CN112934133A - 一种改性固相硅凝胶的制备方法 - Google Patents
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Abstract
本发明公开了一种改性固相硅凝胶的制备方法，固相硅凝胶是由氧化硅、水及金属氧化物合成的络合物，常温是稳定的固相，当温度大于108℃时开始由固相到液相的转移，其相变期有明显的溶胶特征，该特征所具备的可加工性，使其成为一种特殊的硅酸盐材料。以钙中和三氯氢硅固废为部分原料替代石英砂，降低原料成本同时简化了配方，制备了改性固相硅凝胶。该方法具有：简化配方，反应温和、易控的工艺特征。该方法制备的固相硅凝胶制品具有：耐水性明显提升之产品特征。
Description
技术领域
本发明公开了一种改性固相硅凝胶的制备方法，属硅酸盐材料领域。固相硅凝胶是由氧化硅、水及金属氧化物合成的络合物，常温是稳定的固相，当温度大于108℃时开始由固相到液相的转移，其相变期有明显的溶胶特征，该特征所具备的可加工性，使其成为一种特殊的硅酸盐材料。以钙中和三氯氢硅固废为部分原料替代石英砂，降低原料成本同时简化了配方，制备了改性固相硅凝胶。该方法具有：简化配方，反应温和、易控的工艺特征。该方法制备的固相硅凝胶制品具有：耐水性明显提升之产品特征。
背景技术
中国专利CN104174341A《一种固相硅凝胶的制备方法》公开了一种由石英砂制备的固相硅凝胶，阐述了固相硅凝胶是一种人工合成的络合物，常温环境是一种稳定的固相物，当温度大于108℃时开始由固相到液相的转移，由于有宽范的临界区间顾奠定了该材料的特殊理化性能和可加工性能。进一步阐述了氧化硅与金属离子的配比。以锂Li、钠Na、钾K，＋1价离子，镁Mg、钙Ga，＋2价离子，铝Al、铁Fe，＋3价离子的配合比。并且强调了原料砂中已经包含的上述离子，致使配方及其复杂。发明人的目的是强调其原料的通用性和广泛性。但实际生产中，即便是充分计算了原料砂中的上述金属离子，其产品合格率也不高。究其原因，是因为固相硅凝胶是氧化硅水和金属离子，形成的相对稳定的络合物胶体，氧化硅与金属离子配合出络合物胶体的范围很窄，稍有偏差就会在高压环境形成晶体，甚至将反应釜抱死，因此，可以想象CN104174341A的成品率并不高，对设备还存在一定的危险性。
发明内容
了解了多晶硅生产工艺，研究了该工艺产生的工业固废，钙中和三氯氢硅，其成分如下：氧化硅 SiO2 80.6％～81.4％ 氧化钙GaO 12.2%～12.7％ 氧化钠Na2O 4.6％～5.3％ 氧化镁MgO 0.4％ ～1.3％ 氧化铁 Fe2O3 0.1%～0.3%对多个生产批次产生的固废，进行了比对实验，其成分相对稳定。研究了不同氧化硅含量石英砂与上述钙中和三氯氢硅固废配合，合成改性固相硅凝胶的配方，找到了通用性强的简易配比方法。即，上述固废30～75质量份，与氧化硅含量≥92%的石英砂50～100质量份，配合氢氧化锂0.01～0.05质量份，在Oy15渗透剂0.01～0.05质量份存在的环境中，加压反应实现了固相硅凝胶的制备。克服了成品率低，反应不稳定，产品耐水性差的问题。需要强调的是水在配方中的占比，是核心要素之一，氧化硅与水的摩尔比0.75～1.75是形成固相硅凝胶的区间，高则分层产生沉淀，低则会抱死反应釜。
一种改性固相硅凝胶的制备方法，包含7个步骤①预混罐中加入：石英砂50～100质量份，钙中和三氯氢硅固废30～75质量份，氢氧化锂0.1～0.5质量份，Oy15渗透剂0.01～0.05质量份，②预混罐中加入：去离子水，并调整原料中氧化硅与去离子水的摩尔比为1:0.75 至 1.75，③开启预混罐搅拌，将物料混合均匀后泵入带夹套的蒸压反应釜，④关闭反应釜上料阀，开搅拌，开蒸汽阀，给反应釜加压到1MPa，关闭蒸汽阀，继续搅拌，反应压力冲高到3MPa，开夹套蒸汽阀降温，稳压在3MPa，压力回落后关闭夹套蒸汽，⑤上述反应釜压力回落到1MPa，打开出料阀，放料到成品罐，⑥开成品罐搅拌器，加入：0.05～0.1质量份S35表面修饰剂，0.05～0.1质量份y2封头剂，0. 3～0. 6质量份树脂增韧剂，搅拌均匀后打开成品罐底部出料口放料，⑦上述成品罐放出的原料经压制、切割，成块状固相硅凝胶成品；上述石英砂是氧化硅含量≥92%的石英砂；上述钙中和三氯氢硅固废是，多晶硅厂三氯氢硅精馏塔尾气，通入电石法乙炔生产中产生的废水，中和到pH值在7-8，经吸滤脱水干燥后的废渣；上述Oy15渗透剂是复合型Oy15渗透剂；上述S35表面修饰剂是阴离子表面活性剂，表面修饰剂；上述y2封头剂是带有羟基的有机硅封头剂；上述增韧剂是MQ树脂、一甲基三乙烯基硅树脂、PVC树脂中的一种或多种的组合。
