High molecule polymer template synthetic composite hole zeolite molecular sieve and its preparing method

A high-molecular polymer and zeolite molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of large specific surface area, low acidity, high preparation cost, etc., and achieve the effect of high catalytic activity

Inactive Publication Date: 2006-03-22
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since zeolite molecular sieves have a smaller specific surface and narrower pores, the diffusion rate of catalytic reactions and the application of catalytic reactions involving macromolecules are greatly limited [see Corma, A.Chem.Rev.97, (1997) , 2373.]
For this reason, Mobil Company has invented MCM-41 series mesoporous molecular sieves [see Kresge, C.T., Leonowicz, M.E., Roth, W.J., Vartuli, J.C. & Beck, J.S.Nature 352, (1992), 710.], this kind of molecular sieve ratio The large surface area and large pore size overcome the shortcomings of zeolite molecular sieves to a certain extent, but due to the amorphous walls of mesoporous molecular sieves, their stability is low, their acidity is low, and their preparation costs are high. These factors limit the Further application of mesoporous molecular sieves [see Corma, A.Chem.Rev.97, (1997), 2373.]

Method used

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  • High molecule polymer template synthetic composite hole zeolite molecular sieve and its preparing method
  • High molecule polymer template synthetic composite hole zeolite molecular sieve and its preparing method
  • High molecule polymer template synthetic composite hole zeolite molecular sieve and its preparing method

Examples

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Effect test

Embodiment 1

[0020] Example 1: Synthesis of composite pore structure ZSM-5 with polyquaternium and TPAOH as a composite template

[0021] Synthetic raw materials: polyquaternium-7, TPAOH, tetraethyl orthosilicate, NaAlO 2

[0022] Synthetic ratio: (0.01~0.1) Al 2 o 3 / SiO 2 / (0.01~0.1)Na 2 O / (0.04~1.8)TPAOH / (10~60)H 2 o

[0023] Synthesis steps: first dissolve appropriate amount of TPAOH in water, and mix NaAlO 2 and tetraethyl orthosilicate, after the solution is clarified, age at 40-120°C for 1-8 hours, then introduce polyquaternium-7 accounting for 5%-25% of the total mass of the solution, and continue stirring until the added The polymer is completely dissolved, the obtained sol is vigorously stirred at 15-35°C for 4-10 hours, put into a stainless steel reactor with a polytetrafluoroethylene liner, and left to react at 140-180°C for 24-168 hours. Finally, the sample is raised to 550°C at a rate of 1°C / min, and calcined at a temperature of 545-555°C for 6-8 hours.

[0024] Prep...

Embodiment 2

[0030] Example 2: Synthesis of composite pore structure BETA with polyquaternium and TEAOH as a composite template

[0031] Synthetic raw materials: polyquaternium-6, TEAOH, white carbon black, NaAlO 2 , sodium hydroxide

[0032] Synthetic ratio: (0.01~0.03) Al 2 o 3 / SiO 2 / (0.03~0.1)Na 2O / (0.1~1)TEAOH / (10~40)H 2 o

[0033] Synthesis steps: first dissolve appropriate amount of TEAOH in water, and mix NaAlO with a certain stirring intensity 2 and sodium hydroxide, add white carbon black after dissolving, stir until the solution is clarified, age at 60-140°C for 1-8 hours, and then add 5%-25% of the total mass of the solution polyquaternium- 6. Continue to stir until the added polymer is completely dissolved, and the obtained sol is vigorously stirred at 15-35°C for 4-10 hours, then put it into a stainless steel reactor lined with polytetrafluoroethylene and let it stand at 140-180°C React for 24 to 120 hours. Finally, the sample is raised to 550°C at a rate of 1°C / min...

Embodiment 3

[0037] Example 3: Using polyquaternium as a template to synthesize a composite pore structure Y

[0038] Synthetic raw materials: polyquaternium-7, Y-directing agent, NaAlO 2 , Al 2 (SO 4 ) 3 , water glass.

[0039] Synthetic ratio: Al 2 o 3 / (7.6~16)SiO 2 / (2.9~6.6)Na 2 O / (175~320)H 2 o

[0040] Synthesis steps: first dissolve water glass in water, and mix Y-directing agent, NaAlO 2 and Al 2 (SO 4 ) 3 Add, the dosage of Y-directing agent is 5%~20% of the total amount of silicon source in the synthetic solution. After the solution is stirred evenly, introduce polyquaternium-7 accounting for 5%~25% of the total mass of the solution, and continue stirring for 4~10 Hours, put it into a stainless steel reaction kettle with a polytetrafluoroethylene liner and let it stand at 100-110°C for 20-24 hours. Finally, the sample is raised to 550°C at a rate of 1°C / min, and calcined at a temperature of 545-555°C for 6-8 hours.

[0041] The preparation process of the HY cataly...

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Abstract

The present invention relates to inorganic chemistry, physical chemistry and catalytic chemistry technology. The present invention prepares composite pore zeolite molecular sieve with common silicon source, aluminum source and hybrid metal atom source, and through hydrothermal treatment and calcinations process. In the hydrothermal treatment, material powder is prepared with composite template of mixture comprising quaternary ammonium salt polymer and organic amine or organic quaternary ammonium salt, or template of quaternary ammonium salt polymer. The hydrothermal treatment is in 100-180 deg c and has setting time of 1-7 days. The prepared molecular sieve m is then calcined at 300-800 deg c for 0.5-24 hr to obtain opened channels. The prepared molecular sieve has composite pore structure and high catalytic activity, and may have various metal atoms introduced. The prepared molecular sieve may be used widely as adsorbent, catalyst and catalyst carrier.

Description

technical field [0001] The invention belongs to the fields of inorganic chemistry, physical chemistry, material chemistry, catalytic chemistry and chemical engineering, and particularly relates to zeolite molecular sieve synthesized by template method and its preparation technology. Background technique [0002] As an important part of inorganic microporous crystal materials, molecular sieves are increasingly becoming the starting point for the research of new inorganic materials due to their unique pore structure and exchangeable cation positions. High-quality carrier of new materials such as electricity). In 1961, Barrer and Denny introduced tetramethyl cation into molecular sieve synthesis system and successfully synthesized Na-A molecular sieve with Si / Al>1 [see D.W.Breck, W.G.Eversole, and R.M.Milson, J.Chem.Soc. , 78, (1956), 2338. and D.W.Breck, and J.Y.Smith., Scienct.Am.200, 85, 1959], created the era of organic template synthesis of molecular sieves. Thus, var...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 肖丰收王利丰殷成阳林凯峰
Owner JILIN UNIV
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