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Method for preparing cyclohexene oxide

A technology of epoxycyclohexane and cyclohexene, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve unfavorable large-scale industrial application, high cost, and catalyst Complicated preparation process and other problems, to achieve the effect of increasing catalyst performance, low cost, and shortening residence time

Active Publication Date: 2012-11-21
平邑仁安中医药产业发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalysts used have disadvantages such as complicated preparation process and high cost, which are not conducive to large-scale industrial application.

Method used

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  • Method for preparing cyclohexene oxide
  • Method for preparing cyclohexene oxide
  • Method for preparing cyclohexene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0029]Example: Preparation of Heterogeneous Supported Composite Oxide Catalyst

[0030] Add 9.70g (55mmol) ammonium paramolybdate tetrahydrate into 50mL deionized water, heat to 100°C under stirring, add 1.5mL acetic acid to adjust the pH to 4.5, add 5mmol NaH successively 2 PO 4 , 5mmol Fe(SO 4 ) 2 , 0.5M H 2 SO 4 10mL. Continue to stir under heating until a small amount of water remains, and after cooling, the target product solid is precipitated, and the product PMo is obtained after filtration and drying. 11 Fe 1 9.00g;

[0031] Using excessive impregnation method: in a 100mL three-neck round bottom flask, add the Ti silicon ratio of 0.12:1 prepared according to the method of the above-mentioned content of the invention. 0.12 -MCM-41 molecular sieve 3.0g, the heteropolyacid salt PMo prepared above 11 Fe 1 Dissolve 0.60 g in 40 mL deionized water and pour it into a round bottom flask with Ti 0.12 -MCM-41 mixed, stirred continuously in an oil bath at 60°C until...

Embodiment 2~4

[0032] Embodiment 2~4: the complex oxide that different roasting temperature makes is catalyzed to prepare epoxycyclohexane

[0033] In three 50mL three-neck round bottom flasks, add the PMo prepared above with a loading capacity of 20%. 11 Fe 1 / Ti 0.12 -MCM-41-400°C / 500°C / 600°C catalyst 0.2g, cyclohexene 1.64g (20mmol), acetonitrile 4.9g (0.12mol), the flask was reacted at a constant temperature in a 60°C oil bath, refluxed for 10 hours, and continuously Stir, and add 2.05mL (20mmol) of 30% hydrogen peroxide at a constant speed with a micro-sampling pump, and the dropwise addition time is half of the reaction time (5h). After the reaction, the catalyst was separated by filtration, and the filtrate was analyzed by gas chromatography for the content of cyclohexene, epoxycyclohexane and the selectivity of epoxycyclohexane. The filtrate is rectified, and the fraction at 130~135°C is collected to obtain the product epoxycyclohexane. The product was qualitatively analyzed by G...

Embodiment example 5~8

[0036] Implementation Cases 5~8: Catalyzed Preparation of Epoxycyclohexane by Heterogeneous Composite Oxide Catalysts Prepared from Molybdophosphorus Heteropolysalts with Different Molar Ratio of Fe and P

[0037] Use 20% PMo 12-n Fe n / Ti 0.2 -MCM-41-600°C is used as catalyst, other preparation conditions are the same as cases 1~3. The difference is that the heteropoly acid salt PMo 12-n Fe n The molar ratio of Fe and P (namely n) in the case, n=0.5 in case 5, n=1 in case 6, n=2 in case 7, and n=3 in case 8. The catalytic performance of these three catalysts was investigated under the same reaction conditions as in Cases 2-4, and the results are shown in Table 2.

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Abstract

The invention discloses a method for preparing cyclohexene oxide, belonging to the technical field of a fine chemical product. The method comprises the steps of: taking cyclohexene as a substrate and acetonitrile as a reaction solvent, taking 30wt% of hydrogen peroxide as an oxidizing agent, carrying out olefin epoxidation under the action of a catalyst taking a Ti-MCM-41 mesoporous molecular sieve as a carrier to load phosphorus molybdenum iron composite oxide, rectifying the reaction liquid, and taking fraction at 130-135 DEG C to obtain cyclohexene oxide. The load type composite oxide disclosed by the invention has good catalytic activity, and can be repeatedly used; the hydrogen peroxide is used as an oxygen source in the reaction; a byproduct is water and accords with green chemical requirements; the condition is mild at constant pressure; reactant and the byproducts are easily separated; the reaction selectivity is good; the reaction energy consumption is low; and the demand on the reaction device is low; the obtained product cyclohexene oxide is easily separated, and the yield of the cyclohexene oxide is high.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemical products, and specifically relates to a method for preparing epoxycyclohexane by heterogeneous catalytic reaction with mild reaction conditions, simple catalyst preparation and easy separation from reaction solution, convenient product post-treatment, and less environmental pollution. Background technique [0002] There are active epoxy groups in the molecular structure of 1,2-epoxycyclohexane. Under the action of acid or alkali catalyst, the ternary oxygen-containing ring is very easy to ring-open, and it can react with ammonia, amine, alcohol, phenol, carboxylic acid, Water and other substances react to form a high value-added compound. Therefore, epoxycyclohexane is an important organic intermediate, and its industrial applications include the synthesis of epoxy resin active diluents and new pesticides such as dexamethasone. [0003] Most of the main methods for producing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/04C07D301/12B01J31/38
Inventor 吴磊张波汤明慧
Owner 平邑仁安中医药产业发展有限公司
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