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Synthesis,Characterization And Catalyst Performance Of Titanosilicate ETS-10

Posted on:2022-09-30Degree:MasterType:Thesis
Country:ChinaCandidate:H Y XiaFull Text:PDF
GTID:2491306518973179Subject:Chemical Engineering
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As a basic catalytic material,ETS-10 zeolite has excellent ion exchange ability and stable hydrothermal stability.In this paper,ETS-10 zeolite as the research object,the synthesis and application of ETS-10 zeolite were studied from the low cost and high efficiency of the synthesis system.This paper mainly includes the following contents:In the first part,ETS-10 zeolite with microporous structure was synthesized by hydrothermal synthesis using industrial sodium silicate as silicon source,titanium trichloride and tetra-butyl titanate as titanium source,and KF,KCl and KOH as potassium source.In addition,the effects of silicon/titanium ratio,crystallization temperature and crystallization time on the synthesis of ETS-10 zeolite were investigated.The results showed that the crystallization time of the formula could be shortened to 12 h or even less,and the synthesis efficiency of the zeolite was improved.In the second part,ETS-10 zeolite with mesoporous structure can be synthesized in the presence or absence of template with titanium trichloride as the titanium source and KF as the potassium source under hydrothermal conditions.Template DM-3010 is more favorable to the formation of mesoporous ETS-10 zeolite when the silicon source modulus in the synthesis system is less.Similarly,the ratio of silicon to titanium,the type of template and the dosage of the template were studied.The results show that the ratio of silicon to titanium in the synthetic system varies from 5.5 to 6.3.Both template DM-3010 and 7~#are favorable for the synthesis of mesoporous ETS-10 zeolite.In the third part,transition metals such as Fe,Co,Ni,Cu and Zn were introduced into the silicon-titanium gel in the form of nitrate to synthesize transition metal-doped ETS-10 catalytic materials,and the influence of metal introduction on the crystallinity and morphology of ETS-10 zeolite was investigated.The addition of Fe,Co,Ni and Cu species can improve the crystallinity of ETS-10 zeolite materials,and Cu species can promote the growth of ETS-10 zeolite in the early stage.On the other hand,good texture properties of ETS-10 zeolite can still be synthesized when the doping amount of transition metal is reduced to 0.2%.The experimental results also show that the heteroatomic ETS-10 zeolite can be produced in large quantities on the scale of 5 L kettle.In the fourth part,different transition metals and 7~#template were introduced into the silicon-titanium gel to synthesize high specific surface area ETS-10 zeolite materials.The results show that the nitrate-doped metals(Ni,Co,Mn and Mg)promote the formation of mesoporous structure in ETS-10 zeolite with the help of template 7~#.In addition,pure phase ETS-10zeolite can be synthesized by changing the doping form of the metal(copper acetate,magnesium sulfate).In the fifth part,the prepared ETS-10 zeolite was used as catalyst for the reaction of o-phenylenediamine and aldehyde condensation to investigate its conversion and selectivity.
Keywords/Search Tags:ETS-10 zeolite, hydrothermal synthesis, heteroatomic zeolite, o-phenylenediamine and aldehyde condensation reaction
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