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Process for preparing fine-grain X zeolite

A technology of small crystal grains and zeolite, applied in the field of preparing small crystal grain X zeolite, can solve problems such as low utilization rate of zeolite

Inactive Publication Date: 2003-10-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The adsorbent made of this zeolite has a low utilization rate of zeolite under the operating conditions of adsorption and separation

Method used

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  • Process for preparing fine-grain X zeolite

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preparation example Construction

[0008] The method for preparing small grain X zeolite provided by the invention comprises the following steps:

[0009] (1) The silicon-containing compound, aluminum-containing compound, sodium hydroxide and water are (11~18)Na according to the molar ratio 2 O:Al 2 o 3 :(10~17)SiO 2 :(100~350)H 2 Mixed with the ratio of O, aged at 0-10°C to make the directing agent,

[0010] (2) Mix silicon-containing compound, aluminum-containing compound and water with the directing agent prepared in (1) uniformly at 0-10°C, so that the molar composition of the total mixture obtained after adding the directing agent is (2.5-5)Na 2 O:Al 2 o 3 :(3~5)SiO 2 :(40~200)H 2 O,

[0011] (3) crystallize the total mixture prepared in (2) at 80-120° C. for 2-40 hours, wash with water, filter and dry.

[0012] Step (1) of the above-mentioned preparation method is to prepare a directing agent, and the raw material ratio of the directing agent can be prepared by a conventional method, such as pre...

example 1

[0024] The small crystal X zeolite was prepared according to the method described in the present invention.

[0025] (1) Preparation of directing agent

[0026] In 264 ml of water glass (Na 2 O1.384 mol / L, SiO 2 4.644 mol / liter, specific gravity 1.278 kilogram / liter), add 155 milliliters of high alkali sodium metaaluminate solutions (Na 2 O5.226 mol / L, Al 2 o 3 0.529 mol / liter, specific gravity 1.310 kilogram / liter), 28 milliliters of NaOH solution (NaOH 2 (5.306 mol / liter, specific gravity 1.335 kg / liter) and 28 milliliters of water, after stirring uniformly at a speed of 350 rpm, leave it to stand at 10° C. for aging for 18 hours to obtain the directing agent.

[0027] (2) Preparation of X zeolite

[0028] At 5°C, add 374 ml of low-alkali sodium metaaluminate solution (Na 2 O2.581 mol / L, Al 2 o 3 0.9584 mol / L, specific gravity 1.264 kg / L), then add 214 ml of the directing agent prepared in step (1) and 513 ml of water, stir at 350 rpm for 0.5 hour, heat up to 100°C,...

example 2

[0030] Zeolite X was prepared according to the method of Example 1, except that the aging temperature of the directing agent was 5°C for 6 hours, and the low-alkali sodium metaaluminate solution was added to the water glass at 10°C. The performance data of the prepared zeolite are shown in Table 1.

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Abstract

The preparation of small crystal grain X zeolite includes the steps of: mixing siliceous compound, aluminum compound, sodium hydroxide and water and ageing at 0-10 deg.c to prepare guide agent in thecomposition of (11-18)Na2O:Al2O3:(10-17)SiO2:(100-350)H2O; mixing siliceous compound, aluminum compound, water and the guide agent to prepare the mixture of molar composition of (2.5-5)Na2O:Al2O3:(3-5)SiO2:(100-200)H2O; crystallization at 80-120 deg.c for 2-40 hr; water washing, filtering and drying. The X zeolite thus prepared has crystal grain of 0.5-1.0 micron and excellent thermal stability.

Description

technical field [0001] The invention relates to a preparation method of small-grain X-type zeolite. Specifically, it is a method of preparing small crystal X zeolite by the directing agent method. Background technique [0002] In the adsorption process, the active component of the commonly used adsorbent is X zeolite. As in adsorption separation C 8 For aromatic hydrocarbons, the active component of the adsorbent is BaX, KX or KBaX. There are many synthesis methods of X zeolite, one of which is the synthesis method using a directing agent as introduced in USP4,166,099. This method first prepares a Na 2 O-Al 2 o 3 -SiO 2 Then, the mixture is aged at 20-25°C for at least 2 hours to prepare a directing agent, and then the directing agent is mixed with zeolite raw materials, and X zeolite can be obtained after hydrothermal crystallization. However, the crystal grains of zeolite synthesized by this method are relatively large, about 3 microns. The adsorbent prepared from...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C01B39/22
Inventor 郁灼王辉国于永军
Owner CHINA PETROLEUM & CHEM CORP
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