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High-strength composite zeolite deioidining adsorbent and its preparing method

A composite zeolite and adsorbent technology, applied in chemical instruments and methods, other chemical processes, separation/purification of carboxylic acid compounds, etc., can solve the problems of low particle strength, reduced service life, easy crushing and pulverization, and achieve high Effect of deiodination efficiency and long service life

Inactive Publication Date: 2007-07-25
FUDAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these two kinds of deiodination adsorbents with high silver loading have good deiodination effect and long life expectancy in actual use, they are easy to break and pulverize when used in acetic acid for a long time because of their low particle strength after molding, reducing the its actual service life

Method used

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  • High-strength composite zeolite deioidining adsorbent and its preparing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] STI mineral raw powder is subjected to cation exchange according to the following steps to make H-STI zeolite:

[0026] 1. Add the original STI powder to 1.0mol / L ammonium chloride solution, the solid-to-liquid ratio is 1:10, heat to 95-103°C and reflux for 2 hours, exchange four times, wash and dry with water.

[0027] 2. The ammonium chloride-exchanged STI powder is roasted at 500°C for 3 hours to convert it into a hydrogen-type zeolite.

[0028] 3. Add the calcined hydrogen-type zeolite to 0.5mol / L acetic acid with a solid-to-liquid ratio of 1:10, heat to 95-100°C for 2 hours, wash and dry to obtain H-STI powder.

Embodiment 2

[0030] H-STI powder and H-ZSM-5 powder are mixed in a ratio of 70 / 30, and then mixed with binder silica sol (SiO 2 Content 25wt%) mixes, makes the bead of diameter 2 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.

[0031] The X-ray diffraction pattern of this bead is shown in accompanying drawing 1. Its main feature is that the ratio of the total net intensity / total diffraction intensity reflecting the relative content of its crystalline substances is 0.28. The pellets had an average crush strength of 18 Newtons / pellet.

Embodiment 3

[0033] The pellets prepared in Example 2 were heated in a closed stainless steel reactor for hydrothermal strengthening treatment at a temperature of 180 degrees for 24 hours. After the treatment, pellets of the composite substrate adsorbent are obtained, and the X-ray diffraction pattern thereof is shown in accompanying drawing 2. The ratio of total net intensity / total diffraction intensity reflecting the relative content of its crystalline substances is 0.38. Its main characteristic diffraction peak d=10.9~11.3(vs); 9.6~10.0(vs); .9.0~9.2(vs); 8.7~8.9(ms); 7.8~8.1(ms); 4.4~4.7(ms); 4.2~4.3(ms); 3.9~4.1(vs); 3.7~3.9(vs); 3.6~3.8(ms); 3.2~3.4(vs); 3.0~3.1(ms). Comparing the accompanying drawings 1 and 2, it can be seen that after the hydrothermal strengthening treatment, the total relative content of zeolite in the pellets has increased by 36%. The average crushing strength of the pellets after the strengthening treatment has increased by 2.2 times compared with that before t...

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Abstract

The invention is a kind of high intensity compound zeolite deiodination sorbent and preparation method. The sorbent is prepared from a kind of natural mineral zeolite - stilbite (its Chinese code name is CXN, its English code name is STI, and its scientific name is stilbite); through positive ion exchange produce H-STI, mix with artificial compounded commodity H-ZSM-5 zeolite, add cementing agent to molding, after strengthening process, then through silver carrying to produce. The small ball of the sorbent of 1 mm diameter can get 40 Newton per grain. The sorbent can effectively eliminate the organic iodide, inorganic iodide and idodine molecule in the car-bonyl compounded products.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a composite deiodination adsorbent 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 acetic acid and ethyle...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/18C07C51/47C07C45/79
Inventor 龙英才张玲妹夏晓慧高蕾孙飞曹智龙李彩云
Owner FUDAN UNIV
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