Synthesis method for ZSM-5 zeolite

A synthesis method, the technology of ZSM-5, is applied in the directions of crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc. Synthesis cost, effect of good reaction performance

Inactive Publication Date: 2007-03-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1082510A and USP5240892 adopted silica-alumina gel as raw material, but silica-alumina gel is prepared from water glass as a raw material, and the process is more complicated; the silicon source adopted in CN1194942A and CN1235875A is solid silica gel, and its price is relatively expensive; CN1194943A The raw material used in the preparation method of ZSM-5 zeolite reported in is the silica-alumina microspheres prepared from NaY mother liquor
Existing metal zirconium refining plants, in the process of extracting zirconium from zirconium ore, in addition to generating the required zirconium compounds, will also produce a large amount of by-products whose main component is silicon dioxide. Finding a suitable use and being treated as waste for a long time will not only cause a waste of resources, but also cause environmental pollution and cause bad social impact

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] This example illustrates the treatment of zirconium refinery silicon by-products used as feedstock for zeolite synthesis.

[0015] The silicon by-product (taken from Jiangxi Jin'an Company) was beaten with 5 times of 60°C water for 10 minutes, filtered, and rinsed with 5 times of room temperature water, and the filter cake was dried at 120°C for 5 hours to obtain the synthetic ZSM- 5 Raw materials used for zeolite. Analysis showed that its SiO 2 The content is 94% by weight.

Embodiment 2

[0018] Dissolve 0.56 g of NaOH in 28 g of deionized water and add 1.34 g of Al with stirring 2 (SO 4 ) 3 18H 2 0 and 1.46 gram n-butylamine, then add the silicon by-product that 11.5 gram embodiment 1 handles, the reaction mixture molar ratio that obtains is: SiO 2 / Al 2 o 3 =100,H 2 O / SiO 2 =7.8, Na 2 O / SiO 2 =0.05, n-butylamine / SiO 2 = 0.1. The mixture was placed in a sealed stainless steel reaction vessel, and crystallized at 170°C for 24 hours. After cooling, the product was filtered, washed and dried. Through XRD detection, the obtained zeolite is ZSM-5, and its relative crystallinity is 84%, and the sample SiO 2 / Al 2 o 3 =80.

Embodiment 3

[0020] Dissolve 1.92 g of NaOH in 28 g of deionized water and add 2.66 g of Al with stirring 2 (SO 4 ) 3 18H 2 O and 1.02 grams of n-butylamine, then add the silicon by-product that 11.5 grams of embodiment 1 handles, the reaction mixture molar ratio that obtains is: SiO 2 / Al 2 o 3 =50,H 2 O / SiO 2 =7.8, Na 2 O / SiO 2 =0.06, n-butylamine / SiO 2 = 0.07. The mixture was placed in a sealed stainless steel reaction vessel, and crystallized at 175°C for 20 hours. After cooling, the product was filtered, washed and dried. Through XRD detection, the obtained zeolite is ZSM-5, and its relative crystallinity is 96%, and the sample SiO 2 / Al 2 o 3 =40.

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Abstract

The invention discloses a synthesizing method of ZSM-5 zeolite, which is characterized by the following: blending silicon source, aluminum source, alkaline, organic molding agent Q and water evenly with molar component of SiO2 / Al2O3 at 20-1000, Na2O / SiO2 at 0.03-0.5,Q / SiO2 at 0.03-0.5,H2O / SiO2 at 5-20; proceeding thermal crystallization for compound. The main component of silicon source is by-product of silica, which is generated in the zirconium extracting course.

Description

technical field [0001] The present invention relates to a method for synthesizing ZSM-5 zeolite, more specifically, relates to a method for synthesizing ZSM-5 zeolite with a by-product mainly composed of silicon dioxide produced in the production process of a metal zirconium refinery Methods. Background technique [0002] Since ZSM-5 zeolite was synthesized by MOBIL company in 1972, it has been widely used in many fields of petrochemical industry, and its preparation technology has also become the focus of research. What the silicon source that is used for synthesizing this zeolite early technology adopts is water glass or silica sol, as the silicon source that adopts in CN1072654A is water glass or silica sol; The silicon source that adopts in USP4061724 is silica sol etc. In the conventional hydrothermal synthesis method using water glass or silica sol as a silicon source, the original feed water silicon is relatively large, and the single-pot yield is low during producti...

Claims

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Application Information

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IPC IPC(8): C01B39/40
Inventor 王殿中舒兴田何鸣元冯强
Owner CHINA PETROLEUM & CHEM CORP
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