Preparation method of binderless spherical faujasite particles

A faujasite and binder-free technology, which is applied in the field of preparation of spherical zeolite particles, can solve problems such as the decline in adsorption capacity and mass transfer performance, and achieve the effects of good crushing strength, simple method, and high zeolite content

Active Publication Date: 2014-01-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The mechanical strength of the zeolite particles prepared in this way is directly proportional to the amount of the binder. The higher the binder content, the better the strength, but it will cause a significant decline in adsorption capacity and mass transfer performance. Find a balance between

Method used

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  • Preparation method of binderless spherical faujasite particles
  • Preparation method of binderless spherical faujasite particles
  • Preparation method of binderless spherical faujasite particles

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0041] Silica gel pellets are prepared according to the method of the present invention.

[0042] Take sodium silicate solution A (produced by Sinopec Catalyst Qilu Branch), which contains SiO 2 19.9% ​​by mass, Na 2 O 6.1% by mass, density at 25°C is 1.253g / cm 3 .

[0043] Slowly add 7.14 kg of concentrated sulfuric acid with a concentration of 98% by mass into 42.84 kg of deionized water under stirring conditions, and then add 6.50 kg of ammonium sulfate, stir and dissolve evenly, and record it as solution B. H in solution B 2 SO 4 The concentration is 12.39% by mass, (NH 4 ) 2 SO 4 The concentration is 11.51% by mass, and the density at 25°C is 1.135g / cm 3 .

[0044] Cool the two solutions of A and B to 5°C, inject the A and B solutions into the nozzle at a certain flow rate through the metering pump and quickly mix them to form a sol, adjust the injection ratio of the A and B solutions, and control the pH value of the sol to 6.7, The silica content in this was 11...

example 2

[0046] According to the method of the present invention, X zeolite particles are prepared by in-situ crystallization of silica gel beads.

[0047] (1) Preparation of directing agent

[0048] In a 500 ml beaker, add 27.6 g of sodium metaaluminate solution (produced by Sinopec Catalyst Qilu Branch, containing Al 2 o 3 10.6% by mass, Na 2 O 12.5% ​​by mass), 56.8 grams of deionized water and 29.9 grams of sodium hydroxide (produced by Beijing Chemical Plant, with a purity of 99% by mass), stirred to completely dissolve the solid sodium hydroxide, and added 155.8 grams of sodium silicate solution (Sinopec catalyst Qilu Branch production, including SiO 2 19.9% ​​by mass, Na 2 O 6.1% by mass). The molar composition of the mixture in terms of oxides is 20.2Na 2 O:Al 2 o 3 : 18SiO2 2 : 387H 2 O, stirred at 400 rpm until uniformly mixed, and aged at 25°C for 16 hours to prepare the directing agent.

[0049] (2) Preparation of X zeolite particles

[0050] Add 403.9 grams of ...

example 3

[0053] Prepare X zeolite particle by the method for example 2, difference is (2) in step, add 767.3 gram sodium metaaluminate solutions, 596.5 gram deionized water, 29.1 gram sodium hydroxide, stir and make it fully mix, in synthesis kettle Add 142.9 grams of the silica gel pellets prepared in Example 1 at a stirring speed of 150 rpm, age under stirring at 40°C for 4 hours, then add 30.7 grams of directing agent, and the molar composition of the total mixture in terms of oxides is 2.4Na 2 O:Al 2 o 3 ︰3.0SiO2 2 : 105H 2 O, then crystallized, washed, filtered, and dried to obtain the X zeolite granular product. The detailed test results of its physical and chemical properties are shown in Table 1.

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Abstract

A preparation method of binderless spherical faujasite particles comprises the following steps: 1, mixing an aqueous solution of sodium silicate with a solution of a peptizing agent at -5-10DEG C to prepare a sol having a pH value of 5.0-8.0, adding the sol into an oil column in a dropwise manner to generate hydrogel beads, collecting the hydrogel beads, washing with water, ageing, drying, and roasting to prepare silica gel beads, wherein the specific surface area and pore volume of the silica gel beads, determined through a BET method, are 200-500m<2>/g and 0.6-1.5mL/g respectively, and the peptizing agent comprises an inorganic acid and an inorganic ammonium salt; 2, uniformly mixing sodium silicate, sodium metaaluminate, sodium hydroxide and water according to a molar ratio of (16-24)Na2O:Al2O3:(15-20)SiO2:(300-500)H2O, and ageing at 0-30DEG C for 10-30h to prepare a liquid phase directing agent; and 3, mixing the silica gel beads with a sodium metaaluminate solution to obtain a mixed material, ageing the mixed material at 30-60DEG C, adding the directing agent prepared in step 2 to the mixed material, heating to 90-110DEG C, crystallizing, washing obtained crystallized products with water, and drying. The method is simple to operate, and the prepared faujasite particles have a high strength and a large adsorption capacity.

Description

technical field [0001] The invention is a method for preparing spherical zeolite particles, in particular, a method for preparing spherical zeolite particles without binder. Background technique [0002] Faujasite is widely used in many fields of petroleum refining and petrochemical industry because of its good adsorption and catalytic properties. According to different silicon-aluminum ratios, artificially synthesized faujasite can be divided into low-silicon X-type zeolite and high-silicon Y-type zeolite. Among them, X zeolite is mainly used as an adsorbent for adsorption separation and purification of gases, adsorption separation of aromatic hydrocarbon isomers, desulfurization agent and desiccant, etc. Y zeolite is the main active component of heavy oil catalytic cracking and hydrocracking catalysts, and is also used It can be used as an adsorbent for separating aromatic hydrocarbon isomers. Industrial production of faujasite generally uses water glass, sodium metaalum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02
Inventor 王辉国马剑锋王德华郁灼
Owner CHINA PETROLEUM & CHEM CORP
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