CN104258806B - 多孔硅胶空气净化颗粒的制备方法 - Google Patents
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Abstract
本发明公开了多孔硅胶空气净化颗粒的制备方法，颗粒的比表面积为250‑500m2/g、孔体积为1.2‑2.0mL/g、平均孔径5‑50nm、平均粒径为10‑100μm，具有比表面积大、孔隙发达、吸附能力强等特点，可以用于吸附甲醛、氨、TVOC等气体，能够用于空气净化，祛除有害气体。硅胶表面带有自由羟基，对甲醛这类的极性物质的吸附能力强，甲醛去除率可以达到85%以上。另外，本发明的硅胶二氧化硅纯度高，其本身无毒无害且不含任何重金属，是绿色环保的空气净化产品。本发明制备方法工艺成熟，易于实现工业化生产。
Description
技术领域
本发明属于环保材料技术领域，特别是涉及一种多孔硅胶空气净化颗粒的制备方法。
背景技术
硅胶是一种高活性吸附性材料，属于无定形态物质，其主要成分是二氧化硅，化学式为SiO2·nH2O。二氧化硅具有比表面积大、孔隙率高、纯度高等特点，被广泛应用于涂料、造纸、石油化工、日用化工、塑料、农药等诸多领域，是最热门的化工产品之一。作为吸附剂的硅胶，由于硅胶具有较高的吸附活性，可以选择性吸附气体的甲醛、氨等有害气体，或吸附空气中的水分用作干燥剂，也可用于物质的吸附分离、作为催化剂载体等。目前，市场上的主要空气净化产品有活性炭和硅藻纯等，硅藻纯是采用一些松散、质轻、多孔的天然矿物原料混合制备而成的球状颗粒，如中国专利一种光触媒多功能硅藻纯净化颗粒（专利号201310142911）包括以下重量份的组分制成：硅藻土50~70份、凹凸棒土5~15份、沸石粉10~20份、海泡石5~10份、负离子粉5~8份、远红外陶瓷粉3~5份、高岭土20~30份；纳米光触媒5~15份。该多功能硅藻纯净化颗粒具有比活性炭更高的孔隙率，是新一代的环保型空气净化产品，其SiO2含量可以达到80%以上。但是，硅藻纯的比表面积仅有40-65m2/g，孔体积小于1.0mL/g，因此有效吸附面积有限，吸附容量小。根据孔径的不同，硅胶可以分为微孔硅胶（孔径＜2nm）、介孔硅胶（孔径在2-50nm之间）和大孔硅胶（孔径＞50nm），其中，硅胶的SiO2含量可达98%以上，比表面积大于300m2/g，孔体积大于1.2mL/g，与硅藻纯和活性炭相比，它的吸附容量较大，并且能够提供更大的吸附面积。硅胶主要以碱金属硅酸盐或有机硅源为原料，采用凝胶法制备，如中国专利高纯度硅胶的制备工艺（CN 102079526）、一种多孔二氧化硅是以硅酸盐（CN101885488）、美国专利（US 6103004）等，然而，这种硅胶主要应用于工业用途，很少将其直接用于居住环境空气污染治理。
多孔硅胶颗粒兼有活性炭大比表面积和硅藻纯高孔隙率的特点，并且比表面积远大于硅藻纯，作为空气净化剂具有比硅藻纯更大的有效吸面积和吸附容量。并且，硅胶本身二氧化硅含量高，无毒无害，制备过程简单，是一种安全的环保材料。
发明内容
本发明的一个目的在于提供一种易于实现工业化生产的多孔硅胶空气净化颗粒的制备方法。
为实现上述目的，本发明的技术解决方案是：
本发明是一种多孔硅胶空气净化颗粒,其结构特征为：1)比表面积为250-500m2/g；2）孔体积为1.2-2.0mL/g；3）平均孔径5-50nm；4）平均粒径为10-100μm，且平均粒径可控；5）SiO2含量≥98%；6）加热减量≤5%。
