Device and method for preparing cyclohexenyl cyclohexanone

A technology for preparing cyclohexenyl cyclohexanone and a device, which is applied in the field of preparation of cyclohexenyl cyclohexanone with high selectivity, and can solve the problem of selectivity decline, increased chance of by-products, and single-pass conversion rate of cyclohexanone No high problems, to achieve the effect of reducing wastewater discharge

Inactive Publication Date: 2009-12-30
江苏华派新材料科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As the reaction proceeds, the concentration of moisture and product cyclohexenyl cyclohexanone in the system increases constantly, and the high water concentration increases the reverse reaction rate, so the single-pass conversion rate of cyclohexanone is not high; the product cyclohexenyl cyclohexanone in the system The increase of ketone concentration

Method used

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  • Device and method for preparing cyclohexenyl cyclohexanone
  • Device and method for preparing cyclohexenyl cyclohexanone
  • Device and method for preparing cyclohexenyl cyclohexanone

Examples

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Embodiment 1

[0029] exist figure 1Coupling of cyclohexanone condensation and separation to prepare cyclohexenyl cyclohexanone The tower kettle is 1000L, heated with electricity; the inner diameter of the tower is Φ300mm, the separation section is filled with high-efficiency wire mesh corrugated packing, and the height is 3m; the reaction separation section has a total of 10 The first sieve plate is equipped with a catalyst frame on the 1st, 3rd, 5th, 7th, and 9th sieve plate from top to bottom. The catalyst frame is made of a 1mm thick perforated plate with an outer diameter of Φ290mm and a frame height of 8cm. The plate is 3cm, and the downcomer is 12cm high. Each frame is equipped with a catalyst package, and the catalyst package contains 1kg of phosphotungstic acid solid acid catalyst supported by 20-40 mesh activated carbon, and 5kg of catalyst is installed in five frames. Add 700 kg of cyclohexanone into the 1000 L tower kettle 1, and heat it to boiling under normal pressure. A liqu...

Embodiment 2

[0033] The same device as in Example 1, a catalyst bag is housed in each frame, and 20-40 mesh cationic resins are loaded with FeCl in the catalyst bag. 3 0.5kg of solid acid catalyst, 2.5kg of catalyst in five frames, and other conditions are the same.

[0034] After the reaction, the heating was stopped, and the gas chromatographic analysis was adopted for sampling and the condensation product was composed of: 3.0% cyclohexanone, 96.15% cyclohexenyl cyclohexanone, 0.85% polycondensate, and about 96.5% cyclohexanone single-pass conversion rate. The reaction selectivity is 98.8%, and the purity of cyclohexenyl cyclohexanone after direct distillation of the condensation product reaches 99.7%.

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Abstract

The invention relates to a device and a method for preparing cyclohexenyl cyclohexanone as an intermediate of o-phenylphenol. The device comprises a column bottom 6, a tower reactor 5, an all-reflex condenser 1 and an oil-water separator 2, wherein the reactor 5 consists of a reaction separation section 3 and a separation section 4; a catalyst bag is placed in a catalyst frame on a tower plate of the reaction separation section 3 of the tower separator, cyclohexanone in the column bottom is heated and steamed out and enters the tower plate of the reaction separation section 3 through the separation section 4 to form a liquid layer so that the catalyst in the catalyst frame is immersed in the cyclohexanone liquid, cyclohexanone undergoes a condensation reaction under the action of the catalyst to generate cyclohexenyl cyclohexanone and water, the cyclohexenyl cyclohexanone leaves the reaction section and moves towards the lower part of the tower under the separation action of the tower plate, and finally enters the column bottom, the generated water and cyclohexanone are steamed out together from the top of the tower and undergo phase splitting in the oil-water separator after being condensed. The once-through conversion of the cyclohexanone can reach over 95 percent and the selectivity of the cyclohexenyl cyclohexanone can reach over 98 percent.

Description

technical field [0001] The present invention relates to a preparation device and method of cyclohexenyl cyclohexanone, an intermediate of o-phenylphenol, in particular to a method for preparing cyclohexenyl cyclohexanone with cyclohexanone as a raw material with high conversion rate and high selectivity Preparation method and device thereof. Background technique [0002] O-phenylphenol (OPP) is a fine chemical and organic intermediate with a wide range of uses. It can be used as antiseptic, antifungal agent, broad-spectrum fungicide, used for fruit preservation, cosmetics, wood preservation, and household, public places, Disinfection of swimming pools and hospitals, it can also be used to produce oil-soluble o-phenylphenol formaldehyde resins, non-ionic emulsifiers, synthetic dyes, water-based cutting fluids, etc. Agents and intermediates of flame retardant polymer materials, etc. At present, cyclohexanone is mainly used as raw material at home and abroad, and the intermed...

Claims

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Application Information

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IPC IPC(8): C07C45/74C07C49/613
Inventor 曾崇余张银华钱菊玲游本刚
Owner 江苏华派新材料科技有限公司
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