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SO42-/nano TiO2 catalyst and application thereof to preparing cyclohexenyl cyclohexanone

A catalyst, cyclohexanone technology, applied in physical/chemical process catalysts, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of low rush selectivity, polluting the environment, and many by-products, etc.

Inactive Publication Date: 2012-06-20
NANJING UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The solid acid catalyst of above-mentioned research is on the low side in preparing cyclohexenyl cyclohexanone, and the by-product is more, and the catalyst used in production is mostly organic acid or inorganic acid, has serious corrosion to production equipment, simultaneously It is difficult to separate the product from the catalyst, and it needs to undergo neutralization, washing and other processes, resulting in a large amount of acidic wastewater, which seriously pollutes the environment

Method used

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  • SO42-/nano TiO2 catalyst and application thereof to preparing cyclohexenyl cyclohexanone
  • SO42-/nano TiO2 catalyst and application thereof to preparing cyclohexenyl cyclohexanone
  • SO42-/nano TiO2 catalyst and application thereof to preparing cyclohexenyl cyclohexanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 16.0g with an average particle size of 10nm and a specific surface area of ​​82m 2 / g Nano-TiO 2 In a beaker, add 50ml, 2mol / L sulfuric acid while stirring, the molar ratio of nano-titanium dioxide to sulfuric acid is 2:1. Nano TiO 2 After complete impregnation, promote at 30°C for 3h, filter the impregnation solution, put the obtained filter cake in a drying oven at 100°C for 5h, and then bake in a muffle furnace at 300°C for 5h to prepare the catalyst.

[0020] The prepared catalyst is used for self-condensation of cyclohexanone to prepare cyclohexenyl cyclohexanone. The reaction is carried out in a tank reactor with stirring. Add 100g of cyclohexanone to the reactor, heat it to 140°C, add 3 grams of catalyst to the tank, and react for 2 hours under stirring. Then, take a sample and analyze the reaction in gas chromatography. The composition of the product, and the conversion rate of cyclohexanone calculated from this data is 51.5%, and the selectivity of cyc...

Embodiment 2-4

[0022] Catalyst preparation method is the same as embodiment 1, changes H 2 SO 4 with nano TiO 2 Molar ratio, the prepared catalyst was carried out under the same activity evaluation conditions as in Example 1, and the obtained cyclohexanone conversion rate and cyclohexenyl cyclohexanone selectivity were shown in Table 1.

[0023] Table 1 Nano TiO 2 with H 2 SO 4 Catalytic Activity of Catalysts Prepared by Different Molar Ratio

[0024]

Embodiment 5-7

[0026] Catalyst preparation method is the same as embodiment 1, changes H 2 SO 4 Nano TiO 2 Acceleration time, the prepared catalyst was carried out under the same activity evaluation conditions as in Example 1, and the obtained cyclohexanone conversion rate and cyclohexenyl cyclohexanone selectivity are shown in Table 2.

[0027] Table 2H 2 SO 4 Catalytic Activity of Catalysts Prepared by Different Promoting Time

[0028]

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Abstract

The invention belongs to the technical field of catalysts, and particularly relates to a SO42- / nano TiO2 catalyst used in preparation of cyclohexenyl cyclohexanone through cyclohexanone self-condensation and a preparation method. In the invention, nano titanium dioxide is used as a raw material; mixing of sulfuric acid and nano titanium dioxide is promoted by using an impregnation method; and then drying and high-temperature roasting are performed to prepare the SO42- / nano TiO2 slid super acidic catalyst. The catalyst is applied to cyclohexanone self-condensation for catalytic synthesis of the cyclohexenyl cyclohexanone; and at the reaction temperature of 130-150 DEG C, the using amount of the SO42- / nano TiO2 catalyst is 2-5 percent, the reaction time is 2-3 hours, the cyclohexanone conversion rate is 45-65 percent, and the cyclohexenyl cyclohexanone selectivity reaches 97-99 percent.

Description

technical field [0001] The invention belongs to the field of catalysts, in particular to a SO 4 2- / nano-TiO 2 Catalyst, and the application of this catalyst in cyclohexanone self-condensation preparation cyclohexenyl cyclohexanone. Background technique [0002] Cyclohexenyl cyclohexanone is an important fine chemical, which can be used as a special solvent in carbamate herbicides, wood preservatives, insecticides, etc., and its large-scale application is as the production of o-phenylphenol ( OPP) raw material. OPP is an organic chemical product with a wide range of uses. This compound can be used as a carrier for hydrophobic synthetic fibers when dyed with a carrier, a heat stabilizer for plastics, a surfactant, a bactericidal preservative, and a dye intermediate. O-phenylphenol and its sodium salt can be used for antisepsis of vegetables, apples, pears, pineapples, citrus, etc., which can minimize the rot. It is also a powerful bactericide, disinfectant, antiseptic an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053C07C45/74C07C49/653
Inventor 孙中森张银华曾崇余武文良徐建东
Owner NANJING UNIV OF TECH
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