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Catalyst for synthesizing caprolactam in one step by ammoxidation of cyclohexanone and preparation and application method thereof

A caprolactam and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of separation of intermediate products and energy consumption, and solve the problems of equipment corrosion and environmental pollution, low production cost, The effect of long preparation cycle

Inactive Publication Date: 2010-03-17
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The technical problem to be solved by the present invention is to provide a catalyst for one-step synthesis of caprolactam by ammoxidation of cyclohexanone and its preparation and application method in view of the problems of intermediate product separation and energy consumption in the existing production technology

Method used

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  • Catalyst for synthesizing caprolactam in one step by ammoxidation of cyclohexanone and preparation and application method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The preparation of supported catalyst, the steps are as follows:

[0029] In the first step, get tetraethyl orthosilicate (TEOS), aluminum sec-butoxide, and dehydrated ethanol and place them in a 100ml three-necked flask, the molar ratio of which is tetraethyl orthosilicate: aluminum sec-butoxide: dehydrated ethanol=0.93 : 1:8 After stirring mechanically at room temperature for 10 minutes, place the there-necked flask in a water bath at 70°C, slowly add aqueous hydrochloric acid solution with a mass concentration of 12% until the pH of the reaction system is 3, stir in a constant temperature water bath at 70°C for 1.5 hours, take out Distillation under reduced pressure was performed to remove water, ethanol and butanol.

[0030] In the second step, the material obtained in the first step is calcined in a tube furnace at a high temperature of 550° C. for 5 hours in an oxygen atmosphere to obtain a composite oxide of silicon oxide and aluminum oxide.

[0031] In the thir...

Embodiment 2

[0035] Step is the same as Example 1, and the difference is that in the first step, the mol ratio of tetraethyl orthosilicate (TEOS), aluminum sec-butoxide, dehydrated alcohol is 0.73: 1: 8; Get 0.23g mass concentration in the 3rd step It is 85% phosphoric acid, dissolved in 1.45g of distilled water to form an impregnation solution. In the fifth step, 1.90 g of a supported bifunctional catalyst product for the one-step synthesis of caprolactam from cyclohexanone was obtained.

Embodiment 3

[0037] Step is the same as Example 1, and difference is that, in the first step, the mol ratio of tetraethyl orthosilicate (TEOS), aluminum sec-butoxide, dehydrated alcohol is 1.13: 1: 8; Get 1.33g mass concentration in the 3rd step It is 85% phosphoric acid, dissolved in 1.29g of distilled water to form an impregnation solution. In the fifth step, 2.83 g of a supported bifunctional catalyst product for the one-step synthesis of caprolactam from cyclohexanone was obtained.

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Abstract

The invention relates to a supported solid-acid catalyst for synthesizing caprolactam in one step by cyclohexanone as well as a preparation and an application method thereof. The catalyst is a supported dual-function type catalyst and comprises a carrier and active components, wherein the carrier is a composite oxide of silicon oxide and aluminum oxide, and the active component is phosphoric acid;the mol ratio between silicon and aluminum in the carrier is 0.73 to 1.13: 1, the load amount of the phosphoric acid is 10 percent to 40 percent, and the load amount is the mass percentage content ofthe phosphoric acid in the whole supported dual-functional type catalyst. The supported dual-functional type catalyst has the advantages of simple preparation method, low-price and easily-obtained raw materials and lower production cost, can be repeatedly used for more than three times and can recover the activity just by simple washing and roasting.

Description

technical field [0001] The technical scheme of the present invention relates to a solid acid catalyst for preparing caprolactam, specifically a supported solid acid catalyst for one-step synthesis of caprolactam from cyclohexanone and a preparation and application method thereof. technical background [0002] Caprolactam is one of the important organic chemical raw materials, which can be processed into nylon-6 fiber, nylon-6 resin and nylon-6 film, etc.; it is mainly used in automobiles, ships, electronic appliances, industrial machinery, textiles, components of daily consumer goods and Film products such as food preservation film. In recent years, with the development of a new environment-friendly process for the synthesis of high-quality chemical fibers from caprolactam and nylon-6, the technology of clean production of caprolactam has become a hot spot in the chemical industry at home and abroad. [0003] The current industrial production adopts a two-step production pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/182C07D223/10
CPCY02P20/52
Inventor 王延吉赵江琨王荷芳赵新强裴新彬
Owner HEBEI UNIV OF TECH
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