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Preparation method of cyclohexanone oxime

A technology of cyclohexanone oxime and cyclohexanone, which is applied in the field of preparation of organic compounds, can solve the problems of difficult separation of impurities, poor product quality, and many impurities, and achieve the effect of low-cost and high-quality production

Inactive Publication Date: 2014-01-01
刘建青
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The process uses titanium-silicon molecular sieves as catalysts, does not require precious metals as catalysts, and can effectively reduce production costs, but cyclohexanone oxime contains many impurities, such as 1-cyclohexylcyclohexene, nitrocyclohexane, 1,1 Impurities such as '-bicyclohexane-1,1'-diol and 2-cyclohexylcyclohexanone are difficult to separate, resulting in poor product quality and a large amount of waste water

Method used

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  • Preparation method of cyclohexanone oxime

Examples

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Effect test

Embodiment 1

[0034] As shown in the attached figure, 100 g of phosphoric acid with a concentration of 85% by mass and 300 g of aqueous ammonia with a concentration of 5% by mass were prepared to prepare 400 g of phosphate buffer solution (phosphate concentration 2.2 mol / kg).

[0035] In the acidolysis reactor, drop 40g of butanone oxime into a mixture containing 400g of phosphate buffer solution and 65g of 85% phosphoric acid for reaction (the molar ratio of oxime to free phosphoric acid is 0.8:1) to obtain of inorganic fluids. The reaction temperature is controlled at 110° C., and the reaction time is 3 hours; the obtained reaction solution is passed through a stripping tower to remove organic matter butanone oxime and butanone by stripping.

[0036] Dissolve 50g of cyclohexanone in 200g of toluene, and then drop it into an oximation reactor equipped with 400g of inorganic liquid for removing organic matter to perform oximation reaction to obtain a reaction mixture. The reaction temperatu...

Embodiment 2

[0041] 346g of phosphoric acid with a mass percent concentration of 50% and 200g of ammonia water with a mass percent concentration of 15% were configured to form 546g of phosphate buffer solution (phosphate concentration: 3.23mol / kg).

[0042] Add 95g of butanone oxime dropwise to the mixed solution containing 500g of phosphate buffer solution and 65g of 85% phosphoric acid (the molar ratio of oxime to free phosphoric acid is 1.95:1) to obtain an inorganic liquid containing hydroxylamine phosphate. The reaction temperature was controlled at 60° C., and the reaction time was 4 hours; the obtained reaction solution was stripped to remove organic matter.

[0043] Dissolve 50g of cyclohexanone in 200g of toluene, and then drop it into a reactor equipped with 400g of inorganic liquid to remove organic matter for oximation reaction to obtain a reaction mixture. The reaction temperature is 90°C and the reaction time is 1h. The reaction mixture is separated from oil and water, and th...

Embodiment 3

[0047] 247g of phosphoric acid with a mass percent concentration of 70% and 100g of ammonia water with a mass percent concentration of 30% were prepared to form 347g of phosphate buffer solution (phosphate concentration 5.0mol / kg).

[0048]Add 25g of butanone oxime dropwise to a mixed solution containing 300g of phosphate buffer solution and 65g of 85% phosphoric acid (the molar ratio of oxime to free phosphoric acid is 0.5:1) to obtain an inorganic liquid containing hydroxylamine phosphate. The reaction temperature was controlled at 140° C., and the reaction time was 1 h; the obtained reaction solution was stripped to remove organic matter.

[0049] 50g of cyclohexanone was dissolved in 200g of toluene, and then dropped into a reactor equipped with 400g of inorganic liquid to remove organic matter for oximation reaction to obtain a reaction mixture. The reaction temperature was 30°C and the reaction time was 3h. The reaction mixture is separated from oil and water, and the wa...

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Abstract

The invention provides a new preparation method of cyclohexanone oxime, and the preparation method comprises performing a hydrolysis reaction of 4 or less than 4 carbon atom containing oxime such as acetaldoxime, acetone oxime or butanone oxime and the like which is produced by an ammoxidation method and phosphoric acid added in a phosphate buffer solution to obtain an inorganic liquid containing hydroxylamine phosphate, then performing an oximation reaction of the inorganic liquid and cyclohexanone to obtain the high purity cyclohexanone oxime. According to the preparation method, due to the direct oximation reaction of the hydroxylamine phosphate and the cyclohexanone, the shortcoming that the cyclohexanone oxime prepared by the direct ammoxidation method is high in impurity content and is difficult to separate, and thus affecting the quality of caprolactam prepared from the cyclohexanone oxime can be overcomed; at the same time, the advantages of a plurality of processes for industrial production of the cyclohexanone oxime are combined, the inorganic liquid cycle can be realized, the high purity cyclohexanone oxime is prepared, the process cycle is realized, and the preparation method is conducive to energy saving and consumption reduction, and the realization of safe, environmentally friendly, low-cost and high-quality production.

Description

technical field [0001] The invention relates to a preparation method of an organic compound, in particular to a preparation method of cyclohexanone oxime. Background technique [0002] Cyclohexanone oxime is an important intermediate product in the production of caprolactam, which can be prepared by reacting hydroxylamine with cyclohexanone, or by other methods. The production process mainly includes hydroxylamine phosphate method, cyclohexanone ammoximation method, etc. [0003] 1. Hydroxylamine phosphate method (HPO method): at 60 o C. Use noble metals Pt and Pd supported on activated carbon as catalysts at 2.6 MPa, and use hydrogen to reduce nitrate in HPO buffer solution (called inorganic process solution in the device) in the hydroxylamine reactor to prepare hydroxylamine phosphate. Hydroxylamine phosphate and cyclohexanone are oximated in a pulse oximation reaction tower with toluene as a solvent to generate cyclohexanone oxime. This process does not generate ammoni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/44C07C249/12
Inventor 刘建青陈孚康
Owner 刘建青
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