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Iron-molybdenum catalyst for preparing formaldehyde through methanol oxidation, preparation and application of iron-molybdenum catalyst

A catalyst, oxidation technology, applied in physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, carbon-based compound preparation, etc., can solve the complicated preparation process, easy deactivation of catalyst, catalyst preparation cost Advanced problems, to achieve the effect of improving mixing uniformity

Active Publication Date: 2021-06-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN108816241 A, CN100413584C, CN108435192 A, US4420421, US 4829042 etc. have carried out the preparation of iron-molybdenum catalyst by co-precipitation method, although can make the iron-molybdenum catalyst that activity is good enough, strength also meets the requirements for methanol oxidation to formaldehyde, but However, there are problems such as high catalyst preparation cost and easy deactivation of the catalyst, which limit its further industrial application.
[0004] To sum up, the existing iron-molybdenum-based catalysts for methanol oxidation to formaldehyde are mostly prepared by coprecipitation method, usually the preparation process is cumbersome, and the mixing uniformity of molybdenum oxide and iron molybdate components is not enough, which leads to the easy deactivation of the catalyst

Method used

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  • Iron-molybdenum catalyst for preparing formaldehyde through methanol oxidation, preparation and application of iron-molybdenum catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] First, 40.0 g of hematite (50% iron oxide mass content) was mechanically pulverized, and then roasted at 500° C. for 12 hours; then ammonium heptamolybdate was added according to the molybdenum-iron atomic ratio of 2.4, solid-state grinding for 8 hours and mixed; Add 500mL of deionized water at 60°C, then slowly add concentrated nitric acid with a mass concentration of 65% under stirring conditions for acidification, adjust the pH value of the system to 1.0, and obtain a mixed slurry of ferric molybdate and orthomolybdic acid; The resulting slurry was aged at 90°C for 12 hours, and finally filtered and separated to obtain a filter cake; the filter cake was dried at 80°C, pulverized, shaped, and roasted at 400°C for 8 hours to obtain an iron-molybdenum catalyst (MoO 3 -Fe 2 (MoO 4 ) 3 ).

Embodiment 2

[0021] Embodiment 2: iron ore kind (magnetite)

[0022] First, 57.9g of magnetite (70% iron carbonate content) was mechanically pulverized, then roasted at 500°C for 12 hours; then ammonium heptamolybdate was added at an atomic ratio of molybdenum to iron of 2.4, solid-state ground for 8 hours and mixed; then Add 500mL of deionized water at 60°C, then slowly add concentrated nitric acid with a mass concentration of 65% under stirring conditions for acidification, adjust the pH value of the system to 1.0, and obtain a mixed slurry of ferric molybdate and orthomolybdic acid The resulting slurry was aged at 90°C for 12h, and finally filtered and separated to obtain a filter cake; the filter cake was dried at 80°C, pulverized, molded, and roasted at 400°C for 8h to obtain an iron-molybdenum catalyst ( MoO 3 -Fe 2 (MoO 4 ) 3 ).

Embodiment 3

[0023] Embodiment 3: iron ore kind (siderite)

[0024] Firstly, after crushing 28.9g of siderite mechanically, it was roasted at 500°C for 12 hours; then ammonium heptamolybdate was added according to the molybdenum-iron atomic ratio of 2.4, solid-state ground for 8 hours and mixed; then 500mL was added at 60°C to remove Ionized water, and then slowly add concentrated nitric acid with a mass concentration of 65% under stirring conditions for acidification treatment, adjust the pH value of the system to 1.0, and obtain a mixed slurry of ferric molybdate and orthomolybdic acid; the obtained slurry is at 90 ° C Aged for 12 hours under high temperature, and finally filtered and separated to obtain a filter cake; the filter cake was dried at 80°C, pulverized, shaped, and roasted at 400°C for 8 hours to obtain an iron-molybdenum catalyst (MoO 3 -Fe 2 (MoO 4 ) 3 ).

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Abstract

The invention relates to a preparation method of an iron-molybdenum catalyst for preparing formaldehyde through methanol oxidation. The preparation method of the iron-molybdenum catalyst comprises the following steps: by taking ammonium molybdate and iron ore as raw materials, firstly, mechanically crushing the iron ore, and then roasting; adding ammonium molybdate into the roasted iron ore according to different molybdenum-iron atomic ratios, and carrying out solid-state grinding and uniform mixing; adding deionized water and inorganic acid at a certain temperature for acidification treatment to obtain mixed slurry of iron molybdate and molybdic acid; carrying out aging treatment on the obtained slurry, and then filtering and separating to obtain a filter cake; and drying, crushing, forming and roasting the filter cake to obtain the iron-molybdenum catalyst for preparing formaldehyde by methanol oxidation. In the preparation process, iron salts such as ferric nitrate and the like are replaced by the iron ore so as to reduce the raw material cost of the iron-molybdenum catalyst, and the mixing uniformity of molybdenum oxide and iron molybdate components is improved on the microscopic scale so as to prolong the service life of the iron-molybdenum catalyst.

Description

technical field [0001] The invention belongs to the field of preparation of novel catalytic materials, and in particular relates to a long-life methanol oxidation to formaldehyde iron-molybdenum catalyst (MoO 3 -Fe 2 (MoO 4 ) 3 ) preparation method. Background technique [0002] As a basic chemical product, formaldehyde has a very wide range of applications. In recent years, my country's methanol production has leapt to the first place in the world. Among the existing domestic formaldehyde production processes, the methanol oxidation process is the main one. According to the type of catalyst used, it is divided into "silver method" and "iron molybdenum method". Compared with the "silver method", the "iron-molybdenum method" production device has the advantages of large single-set production capacity, small methanol unit consumption, and long service life of the catalyst. Therefore, in recent years, most of the new and expanded formaldehyde plants adopt the iron-molybd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/881C07C45/38C07C47/052
CPCB01J23/881C07C45/38C07C47/04
Inventor 王峰李书双张志鑫张健
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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