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Device for preparing fluorenone by means of liquid phase oxidation and preparation method thereof

A liquid-phase oxidation method and the technology of fluorenone, which are applied in the preparation of carbon-based compounds, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of increasing equipment, large amount of solvent and catalyst, and inability to carry out the reaction, so as to avoid Caking and clogging, easy control of fluorene oxidation reaction, sufficient effect of fluorene oxidation reaction

Active Publication Date: 2013-03-13
WUHAN RUIKAIXING SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the fluorene oxidation reaction in Comparative Document 1 is better, the fluorene oxidation reaction is an exothermic reaction, and a large amount of heat is released during the reaction. If it is not taken away in time, it will seriously affect the progress of the reaction; it adopts a jacket to pass cooling water to take away the heat , if there is a large temperature difference between the cooling water temperature and the material temperature, due to the high freezing point of the reaction material, it will inevitably lead to material caking on the tower wall. Carried out in different equipment, whi

Method used

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  • Device for preparing fluorenone by means of liquid phase oxidation and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] like figure 1 A device for preparing fluorenone by liquid-phase oxidation method is shown, including reactor 1, static mixer 2, material circulation equipment 3 and hot water circulation equipment 4, and the volume in static mixer 2 is about the same as that of reactor 1 About 1 / 10 of the internal volume, the reactor 1 is provided with a stirrer 5, the top of the reactor 1 is provided with a feeding port 11, a solvent inflow pipe 12, a vacuum input pipe 13 and a thermometer 15, and the bottom of the reactor 1 is provided with Outlet pipe 14, water bath 6 is arranged on the outside of the bottom of reactor 1, jacket 7 is arranged on the outside of static mixer 2, material circulation equipment 3 comprises material output pipe 31, material input pipe 32 and circulation pump 33, material output pipe 31 is connected with the bottom of the reactor 1 and the bottom of the static mixer 2, the material input pipe 32 is connected with the top of the reactor 1 and the top of the ...

Embodiment 2

[0023]The method for preparing fluorenone with the device of Example 1, after opening the vacuum input pipe 13, 40kg dimethyl sulfoxide and 0.55kg catalyst (sodium hydroxide or potassium hydroxide, etc.) are imported into the reactor 1 from the solvent inflow pipe 12 , close the vacuum input pipe 13, and then put 50kg of industrial fluorene into the reactor 1 from the feeding port 11, so that the fluorene, dimethyl sulfoxide and catalyst are dissolved and mixed into materials, and the hot water circulation equipment 4 is opened, and the steam input pipe 91 Input steam, let the water temperature in the water tank 9 be about 50~75 ℃, the temperature is controlled by the temperature control meter 94 on the water tank 9, when the water temperature is too high, input normal temperature water from the supplementary water input pipe 92 to cool down, and then use the hot water pump 43 Let the hot water circulate between the water tank 9-hot water output pipe 41-water bath 6 and the jac...

Embodiment 3

[0025] It is basically the same as Example 2, except that the consumption of industrial fluorene is 250kg, the consumption of dimethyl sulfoxide is 200kg, the consumption of catalyst is 2.5kg, and the flow rate of industrial oxygen is 6m 3 / hr, the fluorene cycle oxidation reaction time is 4 hours, and the yield of fluorene into fluorenone is above 99.7%.

[0026] The ratio of fluorene consumption and dimethyl sulfoxide consumption in embodiment 2 and embodiment 3 also can be 1: 0.9, 1: 1.0 or 1: 0.7 etc.; The ratio of fluorene consumption and catalyst consumption also can be 1: 0.013 or 1 : 0.015, etc., and 1: 0.03, 1: 0.05, 1: 0.08KG 1: 0.1, etc.; the fluorene cycle oxidation reaction time can also be 5 hours or 2.5 hours, etc., which are not listed here.

[0027] Dimethyl sulfoxide in Example 2 and Example 3 can also be replaced by other solvents.

[0028] Embodiment 2 and embodiment 3 compare with the reaction parameter of comparative document 1 and comparative document 2...

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Abstract

The invention discloses a device for preparing fluorenone by means of liquid phase oxidation and a preparation method thereof. The device comprises a reactor and a static mixer. The volume in the static mixer is less than the volume in reactor; the upper part of the reactor is provided with a feed inlet and a solvent inflow pipe; the bottom of the reactor is provided with a discharge pipe; the lower part of the reactor is provided with water bath; the static mixer is externally provided with a clamp sleeve; material recycle equipment is arranged between the reactor and the static mixer; the material recycle equipment front the static mixer is provided with am oxygen input pipe; and the water batch and the clamp sleeve are provided with hot water recycle equipment. The device has the advantages that oxygen is better contacted with the material and is better distributed; the fluorine oxidation reaction is complete; the inner part of the reactor can be prevent from being accumulated by the material and blocked, etc. The method can use less usage of the solvent and the oxygen when oxidizing the fluorine with the same weight, save the cost of raw material, improve the yield coefficient of the fluorine, reduce energy consumption, and decrease exhaust emission.

Description

technical field [0001] The invention relates to the preparation of fluorenone, in particular to a device for preparing fluorenone by a liquid-phase oxidation method and a preparation method thereof. Background technique [0002] Fluorenone, also known as benzophenone, has a molecular weight of 180.21 and is a yellow orthorhombic crystal with a melting point of 84°C and a boiling point of 341.5°C. It is an important fine chemical raw material. As early as the 1930s to 1950s, foreign countries have studied fluorenone in dyes, medicines, pesticides, etc., mainly using fluorenone as raw material to synthesize monomers or derivatives containing fluorene structure, which are used for modification or synthesis. Polymer materials (such as epoxy resin, polyester, polycarbonate and polyimide containing fluorene structure) are widely used in high-tech fields such as aerospace, non-silver photosensitive materials for synthetic electronic photography, medicine And pesticide intermediate...

Claims

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Application Information

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IPC IPC(8): C07C49/675C07C45/36
Inventor 邱孟杰姜琦张兴耀
Owner WUHAN RUIKAIXING SCI & TECH