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Synthesis of porous ZSM-5 zeolite and gamma-Al2O3 composite material and preparation of hydrodesulfurization catalyst

A MZSM-5-A, composite material technology, applied in physical/chemical process catalysts, molecular sieve catalysts, refined hydrocarbon oil, etc., can solve the problems of low mechanical strength of porous zeolite, difficult to apply, difficult to shape, etc., to achieve repeatability High sex, improve interaction, avoid the effect of agglomeration

Active Publication Date: 2017-02-15
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the mechanical strength of porous zeolite is not high, it is difficult to form in the catalyst forming process, and it is difficult to apply to the actual industry

Method used

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  • Synthesis of porous ZSM-5 zeolite and gamma-Al2O3 composite material and preparation of hydrodesulfurization catalyst
  • Synthesis of porous ZSM-5 zeolite and gamma-Al2O3 composite material and preparation of hydrodesulfurization catalyst
  • Synthesis of porous ZSM-5 zeolite and gamma-Al2O3 composite material and preparation of hydrodesulfurization catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Preparation of ZSM-5: γ-Al 2 O 3 = 9:1 The composite material method is realized by the following steps:

[0030] (1) Weigh 0.357g NaAlO 2 And 0.522g NaOH dissolved in 19.6mL water, add a mixed solution of ethyl orthosilicate and TAPOH (10mL TEOS and 26mL 25wt.% TPAOH), when it is completely dissolved, the NaAlO 2 Take Al 2 O 3 Calculated, TEOS is SiO 2 Calculate, then add 2.5mL DEAB, the molar ratio of each material is Al 2 O 3 :Na 2 O:TPAOH:SiO 2 :DEAB:H 2 O=1:4:20:20:2:500. After the reaction is complete, 0.72 g of pseudo-boehmite is added and stirred until it is completely dissolved. The reacted mixture was added to a 50mL hydrothermal kettle, and then crystallized at 180°C for 3 days. After natural cooling, wash with water at room temperature, suction filtration, 100℃ oven, 550℃ calcination for 5h. The texture properties of the resulting carrier are shown in Table 1.

[0031] (2) Add 0.0699g (NH 4 ) 6 Mo 7 O 24 ·4H 2 O, 0.0576g Co(NO 3 ) 2 ·6H 2 O and 0.0579g EDTA dis...

Embodiment 2

[0033] Preparation of ZSM-5: γ-Al 2 O 3 = 9:1 The composite material method is realized by the following steps:

[0034] (1) Weigh 0.357g NaAlO 2 And 0.522g NaOH dissolved in 19.6mL water, add a mixed solution of TEOS and TAPOH (10mL TEOS and 26mL 25wt.% TPAOH), when it is completely dissolved, the NaAlO 2 Take Al 2 O 3 Calculated, TEOS is SiO 2 Calculate, then add 2.5mL DEAB, the molar ratio of each material is Al 2 O 3 :Na 2 O:TPAOH:SiO 2 :DEAB:H 2 O=1:4:20:20:2:500. After the reaction is complete, 0.72 g of pseudo-boehmite is added and stirred until it is completely dissolved. The reacted mixture was added to a 50mL hydrothermal kettle, and then crystallized at 180°C for 3 days. Filter, wash, dry, and calcine at 550°C for 5 hours. The texture properties of the resulting carrier are shown in Table 1.

[0035] (2) 0.2116g (NH 4 ) 6 Mo 7 O 24 ·4H 2 O, 0.1744g Co(NO 3 ) 2 ·6H 2 O and 0.1751g EDTA are dissolved in a certain amount of water, and after all are dissolved, they are dro...

Embodiment 3

[0037] Preparation of ZSM-5: γ-Al 2 O 3 = 9:1 The composite material method is realized by the following steps:

[0038] (1) Weigh 0.357g NaAlO 2 And 0.522g NaOH dissolved in 19.6mL water, add a mixed solution of TEOS and TAPOH (10mL TEOS and 26mL 25wt.% TPAOH), when it is completely dissolved, the NaAlO 2 Take Al 2 O 3 Calculated, TEOS is SiO 2 Calculate, then add 2.5mL DEAB, the molar ratio of each material is Al 2 O 3 :Na 2 O:TPAOH:SiO 2 :DEAB:H 2 O=1:4:40:20:2:500. After the reaction is complete, 0.72 g of pseudo-boehmite is added and stirred until it is completely dissolved. The reacted mixture was added to a 50mL hydrothermal kettle, and then crystallized at 180°C for 3 days. Filter, wash, dry, and calcine at 550°C for 5 hours. The texture properties of the resulting carrier are shown in Table 1.

[0039] (2) 0.1964g (NH 4 ) 6 Mo 7 O 24 ·4H 2 O, 0.1618g Co(NO 3 ) 2 ·6H 2 O and 0.1628g EDTA are dissolved in a certain amount of water, and after all are dissolved, drip into 1g...

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Abstract

The invention discloses synthesis of a porous ZSM-5 zeolite and gamma-Al2O3 composite material and preparation of a hydrodesulfurization catalyst and relates to the technical field of composite materials and the field of hydrodesulfurization catalysts. The composite material is roasted for 3-8 h at the temperature of 450-600 DEG C, and has the following properties that the content of porous ZSM-5 zeolite is 5-95 wt.%, the content of gamma-Al2O3 is 5-95 wt.%, the specific surface area is 400-600 m<2>.g1, the mesopore volume is 0.40-0.85 cm<3>.g1, and the micropore volume is 0.06-0.15 cm<3>. g1. The composite material has multiple stages of porous structures, good hydrothermal stability, high mechanical strength and weak interaction with loaded metal species, changes the existence state of the metal species and promotes reducing and vulcanizing of the metal species, multiple layers of high-activity molybdenum sulfide or tungsten sulfide active phases are easily formed on the composite material, and the hydrodesulfurization performance of the metal sulfide catalyst is improved.

Description

Technical field [0001] The invention relates to the technical field of composite materials and the field of hydrodesulfurization catalysts, in particular to porous ZSM-5 zeolite and γ-Al 2 O 3 The preparation of composite carrier and its application of supporting metal sulfide in hydrodesulfurization reaction. Background technique [0002] In recent years, as the quality of crude oil worldwide has become heavier and worse, the content of difficult-to-remove dibenzothiophene compounds such as 4,6-dimethyldibenzothiophene in the processed diesel fraction Increasingly, these sulfur-containing organic compounds inevitably generate sulfur oxides during the combustion process, resulting in acid rain, which seriously pollutes the atmosphere. Therefore, countries all over the world have issued strict environmental protection regulations. For example, in September 2009, Europe implemented strict European VI standards, which clearly stipulated that the sulfur content of diesel oil should b...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J29/48B01J35/10C10G45/12
CPCC10G45/12B01J29/40B01J29/48C10G2300/202C10G2300/70B01J35/60
Inventor 唐天地俞泉勇傅雯倩张磊
Owner CHANGZHOU UNIV
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