High silver supported zeolite molecular sieve acetate deiodinase adsorber and preparation method thereof

A zeolite molecular sieve and adsorbent technology, applied in the field of deiodination zeolite molecular sieve adsorbent and its preparation, can solve the problems of violent molecular movement, poor deiodination effect, loss, etc., and achieve high crystallization degree, high particle strength, and silver loading capacity high effect

Active Publication Date: 2010-09-15
FUDAN UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] However, due to the single pore structure of the zeolite used in the above-mentioned silver-loaded molecular sieve deiodination adsorbent, the iodide removal effect of the molecular size in the acetic acid is different, and the composition is complex.
The reason is that the intracrystalline pore diffusion resistance of large-pore zeolite is small, which is conducive to the removal of large-sized organic iodine molecules through physical adsorption, but for small-sized inorganic molecular iodine and elemental iodine, the molecular motion is violent, and the macropores Decreased adsorption capacity of zeolite
In medium pore zeolites, the organic iodide with larger molecul

Method used

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  • High silver supported zeolite molecular sieve acetate deiodinase adsorber and preparation method thereof
  • High silver supported zeolite molecular sieve acetate deiodinase adsorber and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Commercially available zeolite mineral raw powder is subjected to cation exchange according to the following steps to make H-STI zeolite:

[0030] 1. Add BEA raw powder to 1.5mol / l ammonium chloride solution, the solid-to-liquid ratio is 1:8, heat to 95-105°C and reflux for 4 hours, exchange three times, wash and dry with water.

[0031]2. The BEA powder exchanged with ammonium chloride was roasted at 550° C. for 5 hours to transform into hydrogen zeolite.

[0032] 3. Add the roasted hydrogen-type zeolite to 1 mol / l acetic acid, the solid-to-liquid ratio is 1:6, heat to 90-95°C and reflux for 4 hours, wash and dry to obtain H-BEA for the preparation of deiodination adsorbent pink.

Embodiment 2

[0034] H-BEA powder and binder silica sol (SiO 2 Content 20wt%) mix, make the bead of diameter 1 millimeter in the rolling ball machine. The amount of zeolite in the pellets and the SiO in the binder 2 The mass ratio is 80 / 20. X-ray powder diffraction showed a relative crystallinity of 80%. The pellets are heated in a closed stainless steel reactor for hydrothermal strengthening treatment at a temperature of 180 degrees for 24 hours. After the treatment, the pellets of the substrate adsorbent were obtained, the relative crystallinity increased to 105%, the strength reached 30 Newton / particle, and the specific surface area was 415m 2 / g.

Embodiment 3

[0036] H-BEA powder and binder silica (SiO 2 Content 25wt%) mix, make the bead of diameter 1.5 millimeters in the rolling ball machine. The amount of zeolite in the pellets and the SiO in the binder 2 The mass ratio is 75 / 25. X-ray powder diffraction showed a relative crystallinity of 78%. The pellets are heated in a closed stainless steel reactor for hydrothermal strengthening treatment at a temperature of 160 degrees for 20 hours. After the treatment, the pellets of the base adsorbent were obtained, the relative crystallinity increased to 103%, the strength reached 28 Newton / particle, and the specific surface area was 410m 2 / g.

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Abstract

The invention belongs to the chemical technical field and relates to a high silver supported zeolite molecular sieve acetate deiodinase adsorber and a preparation method thereof. In the adsorber, the sizes of zeolite cavity openings are respectively 0.66*0.71 nanometers and 0.56*0.56 nanometers, and the adsorber is provided with characteristic X-ray diffraction lines in a BEA (Background Equivalent Activity) type zeolite structure. The deiodinase adsorber is prepared by the steps that saled sodium type zeolite molecular sieve powder with two-dimensional twelve oygen membered ring cavity openings is formed through binder, is in in-situ hydrothermal strengthening treatment to generate chemical bonds and then is treated by ion exchange sodium removal and silver carrying. The adsorber has the advantages of high crystallization degree, strong particle strength, high silver supported and strong adsorption capacity to organic iodide, inorganic iodide and molecular iodide with different sizes contained in strong acidic medium, can enable the total iodide content in product acetic acid after deiodination treatment by the adsorber to be lower than 5ppb and is suitable for being used as raw materials for synthetizing vinyl acetate.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a deiodinated zeolite molecular sieve adsorbent used for removing iodide in the carbonylation synthesis of carboxylic acid or carboxylic anhydride product process and a preparation method thereof. Background technique [0002] In the process of carbonylation of carboxylic acid or carboxylic anhydride, iodide or its derivatives are unavoidably present in the produced carboxylic acid or carboxylic anhydride due to the use of iodide as a catalytic promoter. After traditional distillation, rectification or treatment with certain chemicals, there will still be traces of iodide (derivatives) that are difficult to remove. Its existence limits the application of the products produced by this method. In particular, it cannot be used in the production process using iodine-sensitive metals as catalysts. For example, in the process of producing vinyl acetate from acet...

Claims

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Application Information

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IPC IPC(8): B01J20/18B01J20/30
Inventor 龙英才汪靖程晓维沈杰沈浩然
Owner FUDAN UNIV
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