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Method for preparing caprolactam by beckmann rearrangement for cyclohexanone-oxime
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A technology of cyclohexanone oxime and caprolactam, which is applied in the field of caprolactam preparation, to achieve the effect of strong acidity, strong catalytic activity and simple reaction operation
Active Publication Date: 2012-08-22
JIANGSU SANJILI CHEM
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[0007] The technical problem to be solved by the present invention is aimed at the problems faced in the development of the cyclohexanone oxime rearrangement process without ammoniumsulfate by-product in the prior art, and proposes a more reasonable process design, the conversion rate of cyclohexanone oxime and the selection of caprolactam The method of preparing caprolactam by the Beckmann rearrangement of cyclohexanone oxime that can be applied to large-scale industrial production
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Embodiment 1
[0022] Example 1, a method for preparing caprolactam by rearrangement of cyclohexanone oxime. In this method, after the raw material cyclohexanone oxime is miscible with an organic solvent, a catalyst is added to support a heteropolyacid. Under the protection of an inert gas, a liquid phase reaction occurs Beckmann rearrangement to produce caprolactam;
[0023] The loaded heteropolyacid refers to the heteropolyacid loaded on SiO 2 The tungsten-containing heteropolyacid compound with Keggin structure above, wherein the molar ratio of P:W:V is 1:5:1;
[0024] When the liquid phase reaction is adopted, the organic solvent is polyhalogenated alkanes, polyhalogenated aromatic hydrocarbons or thiophene heterocyclic compounds; when the liquid phase reaction is performed, the temperature is 30°C, and the weight ratio of cyclohexanone oxime to the organic solvent is 1:5 , The reaction time is 1h.
Embodiment 2
[0025] Example 2, a method for preparing caprolactam by rearrangement of cyclohexanone oxime. In this method, after the raw material cyclohexanone oxime is miscible with an organic solvent, a catalyst is added to support a heteropolyacid. Under the protection of an inert gas, a liquid phase reaction occurs Beckman rearrangement to produce caprolactam;
[0026] The loaded heteropolyacid refers to the heteropolyacid loaded on SiO 2 The tungsten-containing heteropolyacid compound with Keggin structure, wherein the molar ratio of P:W:V is 1:15:10;
[0027] When liquid phase reaction is adopted, the organic solvent is polyhalogenated alkanes, polyhalogenated aromatic hydrocarbons or thiophene heterocyclic compounds; during liquid phase reaction, the temperature is 150°C, and the weight ratio of cyclohexanone oxime to organic solvent is 1: 15 , The reaction time is 10h.
Embodiment 3
[0028] Example 3, a method for preparing caprolactam by rearrangement of cyclohexanone oxime. In this method, after the raw material cyclohexanone oxime is miscible with an organic solvent, a catalyst is added to support a heteropolyacid. Under the protection of an inert gas, a liquid phase reaction occurs Beckman rearrangement to produce caprolactam;
[0029] The loaded heteropolyacid refers to the heteropolyacid loaded on SiO 2 The tungsten-containing heteropolyacid compound with Keggin structure above, wherein the molar ratio of P:W:V is 1:10:5;
[0030] When liquid phase reaction is adopted, the organic solvent is polyhalogenated alkanes, polyhalogenated aromatic hydrocarbons or thiophene heterocyclic compounds; during liquid phase reaction, the temperature is 100°C, and the weight ratio of cyclohexanone oxime to organic solvent is 1:10 , The reaction time is 5h.
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Abstract
The invention relates to a method for preparing caprolactam by beckmann rearrangement for cyclohexanone-oxime, which is characterized in that the cyclohexanone-oxime serving as the raw material and organic solvent are dissolved with each other, and then catalyst load heteropoly acid is added into the solution; under the condition of inert gas shielding, liquid-phase or gas-phase reaction is carried out, and the caprolactam can be prepared by the beckmann rearrangement; the load heteropoly acid is tungsten-containing heteropoly acid compound which is obtained by loading heteropoly acid on SiO2 and has a Keggin structure, wherein the molar ratio of P to W to V is 1:(5-15):(1-10); the liquid-phase reaction temperature is 30-150 DEG C, and the weight ratio of the cyclohexanone-oxime to the organic solvent is 1:(5-15); the gas-phase reaction temperature is 250-350 DEG C, and the weight ratio of the cyclohexanone-oxime to the organic solvent is 1:(5-10); and the weight space velocity of the cyclohexanone-oxime is 0.25-25h<-1>. The method is mild in reaction condition and simple in reaction operation, and the conversion rate of the cyclohexanone-oxime and the selectivity of the caprolactam are higher, so that the method is completely suitable for industrial production; and the reaction process is environment-friendly.
Description
technical field [0001] The invention relates to a method for preparing caprolactam, in particular to a method for preparing caprolactam through Beckmann rearrangement of cyclohexanone oxime. Background technique [0002] Caprolactam is an important organic chemical raw material and an important monomer for the manufacture of nylon 6, plastics and films. In industry, cyclohexanone oxime is generally prepared by Beckmann rearrangement under the action of concentrated sulfuric acid or nicotinic acid. The biggest disadvantage of this method is that equipment corrosion and environmental pollution are serious, and a large amount of low-value ammoniumsulfate is produced by-product, which increases production. cost. Therefore, the development of a new Beckmann rearrangement process without ammoniumsulfate by-product is the goal of improving the production process of caprolactam, and it is also in line with the development direction of green chemistry. [0003] In order to solve...
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