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Synthesizing method of phosphorus-containing MCM-22 zeolite

A synthetic method and technology of molecular sieves, applied in molecular sieves and base exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of low alkali content, high price, low stability of sodium oxide, etc.

Active Publication Date: 2017-05-31
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually, the synthesis of MCM-22 molecular sieves requires the use of hexamethyleneimine (HMI) as a template, and HMI is highly toxic and expensive, and its production, transportation, storage and use are strictly controlled
Studies in recent years have shown that low-toxicity and easy-to-obtain piperidine (PI) can replace HMI as a template for the synthesis of MCM-22 molecular sieves. The required amount of alkali is relatively low, and when sodium metaaluminate solution is used as the aluminum source, its sodium oxide (Na 2 O) content is too low then stability is poor, even be difficult to prepare, and increase its Na 2 O content, will lead to Na in the synthetic system 2 O content exceeds the amount of alkali required

Method used

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  • Synthesizing method of phosphorus-containing MCM-22 zeolite
  • Synthesizing method of phosphorus-containing MCM-22 zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Under stirring conditions, 20.0g sodium metaaluminate solution (16.8wt.%Al 2 O 3 , Na 2 O and Al 2 O 3 The molar ratio is 2.45), 206.6g deionized water, 34.0g piperidine, 2.4g phosphoric acid (85wt.%H 3 PO 4 ), 202.0g silica sol (29.7wt.%SiO 2 , 0.3wt.%Na 2 O) and 3.2gMCM-22 seed crystals, the molar ratio is SiO 2 / Al 2 O 3 = 30, Na 2 O / SiO 2 =0.06, PI / SiO 2 = 0.4, H 2 O / SiO 2 =20 and the seed crystal is SiO 2 With Al 2 O 3 The raw material mixture with a total mass of 5.0%, the synthesis kettle was sealed and crystallized at 152°C for 48 hours. The product (A1) obtained was phosphorus-containing MCM-22 molecular sieve with a phosphorus content of 0.14wt.%. XRD of the raw powder and the calcined sample Spectrum is shown in figure 2 . figure 2 versus figure 1 The XRD spectra of the original powder and the calcined sample were similar, indicating that the introduction of phosphorus did not affect the crystal phase structure of MCM-22 molecular sieve.

Embodiment 2

[0020] Under stirring conditions, 21.9g sodium metaaluminate solution (16.8wt.%Al 2 O 3 , Na 2 O and Al 2 O 3 The molar ratio is 2.92), 206g deionized water, 34.0g piperidine, 6.5g phosphoric acid (85wt.%H 3 PO 4 ), 202.0g silica sol (29.7wt.%SiO 2 , 0.3wt.%Na 2 O) and 1.9g MCM-22 seed crystals to obtain a molar ratio of SiO 2 / Al 2 O 3 = 27.8, Na 2 O / SiO 2 =0.03, PI / SiO 2 = 0.4, H 2 O / SiO 2 =20 and the seed crystal is SiO 2 With Al 2 O 3 The raw material mixture with a total mass of 3.0%, the synthesis kettle was sealed and crystallized at 152°C for 48 hours. The product (A2) obtained was phosphorus-containing MCM-22 molecular sieve with a phosphorus content of 0.52wt.%. The XRD of the raw powder and the calcined sample Spectrum and figure 2 similar.

Embodiment 3

[0022] Under stirring conditions, 20.0g sodium metaaluminate solution (16.8wt.%Al 2 O 3 , Na 2 O and Al 2 O 3 The molar ratio is 1.52), 222.6g deionized water, 25.5g piperidine, 3.8g phosphoric acid (85wt.%H 3 PO 4 ), 202.0g silica sol (29.7wt.%SiO 2 , 0.3wt.%Na 2 O) and 3.2g MCM-22 seed crystals to obtain a molar ratio of SiO 2 / Al 2 O 3 = 30, Na 2 O / SiO 2 =0.01、PI / SiO 2 = 0.3, H 2 O / SiO 2 =21 and the seed crystal is SiO 2 With Al 2 O 3 The raw material mixture of 5% of the total mass is sealed in the synthesis kettle and crystallized at 168°C for 24 hours. The product (A3) obtained is phosphorus-containing MCM-22 molecular sieve with a phosphorus content of 0.24wt.%. The XRD of the raw powder and the calcined sample Spectrum and figure 2 similar.

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Abstract

The invention provides a synthesizing method of a phosphorus-containing MCM-22 zeolite, and belongs to the technical field of chemical synthesis of inorganic materials. The synthesizing method comprises the following steps: uniformly mixing silica sol, a sodium metaaluminate solution, phosphoric acid, piperidine (PI), deionized water and a crystal seed which are used as reaction raw materials; hydrothermally crystallizing for 20 to 72 hours under the temperature of 140-170 DEG C; then washing, separating and drying to obtain the phosphorus-containing MCM-22 zeolite. The method capable of synthesizing the phosphorus-containing MCM-22 zeolite in one step is simple and easy to carry out, so that the convenience of mass production is ensured; the synthesized product has a high application value.

Description

Technical field [0001] The invention belongs to the technical field of inorganic material chemical synthesis, and specifically relates to a method for synthesizing phosphorus-containing MCM-22 molecular sieve. Background technique [0002] Molecular sieves have uniform pore structure, good adsorption performance and ion exchange capacity, and suitable acidity. They can be widely used in adsorption and separation, ion exchange and catalytic reaction processes, especially in the petrochemical industry. Generally, molecular sieves are obtained through hydrothermal synthesis reactions. The hydrothermal synthesis of molecular sieves mainly includes two basic processes: the formation of aluminosilicate hydrated gels and the crystallization of hydrated gels. Crystallization is a very complicated process and there is still a lack of clear theoretical understanding. Therefore, the synthesis of molecular sieves It is a highly experimental subject area, and various opinions and conclusions...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/10C01B39/04
CPCC01B39/04C01B39/10C01P2002/72
Inventor 谢素娟高扬徐龙伢刘盛林朱向学陈福存李秀杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI