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Method for milling of catalyst for preparation of acrylic acid by reactive ball mill

A catalyst and acrylic acid technology, applied in chemical instruments and methods, carboxylate preparation, organic compound preparation, etc., can solve the problems of low selectivity, low activity, etc., and achieve the effect of high acrylic acid selectivity and high propane conversion rate

Inactive Publication Date: 2016-04-20
QINGDAO SEIICHI INTPROP SERVICE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the problem of low activity and low selectivity of 4-component catalysts for the production of acrylic acid, the present inventors attempted to remove impurities inevitably generated during catalyst synthesis or calcination to improve catalytic activity, and as a result, the present inventors accomplished the present invention

Method used

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  • Method for milling of catalyst for preparation of acrylic acid by reactive ball mill

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1 g of the catalyst prepared in Comparative Example 1 was loaded into a 60 ml container, and 15 zirconia balls with a diameter of 10 mm and 80 zirconia balls with a diameter of 5 mm were added thereto. 15 ml of water was added thereto, followed by ball milling at 150 rpm for 15 hours.

[0032] After ball milling, the catalyst and solvent are recovered. 30 cc of solvent was added thereto, followed by centrifugation at 4000 rpm for 2 hours. To detect whether impurities are leached from the catalyst, recover and observe the centrifuged solution. It was tan in color, indicating that impurities were leached. The catalyst precipitated at the bottom of the bottle was recovered, dried at 80 °C for 4 h, and then ground in agate to obtain the final catalyst.

Embodiment 2

[0034] 1 g of the catalyst prepared in Comparative Example 1 was loaded into a 60 ml container, and 15 zirconia balls with a diameter of 10 mm and 80 zirconia balls with a diameter of 5 mm were added thereto. 15 ml of ethanol was added thereto, followed by ball milling at 150 rpm for 15 hours.

[0035]After ball milling, the catalyst and solvent are recovered. 30 cc of solvent was added thereto, followed by centrifugation at 4000 rpm for 2 hours. To detect whether impurities are leached from the catalyst, recover and observe the centrifuged solution. It was tan in color, indicating that impurities were leached. The catalyst precipitated at the bottom of the bottle was recovered, dried at 80 °C for 4 h, and then ground in agate to obtain the final catalyst.

Embodiment 3

[0037] 1 g of the catalyst prepared in Comparative Example 1 was loaded into a 60 ml container, and 15 zirconia balls with a diameter of 10 mm and 80 zirconia balls with a diameter of 5 mm were added thereto. 15 ml of 1-propanol was added thereto, followed by ball milling at 150 rpm for 15 hours.

[0038] After ball milling, the catalyst and solvent are recovered. 30 cc of solvent was added thereto, followed by centrifugation at 4000 rpm for 2 hours. To detect whether impurities are leached from the catalyst, recover and observe the centrifuged solution. It was tan in color, indicating that impurities were leached. The catalyst precipitated at the bottom of the bottle was recovered, dried at 80 °C for 4 h, and then ground in agate to obtain the final catalyst.

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Abstract

The invention provides a preparation method of an oxide catalyst for preparation of acrylic acid. The method comprises the steps of: employing a solution mixture containing a molybdenum salt, a vanadium salt, a tellurium salt and a niobium salt to prepare a catalyst precursor, and then drying and calcining the catalyst precursor. The method provided by the invention is characterized by ball milling of a prepared catalyst in the presence of a polar solvent so as to remove impurities. Therefore, the method provided by the invention can be used for preparation of the oxide catalyst that has excellent catalytic activity and can be applicable to preparation of acrylic acid.

Description

technical field [0001] The present invention relates to a method for preparing an oxide catalyst for acrylic acid, more specifically, relates to a method for preparing an oxide catalyst for acrylic acid, which is characterized in that, in the presence of a polar solvent, ball milling The catalyst was prepared to remove impurities to produce acrylic acid with higher activity than acrylic acid prepared by conventional methods. Background technique [0002] For the production of acrylic acid by direct oxidation of propane, extensive research has been conducted on 4-component composite oxide catalysts such as MoVTeNbO. US Patent No. 5,380,933 reported the synthesis of acrylic acid with a high selectivity of 60.5% using a MoVTeNbO type 4-component catalyst. Since then, attempts have been made to increase the catalytic activity or to modify the synthesis of the catalyst by adding additional components to the basic 4 components. However, synthetic methods using co-catalysts or al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/051C07C57/05C07C51/215
Inventor 徐聪
Owner QINGDAO SEIICHI INTPROP SERVICE CO LTD
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