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Method for catalysis of pimelinketone oxamidine

A technology of cyclohexanone ammonia oxime and cyclohexanone, which is applied in the field of cyclohexanone ammonia oximation catalyzed by titanium silicon materials

Active Publication Date: 2008-12-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there is no report on the preparation of cyclohexanone oxime by ammoxidation of cyclohexanone

Method used

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  • Method for catalysis of pimelinketone oxamidine
  • Method for catalysis of pimelinketone oxamidine
  • Method for catalysis of pimelinketone oxamidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] Take 20 grams of titanium silicon molecular sieve TS-1, ammonium nitrate palladium complex solution with a concentration of 0.01g / ml (calculated as palladium atom), and an appropriate amount of hydrazine hydrate and cetyltrimethylammonium bromide and add to the tetrapropyl group Stir and mix uniformly in an aqueous solution of ammonium hydroxide (10% by mass), in which titanium silicon molecular sieve (g): cetyltrimethylammonium bromide (mole): tetrapropylammonium hydroxide (mole): hydrated Hydrazine (mole): ammonium nitrate palladium complex (g, in terms of palladium): water (mole)=100:0.005:0.5:3.0:2.0:1000. Then it was put into a stainless steel sealed reaction kettle and hydrothermally treated at a temperature of 150°C and autogenous pressure for 48 hours. The resultant was filtered, washed with water, dried naturally, and dried at 180°C for 3 hours to obtain the new type of the present invention. Noble metal microporous titanium silicon material A. After characterizati...

Embodiment 2

[0076] Take 20 grams of titanium silicon molecular sieve TS-1, a palladium chloride solution with a concentration of 0.01g / ml (based on palladium atoms), and an appropriate amount of hydrazine hydrochloride and polypropylene, add them to the aqueous solution of sodium hydroxide (15% by mass) and stir. Mix uniformly, in which titanium silicon molecular sieve (g): polypropylene (mol): sodium hydroxide (mol): hydrazine hydrochloride (mol): palladium chloride (g, calculated as palladium): water (mol) = 100: 0.9: 1.8:0.15:0.1:4600. Then it was put into a stainless steel sealed reaction kettle, hydrothermally treated at a temperature of 180°C and autogenous pressure for 24 hours, the resultant was filtered, washed with water, dried naturally, and dried at 110°C for 3 hours to obtain the novel containing material of the present invention. Noble metal microporous titanium silicon material B. After characterization, its composition can be expressed as 8TiO in the form of oxide 2 ·100SiO 2 ...

Embodiment 3

[0078] Add tetraethyl orthosilicate, tetrabutyl titanate, a palladium acetate solution with a concentration of 0.01g / ml (in terms of palladium atom) and Tween 80 to the aqueous solution of tetrapropylammonium hydroxide and butanediamine (quality The percentage concentration is 10%), stir and mix evenly, and the molar composition is silicon source: titanium source: tetrapropyl ammonium hydroxide: butanediamine: palladium source: protective agent: water = 100: 0.03: 0.5: 0.1: 0.05: 0.02:550, silicon source is SiO 2 Calculated, the titanium source is TiO 2 The palladium source is calculated as Pd. Then, it is put into a sealed reactor, and is subjected to a hydrothermal treatment at a temperature of 120° C. and autogenous pressure for 120 hours. The resultant is taken out, filtered, dried, and calcined to obtain an intermediate crystalline material. Transfer the intermediate crystalline material to the remaining filtrate, add an appropriate amount of hydrazine hydrate, and hydrotherm...

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Abstract

The invention discloses a method for catalyzing ammoximation of cyclohexanone. The method comprises the steps as follows: subjecting cyclohexanone, ammonia, oxygen, hydrogen, diluent gas and a solvent to coming in contact with a catalyst. The mole ratio of cyclohexanone, to ammonia, oxygen, hydrogen and diluent gas is 1:(0.1-10.0):(0.1-10.0):(0.1-10.0):(0-100). The mass ratio of the solvent to the catalyst is (20-1000):1. The catalyst is a microporous titanium-silicon material or a compound containing the microporous titanium-silicon material. The composition of the microporous titanium-silicon material is expressed as xTiO2*100SiO2*yEmOn*zE in an oxide form, wherein x ranges from 0.001 to 50.0; the sum of y plus z ranges from 0.005 to 20.0; the ratio of y to z is smaller than 1; E is one or more metal noble metals selected from Ru, Rh, Pd, Re, Os, Ir, P and Au; m and n are numbers required for meeting the oxidation state of the E; and material grains are partially or totally hollow-structured. The method has the advantages of high selectivity of cyclohexanone oxime, high product activity and stability, environment friendliness and low cost.

Description

Technical field [0001] The invention relates to a method for catalyzing the ammoximation of cyclohexanone, and more particularly to a method for catalyzing the ammoximation of cyclohexanone by a titanium-silicon material containing noble metals. Background technique [0002] Cyclohexanone oxime is a key intermediate for the production of ε-caprolactam, and ε-caprolactam is an important organic chemical raw material, mainly used as a monomer for synthetic fibers and engineering plastics (such as nylon-6). About 91% of caprolactam in industry is produced through the cyclohexanone oxime route, that is, the cyclohexanone-hydroxylamine process. This process is not only complex, long production process, high equipment investment, but also due to the production or use of NO X , SO X And there are serious corrosion and pollution problems. With the increasing awareness of environmental protection in our country, the research and development of a method for producing cyclohexanone oxime wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/44C07C249/04B01J29/89
Inventor 林民史春风龙军朱斌舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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