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以硅藻土为原料合成沸石分子筛的探索研究

Exploratory Study on Synthesis of Zeolites by Diatomite

【作者】 满卓

【导师】 孟长功;

【作者基本信息】 大连理工大学 , 无机化学, 2006, 硕士

【摘要】 沸石分子筛是一种结晶态的硅铝酸盐,可作为良好的吸附剂、离子交换剂和催化剂,用化学原料合成分子筛具有成本高、母液排放量大且污染环境等诸多弊端。本文在综合分析国内外有关沸石分子筛的合成与应用的大量文献的基础上,采用吉林敦化的硅藻土为主要原料成功合成出了NaP、NaA和NaY型分子筛,既提高了硅藻土的高层次开发利用,又为沸石分子筛的合成提供了一种来源丰富的新原料。本论文对硅藻土水热法合成分子筛结晶变化过程中的影响因素进行了全面系统的研究,主要内容如下: 探索以硅藻土为主要原料,不采用传统的高温焙烧,直接与碱液反应,水热合成系列低品位沸石分子筛(NaP、NaA和NaY型)。通过XRD、IR、SEM及CEC等测试手段对合成的产品进行了测试与表征,系统考察了合成过程中的影响因素,如反应体系配比、陈化条件、晶化温度及晶化时间等,从而确定了分子筛水热合成的最佳工艺参数。该合成方法工艺简单、反应条件易控制,而且原料来源丰富、合成成本低,可进行工业化生产。 探索以硅藻土为主要原料,采用碱熔、添加导向剂合成结晶度高的高品位NaY型沸石分子筛。以硅藻土为原料,采用优化的水热反应合成新工艺:碱焙烧硅藻土→添加导向剂→晶化合成→过滤、洗涤→烘干→NAY型分子筛产品。最佳工艺参数为:先将硅藻土与氢氧化钠按Na2O/SiO2=1∶1混合,在550℃焙烧1h,再将碱土与偏铝酸钠、水按照摩尔比6SiO2∶Al2O3∶6Na2O∶219.6H2O配制,并加入少量的导向剂(组成为15SiO2∶Al2o3∶21.6Na2O∶569H2O),在100℃下恒温晶化10h。所得产品的结晶度接近100%,饱和静态水吸附量可达到27.3%。研究发现,碱熔焙烧、导向剂和反应体系配比对合成产品晶相的影响起了决定性作用。

【Abstract】 Zeolites are widely used as absorbents, ion exchanges and catalysts. There are many shortcomings in synthesizing zeolites from chemical materials, such as high cost, and serious pollution from reactant liquids and so on. Based on lots of literatures of zeolites synthesis, a series of zeolites are hydrothermally synthesized successfully from diatomite. Besides, the influence of treatment conditions is studied systematically.Using diatomite and alkali solution directly, this paper synthesizes a series of zeolite products (NaP, NaA and NaY type) through the hydrothermal method. It is discussed in depth the effects on synthesis of zeolites, including the composition of the reaction mixture and the hydrothermal conditions. Then the technical parameters of hydrothermal treatment of zeolites are optimized.In existing of the structure directing agent (SDA), Zeolite NaY of high crystallinity is hydrothermally synthesized by diatomite, which is calcined with alkali in advance. The crystal phase is identified by X-ray diffraction. And the static water absorption capacity data of zeolite NaY is gained. The reaction conditions are discussed and the results show that the alkali fusion, the action of SDA and the composition of reactant system are the main impacting factors on zeolite NaY synthesis. The optimum technical conditions are as follows. Diatomite is calcined with sodium hydroxide under the Na2O/SiO2 ratio of 1:1 at the temperature of 550℃. Afterwards, the composition of reactant mixture is 6SiO2: Al2O3: 6Na2O: 219.6H2O, with adding little amounts of SDA composed of 15SiO2:Al2O3:21.6Na2O: 569H2O. And then the reactants are crystallized 10h at the temperature of 100℃. The crystallinity of product reaches to the maximum, and its water absorption capacity comes to 27.3%.

【关键词】 硅藻土水热合成沸石分子筛
【Key words】 DiatomiteHydrothermal treatmentZeolites
  • 【分类号】O643.36
  • 【被引频次】9
  • 【下载频次】692
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