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Preparation of rod-shaped nano tungsten trioxide and technology of catalytic synthesis of adipic acid therethrough

A technology of nano-tungsten trioxide and adipic acid, which is applied in the direction of oxidative preparation of carboxylic acid, tungsten oxide/tungsten hydroxide, organic chemistry, etc., which can solve the problem of low yield

Inactive Publication Date: 2013-12-04
XINJIANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the yield of adipic acid is lower than that of tungstic acid and phosphotungstic acid, further research is needed to improve the yield of adipic acid

Method used

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  • Preparation of rod-shaped nano tungsten trioxide and technology of catalytic synthesis of adipic acid therethrough
  • Preparation of rod-shaped nano tungsten trioxide and technology of catalytic synthesis of adipic acid therethrough

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 6.6 g Na 2 WO 4 . 2H 2 O (0.02 mol) was added to 50 mL of water, and HCl (9 mL) with a metering ratio of 1:1 was added dropwise under the condition of magnetic stirring. After stirring evenly, 5.48 g (0.04 mol) of p-aminobenzoic acid was added, stirred for another 0.5 h, and the mixture was poured into the reaction kettle. React at 180°C for 24 h in a blast oven. The obtained substance was repeatedly washed with ethanol and water, filtered with suction, and dried to obtain the final product.

[0020] 0.0356 g of the catalyst synthesized above, 0.1 g of oxalic acid, 4.1 ml of 30% H 2 o 2 and 8 mmol cyclohexene into a 10mL reaction vessel, put the reaction kettle in an oven at 90°C for 12 h, add a certain amount of acetone after the reaction, centrifuge the mixed solution to remove the catalyst, take the supernatant, spin evaporate, and air-dry , to obtain the product. The product is weighed, and the yield is calculated, and the results are shown in the attached ...

Embodiment 2

[0022] Accurately weigh 33 g Na 2 WO 4 . 2H 2 O (0.1 mol) was added to 250 mL of water, and HCl (45 mL) with a metering ratio of 1:1 was added dropwise under the condition of magnetic stirring. After stirring evenly, 27.4 g (0.2 mol) of p-aminobenzoic acid was added, stirred for another 0.5 h, and the mixture was poured into the reaction kettle. React at 180°C for 24 h in a blast oven. The obtained substance was repeatedly washed with ethanol and water, filtered with suction, and dried to obtain the final product.

[0023] Add 1.5 mmol of the catalyst synthesized above, 0.4 mol of 30% H to the reaction vessel 2 o 2 , 0.12 mol oxalic acid, stirred at room temperature for 15 min, then added the calculated amount of cyclohexene, stirred vigorously, heated at 73°C for 2 h, then rose to 90°C and refluxed for 10 h. After the reaction, a transparent liquid was obtained by suction filtration, which was left standing at 0°C overnight, and a large amount of white crystals were pr...

Embodiment 3

[0025] Accurately weigh 33 g Na 2 WO 4 . 2H 2O (0.1 mol) was added to 250 mL of water, and HCl (45 mL) with a metering ratio of 1:1 was added dropwise under the condition of magnetic stirring. After stirring evenly, 27.4 g (0.2 mol) of p-aminobenzoic acid was added, stirred for another 0.5 h, and the mixture was poured into the reaction kettle. React at 180°C for 24 h in a blast oven. The obtained substance was repeatedly washed with ethanol and water, filtered with suction, and dried to obtain the final product.

[0026] Add 1.5 mmol of the catalyst synthesized above, 0.4 mol of 30% H to the reaction vessel 2 o 2 , 0.196 g sulfuric acid, 0.0161 g phosphoric acid, stirred at room temperature for 15 min, then added the calculated amount of cyclohexene, stirred vigorously, heated at 73 °C for 2 h, then rose to 90 °C and refluxed for 10 h. After the reaction, a transparent liquid was obtained by suction filtration, which was left standing at 0°C overnight, and a large amou...

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Abstract

The invention provides a method for hydro-thermal synthesis of rod-shaped nano tungsten trioxide using p-aminobenzoic acid as an adjuvant, as well as a method for catalytic synthesis of adipic acid. According to the invention, tungstate is used as tungsten source, p-aminobenzoic acid is used as a morphological control agent, and the rod-shaped nano tungsten trioxide is obtained through hydro-thermal synthesis; then, hydrogen peroxide is used as an oxidant, rod-shaped nano tungsten trioxide is used as a catalyst for catalytic synthesis of adipic acid. The method is mainly characterized in two points: firstly, a new approach is adopted to synthesize the nano tungsten trioxide; secondly, adipic acid can be obtained through catalytic synthesis via the synthesized catalyst cleanly and efficiently (the yield of adipic acid can reach 51.92%-82.20%) without an organic solvent and a phase transfer catalyst.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and specifically relates to a rod-shaped nano-tungsten trioxide catalyst, a preparation method and a technology for synthesizing adipic acid by catalytic oxidation. [0002] Background technique [0003] Adipic acid is an important organic dibasic acid, mainly used in synthetic fibers, namely nylon-66. The annual consumption of adipic acid is very large. At present, the industrial synthesis of adipic acid generally uses the traditional production process, that is, using concentrated HNO 3 As an oxidizing agent, this process is very harmful to the environment. The main disadvantage of the traditional production process is that the oxidant used is highly corrosive concentrated HNO 3 , and a large amount of N will be emitted during the production process 2 O, and N 2 O gas is a greenhouse gas that can deplete the ozone layer and contribute to the formation of acid rain. Therefore, f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/02C07C51/31C07C55/14
Inventor 肖峰董泽娟宿新泰
Owner XINJIANG UNIVERSITY
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