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Method for preparing beta zeolite

A technology of beta zeolite and seed crystal, which is applied in the field of inorganic material synthesis and catalytic application, can solve the problem that the synthesis cost accounts for the main part, and achieve the effect of improving synthesis efficiency, reducing synthesis cost and reducing dosage

Active Publication Date: 2011-10-12
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in essence, all patented technologies use TEAOH as a template. Even if only a small amount of this template is used, it still accounts for a major part of the synthesis cost.

Method used

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  • Method for preparing beta zeolite
  • Method for preparing beta zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Take 2.16 parts of TEABr template agent and 0.12 parts of organic accelerator A, add to 8.3 parts of 12% sodium hydroxide solution, stir and dissolve, then add 1.88 parts of sodium aluminate, continue to stir until the system is uniform and transparent, and then add 12.5 parts Slowly add silica sol to the above solution, and add 5 parts of solid silica gel under stirring, stir vigorously for 20 minutes, transfer to a closed stainless steel reaction kettle lined with polytetrafluoroethylene, and crystallize at 140°C for 48 hours , and continued to crystallize at 160° C. for 32 hours, and the obtained product was filtered, washed and dried to obtain zeolite beta.

[0047] The molar ratio of raw materials in the reaction system is: Na 2 O / SiO 2 =0.12,H 2 O / SiO 2 =5, (TEA) 2 O / SiO 2 =0.03, SiO 2 / Al 2 o 3 =20.

[0048] The relative crystallinity of the beta zeolite prepared in this example and the beta zeolite obtained in comparative example 1 is 106%. A small amou...

Embodiment 2～5

[0053] Preparation of the seed liquid: take the raw powder of zeolite beta, add it into 15% sodium hydroxide solution according to the solid-liquid ratio of 1:5.5, and treat it at 55° C. for 30 minutes.

[0054] According to the material ratio given in Table 1 and the addition of each substance, the specific steps are to first take TEABr template agent, organic accelerator A or inorganic accelerator C, add them to the sodium hydroxide solution under stirring, and stir to dissolve. , add pseudo-boehmite, continue to stir until the system is uniform, then add solid silica gel, stir vigorously, add seed liquid, continue to stir for 20 minutes, transfer to a closed stainless steel reaction kettle lined with polytetrafluoroethylene to crystallize The product was filtered, washed and dried to obtain zeolite beta.

[0055] The relative crystallinity of the product was determined by X-ray diffraction analysis, and the crystallinity of zeolite beta prepared in Comparative Example 1 was...

Embodiment 6～9

[0060] Preparation of the seed crystal liquid: take the raw powder of zeolite beta, add it into 12% sodium hydroxide solution at a solid-to-liquid ratio of 1:7, and treat it at 60° C. for 20 minutes.

[0061] According to the ratio of materials given in Table 1 and the addition of each material, feed intake, get TEABr template agent, surfactant (A is sodium dodecylbenzenesulfonate, B is cetyltrimethylammonium bromide ) and phosphate (C is magnesium phosphate, D is potassium hydrogen phosphate), added to the sodium hydroxide solution under stirring, after stirring and dissolving, adding sodium aluminate, continuing to stir until the system is uniform, then adding silica sol, solid silica gel, After vigorously stirring evenly, add a certain amount of seed liquid, continue stirring for 20 minutes, transfer to a closed stainless steel reaction kettle lined with polytetrafluoroethylene for crystallization, and filter, wash and dry the product to obtain zeolite beta. The amount of m...

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Abstract

The invention discloses a method for preparing beta zeolite. The method is low in cost and high in efficiency. The method specifically comprises the following steps of: adding a sodium source, an aluminum source, a template agent, and an organic accelerator and / or inorganic accelerator into water, stirring uniformly and mixing the mixture and a silicon source, and violently stirring until the system materials form a uniformly dispersed mixture; and crystallizing the reaction mixture and filtering a crystallization product, washing and drying to obtain the beta zeolite with relatively high crystallinity. The method has the characteristics that: the using amount of a tetraethylammonium cation template agent is reduced by adding the organic accelerator and / or inorganic accelerator, the solid content in a synthesis system is high, the crystallization time is short, and the single-kettle yield of the product is high, so that the synthesis cost of the beta zeolite can be reduced.

Description

technical field [0001] The invention belongs to the field of inorganic material synthesis and catalytic application, and relates to a preparation method of zeolite materials. Specifically, it is a method for preparing zeolite beta in the presence of trace amounts of tetraethylammonium ions. technical background [0002] Beta zeolite is a patented product USP3308069 researched and developed by Mobil Petroleum Company of the United States in 1967. The method is to contain Na 2 O, Al 2 o 3 , tetraethylammonium hydroxide (TEAOH), SiO 2 The mixture with water is made into a slurry, and the crystallization reaction is carried out in an autoclave at 75-200°C for 3-60 days. Reaction system feed molar ratio: SiO 2 / Al 2 o 3 =10~200, TEAOH / SiO 2 = 0.1 ~ 1.0, Na 2 O / TEAOH=0.0~0.1, H 2 O / TEAOH = 20-75. In this method, the water content in the system is large, which leads to a large dosage of the template agent TEAOH and a long crystallization time, which brings about the pro...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 窦涛潘惠芳庞新梅李强巩雁军徐庆虎张瑛邢法猛李阳阎立军
Owner PETROCHINA CO LTD
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