅酸钙C-S-H和水化铝酸钙C-A-H等凝胶材料,而无机-有机杂化激发单体主要在水化后期提供OH-进一步激发粉煤灰的活性生成活性Ca(OH)2,并且无机-有机杂化激发单体可填充在网状骨架结构的间隙中,其中的笼型POSS结构可以提高硅酸盐骨料的强度,并且POSS上延伸的有机结构对于硅酸盐骨料的柔韧性能也能够产生一定的改善作用。
本发明使用的大宗原材料都是尾矿和工业废弃物,生产过程中降低了能耗,节约了能源,减少环境污染,并且其制备得到了性能优异的硅酸盐骨料。
附图说明
图1为无机-有机杂化激发单体的化学结构式。
具体实施方式
下面将结合本发明实施例,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的一部分实施例,而不是全部的实施例。在不冲突的情况下,本申请中的实施例及实施例中的特征可以相互组合。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他实施例,都属于本发明保护的范围。
以下实施例中所用试剂,均可从本领域常规厂商购得;所用实验方法,均为本领域技术人员知晓的常规实验方法。
实施例1:
八巯基丙基笼状聚倍硅氧烷(POSS-SH8)的制备:量取31.8g(3-巯基丙基)三甲氧基硅烷溶于450mL甲醇溶液,将甲醇混合液加入装有搅拌装置的三口烧瓶中,搅拌状态下一次性加入60mL浓盐酸溶液,混合溶液在90℃下回流、搅拌24h,冷却后,首先在冰水浴中静置倒去上层清液,然后用10mL二氯甲烷溶解、加入250mL甲醇溶液搅拌、在冰水浴中静置,最后在-0.1MPa下70℃旋转蒸馏,得到八巯基丙基笼状聚倍硅氧烷(POSS-SH8);
无机-有机杂化激发单体的制备:将10.2g八巯基丙基笼状聚倍硅氧烷(POSS-SH8)、17.3g2-甲基-3-丁烯-2-醇和300mL的四氢呋喃THF加入石英圆底瓶中,待搅拌溶解后加入光引发剂DMPA,在紫外灯(UV365nm)照射下搅拌反应1h,反应过程中用深色布覆盖反应装置,以防止紫外光外漏,将反应液浓缩并用冰的无水乙醚沉淀,过滤收集产物放入30℃真空烘箱中干燥24h,得到无机-有机杂化激发单体,其结构式如图1所示。
实施例2:
一种水热合成粉煤灰硅酸盐骨料的制备方法,包括如下步骤:
步骤一,制备无机-有机复合型激发剂,其制备方法如下:称取1.5重量份的九水硅酸钠、5重量份的氢氧化钾、1.5重量份的实施例1制备的无机-有机杂化激发单体,复配得到无机-有机复合型激发剂;
步骤二,配制硅酸盐骨料的原料,该原料包括:粉煤灰60%,电石渣20%,生石灰15%,膨胀珍珠岩3.85%,玻化微珠1%,无机-有机复合型激发剂0.15%;
其中,粉煤灰的化学组成为:50.16%SiO2、35.25%Al2O3、3.85%CaO、0.36%Na2O、0.6%MgO、1.84%K2O、0.54%SO3、1.18%TiO2、1.02%Loss;
电石渣的化学组成为:60.98%CaO、5.42%SiO2、3.0%Al2O3、0.05%Na2O、0.28%SO3、0.19%Fe2O3、0.75%其他、29.33%Loss;
膨胀珍珠岩的粒径为0.5mm;
步骤三,把计量好的粉煤灰、电石渣、生石灰、玻化微珠搅拌5min,加入无机-有机复合型激发剂继续搅拌3min,制成混合料;
步骤四,成型方式采用成球盘,把成球核膨胀珍珠岩喷水润湿,加入制备好的混合料,边加入边喷水,成型直径在5mm-10mm范围内,静置养护1h,进入蒸压釜,在温度为180℃、压力为1.15MPa的蒸压养护条件下进行熟化活化处理,发生硅钙反应进行水热合成,制出水热合成硅酸盐骨料。
