Preparation method of cyclohexanone-oxime
A technology of cyclohexanone oxime and cyclohexanone amidoxime, which is applied in the field of preparation of cyclohexanone oxime, can solve the loss of titanium silicon molecular sieve, the influence of catalyst pore volume and specific surface area, the conversion rate of cyclohexanone oxime and the selection of cyclohexanone oxime To solve the problems of low cyclohexanone oxime, high cyclohexanone oxime selectivity, improving cyclohexanone conversion rate and cyclohexanone oxime selectivity
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[0016] The preparation method of the cyclohexanone oxime according to the present invention comprises: under the cyclohexanone ammoximation reaction condition, make the reaction raw material that contains cyclohexanone, ammonia, hydrogen peroxide and solvent pass through the polyhedron in the fixed-bed reactor Each catalyst bed layer contains titanium-silicon molecular sieve and resin, and the titanium-silicon molecular sieve contains Ti-MWW-F molecular sieve, along the flow direction of the reaction raw material in the reactor, in the catalyst bed layer The content of the resin is increasing, and the weight percentage of the resin in at least part of the catalyst bed is less than 50%.
[0017] In the present invention, the titanium-silicon molecular sieve may be entirely composed of Ti-MWW-F molecular sieves, or may contain other titanium-silicon molecular sieves conventionally used in the field. Containing Ti-MWW-F molecular sieve can further improve the conversion rate of c...
Embodiment 1
[0051] This example is used to illustrate the preparation method of the cyclohexanone oxime of the present invention.
[0052] (1) Preparation of composite catalyst
[0053] In the polymerization reactor, add Ti-MWW-F molecular sieve, styrene, divinylbenzene and gasoline, stir and mix evenly, when the water bath is heated to 60°C, add benzoyl peroxide, and react at 90°C for 6 hours, Obtain block composite catalyst, then crush to obtain composite catalyst microparticles with a particle size of 1-3 mm, then add 250 ml of 1,2-dichloroethane to swell, keep swelling at normal temperature for 5 hours, then pour out 1,2-dichloroethane, then add 200 ml of ethyl acetate for solvent extraction, the extraction temperature is 55 ° C, the extraction time is 4 hours, and the extraction is repeated three times to obtain a composite catalyst of titanium silicon molecular sieve and resin .
[0054] Composite catalysts A1-A4 of titanium-silicon molecular sieves and resins were prepared accord...
Embodiment 2
[0072] This example is used to illustrate the preparation method of the cyclohexanone oxime of the present invention.
[0073] (1) Preparation of composite catalyst
[0074] According to the method of step (1) of Example 1, the difference is that the composite catalysts B1-B8 are prepared, and the feeding amount of materials in each preparation process is shown in Table 2 below.
[0075] Table 2
[0076]
[0077] (2) Preparation of cyclohexanone oxime
[0078] According to the order of composite catalyst B8 to composite catalyst B1, the composite catalyst that step (1) obtains is packed in diameter and is 20 millimeters, and length is in the fixed-bed reactor of 1200 millimeters, and total filling volume is 50 milliliters, and each The packing heights of the composite catalysts are the same. Then, the reaction raw material (made up of cyclohexanone, hydrogen peroxide, ammonia and water) is injected in the fixed bed reactor, makes the reaction raw material flow along the ...
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