附图说明 图1固相硅凝胶生产线示意图
附图标注
1预混罐，2蒸压反应釜，3反应釜上料阀，4蒸汽阀，5夹套蒸汽阀，6出料阀，7成品罐，8成品罐底部出料口。
具体实施例1
结合附图，图1：固相硅凝胶生产线，以实际生产为例
原料：阿勒泰北屯石英砂，其成分为：SiO2氧化硅92%、氧化钙GaO 2.2%、氧化钠Na2O1.6％、氧化镁MgO 0.7％氧化铁 Fe2O3 11.3%，新特能源股份有限公司多晶硅1分厂废渣，其成分为：SiO2氧化硅81.1％、GaO氧化钙12.5%、Na2O氧化钠5.1％ 、MgO氧化镁1.3％、Fe2O3氧化铁0.2%，pH值7.5,新疆锂盐厂氢氧化锂（工业纯）。
制备：①预混罐1中加入：石英砂900Kg，钙中和三氯氢硅固废550Kg，氢氧化锂2.5Kg，Oy15渗透剂270g，②预混罐中加入：去离子水670Kg，③开启预混罐搅拌，将物料混合均匀后泵入带夹套的蒸压反应釜2，④关闭反应釜上料阀3，开搅拌，开蒸汽阀4，给反应釜加压到1MPa，关闭蒸汽阀4，继续搅拌，反应压力冲高到3MPa，开夹套蒸汽阀5降温，稳压在3MPa，压力回落后关闭夹套蒸汽阀5，⑤上述反应釜压力回落到1MPa，打开出料阀6，放料到成品罐7，⑥打开成品罐搅拌器，加入：750g S35表面修饰剂，900g y2封头剂，5Kg一甲基三乙烯基硅树脂增韧剂，搅拌均匀后打开成品罐底部出料口8放料，⑦上述成品罐放出的原料经压制、切割，成块状固相硅凝胶成品。
上述块状固相硅凝胶成品，经微波发泡、近红外转晶，制备出固相硅凝胶泡沫产品。该产品经检测：容重106Kg/m3、导热系数0.039W/(m·K)、抗压强度187KPa、拉拔强度212KPa、100℃沸水浸泡1h质量损失率0.26％。与普通固相硅凝胶泡沫产品比较，100℃沸水浸泡1h质量损失率，下降了一半以上。充分验证了其耐水性提高的事实。
Claims (1)
1.一种改性固相硅凝胶的制备方法，其区别特征是：以多晶硅厂的固体废弃物，钙中和三氯氢硅为部分原料和改性剂，制备方法包含①预混罐中加入：石英砂50～100质量份，钙中和三氯氢硅固废30～75质量份，氢氧化锂0. 1～0. 5质量份，Oy15渗透剂0.01～0.05质量份，②预混罐中加入：去离子水，并调整原料中氧化硅与去离子水的摩尔比为1: 0.75～1.75，③开启预混罐搅拌，将物料混合均匀后泵入带夹套的蒸压反应釜，④关闭反应釜上料阀，开搅拌，开蒸汽阀，给反应釜加压到1MPa，关闭蒸汽阀，继续搅拌，反应压力冲高到3MPa，开夹套蒸汽阀降温，稳压在3MPa，压力回落后关闭夹套蒸汽，⑤上述反应釜压力回落到1MPa，打开出料阀，放料到成品罐，⑥打开成品罐搅拌器，加入：0.05～0. 1质量份S35表面修饰剂，0.05～0.1质量份y2封头剂，0.3～0.6质量份树脂增韧剂，搅拌均匀后打开成品罐底部出料口放料，⑦上述成品罐放出的原料经压制、切割，成块状固相硅凝胶成品；上述石英砂是氧化硅含量≥92%的石英砂；上述钙中和三氯氢硅固废是，多晶硅厂三氯氢硅精馏塔尾气，通入电石法乙炔生产中产生的废水，中和到pH值在7-8，经吸滤脱水后的废渣；上述Oy15渗透剂是复合型Oy15渗透剂；上述S35表面修饰剂是阴离子表面活性剂，表面修饰剂；上述y2封头剂是带有羟基的有机硅封头剂；上述增韧剂是MQ树脂、一甲基三乙烯基硅树脂、PVC树脂中的一种或多种的组合。
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