ZSM-5 molecular sieve containing phosphorus in crystal, synthetic method and application thereof

A ZSM-5, synthesis method technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., can solve the problems of high price, affecting the catalytic activity of molecular sieve catalysts, and affecting the stability of molecular sieves. The effect of catalytic activity

Active Publication Date: 2017-01-11
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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  • Claims
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Problems solved by technology

[0007] Nichiappan lingappan et al. (Bull.Chem.Soc.Jpn, 1996,69,1125-1128) used quaternary phosphorus salts as templates and roasted them after synthesis to obtain phosphorus-containing ZSM-5 molecular sieves, wherein the phosphorus content was between 0.4 and 0.6wt% range, but quaterna

Method used

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Examples

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preparation example Construction

[0021] A method for synthesizing ZSM-5 molecular sieves containing phosphorus in crystals, comprising the following steps:

[0022] (1) Mix the quaternary ammonium base, tetrabutylphosphorus hydroxide and the aluminum source. The mixture is treated in a closed reaction kettle at 50-190°C for 0.1-5 hours and then cooled to obtain an intermediate product. The aluminum source does not contain alkali Aluminum source of metal ions;

[0023] (2) mixing the intermediate product of step (1) with silicon source and water to obtain a mixture;

[0024] (3) The mixture in step (2) is placed in a closed reactor for hydrothermal crystallization and the product is recovered.

[0025] In the synthetic method provided by the invention, in the mixture described in step (1), the sum of the moles of quaternary ammonium base and tetrabutylphosphorus hydroxide 2 o 3 The ratio of the number of moles of the aluminum source is 0.2 to 40:1; preferably, the sum of the number of moles of the quaternar...

Embodiment 1

[0050] This example illustrates the synthetic method provided by the present invention.

[0051] Weigh 0.21 gram of pseudo-boehmite (Hunan Jianchang Company, Al 2 o 3 content 70.11%), with 16.56g tetramethylammonium hydroxide aqueous solution (Beijing Jiayousheng New Technology Development Center, analytically pure, TMAOH content 10%) and 4.08g tetrabutylphosphine hydroxide (TBPOH, Sinopharm Chemical Reagent Co., Ltd. company, content 40%,) mixing, mixture molar ratio TMAOH / TBPOH=3, organic template agent / Al 2 o 3 = 10.6.

[0052] It was placed in a crystallization kettle containing a polytetrafluoroethylene liner, cooled to room temperature after reacting for 3 hours at 150° C., and then mixed with 30 g of silica gel (Qingdao Ocean Chemical Co., Ltd., SiO 2 Content 99% solid content 92%) mixes with 33.20g water, mixture molar ratio SiO 2 / Al 2 o 3 =200,H 2 O / SiO 2 = 6.5. The mixture was subjected to hydrothermal crystallization at 120° C. for 73 hours in an autoclav...

Embodiment 2

[0062] This example illustrates the synthetic method provided by the present invention.

[0063] Weigh 0.5 gram of pseudo-boehmite (Hunan Jianchang Company, Al 2 o 3content 75%), it was mixed with 8.36g tetraethylammonium hydroxide aqueous solution (Shanghai Yongsheng Reagent Factory, analytically pure, TEAOH content 40%) and 4.71g tetrabutylphosphine hydroxide (TBPOH, Sinopharm Group Chemical Reagent Co., Ltd., content 40%) %) mixed, mixture molar ratio TEAOH / TBPOH=3.33, organic template / Al 2 o 3 = 6.5. It was placed in a crystallization kettle containing a polytetrafluoroethylene lining, cooled to room temperature after reacting for 2 hours at 150°C, after that, it was mixed with 30g silica gel (Qingdao Ocean Chemical Co., Ltd., SiO 2 Content 99% solid content 92%) mixes with 54.9g water, mixture molar ratio SiO 2 / Al 2 o 3 =100,H 2 O / SiO 2 =8. The mixture was subjected to hydrothermal crystallization at 130° C. for 40 hours in an autoclave. After crystallization,...

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Abstract

The invention discloses a synthetic method of ZSM-5 molecular sieve containing phosphorus in crystal. The method comprises the following steps: (1) quaternary ammonium hydroxide and tetrabutylphosphonium hydroxide and an aluminium source are mixed, a mixture is treated in an enclosed reaction vessel for 0.1-5 hours at 50-190 DEG C and cooled, an intermediate product is obtained, and an aluminium source is an aluminium source without alkali metal ions; (2) the intermediate product in the step (1) and a silicon source and water are uniformly mixed in order to obtain a mixture; (3) the mixture in the step (2) is placed in the enclosed reaction vessel for hydrothermal crystallization and products are recycled. The synthesized ZSM-5 molecular sieve containing phosphorus in crystal can be used as an active component for catalysis of tetradecane with higher cracking conversion rate.

Description

technical field [0001] The invention relates to a phosphorus-containing ZSM-5 molecular sieve, a synthesis method and its application, more specifically to a phosphorus-containing ZSM-5 molecular sieve in crystals, a synthesis method of an alkali-free metal system and its application. Background technique [0002] ZSM-5 molecular sieve is a high silicon medium pore molecular sieve with MFI structure. It has a unique pore structure and is widely used in important petrochemical units such as catalytic cracking, aromatization, and alkylation. Phosphorus-modified ZSM-5 has good catalytic performance, high thermal stability and hydrothermal stability, and is widely used in catalytic cracking, alkylation and other reaction processes. [0003] The synthesis system of ZSM-5 molecular sieves usually uses inorganic bases (such as sodium hydroxide) to form an alkaline environment suitable for the crystallization of molecular sieves. The synthesized molecular sieves are sodium-type ZSM-...

Claims

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Application Information

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IPC IPC(8): C01B39/40B01J29/40C10G11/05C10G47/16
Inventor 王萍王殿中罗一斌慕旭宏舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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