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Synthetic method for phosphorus-containing ZSM-5 molecular sieve

A technology of ZSM-5 and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of unfavorable industrial production and high cost of silica-alumina gel, and reduce the synthesis cost , the effect of reducing pollution

Active Publication Date: 2014-08-06
CHINA PETROLEUM & CHEM CORP +1
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AI Technical Summary

Problems solved by technology

The preparation method uses solid silica-alumina gel as raw material, and the single-pot yield is high, but the cost of silica-alumina gel is relatively high, which is not conducive to large-scale industrial production

Method used

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Examples

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preparation example Construction

[0014] The synthetic method of phosphorus-containing ZSM-5 molecular sieve provided by the invention comprises the following steps:

[0015] (1) Mix the first organic template agent with the aluminum source, the first organic template agent in the mixture and the Al in the aluminum source 2 o 3 The molar ratio is 0.2-40:1, and the mixture is treated in a closed reactor at 50-190°C for 0.1-5 hours and then cooled to obtain an intermediate product, wherein the aluminum source is selected from aluminum phosphate molecular sieves and / or silicon Aluminum phosphorus molecular sieve;

[0016] (2) Mix the intermediate product of step (1) with the second organic template agent, silicon source and water evenly, and the SiO in the mixture is calculated by mole 2 / Al 2 o 3 =20~300, the second organic template: SiO 2 =0.01~0.2,H 2 O / SiO 2 =6~10;

[0017] (3) Transfer the mixture obtained in step (2) to a high-pressure reactor for hydrothermal crystallization. The temperature and ti...

Embodiment 1

[0027] This example illustrates the synthesis method of the phosphorus-containing ZSM-5 molecular sieve provided by the present invention.

[0028] Weigh 2 grams of SAPO-34 molecular sieve (Hunan Jianchang Company, SiO 2 Content 9.39%, Al 2 o 3 Content 43.1%, P 2 o 5 Content 47.4%), mix it with 30.84g tetramethylammonium hydroxide aqueous solution (Beijing Jiayousheng New Technology Development Center, analytically pure, TMAOH content 10%), the mixture molar ratio TMAOH / Al 2 o 3 =4. The mixture was placed in a polytetrafluoro-lined crystallization kettle, reacted at 150°C for 4 hours and then cooled to room temperature. After that, it was mixed with 25.58g of silica gel (Qingdao Ocean Chemical Co., Ltd., SiO 2 content 98.4%), 4.56g tetrapropylammonium bromide (Sinopharm Chemical Reagent Co., Ltd., chemically pure) and 32.67g water are mixed, and the molar ratio of the mixture is SiO 2 / Al 2 o 3 =50, TPABr / SiO 2 =0.04,H 2 O / SiO 2 =8. The mixture was subjected to hy...

Embodiment 2

[0030] This example illustrates the synthesis method of the phosphorus-containing ZSM-5 molecular sieve provided by the present invention.

[0031] Weigh 0.5 gram of AlPO4 molecular sieve (Hunan Jianchang Company, Al 2 o 3 Content 46.1%, P 2 o 5 Content 52.9%), mix it with 6.66g tetraethylammonium hydroxide aqueous solution (Shanghai Yongsheng Reagent Factory, analytical grade, TEAOH content 40%), the mixture molar ratio TEAOH / Al 2 o 3 =8. It was placed in a crystallization kettle with polytetrafluoroethylene lining, reacted at 150°C for 4 hours and then cooled to room temperature. After that, it was mixed with 27.57g of silica gel (Qingdao Ocean Chemical Co., Ltd., SiO 2 content 98.4%), 22.07g tetrapropylammonium hydroxide aqueous solution (Beijing Jiayousheng New Technology Development Center, analytically pure, TPAOH content 25%) and 28.29g water, the mixture molar ratio SiO 2 / Al 2 o 3 =200,TPAOH / SiO 2 =0.06,H 2 O / SiO 2 =6. The mixture was subjected to hydrothe...

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Abstract

The invention discloses a synthetic method for a phosphorus-containing ZSM-5 molecular sieve. The method comprises the following steps: mixing a first organic template with an aluminum source, wherein in the obtained mixture, a mol ratio of the first organic template to Al2O3 in the aluminum source is 0.2-40: 1; treating the mixture in an enclosed reaction vessel at a temperature of 50 to 190 DEG C for 0.1 to 5 h and then carrying out cooling so as to obtain an intermediate product; and uniformly mixing the intermediate product with a second organic template, a silicon source and water and carrying out hydrothermal crystallization so as to obtain the phosphorus-containing ZSM-5 molecular sieve; wherein the aluminum source is an aluminum phosphate molecular sieve and / or silicon-phosphorus-aluminum molecular sieve. The method adopts a synthetic process route different from that in the prior art, abandons usage of high-cost silica-alumina gel as the silicon source and the aluminum source and can directly prepare the phosphorus-containing ZSM-5 molecular sieve, so synthesis cost is reduced.

Description

technical field [0001] The invention relates to a method for synthesizing a phosphorus-containing ZSM-5 molecular sieve, and more specifically relates to a method for synthesizing a phosphorus-containing ZSM-5 molecular sieve in a sodium-free system. 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. [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-5, which must be converted into hydrogen-type molecular sieves through ion exchange. catalyst. The ion exchange process produces a large amount of ammonia-nitrogen wastewater or acid-containing wastewater, which puts a lot of ...

Claims

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Application Information

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