根据GB/T17431.1-2010《轻集料及其试验方法第1部分:轻集料》进行性能测试,检测结果为:吸水率为6.2%、堆积密度为710kg/m3、筒压强度为17.5MPa。
实施例3:
一种水热合成粉煤灰硅酸盐骨料的制备方法,包括如下步骤:
步骤一,制备无机-有机复合型激发剂,其制备方法如下:称取5重量份的氢氧化钾、1.5重量份的实施例1制备的无机-有机杂化激发单体,复配得到无机-有机复合型激发剂;
步骤二,配制硅酸盐骨料的原料,该原料包括:粉煤灰60%,电石渣20%,生石灰15%,膨胀珍珠岩3.85%,玻化微珠1%,无机-有机复合型激发剂0.15%;
膨胀珍珠岩的粒径为0.5mm;
步骤三,把计量好的粉煤灰、电石渣、生石灰、玻化微珠搅拌5min,加入无机-有机复合型激发剂继续搅拌3min,制成混合料;
步骤四,成型方式采用成球盘,把成球核膨胀珍珠岩喷水润湿,加入制备好的混合料,边加入边喷水,成型直径在5mm-10mm范围内,静置养护1h,进入蒸压釜,在温度为180℃、压力为1.15MPa的蒸压养护条件下进行熟化活化处理,发生硅钙反应进行水热合成,制出水热合成硅酸盐骨料。
根据GB/T17431.1-2010《轻集料及其试验方法第1部分:轻集料》进行性能测试,检测结果为:吸水率为6.9%、堆积密度为691kg/m3、筒压强度为13.9MPa。
实施例4:
一种水热合成粉煤灰硅酸盐骨料的制备方法,包括如下步骤:
步骤一,制备无机-有机复合型激发剂,其制备方法如下:称取1.5重量份的九水硅酸钠、1.5重量份的实施例1制备的无机-有机杂化激发单体,复配得到无机-有机复合型激发剂;
步骤二,配制硅酸盐骨料的原料,该原料包括:粉煤灰60%,电石渣20%,生石灰15%,膨胀珍珠岩3.85%,玻化微珠1%,无机-有机复合型激发剂0.15%;
膨胀珍珠岩的粒径为0.5mm;
步骤三,把计量好的粉煤灰、电石渣、生石灰、玻化微珠搅拌5min,加入无机-有机复合型激发剂继续搅拌3min,制成混合料;
步骤四,成型方式采用成球盘,把成球核膨胀珍珠岩喷水润湿,加入制备好的混合料,边加入边喷水,成型直径在5mm-10mm范围内,静置养护1h,进入蒸压釜,在温度为180℃、压力为1.15MPa的蒸压养护条件下进行熟化活化处理,发生硅钙反应进行水热合成,制出水热合成硅酸盐骨料。
根据GB/T17431.1-2010《轻集料及其试验方法第1部分:轻集料》进行性能测试,检测结果为:吸水率为7.2%、堆积密度为689kg/m3、筒压强度为14.2MPa。
实施例5:
一种水热合成粉煤灰硅酸盐骨料的制备方法,包括如下步骤:
步骤一,制备无机-有机复合型激发剂,其制备方法如下:称取1.5重量份的九水硅酸钠、5重量份的氢氧化钾,复配得到无机-有机复合型激发剂;
步骤二,配制硅酸盐骨料的原料,该原料包括:粉煤灰60%,电石渣20%,生石灰15%,膨胀珍珠岩3.85%,玻化微珠1%,无机-有机复合型激发剂0.15%;
膨胀珍珠岩的粒径为0.5mm;
步骤三,把计量好的粉煤灰、电石渣、生石灰、玻化微珠搅拌5min,加入无机-有机复合型激发剂继续搅拌3min,制成混合料;
步骤四,成型方式采用成球盘,把成球核膨胀珍珠岩喷水润湿,加入制备好的混合料,边加入边喷水,成型直径在5mm-10mm范围内,静置养护1h,进入蒸压釜,在温度为180℃、压力为1.15MPa的蒸压养护条件下进行熟化活化处理,发生硅钙反应进行水热合成,制出水热合成硅酸盐骨料。