本发明是一种多孔硅胶空气净化颗粒的制备方法，包括以下步骤：
1)提前在反应釜中预先加入底液和表面活性剂，保持搅拌并控制温度为25-80oC；加热后向反应釜中同时打入水玻璃溶液和硫酸溶液，控制反应釜内的pH值为4-10；
2）形成二氧化硅凝胶后，继续反应20-40min，然后升高温度至90-100oC，调节pH值为2-9，老化1-5小时，目的是促进扩孔和增大比表面积；
3）老化结束后，用水玻璃溶液或硫酸溶液调节二氧化硅凝胶浆料的pH值至6-7；
4）将二氧化硅凝胶浆料打入板框过滤机，进行固液分离，得到硅胶滤饼，用去离子水洗涤硅胶滤饼至洗涤液电导率＜0.4μs/cm；
5）将得到的硅胶滤饼进行干燥和粉碎，得到硅胶微颗粒，最后用包装材料进行制袋包装。
步骤1）中，所述的表面活性剂选自聚乙二醇、硬脂酸聚乙二醇酯、烷基磺酸胺、蓖麻油聚氧乙烯醚中的一种或一种以上；按质量百分比表面活性剂为水玻璃溶液的0.01-5%。
步骤1）中，所述的水玻璃溶液质量浓度为5-25%，模数为3.0-3.4。
步骤1）中，所述的硫酸溶液质量浓度为15-50%。
步骤1）中，水玻璃溶液和硫酸溶液的比例为4:1。
步骤1）所述包装材料为透气软质包材，选自无纺布、杜邦纸、太华纸、无纺布覆膜、高密度纸、大邦纸中的一种，优选为透气无纺布。
采用上述方案后，由于本发明颗粒的比表面积为250-500m2/g、孔体积为1.2-2.0mL/g、平均孔径5-50nm、平均粒径为10-100μm，具有比表面积大、孔隙发达、吸附能力强等特点，可以用于吸附甲醛、氨、TVOC等气体，能够用于空气净化，祛除有害气体。硅胶表面带有自由羟基，对甲醛这类的极性物质的吸附能力强，甲醛去除率可以达到85%以上。另外，本发明的硅胶二氧化硅纯度高，其本身无毒无害且不含任何重金属，是绿色环保的空气净化产品。本发明制备方法工艺成熟，易于实现工业化生产。
下面结合附图和具体实施例对本发明作进一步的说明。
附图说明
图1是本发明的工艺流程示意图。
具体实施方式
一、颗粒
本发明是一种多孔硅胶空气净化颗粒,其结构特征为： 1)比表面积为250-500m2/g；2）孔体积为1.2-2.0mL/g；3）平均孔径5-50nm；4）平均粒径为10-100μm，且平均粒径可控；5）SiO2含量≥98%；6）加热减量≤5%。
二、生产设备
如图1所示，一种多孔硅胶空气净化颗粒生产设备,包括水玻璃溶液储罐1、硫酸溶液储罐2、耐碱泵3、耐酸泵4、反应釜5、浆料储罐6、砂浆泵7、压滤洗涤装置8、干燥机9、粉碎机10。
所述的水玻璃溶液储罐1和硫酸溶液储罐2分别通过管道连接带有搅拌器51的反应釜5上部的进料口，在水玻璃溶液储罐1与反应釜5的进料口之间的管道上设置耐碱泵3，在硫酸溶液储罐2与反应釜5的进料口之间的管道上设置耐酸泵4。所述的反应釜5底部的出料口与浆料储罐6上部的进料口通过管道连接，反应釜5底部的出料口上设有放料阀52；浆料储罐6底部的出料口通过管道与压滤洗涤装置8连接，在浆料储罐6出料口与压滤洗涤装置8之间的管道上设有砂浆泵7。
所述的干燥机9、粉碎机10据工艺步骤依次设置压滤洗涤装置8的一侧。在压滤洗涤装置8与干燥机9之间、干燥机9与粉碎机10之间分别设有输送装置。
三、制备方法
本发明是一种多孔硅胶空气净化颗粒的制备方法，包括以下步骤：
