Ammoxidation method for cyclohexanone

A cyclohexanone ammonia and cyclohexanone technology is applied in the field of cyclohexanone ammoxidation, which can solve the problems that the active component titanium silicon is easy to fall off, the specific surface of graphite is small, the catalyst activity is decreased, etc., and the catalytic effect is excellent and the thermal effect is moderated. , the effect of improving the reaction selectivity

Active Publication Date: 2014-05-21
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The composite titanium silicon catalyst is used for the ammoximation reaction of cyclohexanone, the conversion rate of cyclohexanone and the selectivity of cyclohexanone oxime can reach more than 95%, but the specific surface of graphite is small, the surface is smooth and chemically inert, and the active group Titanium and silicon are easy to fall off, resulting in a decrease in catalyst activity

Method used

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  • Ammoxidation method for cyclohexanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In the polymerization kettle, add 7.5g of titanium-silicon molecular sieve powder, 90g of polymerized monomer styrene and 30g of divinylbenzene, and 60g of pore-forming agent liquid wax. Benzoyl 1.Sg, polymerized at 90°C for 6 hours to obtain block titanium silicon molecular sieve catalyst. Then carry out crushing and granulation, select a catalyst with a suitable particle size after screening, add 250 ml of 1,2-dichloroethane to swell, and swell for 5 hours at normal temperature. After pouring out 1,2-dichloroethane, add 200ml of ethyl acetate for solvent extraction. The extraction reaction temperature is 55°C, and the extraction time is 4 hours. The same method is used for three extractions to obtain a composite of titanium silicon molecular sieve and resin. Catalyst A, its physical and chemical properties are shown in Table 1.

Embodiment 2

[0039] In the polymerization kettle, add 15g of titanium-silicon molecular sieve powder, 90g of polymerized monomer styrene, 15g of divinyltoluene, 25g of divinylxylene, and pore-forming agent C 5 60g of aliphatic alcohol, stirred and mixed evenly, when the temperature of the water bath was raised to 80°C, 2.0g of initiator azobisisobutanol was added, and the reaction temperature was polymerized at 100°C for 6 hours to obtain a block titanium silicon molecular sieve catalyst. Then carry out crushing and granulation, select a catalyst with a suitable particle size after screening, add 250 ml of 1,2-dichloroethane to swell, and swell for 5 hours at normal temperature. After pouring out 1,2-dichloroethane, add 200ml of xylene for solvent extraction. The extraction reaction temperature is 55°C, and the extraction time is 4 hours. The same method is used for three extractions to obtain a titanium-silicon molecular sieve and resin composite catalyst. B, its physical and chemical pro...

Embodiment 3

[0041] The weight of the titanium-silicon molecular sieve powder in Example 1 was changed to 30 g, the extraction solvent was replaced with chloroform, and the rest was the same as in Example 1 to obtain a titanium-silicon molecular sieve and resin composite catalyst C, whose physical and chemical properties are shown in Table 1.

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Abstract

A composite catalyst of Ti-Si molecular sieve and resin, preparation method and application thereof are disclosed. The catalyst is mainly consisted of Ti-Si molecular sieve and resin. The preparation method is as follows: mixing Ti-Si molecular sieve, polymerizing monomers, and pore-forming materials sufficiently in the presence of an initiator; then perfoming polymerization reaction to obtain a catalyst solid; adding the catalyst solid into halohydrocarbon to swell; solvent extracting to obtain a shaped catalyst.The obtained catalyst may be applied in the catalytic reactions of olefine epoxidation and cyclohexanone ammoxidation to prepare cyclohexanone oxime with fixed bed process, thus simplifying the operation steps, improving the slectivity for the target product, at the same time, solving the difficult problem of separating the catalyst powder containing Ti-Si molecular sieve from the reaction liquid, and increasing the reaction efficiency.

Description

technical field [0001] The invention belongs to a method for ammoxidation of cyclohexanone, in particular to a method for ammoxidation of fixed bed cyclohexanone. Background technique [0002] Since the Italian Enichem company first synthesized the lattice oxygen-selective titania-silicon molecular sieve catalyst TS-1 in 1983, it has become a hot spot in the research of oxidation catalysts due to its excellent oxidation selectivity and mild reaction conditions, and this discovery is regarded as environmentally friendly. A major breakthrough in catalyst development. [0003] Titanium-silicon molecular sieve catalysts play a very important role in the selective oxidation of organic compounds, such as the ammoxidation of cyclohexanone with hydrogen peroxide under the action of titanium-silicon molecular sieve catalysts to prepare cyclohexanone oxime. In industrial applications, titanium-silicon molecular sieve catalysts exhibit excellent shape-selective catalytic performance. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C251/44C07C249/04B01J31/38
CPCB01J35/1038C07C249/04B01J35/002B01J35/1019B01J37/0018B01J29/89
Inventor 王海波黎元生勾连科宋丽芝薛冬
Owner CHINA PETROLEUM & CHEM CORP
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