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Zeolite deiodination adsorbent with high silver carrying amount and its prepn process

An adsorbent, zeolite technology, applied in chemical instruments and methods, other chemical processes, silicates, etc., can solve the problems of reduced total iodine content, no description, and high price, and achieves simple methods, mild preparation conditions, and reduced costs. Effect

Inactive Publication Date: 2005-06-22
FUDAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] All of these patents use synthetic zeolite molecular sieves, the price is relatively high, and there is no description of the level that can reduce the total iodine content in acetic acid

Method used

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  • Zeolite deiodination adsorbent with high silver carrying amount and its prepn process
  • Zeolite deiodination adsorbent with high silver carrying amount and its prepn process
  • Zeolite deiodination adsorbent with high silver carrying amount and its prepn process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] STI mineral raw powder is exchanged and modified according to the following steps:

[0043] 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.

[0044] 2. The ammonium chloride-exchanged STI powder is roasted at 500°C for 3 hours to convert it into a hydrogen-type zeolite.

[0045] 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 and reflux for 2 hours, wash and dry with water. Obtain H-STI-I samples.

[0046] STI zeolite was exchanged with ammonium chloride, calcined at 500°C for 3 hours, and then treated with acetic acid, its structure remained stable. XRD spectrum see figure 2 (Online is before processing).

Embodiment 2

[0048] STI raw powder is modified according to the following steps

[0049] 1. Add STI raw powder into 1.5mol / L ammonium nitrate solution, the solid-to-liquid ratio is 1:15, heat to 105-115°C and reflux for 5 hours, exchange four times, wash and dry.

[0050] 2. Add the ammonium-exchanged STI to 1.0mol / L acetic acid, the solid-to-liquid ratio is 1:10, heat to 80-90°C and reflux for 1 hour, exchange twice, wash and dry with water. That is, H-STI-II was obtained.

[0051] Apparently after being treated with ammonium nitrate and then treated with acetic acid, the obtained H-STI-II still has high crystallinity and structural stability. The powder XRD spectrum of H-STI-II calcined at different temperatures is shown in image 3 . From top to bottom are the sample powder XRD spectra of uncalcined H-STI-II, calcined at 300°C for 4 hours, and calcined at 500°C for 1.0 hour.

Embodiment 3

[0053] H-STI-I powder uses 0.05 mol / l silver nitrate as the exchange liquid, liquid / solid = 15 / 1, carries out silver ion exchange under the condition of stirring at room temperature for 12 hours. After the sample was filtered, washed, and dried, it was analyzed by EDX to have a silver content of 5.6%. The powder XRD spectrum of the obtained Ag-STI is shown in Figure 4 .

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Abstract

The invention relates to a high-silver-loaded zeolite adsorbent for removing iodide in acetic acid and a preparation method thereof. The prior art has high cost, high price and complicated production operation process. The adsorbent of the present invention is made of a natural mineral zeolite-stilbite (Chinese code name CXN, English code STI, scientific name stilbite), which is made through modification and cation exchange. After silver ion exchange, its maximum silver loading can reach 26%. The adsorbent can effectively remove organic iodide, inorganic iodide and molecular iodine in acetic acid.

Description

technical field [0001] The invention relates to a zeolite deiodination adsorbent with high silver loading and a preparation method thereof. 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 production...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/16B01J20/30C07C51/47
Inventor 龙英才张玲妹杨波夏晓慧周伟正曹智龙李彩云
Owner FUDAN UNIV
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