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Preparation method of catalyst for alkane oxidation

A technology of oxygen catalyst and catalyst, which is applied in the direction of catalyst activation/preparation, preparation of organic compounds, physical/chemical process catalysts, etc. It can solve the problems of unfavorable large-scale production, high production cost, complicated methods, etc., and achieve selectivity and easy control , low production cost, good selectivity

Active Publication Date: 2014-07-16
大连进化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In recent years, phosphorus vanadium series catalyst development is more, but all synthesis is more difficult, as: the catalyst preparation method of the fluidized-bed method n-butane oxidation of maleic anhydride of invention such as CN1059297A Tianjin University Xu Genhui and CN1090224A Montecatini company consultant In the n-butane oxidative maleic anhydride catalyst invented by Min et al., mixture alcohols such as butanol and benzyl alcohol are used to reduce the valence state of vanadium in the catalyst precursor containing phosphorus and vanadium, which makes it difficult to separate a large amount of aldehyde contained in the mixed alcohol, and the production cost is relatively high. high
The synthesis method and product separation method of the products in the above processes are either too complicated, or the reagents used are toxic, costly, or have problems such as large energy consumption and serious environmental pollution, which are not conducive to large-scale production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: synthesize catalyst by the inventive method

[0021] 1. Use a 3000-liter 316L stainless steel reactor, put 1500 kg of water into the reactor, and add 150 kg of ammonium vanadate. Stir and heat up to 100°C, the water boils and refluxes, and slowly add 200 kg of phosphoric acid with a concentration of 75%. The feed rate is controlled by moderate reflux of water. After the addition of phosphoric acid, continue to react for at least 4 hours under the condition of water reflux, cool down to normal temperature, centrifugally filter, and dry the filter cake at 80-100°C to obtain 300 kg of ammonium phosphovanadium powder.

[0022] 2. Configure 10% ammonium molybdate aqueous solution, put 1800 kg of water and 200 kg of ammonium molybdate into a 3000 liter enamel reaction kettle. Stir at room temperature for 1 hour, and put into buckets for later use.

[0023] 3. Weigh 300 kg of ammonium vanadium phosphate powder and add it to the silo with solid material auger s...

Embodiment 2

[0028] Synthesis of acetic acid prepared by oxidation of ethane with the catalyst of the invention.

[0029] Take 400 grams of catalyst and fill it into a single-tube reactor with molten salt control, and the catalyst layer is about 5 meters high. The air feed was 20 liters per minute and the ethane feed was 300 ml per minute. When the molten salt temperature is controlled at 390°C, the reaction bed temperature is at 445°C. Product water absorbs. The product gas chromatographic analysis shows that the acetic acid content is more than 95%, and the product contains about 3% acetaldehyde.

[0030] time Middle temperature control / ℃ Hot spot temperature / ℃ Air flowL / min Ethane flow mL / min Ethane inlet volume concentration Ethane outlet volume concentration Conversion rate CO% CO2% selectivity 9:30 412 285.6 20.0 300 1.646% 10:10 410 461.5 20.0 300 1.652% 0.38...

Embodiment 3

[0032] Synthesis of acrylic acid prepared by oxidation of propane with the catalyst of the present invention.

[0033] Take 400 grams of catalyst and fill it into a single-tube reactor with molten salt control, and the catalyst layer is about 5 meters high. The air feed was 20 liters per minute and the ethane feed was 300 ml per minute. When the molten salt temperature is controlled at 380°C, the reaction bed temperature is at 440°C. Product water absorbs. The content of acrylic acid in the product reaches 90%, the content of acetic acid is about 10%, and the content of propionic acid is about 8%.

[0034] time Middle temperature control / ℃ Hot spot temperature / ℃ Air flowL / min Propane flow mL / min Propane inlet volume concentration Propane outlet volume concentration Conversion rate CO% CO2% selectivity 9:30 407 285.6 20.0 300 1.851% 10:00 401 449.7 20.0 300 ...

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PUM

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Abstract

The invention discloses a catalyst for alkane oxidation, wherein the phosphorus-vanadium atom ratio is 1: (0.9-1.0), the phosphorus-molybdenum atom ratio is 1: (0.001-0.1), the phosphorus-aluminum atom ratio is 1: (0.9-1.1), and the phosphorus-oxygen atom ratio is 1: (7-10). A preparation method of the catalyst comprises the following steps: synthetizing a phosphorus-vanadium-oxygen precursor, synthetizing immobilized ammonium molybdate, synthetizing the catalyst, and activating the catalyst. The catalyst is used for preparing acetic acid through ethane oxidation, preparing crylic acid through dimethylmethane oxidation, and preparing fumaric acid and / or cis-butenedioic anhydride through butane oxidation. The preparation method has the advantages of simple technology, low production cost, nontoxicity, and low energy consumption and environment friendless during the production process.

Description

technical field [0001] The present invention relates to a catalyst preparation method, especially a catalyst preparation method that can be used for the oxidation of alkane, more specifically, it can be used for the oxidation of ethane, propane and butane to prepare acetic acid, acrylic acid, fumaric acid, maleic anhydride, etc. Catalyst preparation method. It belongs to the field of chemical product synthesis. Background technique [0002] As we all know, a large amount of low-carbon alkanes are produced in petroleum refining, most of which are used as fuel, and the waste of resources is serious. There are not many comprehensive utilization methods, and the catalyst life is short. Acetic acid and acrylic acid are industrial bulk raw materials, and maleic anhydride is an important raw material for preparing polyester, etc., with high economic value. [0003] In recent years, phosphorus vanadium series catalyst development is more, but all synthesis is more difficult, as: ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/199B01J37/16C07C51/215C07C53/08C07C57/05C07C57/03
Inventor 高丽娜
Owner 大连进化科技有限公司
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