根据GB/T17431.1-2010《轻集料及其试验方法第1部分:轻集料》进行性能测试,检测结果为:吸水率为7.5%、堆积密度为662kg/m3、筒压强度为11.8MPa。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
Claims (9)
1.一种水热合成粉煤灰硅酸盐骨料的制备方法,其特征在于,所述制备方法包括如下步骤:
步骤一,制备无机-有机复合型激发剂,其制备方法如下:
步骤Step1,制备无机-有机杂化激发单体,该无机-有机杂化激发单体通过八巯基丙基笼状聚倍硅氧烷的巯基官能团与丁烯醇单体的烯基官能团发生巯基-烯点击化学反应制备而成;
步骤Step2,称取1-2重量份的九水硅酸钠、2-10重量份的氢氧化钾、0.3-1.5重量份的无机-有机杂化激发单体,复配得到无机-有机复合型激发剂;
步骤二,配制硅酸盐骨料的原料,该原料包括:粉煤灰55%-75%,电石渣15%-25%,生石灰10%-20%,膨胀珍珠岩3%-5%,玻化微珠0.55%-1.50%,无机-有机复合型激发剂0.05-0.2%;
步骤三,把计量好的粉煤灰、电石渣、生石灰、玻化微珠搅拌,加入无机-有机复合型激发剂继续搅拌,制成混合料;
步骤四,成型方式采用成球盘,把成球核膨胀珍珠岩喷水润湿,加入制备好的混合料,边加入边喷水,静置养护,进入蒸压釜熟化活化处理,发生硅钙反应进行水热合成得到水热合成硅酸盐骨料。
2.根据权利要求1所述的一种水热合成粉煤灰硅酸盐骨料的制备方法,其特征在于,所述无机-有机杂化激发单体的制备如下:将八巯基丙基笼状聚倍硅氧烷、丁烯醇单体和四氢呋喃加入反应器中,待搅拌溶解后加入光引发剂,在UV灯照射下搅拌反应,反应过程中在暗室内进行,得到无机-有机杂化激发单体。
3.根据权利要求2所述的一种水热合成粉煤灰硅酸盐骨料的制备方法,其特征在于,所述丁烯醇单体为2-甲基-3-丁烯-2-醇、2,3-二甲基-3-丁烯-2-醇、3-甲基-3-丁烯-2-醇、3-丁烯-2-醇中的一种或几种组合。
4.根据权利要求2所述的一种水热合成粉煤灰硅酸盐骨料的制备方法,其特征在于,所述光引发剂为光引发剂DMPA、光引发剂1173、光引发剂I907、光引发剂369、光引发剂2959中的一种。
5.根据权利要求1所述的一种水热合成粉煤灰硅酸盐骨料的制备方法,其特征在于,所述膨胀珍珠岩的粒径为0.5-1mm。
6.根据权利要求1所述的一种水热合成粉煤灰硅酸盐骨料的制备方法,其特征在于,所述步骤四,成型直径5mm-10mm。
7.根据权利要求1所述的一种水热合成粉煤灰硅酸盐骨料的制备方法,其特征在于,所述步骤四,静置养护1-3h,进入蒸压釜,在温度为160-200℃、压力为1-1.3MPa的蒸压养护条件下进行熟化活化处理。
8.根据权利要求1-7任一项所述的制备方法的一种水热合成粉煤灰硅酸盐骨料,其特征在于,所述粉煤灰硅酸盐骨料包括如下重量份的原料:粉煤灰55%-75%,电石渣15%-25%,生石灰10%-20%,膨胀珍珠岩3%-5%,玻化微珠0.55%-1.50%,无机-有机复合型激发剂0.05-0.2%。
9.根据权利要求8所述的一种水热合成粉煤灰硅酸盐骨料,其特征在于,所述硅酸盐骨料的吸水率为5.4%-7.8%、堆积密度为690-730kg/m3、筒压强度为10.7-18.3MPa。
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