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Process for preparing beta zeolite containing phosphorus

A technology of beta zeolite and phosphoric acid, applied in chemical instruments and methods, molecular sieve and alkali exchange of phosphate, inorganic chemistry, etc., to achieve the effect of high catalytic selectivity

Active Publication Date: 2005-05-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] So far, there is no other report on the method of adding phosphorus element during the preparation process to synthesize phosphorus-containing zeolite beta

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

[0026]These examples illustrate the first step in the method of the invention: the preparation of the seed gel.

[0027] Synthesize beta zeolite crystal seed glue by the method that CN1154342A proposes: Pseudo-boehmite (containing Al 2 o 3 56.9% by weight, Zhoucun Catalyst Factory), sodium hydroxide (chemically pure, Beijing Chemical Plant), tetraethylammonium hydroxide (2.417N, Daxing Xingfu Fine Chemical Research Institute) were added to deionized water, heated to dissolve, and stirred evenly , to make a working solution, mix coarse-porous silica gel (80-100 mesh, 4.5% ignition loss, Qingdao Ocean Chemical Factory) with the above-mentioned working solution, make the surface of the silica gel wet by the working solution, and crystallize the resulting reaction mixture That is to obtain the seed glue used in the method of the present invention.

[0028] The relevant parameters are listed in Table 1.

[0029] Example 1

Embodiment 4-13

[0031] These examples illustrate the second step in the method of the invention: the introduction of phosphorus.

[0032] Aluminum phosphate was added to the seed gel prepared in Examples 1-3 to synthesize phosphorus-containing zeolite beta. The aluminum phosphate mentioned is composed of pseudoboehmite and phosphoric acid according to Al 2 o 3 with P 2 o 5 It is prepared by uniformly mixing pseudo-boehmite, phosphoric acid and water at a molar ratio of 1:1 and a volume ratio of water to phosphoric acid of 6:1.

[0033] The amount of aluminum phosphate used, crystallization temperature, crystallization time and relative crystallinity, particle size, P 2 o 5 The contents are listed in Table 2.

[0034] The samples prepared in these examples all have the same XRD patterns as zeolite beta. The test results prove that the added aluminum phosphate does not affect the crystallization of the zeolite by adopting the method provided by the invention. After the seed glue continue...

Embodiment 14

[0036] This example shows that the phosphorus-containing zeolite prepared by the method provided by the present invention has good alkylation reaction performance.

[0037] Take 10 g of the zeolite samples prepared in the comparative example and the example and exchange ammonium with 1.5N ammonium chloride solution for 4 times, each time for 2 hours; the filter cake after filtration is washed with water and dried at 110° C. for two hours. The treated zeolite was mixed with pseudo-boehmite according to zeolite (dry basis): Al 2 o 3 =35:65 weight ratio mixing, then adding 3-8% by weight of the total solids, the concentration of 1N nitric acid aqueous solution, kneading, molding, drying and roasting at 550 ° C for 2 hours, the obtained sample is used for the alkyl of benzene and ethylene reaction. The conditions of the alkylation reaction are: benzene / ethylene (molar ratio)=12, reaction temperature 250 DEG C, reaction pressure 3.8 MPa, liquid hourly space velocity 1 hour -1 . ...

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Abstract

During the preparation process of phosphorus containing beta-zeolite, work water solution compounded with aluminum source, alkali source and tetraethyl ammonium cationic solution is mixed with silica gel of granularity 20-300 mesh as silicon source to moisten the surface of the silica gel grain; the mixture is maintained at 80-140 deg.c for 20-80 hr to obtain crystal seed colloid; aluminum phosphate in the amount of 5-30 wt% of the crystal seed colloid is thrown into the crystal seed colloid, and through homogeneous mixing, crystallization at 140-170 deg.c for 50-100 hr, separation of solid matter, washing to Na2O content less than 0.1 wt% and drying, phosphorus containing beta-zeolite is prepared. The beta-zeolite product may contain phosphorus up to 5 wt% and has relatively high catalytic selectivity when being used in alkylation.

Description

technical field [0001] The invention relates to a preparation method of phosphorus-containing beta zeolite. technical background [0002] Beta zeolite, as a catalytically active component, is suitable for hydrocarbon transfer reactions such as hydrocracking, hydroisomerization, hydrofinishing, hydrodewaxing, diesel oil decondensation, hydrocarbon cracking, alkylation, and olefin hydration. catalyst. The zeolite was synthesized by the classic hydrothermal crystallization method for the first time in 1967 by the Mobile Company of the United States (USP3,308,069). According to the patent, zeolite beta is synthesized as follows: will contain Na 2 O source, Al 2 o 3 source, tetraethylammonium hydroxide (TEAOH), SiO 2 The mixture of source and water is made into a slurry, and the crystallization reaction is carried out in an autoclave at 75-200°C for 3-60 days. The molar ratio of the reaction system is: SiO 2 / Al 2 o 3 =10-200, Na 2 O / TEAOH=0.0-0.1, TEAOH / SiO 2 = 0.1-1.0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/10C01B39/54
Inventor 贾晓梅刘冠华高扬舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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