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Catalyst for synthesizing cyclopentanone, preparation method thereof and application in synthesizing cyclopentanone

A cyclopentanone and catalyst technology, applied in the field of catalytic synthesis, can solve the problems of shortage of adipic acid raw material sources, low use value, high price of adipic acid, etc., and achieve the effect of simple structure, less equipment and high product selectivity

Active Publication Date: 2017-01-04
SHANDONG NHU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the shortage of adipic acid raw materials, the price of adipic acid is relatively high, and the reaction produces a large amount of pollutants, this method is facing elimination; BASF uses N 2 Oxidation of cyclopentene method, cyclopentanone has good selectivity and strong market competitiveness, but the reaction needs to be carried out under high temperature and high pressure conditions. When the temperature is 230 ° C, the pressure in the reactor can reach 11.5 MPa, The requirements for reaction equipment and operation are relatively high, and the N 2 O is a downstream product of Ludwigshafen, Germany, and it is of little value to be widely used in China

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0030] A kind of synthetic technique of cyclopentanone and the preparation of catalyst thereof, comprises the following steps:

[0031] 1. Preparation of catalyst

[0032] A certain amount of Na 2 HPO 4 12H 2 O, Na 2 MoO 4 2H 2 O and NaVO 3 2H 2 O was put into boiling water step by step, stirred and dissolved, reacted for 1 hour, cooled to room temperature, added sulfuric acid to adjust the pH to about 2, extracted with ether and separated to separate the ether polyacid complex, purged with air to remove ether, and dried in vacuo to obtain Solid polyacid.

[0033] Dissolve the obtained solid acid in water, heat to 90°C, slowly add a certain amount of X metal salt solution, stir and precipitate, separate and dry the precipitate to obtain the finished catalyst.

[0034] The prepared heteropolyacid catalyst consists of:

[0035] P—Mo—V—X

[0036] Wherein: X is any one in Fe, Co, Pd and Cu;

[0037] As the main catalyst, Mo and V coordinate and restrict each other in t...

Embodiment 1

[0044] Embodiment 1: the preparation of catalyst

[0045] The preparation of catalyst comprises the following steps:

[0046] a. Add raw materials

[0047] 3.8gNa 2 HPO 4 12H 2 O dissolved in 50 mL deionized water, 28.6 g Na 2 MoO 4 2H 2 O was dissolved in 60mL deionized water, the two solutions were mixed, heated to boiling, reacted for 30min, stopped heating, and 1.42gNaVO 3 2H 2 O was dissolved in 20ml of water, and added to the above mixture while stirring, and stirred and refluxed at 90°C for 1h.

[0048] b. Adjust the pH value

[0049] Stop heating, slowly drop in 1:1 (m / m) H 2 SO 4The solution was adjusted to pH=2.0.

[0050] c, static stratification

[0051] Continue to stir to room temperature, add 50 mL of ether to the reaction solution, and after sufficient shaking, add 1:1 (m / m) of H 2 SO 4 Continue to shake until no oily liquid drips. After standing, the solution is divided into three layers, the upper layer is ether, the middle layer is water and i...

example 2

[0056] Example 2: Synthesis of cyclopentanone

[0057] The synthesis of cyclopentanone comprises the following steps:

[0058] a. to react

[0059] Take 2.0 g of the prepared P-Mo-V-Fe type catalyst, 40 ml of cyclopentene, and 150 ml of solvent into the reactor, stir and heat up to 60 ° C, fill with nitrogen to make the pressure reach 0.5 MPa, close the nitrogen, and then add to the reactor. Pure oxygen was introduced into the reaction kettle to make the system pressure reach 0.75MPa, the system pressure was maintained, and the reaction was kept under pressure for 6 hours. After the reaction was completed, it was cooled to room temperature. The single-pass conversion of cyclopentene was 76.1%, and the selectivity of the product cyclopentanone was 96.5%.

[0060] b. Rectification and purification

[0061] The reacted solution is transferred to a vacuum distillation device, and at a certain temperature, the cyclopentene and the solvent are evaporated, the catalyst is precipit...

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PUM

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Abstract

The invention discloses a catalyst for cyclopentanone synthesis. The catalyst comprises the following components: P-Mo-V-X, wherein X is one of Fe, Co, Pd and Cu. The preparation method of the catalyst comprises the following steps: adding raw materials; regulating a pH value; standing for layering; carrying out vacuum drying; and carrying out precipitation separation. The catalyst disclosed by the invention is applied to the cyclopentanone synthesis and achieves the conversion per pass of cyclopentene more than 75%, the selectivity of product cyclopentanone more than 95% and the purity of the cyclopentanone prepared after rectification and purification more than 99%.

Description

technical field [0001] The invention relates to a catalyst and a preparation method thereof, in particular to a catalyst for synthesizing cyclopentanone, a preparation method thereof and an application in synthesizing cyclopentanone, belonging to the technical field of catalytic synthesis. Background technique [0002] Cyclopentanone is an important fine chemical intermediate, molecular formula: C 5 h 8 O; English name: cyclopentanone, is an important fine chemical intermediate. It can be used to prepare new spices such as methyl dihydrojasmonate, brandyne, 2-n-hexylcyclopentanone and various anti-inflammatory and anti-cancer drugs. [0003] Adipic acid pyrolysis is the main method for the production of cyclopentanone. This process uses barium hydroxide as a catalyst. Adipic acid undergoes intramolecular condensation at high temperature to generate cyclopentanone. The produced cyclopentanone accounts for about 10% of the world's total output. more than 90 percent. Howeve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/199C07C49/395C07C45/34
Inventor 于航周剑平于安德王云龙马啸李耀林
Owner SHANDONG NHU PHARMA
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