Metal-doped EDI-type zinc phosphate molecular sieve and synthesis method thereof

A technology of metal doping and synthesis method, which is applied in the direction of molecular sieve compounds, molecular sieves and base exchange phosphates, molecular sieve characteristic metal phosphates, etc.

Active Publication Date: 2019-01-29
LIAONING TECHNICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

How to control metal-substituted zinc phosphate EDI molecular sieves still faces great challenges

Method used

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  • Metal-doped EDI-type zinc phosphate molecular sieve and synthesis method thereof
  • Metal-doped EDI-type zinc phosphate molecular sieve and synthesis method thereof
  • Metal-doped EDI-type zinc phosphate molecular sieve and synthesis method thereof

Examples

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Effect test

example 1

[0024] Mix zinc acetate and water, add ferric chloride, stir magnetically for 0.5h, add isobutanol, continue stirring for 0.5h, add phosphorous acid to the solution, continue stirring for 2h, add template agent 1,2-propylenediamine , and finally stirred for 2h to form an initial reaction mixture and obtain a sol; the molar ratio of the initial reaction mixture is Zn:Fe:H 3 PO 3 :1,2-propanediamine: H 2 O: isobutanol = 1.0: 1.0: 4.0-8.0: 6.0-10.0: 444.4-888.8: 60-100. The obtained sol was left to stand for 0.5h, put into a 25ml polytetrafluoroethylene reactor, and placed in a 180°C oven for crystallization for 3 days. After the reaction was completed, the reactor was taken out and cooled naturally at room temperature to remove the product. The solid product is separated, washed, and dried to obtain an iron-doped EDI molecular sieve. The obtained product is a dark green square crystal and does not contain other amorphous substances, such as Figure 3a shown.

example 2

[0026] Mix zinc acetate and water, add cobalt acetate, stir magnetically for 0.5h, add isobutanol, continue stirring for 0.5h, add phosphorous acid to the solution, continue stirring for 3h, add template agent 1,2-propylenediamine, and finally Stir for 1h to form the initial reaction mixture and obtain a sol; the molar ratio of the initial reaction mixture is Zn:Co:H 3 PO 3 :1,2-propanediamine: H 2 O: isobutanol == 1.0: 1.0: 4.0-8.0: 6.0-10.0: 444.4-888.8: 60-100; the obtained sol was left to stand for 0.5h, put into a 25ml polytetrafluoroethylene reactor, and placed at 180 Crystallize in an oven at ℃ for 7 days. After the reaction is completed, take out the reaction vessel and let it cool naturally at room temperature to remove the product. The solid product is separated, washed and dried to obtain a cobalt-doped EDI molecular sieve. The obtained product is dark blue color cube crystals, such as Figure 3b shown.

example 3

[0028] Mix zinc chloride and water, add nickel chloride, stir magnetically for 0.5h, add isopropanol, continue stirring for 0.5h, add phosphorous acid to the solution, continue stirring for 1h, add template agent 1,2-propanedi Amine, and finally stirred for 1h to form the initial reaction mixture and obtain a sol; the molar ratio of the initial reaction mixture is Zn:Ni:H 3 PO 3 :1,2-propanediamine: H 2 O: Isopropanol = 1.0: 1.0: 4.0-8.0: 6.0-10.0: 444.4-888.8: 60-100; put the obtained sol for 0.5h, put it in a 25ml polytetrafluoroethylene reactor, and place it at 180°C Carry out crystallization in an oven for 5 days. After the reaction is completed, take out the reaction kettle and let it cool naturally at room temperature to remove the product. The solid product is separated, washed and dried to obtain a nickel-doped EDI molecular sieve. The obtained product is light green Cubic crystals with a relatively smooth surface, free of other amorphous phases such as Figure 3c s...

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Abstract

The invention discloses a metal-doped EDI-type zinc phosphate molecular sieve. The molecular sieve is of a metal-doped zinc phosphate double-metal-atom molecular sieve structure and is of a block shape. The invention further discloses a synthesis method of the metal-doped EDI-type zinc phosphate molecular sieve. The synthesis method comprises the following steps: adopting a hydrothermal / solvothermal method, taking phosphorous acid as a phosphorus source, taking zinc acetate as a zinc source, carrying out doping respectively by using iron salt, cobalt salt and nickel salt ions, taking 1,2-diaminopropane as an organic template agent, taking isobutanol and deionized wate as a mixed solvent, carrying out uniform stirring under magnetic stirring according to a certain molar ratio to obtain a gel, putting the gel is put into a 25-ml polytetrafluoroethylene-lining hydrothermal reaction kettle, and carrying out crystallizing at a temperature of 180 DEG C for 3-7 days under a self-generated pressure to obtain the zinc phosphate molecular sieve which is doped with different ions and has an EDI configuration. The method provides a novel synthesis method for synthesizing the EDI-type zinc phosphate molecular sieve material, and the zinc phosphate molecular sieve which is doped with different metals and has the EDI configuration is synthesized. No other impurity phases are contained, and the three different metal-doped zinc phosphate EDI molecular sieve has an anti-ferromagnetic property

Description

technical field [0001] The invention belongs to the technical field of zinc phosphate molecular sieve preparation, in particular to a metal-doped EDI zinc phosphate molecular sieve and a synthesis method thereof. Background technique [0002] Molecular sieves refer to inorganic microporous crystalline materials with regular nanopore or cage structures. From a structural point of view, the basic structural unit of the molecular sieve framework is TO 4 Tetrahedral (T=Si, Al, etc.), T atoms are connected to each other through oxygen bridges to form a structure with specific cages or micropores. Molecular sieves are widely used in fields closely related to energy and the environment, such as petroleum refining, petrochemicals, fine chemicals, and daily chemicals. They also show broad application prospects in the assembly of functional materials and drug embedding. With the development of science and technology, the application of molecular sieves in some emerging fields such a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/00C01B39/54
CPCC01B37/002C01B39/54C01P2004/38C01P2004/61C01P2006/42
Inventor 王学雷庄伟斌王鸣杨绍斌沈丁周晓谦
Owner LIAONING TECHNICAL UNIVERSITY
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