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Anthraquinone degradation product regeneration catalyst and preparation method thereof

A technology for regenerating catalysts and anthraquinone degradation products, which is applied in physical/chemical process catalysts, quinone preparation, chemical instruments and methods, etc., can solve the problems of low regeneration efficiency, difficult separation and recovery, and the stability of aromatic tertiary amines needs to be investigated. To achieve the effect of high regeneration efficiency, saving production cost and long service life

Inactive Publication Date: 2012-10-17
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this catalyst has fewer types of renewable degradation products, low regeneration efficiency, and is not easy to separate and recover, and the stability of aromatic tertiary amines remains to be investigated under harsh anthraquinone hydrogenation and oxidation conditions.

Method used

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  • Anthraquinone degradation product regeneration catalyst and preparation method thereof
  • Anthraquinone degradation product regeneration catalyst and preparation method thereof
  • Anthraquinone degradation product regeneration catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Step A: take by weighing 54.53g Mg(NO 3 ) 2 ·6H 2 O, 89.43g hexamethylenetetramine and 0.70g SDBS were dissolved in 40mL deionized water to form a mixed solution. Wherein the molar ratio of magnesium ions to hexamethylenetetramine is 1:3, and the molar concentration of SDBS is 0.05 mol / L.

[0029] Step B: Add 20g Al 2 o 3 Carrier (spherical carrier prepared by the rolling ball method, the crystal form is γ type, the diameter is 5mm, and the specific surface area is 190m 2 g -1 , the pore volume is 0.85cm 3 / g, crushing strength is 138N / grain) was added to the mixed solution, reacted in the autoclave at 150°C for 6h, took out the sample, washed to pH=7~8, dried at 85°C for 5h to obtain hydrotalcite MgAl-CO 3 -LDHs / Al 2 o 3 Precursor, calcined at 550°C for 4h to obtain 30wt.%MgO / Al 2 o 3 Sample, wherein the mass percentage of MgO is 30wt.%.

[0030] After determination, the specific surface area of ​​the spherical regenerated catalyst is 147m 2 / g, the pore v...

Embodiment 2

[0036] Step A: take by weighing 56.72g Be(NO 3 ) 2 ·3H 2 O, 37.93g Al(NO 3 ) 3 9H 2 O, 91.05g urea and 0.54g SDS were dissolved in 40mL deionized water to form a mixed solution. where the molar ratio Be 2+ : Al 3+ =3, the molar ratio of beryllium ions to urea is 1:5, and the molar concentration of SDS is 0.05mol / L.

[0037] Step B: Add 20g Al 2 o 3 Carrier (spherical carrier prepared by the rolling ball method, the crystal form is γ type, the diameter is 4mm, and the specific surface area is 202m 2 g -1 , the pore volume is 1.15cm 3 / g, crushing strength is 128N / grain) was added to the mixed solution, reacted in the autoclave at 120°C for 8h, took out the sample, washed to pH=7, dried at 90°C for 5h to obtain hydrotalcite BeAl-CO 3 -LDHs / Al 2 o 3 Precursor, calcined at 550°C for 4h to obtain BeO / Al 2 o 3 sample. Wherein the mass percentage of BeO is 20wt%.

[0038] It has been determined that the specific surface area of ​​the spherical regenerated catalyst i...

Embodiment 3

[0043] Step A: take by weighing 13.01g Ca(NO 3 ) 2 4H 2 O, 13.23g Mg(NO 3 ) 2 ·6H 2 O, 21.92g urea and 0.58g CTAB were dissolved in 40mL deionized water to form a mixed solution. where the molar ratio of Ca 2+ : Mg 2+ =1:1, the molar ratio of divalent metal ions to urea is 2:7, and the molar concentration of CTAB is 0.04mol / L.

[0044] Step B: Add 20g Al 2 o 3 Carrier (a spherical carrier prepared by the oil column molding method, the crystal form is γ-type, the diameter is 2.2mm, and the specific surface area is 181m 2 g -1 , the pore volume is 1.01cm 3 / g, crushing strength is 119N / grain) was added to the mixed solution, reacted in the autoclave at 130°C for 6h, took out the sample, washed to pH=7, dried at 80°C for 5h to obtain hydrotalcite CaMgAl-CO 3 -LDHs / Al 2 o 3 Precursor, calcined at 550°C for 4h to obtain the total mass of CaO and MgO in the final product CaO-MgO / Al 2 o 3 A sample with a mass fraction of 20wt.%.

[0045] After measurement, the specif...

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Abstract

The invention provides an anthraquinone degradation product regeneration catalyst and a preparation method thereof. MeO / Al2O3 represents the anthraquinone degradation product regeneration catalyst, wherein MeO represents an alkaline oxide; a crystal form of Al2O3 is a gamma form; Al2O3 crystals are in shapes of balls, strips and whitetip clover; a mass percent of MeO is in a range of 1 to 60wt%; a specific surface area of MeO / Al2O3 is in a range of 100 to 300m<2>.g<-1>; a pore volume is in a range of 0.3 to 1.5cm<3>.g<-1>; and compressive strength is in a range of 50 to 150N / particle. The preparation method comprises the following steps of synthesizing a hydrotalcite MeAlCO3-LDH / Al2O3 precursor on surfaces of Al2O3 carriers and in channels of the Al2O3 carriers and carrying out calcination at a temperature of 500 to 600 DEG C to obtain the anthraquinone degradation product regeneration catalyst. The anthraquinone degradation product regeneration catalyst which is an alkaline composite oxide can be used for regeneration of an anthraquinone working solution used in an anthraquinone process-based hydrogen peroxide preparation industry and has a stable regeneration period of 6 to 20 months. Compared with the existing regeneration catalyst used industrially, the anthraquinone degradation product regeneration catalyst has a service life prolonged by 2-3times and higher regeneration efficiency.

Description

[0001] Field [0002] The invention relates to an anthraquinone degradation product regeneration catalyst and a preparation method thereof. The basic aluminum oxide composite oxide can be used for the regeneration of anthraquinone degradation product in an anthraquinone process hydrogen peroxide working solution. Background technique [0003] Hydrogen peroxide (H 2 o 2 , commonly known as hydrogen peroxide) is an important inorganic chemical raw material and fine chemical product, widely used in textiles, papermaking, organic synthesis and environmental protection and other fields. The anthraquinone method is the current industrial production of H 2 o 2 main method. 2-Ethylanthraquinone (EAQ) is dissolved in an organic solvent to make a working solution, and the working solution is in the load-type Pd / Al 2 o 3 EAQ hydrogenation wherein is converted into 2-ethylhydroanthraquinone (EAQH) under the effect of catalyst such as 2 ), then in pure O 2 or EAQH under the action ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/02B01J23/06C07C50/18C07C46/00
CPCY02P20/584
Inventor 李殿卿郭子添冯俊婷冯拥军
Owner BEIJING UNIV OF CHEM TECH
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