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Method for preparing maleic anhydride by oxidation of n-butane

A process method, n-butane technology, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve the problems of reducing the effective volume of the reactor, reducing the production efficiency, prolonging the stable period, etc., and achieves a smooth reaction hot spot The sharp rise of , to ensure stability, the effect of small reaction heat release

Active Publication Date: 2017-05-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] USP4,855,459 proposes a method for preparing maleic anhydride by oxidation of n-butane, which is carried out by diluting and packing inert silica-alumina balls and catalysts, and reducing the hot spots of reaction by diluting and packing at the hot spots of the reaction tube. temperature, to improve the selectivity of maleic anhydride, the purpose of increasing the yield of maleic anhydride, and at the same time the stability period of the catalyst has been extended, but the unfavorable factor is the addition of inert materials, which reduces the effective volume of the reactor and also reduces the production efficiency

Method used

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  • Method for preparing maleic anhydride by oxidation of n-butane
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  • Method for preparing maleic anhydride by oxidation of n-butane

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Effect test

preparation example Construction

[0051] (2) Preparation of vanadium phosphorus oxygen catalyst

[0052] The vanadium phosphorus oxide obtained in step (1) is first shaped, and the shape of the obtained vanadium phosphorus oxygen catalyst can be a compressed tablet, a spherical shape, an extruded rod, etc., and the phase of the obtained catalyst precursor is (VOHPO 4 0.5H 2 o).

[0053] (3) Oxidation treatment of vanadium phosphorus oxygen catalyst

[0054] The catalyst particles obtained in step (2) are immersed in an organic solvent containing a certain concentration of organic peroxide, and the average valence state of vanadium in the catalyst is regulated by controlling the concentration of the organic peroxide.

[0055] The mass concentration of organic peroxides is generally controlled at 0.1% to 10%.

[0056] (4) Activation of vanadium phosphorus oxygen catalyst

[0057] After the impregnation in step (3), it is filtered and dried, and the dried catalyst is activated in a nitrogen or inert gas atmos...

Embodiment 1

[0063] exist figure 1Add 649L of isobutanol and benzyl alcohol mixture to the reaction kettle shown with a stirring device and a reflux condensing device, the volume ratio of isobutanol / benzyl alcohol is 10:1, 29.53 kg of vanadium pentoxide, and the auxiliary agent hexahydrate Ferric nitrate 0.3kg, auxiliary agent zirconium nitrate 0.5kg, start stirring, increase the reaction temperature and keep it at 100±2°C, carry out reflux reaction, keep reflux time for 4 hours, then add 34.98kg of phosphoric acid with a concentration of 100%, phosphorus / vanadium The molar ratio was 1.1, the reflux was continued for 4 hours, and the reaction ended. After the reaction solution was cooled to room temperature, it was vacuum filtered, and the filter cake was rinsed three times with a small amount of isobutanol to complete the reaction. After the reaction solution was cooled to room temperature, it was vacuum filtered, and the filter cake was rinsed with a small amount of isobutanol three ti...

Embodiment 2

[0068] exist figure 1 Add 649L of isobutanol and benzyl alcohol mixture to the reaction kettle shown with a stirring device and a reflux condensing device, the volume ratio of isobutanol / benzyl alcohol is 10:1, 29.53 kg of vanadium pentoxide, and the auxiliary agent hexahydrate Ferric nitrate 0.3kg, auxiliary agent zirconium nitrate 0.5kg, start stirring, increase the reaction temperature and keep it at 100±2°C, carry out reflux reaction, keep reflux time for 4 hours, then add 34.98kg of phosphoric acid with a concentration of 100%, phosphorus / vanadium The molar ratio was 1.1, the reflux was continued for 4 hours, and the reaction ended. After the reaction solution was cooled to room temperature, it was vacuum filtered, and the filter cake was rinsed three times with a small amount of isobutanol to complete the reaction. After the reaction solution was cooled to room temperature, it was vacuum filtered, and the filter cake was rinsed with a small amount of isobutanol three t...

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Abstract

The invention discloses a method for preparing maleic anhydride by oxidation of n-butane. According to the invention, n-butane, air and cycle tail gas are mixed, a mixture passes through more than two of reaction zones which are connected in series in order, under oxidation reaction condition, the mixture is contacted with a vanadium phosphorus oxide catalyst; besides the most downstream reaction zone, each reaction zone comprises more than two catalyst bed layers; wherein, according to a contact sequence with reaction gas, average valence of vanadium in the catalyst in the downstream reaction zone is higher than the average valence of vanadium in the catalyst in the upstream reaction zone; and, in each reaction zone besides the most downstream reaction zone, average valence of vanadium in the downstream catalyst bed layer is higher than the average valence of vanadium in the upstream catalyst bed layer. The catalyst activity is equally distributed according to reaction requirement, catalytic activity is fully performed, especially in a tail gas cycle utilization technology, influence of decreased conversion rate due to decreased oxygen content in the raw materials can be compensated, reaction hot spot is reduced, and product selectivity is increased.

Description

technical field [0001] The invention relates to a process for preparing maleic anhydride by n-butane oxidation, which can be used in the reaction process of n-butane oxidation for maleic anhydride using a fixed bed process. Background technique [0002] Maleic anhydride, also known as maleic anhydride, is an important organic chemical raw material and the third largest organic anhydride in the world after phthalic anhydride and acetic anhydride. It is widely used in petrochemical, food processing, and pharmaceutical industries. , Building materials and other industries. Its specific applications include the manufacture of unsaturated polyester resins, alkyd resins, maleic acid (maleic acid), fumaric acid (fumaric acid), and pesticides, coatings, glass fiber reinforced plastics, lubricating oil additives, paper chemistry Product additives, surfactants, etc. The advent of the new method of maleic anhydride esterification and low-pressure hydrogenation to produce 1,4-butanedi...

Claims

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Application Information

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IPC IPC(8): C07D307/60B01J27/198
CPCB01J27/198C07D307/60
Inventor 王海波刘新宇勾连科宋丽芝侯学伟
Owner CHINA PETROLEUM & CHEM CORP
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