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Reactor for preparing hydroanthraquinone and preparation method of hydroanthraquinone

A technology of hydrogen anthraquinone and reactor, which is applied in the field of hydrogen peroxide preparation by anthraquinone method, can solve the problems of low utilization rate of catalyst, low yield of anthraquinone hydrogenation, slow velocity of liquid through fluidized bed, etc., so as to improve selectivity and Effects of utilization rate, reduction of diffusion resistance, and reduction of catalyst dosage

Pending Publication Date: 2021-06-08
NANJING UNIV OF TECH +1
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  • Abstract
  • Description
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Problems solved by technology

Usually the hydrogenation reaction occurs at the interface of the gas-liquid-solid three-phase. The supported palladium catalyst is a structure similar to an eggshell. Part of the palladium invades the pores of the carrier and cannot be fully utilized. Only the palladium on the surface of the carrier can Utilization, and the hydrogenation reaction in the form of a fixed bed is subject to the influence of gravity, the velocity of the liquid through the fluidized bed is slow, and the catalyst liquid film is relatively thick, which is not conducive to the full contact reaction of the gas-liquid-solid three-phase, and the catalyst filling in the fixed bed involves catalyst molding and loading Form, easy to form interstitial flow, this kind of fixed-bed hydrogenation in the form of trickle flow has low gas-liquid-solid mass transfer efficiency, and requires a hydrogen-rich environment, which can easily lead to deep hydrogenation of anthraquinone, resulting in serious degradation of anthraquinone and reduced yield ; And increasing the space velocity will inevitably lead to a low conversion rate per pass, which determines the two major shortcomings of the hydrogenation reaction in the form of a fixed bed in the production of hydrogen peroxide by the anthraquinone method:
[0006] 1. A hydrogen-rich environment is required to maintain hydrogenation efficiency, but it is easy to reduce the yield of anthraquinone overhydrogenation, and it is difficult to control the depth of hydrogenation;
[0007] 2. The generated hydroanthraquinone easily leads to an increase in the viscosity of the working fluid, thick catalyst liquid film, and poorer gas-liquid-solid three-phase mass transfer effect, resulting in low catalyst utilization (the quality of anthraquinone converted by a unit catalyst per unit time is expressed in g EAQ / ( g h) meter)
[0009] When using a loop reactor for the preparation of hydroanthraquinone, due to the use of powder catalyst, factors such as catalyst density and liquid injection speed will affect the distribution ratio of the catalyst in the reactor and circulation pipeline, thus affecting the selection of effective hydroanthraquinone sex and utilization

Method used

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  • Reactor for preparing hydroanthraquinone and preparation method of hydroanthraquinone
  • Reactor for preparing hydroanthraquinone and preparation method of hydroanthraquinone
  • Reactor for preparing hydroanthraquinone and preparation method of hydroanthraquinone

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Effect test

preparation Embodiment A

[0056] Weigh the metered gas phase method SiO 2 Add the powder (silicon dioxide prepared by the gas phase method) into a custom-made glass container, and after evacuating for 1 hour, add a certain volume of the above-mentioned PdCl 2 Solution (SiO 2 The amount of powder added and PdCl 2 The amount of solution added is Pd: SiO 2 The mass ratio metering, controlled in Pd:SiO 2 For (0.1-0.3): 100, stirring and impregnating adsorption, stirring and impregnating adsorption, using 0.5mol / L sodium hydroxide solution to adjust pH = 9, reducing formaldehyde in a water bath at 80°C, and filtering and washing with ultrapure water until the end of the reduction The resistivity of the liquid is greater than or equal to 0.1MΩ·CM, and the filter cake is dried in a vacuum drying oven at 50°C, and the bulk density is 0.062-0.165g / cm3 when tested by a Scott density meter 3 .

preparation Embodiment B

[0058] According to the method of embodiment A, gas phase method SiO 2 Change to Al 2 o 3 , all the other operating methods are the same as in Example A, and the bulk density is 0.894g / cm through the Scott density meter test 3 .

