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High-molecular organic polymer template synthesized compound pore structure molecular sieve and preparation method thereof

A technology of molecular sieves and polymers, applied in the direction of crystalline aluminosilicate zeolites, etc., can solve the problems of complex synthesis conditions such as the price of template agents, and achieve the effect of cheap raw materials

Active Publication Date: 2013-06-26
CHANGZHOU YINGZHONG NANO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, many of the methods involving high molecular polymers are difficult to be practically applied to the industrial field due to the price of the template agent and the complexity of the synthesis conditions. Active molecular sieves have important practical significance and industrial value

Method used

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  • High-molecular organic polymer template synthesized compound pore structure molecular sieve and preparation method thereof
  • High-molecular organic polymer template synthesized compound pore structure molecular sieve and preparation method thereof
  • High-molecular organic polymer template synthesized compound pore structure molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1: Synthesis of composite pore structure ZSM-5 with high molecular organic amine polymer and TPABr (tetrapropylammonium bromide) as composite template

[0045] Synthetic raw materials: polyethyleneimine, TPABr, ethyl orthosilicate, Al 2 (SO 4 ) 3 (Aluminum Sulfate), NaOH (Sodium Hydroxide)

[0046] Specific synthesis steps: first dissolve 3gTPABr in 72g water, and mix 0.75gAl 2 (SO 4 ) 3 And add 0.72g NaOH, after the solution is clarified, add 23.5g tetraethyl orthosilicate and continue to stir, use NaOH to adjust the pH to 12, add 1g polyethyleneimine after aging at room temperature for 6 hours, continue to stir until the mixture is uniform The obtained gel was put into a polytetrafluoroethylene-lined stainless steel reactor and reacted at 200°C for 1 day. After the final sample was washed, dried at 110°C, and then calcined at 800°C for 5 hours, a ZSM-5 molecular sieve with a composite pore structure was obtained.

[0047] Molecular sieves with high cr...

Embodiment 2

[0048] Example 2: Synthesis of composite pore structure ZSM-5 with high molecular organic amine polymer and TPABr (tetrapropylammonium bromide) as composite template

[0049] Synthetic raw materials: polyethyleneimine, TPABr, ethyl orthosilicate, Al 2 (SO 4 ) 3 (Aluminum Sulfate), NaOH (Sodium Hydroxide)

[0050] Specific synthesis steps: firstly dissolve 8.43gTPABr in 72g water, and mix 0.75gAl 2 (SO 4 ) 3 And add 0.72g NaOH, after the solution is clarified, add 23.5g tetraethyl orthosilicate and continue to stir, use NaOH to adjust the pH to 13, add 5g polyethyleneimine after aging at room temperature for 6 hours, continue to stir until the mixture is uniform The obtained gel was put into a polytetrafluoroethylene-lined stainless steel reactor and reacted at 180°C for 3 days. After the final sample was washed, dried at 110°C, and calcined at 300°C for 18 hours, a ZSM-5 molecular sieve with a composite pore structure was obtained.

Embodiment 3

[0051] Embodiment 3: Synthesis of compound pore structure L-type molecular sieve with macromolecule organic amine polymer

[0052] Synthetic raw materials: polyethyleneimine, silica sol (30% mass fraction), NaAlO 2 (sodium metaaluminate), NaOH (sodium hydroxide), KOH (potassium hydroxide)

[0053] Concrete synthetic steps:

[0054] First weigh 3.2gNaOH, 5.2gKOH and 1.4gNaAlO 2 , dissolved in 40.8g of water and stirred, after the solution was clarified, 49.4g of silica sol with a mass fraction of 30% was added and continued to stir, and 2g of polyethyleneimine was added and stirred until evenly mixed, and then the obtained gel was loaded into PTFE An ethylene-lined stainless steel autoclave was reacted at 150°C for 80 hours. After the final sample was washed, dried at 110° C., and then calcined at 300° C. for 12 hours, an L-type molecular sieve with a composite pore structure was obtained.

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Abstract

The invention relates to a high-molecular organic polymer template synthesized compound pore structure molecular sieve and a preparation method thereof and belongs to the technical field of compound pore structure molecular sieve preparation. The technical scheme is that the preparation method comprises the following steps of: forming molecular sieve gel, wherein a certain amount of silicon source, aluminum source, template agent and deionized water are uniformly mixed under room temperature; and a certain amount of PEI (Polyethyleneimine) is added to the uniformly mixed molecular sieve gel as a mesoporous structure guide agent for being uniformly stirred; carrying out hydrothermal reaction, wherein the hydrothermal reaction temperature is 100 DEG C to 250 DEG C, the hydrothermal reaction is carried out directly or under stirring conditions and the reaction time is 12 hours to 168 hours; drying, wherein the drying is carried out for 6 hours to 48 hours under 50 DEG C to 150 DEG C; and roasting to obtain the molecular sieve with the compound pore structure, wherein the roasting is carried out for 1 hour to 24 hours under 300 DEG C to 800 DEG C.

Description

technical field [0001] The invention relates to a high-molecular organic polymer template synthesis molecular sieve with a composite pore structure and a preparation method thereof, belonging to the technical field of preparation of molecular sieves with a composite pore structure. Background technique [0002] Zeolite molecular sieve has a regular and uniform pore structure, including the size and shape of the pore, and it has a high specific surface and pore volume, and high hydrothermal stability makes it widely used in catalytic engineering in petroleum refining and processing , such as cracking, alkylation, hydrocracking, and isomerization of hydrocarbons, and secondly, they are also widely used in adsorption and separation processes, such as drying and deCO2 of natural gas, cracked gas, etc. 2 , desulfurization and other purification fields. The most representative one is the synthesis of ZSM-5 series molecular sieves. However, due to the small pore size of zeolite m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 姜兴茂孙龙陈传领盛超
Owner CHANGZHOU YINGZHONG NANO TECH
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