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Method for catalyzing oxidation of methacrolein to methacrylic acid

A technology of methacrolein and methacrylic acid, used in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc.

Pending Publication Date: 2018-10-12
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Carbon materials catalyze the oxidation of methacrolein to methacrylic acid, which has not been reported

Method used

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  • Method for catalyzing oxidation of methacrolein to methacrylic acid
  • Method for catalyzing oxidation of methacrolein to methacrylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] After washing with water, 100 ml of cylindrical activated carbon with a diameter of 2 mm and a height of 4 mm was charged into a fixed bed reactor with a diameter of 25 mm and a length of 2000 mm. The other space in the reactor is filled with inert alumina ceramic balls. The feed rate of methacrolein is 0.2 mol / h, the air feed rate is 60 L / h, the water feed rate is 0.15 mol / h, and the nitrogen feed rate is 36 L / h. The reaction pressure is 1 atmosphere. The reaction temperature was set to 250 oC , 270 oC , 290 oC , 310 oC And 330 oC . After 6 hours of reaction, sampling and analysis were started. Liquid samples were detected by gas chromatography FID detector, and gas samples were detected by gas chromatography TCD detector. 250 o At C, the conversion rate of methacrolein is 30%, and the selectivity of methacrylic acid is 40%; 270 o At C, the conversion rate of methacrolein is 30%, and the selectivity of methacrylic acid is 48%; 290 o At C, the conversion rate of methac...

Embodiment 2

[0024] Take 200g of activated carbon and take 14.8g of 85% phosphoric acid to make a solution of 1.2 times the volume of activated carbon. Put the activated carbon into the prepared phosphoric acid solution and stir vigorously at room temperature for 2 hours. After the phosphoric acid solution is completely absorbed by the activated carbon, 100 o C dry for 24 hours. Put the dried activated carbon at 350 oC Calcined for 12 hours, a carbon catalyst with a phosphorus loading of 2% was prepared.

[0025] The catalyst evaluation reactor, the filling amount and the reactant feed rate are as in Example 1. The filling catalyst is activated carbon doped with 2% phosphorus, and the evaluation temperature is 290 o C and 310 o C. 290 o At C, the conversion rate of methacrolein is 32%, and the selectivity of methacrylic acid is 85%; 310 o At C, the conversion of methacrolein is 30%, and the selectivity of methacrylic acid is 99%. At 310 oC After 200 hours of continuous operation, the conversi...

Embodiment 3

[0027] Take 200g of activated carbon, take 11g of boric acid to make a solution 1.5 times the volume of activated carbon, put the activated carbon into the prepared boric acid solution, stir vigorously at room temperature for 2 hours, wait until the phosphoric acid aqueous solution is completely absorbed by the activated carbon, 100 o C dry for 24 hours. Put the dried activated carbon at 350 oC After calcining for 12 hours, a carbon catalyst with a boron loading of 1% was prepared.

[0028] The catalyst evaluation reactor, the filling amount and the reactant feed rate are as in Example 1. The filling catalyst is activated carbon doped with 1% boron, and the evaluation temperature is 310 o C. The conversion rate of methacrolein was 18%, and the selectivity of methacrylic acid was 93%.

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Abstract

The invention relates to a new method for catalyzing oxidation of methacrolein to methacrylic acid by a gas-solid reaction. The method is characterized in that a catalyst used in the method is a carbon catalyst, and the catalyst comprises activated carbon, graphite, carbon nanotubes, graphene oxide, reduced graphene oxide, graphene and nano diamond; the carbon catalyst is modified by acid washingor solvent washing treatment or doping with nitrogen, sulfur, phosphorus, boron, oxygen, molybdenum, cobalt, copper, iron and zinc elements. When air is an oxidant, the conversion rate of methacroleincan reach 68% or above, and the selectivity of methacrylic acid can reach 92% or above.

Description

Technical field [0001] The invention relates to a new method for catalyzing the oxidation of methacrolein to prepare methacrylic acid, and belongs to the field of catalytic chemical engineering. Background technique [0002] Methacrylic acid is an important chemical intermediate. It can be used to prepare important polymer material monomer methyl methacrylate, and it can also be used to prepare functional plastics, medical materials, thermosetting coatings and synthetic rubbers. The main production methods are acetone cyanohydrin method and methacrolein oxidation method. Because the acetone cyanohydrin method requires highly toxic hydrocyanic acid and highly corrosive sulfuric acid, and generates solid waste such as ammonium sulfate, it does not meet the current requirements of green chemical industry. The methacrolein oxidation method is a green, low energy consumption and pollution-free process. The catalyst used is mainly heteropolyacid catalyst based on phosphomolybdovanadi...

Claims

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Application Information

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IPC IPC(8): C07C51/235C07C57/055
CPCC07C51/235
Inventor 周理龙张珊珊孙烨李正杰张志昆镇崇礼刘润静
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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