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Preparation method of high silver carrying ZSM-5 zeolite deiodine adsorbing agent

A technology of ZSM-5 and adsorbent, which is applied in the field of effective deiodination adsorbent, can solve problems such as hindering the diffusion of silver ions and affecting the silver loading amount of deiodination adsorbent, and achieves the effect of simple operation and low cost

Inactive Publication Date: 2004-03-03
SHANGHAI WUJING CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the SiO of the ZSM-5 zeolite raw material used 2 / Al 2 o 3 Too high, plus the binder blocks the opening of the pore on the surface of the zeolite, hinders the diffusion of silver ions, and also seriously affects the silver loading of the deiodination adsorbent.

Method used

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  • Preparation method of high silver carrying ZSM-5 zeolite deiodine adsorbing agent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] SiO 2 / Al 2 o 3 75g of H-ZSM-5 zeolite powder of ≈26 and 25g of white carbon black are kneaded and dried, then added to a 30% aluminum nitrate solution, soaked for 2 hours, dried, and then sealed in 10% tetrapropylammonium hydroxide solution, after 1.5 days of hydrothermal treatment at 180°C, it was calcined at 600°C for 5 hours. It was determined that its SiO 2 / Al 2 o 3 ≈28, crystallinity>92%, n-hexane adsorption>113mg / g, XRD spectra of samples before and after hydrothermal reaction are shown in Figure 1 (the upper line is after crystal transformation).

Embodiment 2

[0030] SiO 2 / Al 2 o 3 ≈14 85g of H-ZSM-5 zeolite powder with 15g of SiO 2 / Al 2 o 3 ≈14 amorphous silica-alumina adhesive is mixed and dried, then sealed in a sealed reaction kettle filled with 5% ethylamine aqueous solution, heat-treated with ethylamine / water mixed steam at 200°C for 4 days, and then baked at 500°C for 6 hours . It was determined that its SiO 2 / Al 2 o 3 =15, crystallinity>90%, n-hexane adsorption>110mg / g.

Embodiment 3

[0032] The sample that embodiment 1 makes carries out silver ion exchange with 0.05mol / L silver nitrate in ion exchange column, liquid / solid=30 / 1, space velocity 0.5hr -1 , temperature 95 ° C, prepared Ag-ZSM-5 deiodination adsorbent. After washing and drying, the silver content was analyzed by EDX to be 16.0%.

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Abstract

A process for preparing the ZSM-5 zeolite adsorbing containing more carried silver (20%) for removing iodide from acetic acid includes such steps as pulverizing H-ZSM-5 zeolite with the ratio of SiO2 / Al2O3=15-30, adhering for shaping, crystallizing, and silver ion exchange.

Description

technical field [0001] The invention relates to a method for using ZSM-5 zeolite with high silver loading as an effective deiodination adsorbent. Background technique [0002] As an important industrial raw material, acetic acid has a wide range of applications. At present, more than 90% of the products are produced by methanol low pressure oxo synthesis. Since iodide is used as a catalyst promoter in this process, iodide or its derivatives inevitably exist in the final product. Although most iodides can be removed by conventional distillation, rectification or treatment with certain chemicals, trace amounts of iodides (derivatives) will remain in the product. These traces of iodides are difficult to remove by traditional methods, and the existence of these traces of iodides has limited the application of the acetic acid produced by this method. In particular, it cannot be used in the production process using iodine-sensitive metals as catalysts. For example, in the prod...

Claims

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Application Information

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IPC IPC(8): B01J20/18B01J20/30
Inventor 龙英才张玲妹周伟正杨波夏晓慧曹智龙李彩云
Owner SHANGHAI WUJING CHEM
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