1.提前在反应釜5中预先加入底液和表面活性剂，保持搅拌并控制温度为25-80oC；加热后向反应釜5中同时打入水玻璃溶液和硫酸溶液，控制反应釜5内的pH值为4-10。所述的表面活性剂选自聚乙二醇、硬脂酸聚乙二醇酯、烷基磺酸胺、蓖麻油聚氧乙烯醚中的一种或一种以上；按质量百分比表面活性剂为水玻璃溶液的0.01-5%。所述的水玻璃溶液质量浓度为5-25%，模数为3.0-3.4；所述的硫酸溶液质量浓度为15-50%。
2.形成二氧化硅凝胶后，继续反应20-40min，然后升高温度至90-100oC，调节pH值为2-9，老化1-5小时，目的是促进扩孔和增大比表面积调节；
3.老化结束后，用水玻璃溶液或硫酸溶液调节二氧化硅凝胶浆料的pH值至6-7；水玻璃溶液和硫酸溶液的比例为4:1。
4.将二氧化硅凝胶浆料打入板框过滤机，进行固液分离，得到硅胶滤饼，用去离子水洗涤硅胶滤饼至洗涤液电导率＜0.4μs/cm；
5.将得到的硅胶滤饼进行干燥和粉碎，得到硅胶微颗粒，最后用包装材料进行制袋包装。所述包装材料为透气软质包材，选自无纺布、杜邦纸、太华纸、无纺布覆膜、高密度纸、大邦纸中的一种，优选为透气无纺布。
以下为具体实施例：
实施例1
将1000kg去离子水加入到带有搅拌器的反应釜5中，同时加入1kgPEG6000和4kgNaHCO3，控制温度为50oC，在不断搅拌的情况下用蠕动泵将700kg浓度为15%的水玻璃溶液打入反应釜5，同时打入浓度为30%的硫酸控制反应液的pH值为8左右，加料时间约40min。至形成凝胶后，继续反应20min，然后调节反应浆料的pH值为4，升温至90oC老化2小时，老化结束后继续加入10%的水玻璃溶液，至反应浆料的pH值为7。最后，过滤进行固液分离，并用去离子水洗涤滤饼值滤液的电导率小于0.4μs/cm，干燥、粉碎，得到成品。
实施例2
将900kg去离子水加入到带有搅拌器的反应釜5中，同时加入1kgPEG6000和4kgNaHCO3，控制温度为50oC，在不断搅拌的情况下用蠕动泵将800kg浓度为12%的水玻璃溶液打入反应釜5，同时打入浓度为25%的硫酸控制反应液的pH值为9左右，加料时间约40min。至形成凝胶后，继续反应20min，然后调节反应浆料的pH值为5，升温至90oC老化3小时，老化结束后继续加入12%的水玻璃溶液，至反应浆料的pH值为6.5。最后，过滤进行固液分离，并用去离子水洗涤滤饼值滤液的电导率小于0.4μs/cm，干燥、粉碎，得到成品。
实施例3
将1000kg去离子水加入到带有搅拌器的反应釜5中，同时加入1.2kgPEG6000和5kgNaHCO3，控制温度为35oC，在不断搅拌的情况下用蠕动泵将700kg浓度为10%的水玻璃溶液打入反应釜5，同时打入浓度为15%的硫酸控制反应液的pH值为9左右，,加料时间约40min。至形成凝胶后，继续反应20min，然后升温至90oC老化2小时，老化结束后继续加入15%的硫酸溶液，至反应浆料的pH值为6。最后，过滤进行姑爷分离，并用去离子水洗涤滤饼值滤液的电导率小于0.4μs/cm，干燥、粉碎，得到成品。
实施例4
将1200kg去离子水加入到带有搅拌器的反应釜5中，同时加入0.8kgPEG6000和5kgNaHCO3，控制温度为35oC，在不断搅拌的情况下用蠕动泵将400kg浓度为20%的水玻璃溶液打入反应釜5，同时打入浓度为25%的硫酸控制反应液的pH值为9左右，,加料时间约40min。至形成凝胶后，继续反应20min，然后升温至95oC老化2小时，老化结束后继续加入25%的硫酸溶液，至反应浆料的pH值为7。最后，过滤进固液爷分离，并用去离子水洗涤滤饼值滤液的电导率小于0.4μs/cm，干燥、粉碎，得到成品。