[0059] Example of Venturi Injector Size Screening

[0060] In the loop reactor of 5L (reactor volume 5L), add the EAQ working solution of 3kg 15% (the preparation of this working solution is as follows: heavy aromatics: trioctyl phosphate: 2-methylcyclohexyl acetate mass ratio is 70 :20:10 to prepare a mixed solution, add EAQ to the mixed solution to form an EAQ working solution, the mass concentration of EAQ in the EAQ working solution is 15%), add the Pd / SiO prepared by the catalyst preparation embodiment A 2 Catalyst powder (bulk density 0.083g / cm 3 ) is 1% of the mass of EAQ, where Pd:SiO 2=0.15:100, feed nitrogen into the reactor through the air inlet until the system pressure is 1MPa to vent and replace, and so cycle three times, nitrogen...

Embodiment 1

[0066] In the loop reactor of 5L (reactor volume 5L), add the EAQ working solution of 3kg 15%, add the Pd / SiO that catalyst preparation embodiment A prepares 2 Catalyst powder (bulk density 0.062g / cm 3 ) is 0.5% of the mass of EAQ, where Pd:SiO 2 =0.1:100, feed nitrogen into the reactor through the air inlet until the system pressure is 1MPa to vent and replace, so that the cycle is three times, and the nitrogen is switched to a hydrogen-nitrogen mixture (H 2 :N 2 =1:1) Fill the reactor to the reaction pressure of 0.3±0.05MPa, turn on the circulation pump to make the liquid in the kettle flow slowly, raise the temperature to the preset reaction temperature of 40°C (heating time is about 15min), adjust the circulation pump 4 to the flow rate of 60m / s, recorded as the reaction start time. During the reaction, the temperature of the connected reactor was controlled to be 40±1°C. After reacting for 3 hours, immediately reduce the flow rate of the circulation pump 4 and rapidl...

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Abstract

The invention discloses a reactor for preparing hydroanthraquinone and a preparation method of hydroanthraquinone. The reactor comprises a reaction kettle, a circulating pump, a heat exchanger and a Venturi ejector, the Venturi ejector comprises an inlet section, a nozzle, a mixing section and a diffusion section which are communicated in sequence; the inlet section and the nozzle are in a reducing pipe type; the ratio of the inner diameter of an inlet section opening to the inner diameter of a nozzle to the inner diameter of an air chamber closing opening to the length of a mixing section to the length of a diffusion section of the Venturi ejector is 34: (2-5): (3-6): (30-60): (600-1000); and the opening angle of the diffusion section is 10-25 degrees. According to the present invention, the specification and the size of the reactor are optimized, such that the mass transfer process of the reaction is effectively enhanced, the catalyst liquid film thickness is reduced, the conversion from EAQ to EAQH2 can be achieved with low hydrogen partial pressure and low catalyst consumption, the hydrogenation depth is effectively controlled, and the selectivity and the utilization rate of the effective anthraquinone by the catalyst are significantly improved.

Description

technical field [0001] The invention belongs to the field of anthraquinone method for preparing hydrogen peroxide, and in particular relates to a method for catalytically hydrogenating 2-ethylanthraquinone (EAQ) to 2-ethylhydroanthraquinone (EAQH2) by adopting a new type of reactor equipment—a loop reactor method. Background technique [0002] The process of preparing hydrogen peroxide by anthraquinone method is mainly composed of the following steps. First, 2-ethylanthraquinone (EAQ) is dissolved in a specific solvent to form a working fluid. The EAQ dissolved in the solvent has a pressure of 0.3Mpa and a temperature of 40- At 70°C, hydrogenation reaction occurs in the presence of a hydrogenation catalyst to obtain hydroanthraquinone (EAQH 2 ), passing oxygen-containing gas into the hydrogenated working solution can make hydroanthraquinone (EAQH 2 ) is re-oxidized to anthraquinone (EAQ). Meanwhile, during the hydrogenation reaction, EAQH 2 will be further hydrogenated t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J8/18C07C45/62C07C49/675C01B15/023
CPCB01J8/18B01J8/1836B01J8/1809B01J8/1818C07C45/62C01B15/023C07C2603/24C07C49/675
Inventor 於德伟梅华
Owner NANJING UNIV OF TECH
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