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Fe molecular sieve catalyst for purifying NOx in acrylonitrile oxidization tail gas and preparation method of Fe molecular sieve catalyst

A molecular sieve and catalyst technology, which is applied in the field of catalytic purification of tail gas of acrylonitrile plant, achieves the effects of simple preparation process, good repeatability and excellent NOx conversion performance

Inactive Publication Date: 2012-06-27
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the denitrification technology aimed at the control of acrylonitrile tail gas emission in my country has just started, and the current tail gas purification method is only aimed at the oxidation process of acrylonitrile tail gas (such as patents CN101716462A, CN101138699, CN200810200595.X and CN1903415), and does not involve the tail gas after oxidation of acrylonitrile Selective reduction of medium NOx under oxygen-enriched conditions
In addition, although there are about Fe-zeolite NH 3 -Patent reports on the preparation of SCR catalysts (patents CN 200910024336.0 and CN200910090322.9), but this type of catalyst system has not been applied to the field of tail gas NO removal after catalytic oxidation of acrylonitrile for industrialization

Method used

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  • Fe molecular sieve catalyst for purifying NOx in acrylonitrile oxidization tail gas and preparation method of Fe molecular sieve catalyst
  • Fe molecular sieve catalyst for purifying NOx in acrylonitrile oxidization tail gas and preparation method of Fe molecular sieve catalyst
  • Fe molecular sieve catalyst for purifying NOx in acrylonitrile oxidization tail gas and preparation method of Fe molecular sieve catalyst

Examples

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Effect test

Embodiment 1

[0020] Commercial 10g sodium molecular sieve Na-β molecular sieve powder (Zibo Qichuang Chemical Technology Development Co., Ltd.) and 100mL27% NH 4 NO 3 The solution was uniformly mixed, ion-exchanged at 80°C for 4 hours, filtered and washed, dried at 120°C for 12 hours, and calcined at 550°C for 4 hours to obtain hydrogen molecular sieve H-β. 10g H-β with 150mL 0.1M FeCl 3 The solutions were mixed, exchanged for metal ions at 70°C for 8h, filtered and washed, and dried at 120°C for 8h. The dried sample was calcined at 550° C. for 4 hours at a heating rate of 10° C. / min to obtain the Fe-β catalyst sample by the exchange method of Example 1. Its Fe content is 0.8-1% as tested by ICP. The obtained catalyst Fe-β0.5g contains 5% O at 500°C 2 Pre-oxidize in a nitrogen atmosphere for 30 minutes, after cooling down to room temperature, the temperature is programmed at a rate of 10°C / min, and a mixed atmosphere with a total flow rate of 1L / min is introduced, which contains 500ppm...

Embodiment 2

[0022] Commercial 10g sodium molecular sieve Na-β molecular sieve raw powder (Zibo Qichuang Chemical Technology Development Co., Ltd.) and 100mL 27% NH 4 NO 3 The solution was uniformly mixed, ion-exchanged at 80°C for 4 hours, filtered and washed, dried at 120°C for 12 hours, and calcined at 550°C for 4 hours to obtain hydrogen molecular sieve H-β. Then test its water absorption: add water dropwise to a constant mass molecular sieve, grind and stir continuously, dropwise add until obvious liquid appears on the surface of the powder, absorb the excess water with filter paper, and weigh it. Calculate the drop solution volume according to the saturated water absorption rate, add 300mL 0.05M FeCl dropwise to 10g H-β molecular sieve 3 The solution was ground for 30 minutes, aged for 4 hours at room temperature and then dried at 150°C for 4 hours. The dried sample was calcined at 550° C. for 4 hours at a heating rate of 10° C. / min to obtain the impregnated Fe-β catalyst sample of...

Embodiment 3

[0024] Commercial 10g sodium molecular sieve Na-ZSM5 molecular sieve raw powder (Shanghai Zhuoyue Chemical Industry) and 100mL 27% NH 4 NO 3 Mix the solution evenly, ion exchange at 80°C for 4h, filter and wash, dry at 120°C for 12h, and roast at 550°C for 4h to obtain hydrogen molecular sieve H-ZSM5. 10g H-ZSM5 and 200mL of 0.1M FeCl 3 The solutions were mixed, exchanged for metal ions at 70°C for 8h, filtered and washed, and dried at 120°C for 8h. The dried sample was calcined at 550° C. for 4 hours at a heating rate of 10° C. / min to obtain the Fe-ZSM5 catalyst sample by the exchange method in Example 3. Its Fe content is 1-1.2% as tested by ICP. The prepared catalyst Fe-ZSM50.5g contains 5%O at 500°C 2 Pre-oxidize in a nitrogen atmosphere for 30 minutes, after cooling down to room temperature, the temperature is programmed at a rate of 10°C / min, and a mixed atmosphere with a total flow rate of 1L / min is introduced, which contains 500ppm NO, 500ppm NH 3 , 5%O 2 , to det...

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Abstract

The invention relates to a Fe molecular sieve SCR (Selective Catalytic Reduction) catalyst for purifying NOx in acrylonitrile oxidization tail gas and a preparation method of the Fe molecular sieve SCR catalyst. A commercial ZSM-5 molecular sieve, a Y type molecular sieve, ferrierite or a beta molecular sieve is used as a carrier, 0.3-10.0 percent by mass of Fe<3+> is introduced to be used as an active component by adopting an immersion method or ion exchange method, and 0.5-8.0 percent by mass of M (lanthanum La or cobalt Co) is introduced to be used as a modification component. The SCR catalyst prepared by adopting the preparation method furthest realizes NO transformation and efficient catalysis removal of the NOx in the acrylonitrile oxidization tail gas under an oxygen enrichment condition. The preparation method provided by the invention has the advantages of simple process and good repeatability, and is beneficial to industrialized production.

Description

technical field [0001] The invention belongs to the field of catalytic purification of tail gas of an acrylonitrile device, and in particular relates to an Fe-molecular sieve catalyst and a preparation method for purifying tail gas rich in nitrogen oxides (NOx) after oxidation of acrylonitrile. This method is aimed at the application requirements of high-efficiency selective catalytic reduction of NOx-containing tail gas after oxidation treatment of acrylonitrile absorption tower, and lists the preparation method of Fe-molecular sieve ammonia selective catalytic reduction (SCR) catalyst in detail, so as to realize Efficient catalytic removal of NOx under oxygen-enriched conditions. Background technique [0002] As an important chemical intermediate, acrylonitrile is widely used in the production of three major synthetic materials: fiber, rubber and plastic. At present, more than 95% of the devices in the world use propylene ammoxidation technology (also known as the sohio m...

Claims

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Application Information

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IPC IPC(8): B01J29/46B01J29/14B01J29/68B01J29/76B01D53/86B01D53/56
Inventor 沈美庆王军
Owner TIANJIN UNIV
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