三、产品检测
采用本发明的制备方法所制得的颗粒，其孔体积、比表面积、孔径采用MicroTristar II 3020按照DIN66134方法测定；平均粒径采用BT-9300H按照GB/T19077.1方法测定；SiO2含量采用X射线荧光光谱仪分析（XRF）；加热减量按照ISO 787-2方法测定。
甲醛去除率检测方法如下：（1）在两个相同的密闭容器为1.5m3的测试舱中进行，一个为样品舱，另一个为空白舱，将待测样品放在样品舱内，样品数量为1kg；（2）将相同的甲醛不间断缓慢释放到两个测试舱内，开启风扇使舱内气体混合均匀趋于平衡，关闭风扇；（3）24h后分别采样并测定两个舱内空气中的甲醛浓度值；（4）去除率计算公式为：y=（CA-CB）/CA*100%,其中CA为24h空白舱甲醛浓度值，CB为24h样品舱甲醛浓度值。
产品的检测结果如下：
| 实施例1 | 实施例2 | 实施例3 | 实施例4 | |
| 98.7 | 98.5 | 98.3 | 98.6 | |
| 孔体积（mL/g） | 1.58 | 1.54 | 1.62 | 1.65 |
| 315 | 330 | 350 | 342 | |
| 平均孔径（nm） | 21.7 | 25.2 | 23.4 | 27.0 |
| 平均粒径（μm） | 35 | 28 | 43 | 32 |
| 甲醛去除率（%） | 85 | 87 | 89 | 89 |
以上所述，仅为本发明较佳实施例而已，故不能以此限定本发明实施的范围，即依本发明申请专利范围及说明书内容所作的等效变化与修饰，皆应仍属本发明专利涵盖的范围内。
Claims (6)
1.一种多孔硅胶空气净化颗粒的制备方法，其特征在于：包括以下步骤：
1）提前在反应釜中预先加入底液和表面活性剂，保持搅拌并控制温度为25-80oC；加热后向反应釜中同时打入水玻璃溶液和硫酸溶液，控制反应釜内的pH值为4-10；
2）形成二氧化硅凝胶后，继续反应20-40min，然后升高温度至90-100oC，调节pH值为2-9，老化1-5小时；
3）老化结束后，用水玻璃溶液或硫酸溶液调节二氧化硅凝胶浆料的pH值至6-7；
4）将二氧化硅凝胶浆料打入板框过滤机，进行固液分离，得到硅胶滤饼，用去离子水洗涤硅胶滤饼至洗涤液电导率＜0.4μs/cm；
5）将得到的硅胶滤饼进行干燥和粉碎，得到硅胶微颗粒，最后用包装材料进行制袋包装。
2.根据权利要求1所述的多孔硅胶空气净化颗粒的制备方法，其特征在于：步骤1）中，所述的表面活性剂选自聚乙二醇、硬脂酸聚乙二醇酯、烷基磺酸胺、蓖麻油聚氧乙烯醚中的一种以上；按质量百分比表面活性剂为水玻璃溶液的0.01-5%。
3.根据权利要求1所述的多孔硅胶空气净化颗粒的制备方法，其特征在于：步骤1）中，所述的水玻璃溶液质量浓度为5-25%，模数为3.0-3.4。
4.根据权利要求1所述的多孔硅胶空气净化颗粒的制备方法，其特征在于：步骤1）中，所述的硫酸溶液质量浓度为15-50%。
5.根据权利要求1所述的多孔硅胶空气净化颗粒的制备方法，其特征在于：步骤1）中，水玻璃溶液和硫酸溶液的比例为4:1。
6.根据权利要求1所述的多孔硅胶空气净化颗粒的制备方法，其特征在于：步骤5）所述包装材料为透气软质包材，选自无纺布、杜邦纸、太华纸、无纺布覆膜、高密度纸、大邦纸中的一种。
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