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Method for recovering waste iron-molybdenum catalyst for preparing formaldehyde through methanol oxidation

A technology for recycling methanol and catalysts, which is applied in the field of recycling waste catalysts for the oxidation of iron-molybdenum-based methanol to formaldehyde, which can solve the problems of high cost and difficulty, and achieve the effects of convenient operation, high recovery rate and simple process

Pending Publication Date: 2020-06-19
大连瑞克科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods all adopt the oxidation method to ensure the fixed ion form of molybdenum, and when recycling in the workshop, the cost is high and the difficulty is relatively large

Method used

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  • Method for recovering waste iron-molybdenum catalyst for preparing formaldehyde through methanol oxidation
  • Method for recovering waste iron-molybdenum catalyst for preparing formaldehyde through methanol oxidation
  • Method for recovering waste iron-molybdenum catalyst for preparing formaldehyde through methanol oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The spent catalyst was separated by centrifugation, sieved, and calcined at 500°C for four hours, and sampled and analyzed the composition of the catalyst by XRF. Then take 100g of the catalyst after removal of impurities, pulverize and grind it, add 610.76g of 5.03wt% ammonia water into a closed reactor, stir at 103℃ for 10h, filter, and wash the filter cake with 60℃ ammoniated water (pH=9.0). , 300ml each time, wash three times. The filter cake was washed with pure water at 60℃ for the last time. The pH of the fourth washing liquid was 7.73 / 50℃, and the conductivity was 1.9 ms / cm. It was tested that there was no Mo in the fourth washing liquid. 6+ . Collect the filtrate and the first three washing liquids, heat up to 85℃ and steam ammonia for 3.5h under medium-speed stirring, and steam to pH=5.91 / 80℃ to stop the ammonia distillation, and prepare the ammonia solution to Mo 6+ A solution with a concentration of 0.25 mol / L.

[0042] To Fe(OH) 3 Add 49% HNO 3 Make the mixed...

Embodiment 2

[0045] The iron salt and molybdenum salt solutions obtained in Example 1 were co-precipitated at a certain temperature, aged, dried, shaped, and roasted at a high temperature to obtain a methanol oxidation to formaldehyde catalyst product. The recovered catalyst is comparable to the existing industrial methanol oxidation to formaldehyde catalyst in terms of crystal form, component content and performance evaluation results. The analysis and evaluation results are as follows:

[0046] Recovery preparation catalyst

[0047]

[0048] The catalytic performance evaluation conditions and results of the catalyst are as follows

[0049] Evaluation conditions:

[0050] Catalyst filling: 20-40 mesh, filling volume 3ml, sv=24000h -1 , Reaction pressure=0.075Mpa, reaction gas 15% O 2 , The rest N 2 , Methanol feed concentration (mol) 6.5%

[0051] Evaluation results

[0052]

[0053] Note: The above are the laboratory evaluation data for the recovery and preparation of catalysts and industrial cat...

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Abstract

The invention discloses a method for recovering a waste iron-molybdenum catalyst for preparing formaldehyde through methanol oxidation, and belongs to the technical field of catalysts. The method comprises the following steps: crushing an iron-molybdenum formaldehyde waste catalyst, soaking in ammonia water, heating to dissolve molybdenum, forming iron hydroxide precipitate from iron, filtering, separating, and carrying out ammonia distillation treatment on the obtained ammonium molybdate solution to obtain the raw material of the new catalyst; and adding nitric acid to dissolve the iron hydroxide precipitate left after filtering, and filtering to remove impurities to obtain a pure ferric nitrate solution. According to the invention, in the preparation process of the iron-molybdenum formaldehyde catalyst, magnesium stearate is often added as a lubricant during tabletting and forming, and if the catalyst contains magnesium stearate, the pH value is adjusted to precipitate iron ions andenable magnesium ions to be in a free state, the magnesium ions are removed through filtering and washing, and the iron hydroxide precipitate is dissolved with an acid to obtain a magnesium-free ferric nitrate solution capable of being directly used; and the recovery method is high in Fe and Mo recovery rate, simple in process, convenient to operate and low in recycling cost, ad can be used for recovering various iron-molybdenum formaldehyde waste catalysts and other MoO3 / Fe2(MoO4) 3 series non-formaldehyde catalysts.

Description

Technical field [0001] The invention belongs to the field of organic chemical catalysts, and in particular relates to a method for recovering waste catalysts from iron-molybdenum methanol oxidation to formaldehyde. Background technique [0002] Formaldehyde is an important basic organic chemical raw material, widely used in the chemical, pharmaceutical, textile, wood processing and petroleum industries. Modern industrial formaldehyde production mainly adopts methanol oxidation method. The iron-molybdenum formaldehyde catalyst has been widely used due to its advantages in performance. As the demand for formaldehyde increases, a large amount of waste iron-molybdenum formaldehyde catalyst is bound to be produced. The metallic molybdenum is an important component of the catalyst, and because it is a transition metal, the price is relatively high, so whether it is considered from the perspective of environmental protection or the perspective of catalyst manufacturing cost, it is an ...

Claims

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Application Information

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IPC IPC(8): B01J38/02B01J38/60B01J38/66B01J38/68B01J23/881
CPCB01J38/66B01J38/02B01J38/60B01J38/68B01J23/881
Inventor 周焕文曲俊嬴邓少亮乔川
Owner 大连瑞克科技股份有限公司
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