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Preparation method and application of a high-efficiency organosulfur hydrolysis and deoxidation multifunctional catalyst

A catalyst and organic sulfur technology, which is applied in the field of organic sulfur hydrolysis conversion catalysts, can solve the problems of poor thermal stability, low hydrolysis activity, and low organic sulfur conversion efficiency, and achieve high thermal stability, wide use temperature, and excellent deoxidation performance.

Active Publication Date: 2020-05-19
江苏天东新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Not only overcomes the low-temperature catalytic CS of industrial hydrolysis catalysts 2 Low hydrolysis activity, low conversion efficiency of total organic sulfur, easy sulfation poisoning at high temperature and poor thermal stability, and by adjusting the alkalinity of the catalyst and introducing additives, the catalyst can be used at a wider temperature, while reducing CO 2 Influence on Hydrolysis Performance of Organosulfur

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Prepare AlCl with a concentration of 0.3mol / L 3 and ZrOCl 2 mixed solution, control AlCl 3 with ZrOCl 2 The molar ratio of the former is 20:1, and the ethanol solution with a molar concentration of 0.5% polyethylene glycol 20000 is added, and the volume ratio of the former to the latter is controlled to be 5:1, and after being hydrolyzed at 50°C for 2 hours under the condition of stirring, Aged for 40 hours to obtain a gel, then dried at 100°C for 7 hours, and baked in a microwave oven at 650°C for 1 hour to obtain the first Al 2 o 3 -ZrOCl 2 The carrier powder is ready for use;

[0032] (2) preparation volume concentration is the ethanol solution of tetrabutyl titanate of 10%, then adds the Al prepared in step (1) 2 o 3 -ZrOCl 2 powder, fully stirred for 30 minutes, prepared an aqueous solution of acetic acid with a volume concentration of 10%, and added dropwise to the ethanol solution of tetrabutyl titanate under stirring conditions, and controlled the vo...

Embodiment 2

[0039] (1) Prepare AlCl with a concentration of 0.4mol / L 3 and ZrOCl 2 mixed solution, control AlCl 3 with ZrOCl 2 The molar ratio of the former is 22:1, and the ethanol solution with a molar concentration of 0.6% polyethylene glycol 20000 is added, and the volume ratio of the former to the latter is controlled to be 4:1, after hydrolysis at 40°C for 2.5h under stirring conditions , aged for 30 hours to obtain a gel, then dried at 102°C for 6 hours, and baked in a microwave oven at 630°C for 2 hours to obtain the first Al 2 o 3 -ZrOCl 2 The carrier powder is ready for use;

[0040] (2) preparation volume concentration is the ethanol solution of tetrabutyl titanate of 12%, then adds the Al prepared in step (1) 2 o 3 -ZrOCl 2 Powder, fully stirred for 25 minutes, prepared an aqueous solution of acetic acid with a volume concentration of 15%, added dropwise to the ethanol solution of tetrabutyl titanate under stirring conditions, and controlled the volume ratio of the eth...

Embodiment 3

[0047] (1) Prepare AlCl with a concentration of 0.5mol / L 3 and ZrOCl 2 mixed solution, control AlCl 3 with ZrOCl 2 The molar ratio is 25:1, and the ethanol solution with a molar concentration of 0.7% polyethylene glycol 20000 is added, and the volume ratio of the former to the latter is controlled to be 4:1. After hydrolysis at 30°C for 3.0h under stirring conditions , aged for 25 hours to obtain a gel, then dried at 105°C for 5 hours, and baked in a microwave oven at 600°C for 3 hours to obtain the first Al 2 o 3 -ZrOCl 2 The carrier powder is ready for use;

[0048] (2) preparation volume concentration is the ethanol solution of tetrabutyl titanate of 15%, then adds the Al prepared in step (1) 2 o 3 -ZrOCl 2 powder, fully stirred for 20 minutes, prepared an aqueous solution of acetic acid with a volume concentration of 20%, and added dropwise to the ethanol solution of tetrabutyl titanate under stirring conditions, and controlled the volume ratio of the ethanol solut...

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PUM

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Abstract

The invention provides a preparation method of an efficient organic sulfur hydrolysis and deoxygenation multifunctional catalyst. The preparation method comprises the following steps: preparing a mixed solution of AlCl3 and ZrOCl2; adding an ethanol solution of polyethylene glycol and carrying out hydrolysis; carrying out microwave roasting to obtain Al2O3-ZrOCl2 powder; adding the Al2O3-ZrOCl2 powder into an ethanol solution of tetrabutyl titanate into the Al2O3-ZrOCl2 powder; adding an acetic acid solution and reacting; carrying out the microwave roasting to obtain Al2O3-ZrOCl2-TiO2 powder; preparing a mixed solution of KOH, K2CO3 and first active auxiliary agent soluble salt and adding the Al2O3-ZrOCl2-TiO2 powder; carrying out ultrasonic impregnation and roasting a mixture in by microwaves to obtain first powder; adding the first powder into a second auxiliary agent soluble salt solution into the first powder; carrying out the ultrasonic impregnation and carrying out the microwave roasting to obtain semi-finished-product catalyst powder; after uniformly mixing the semi-finished-product catalyst powder, a binding agent, a pore-forming agent and water, carrying out the microwave roasting to obtain the efficient organic sulfur hydrolysis and deoxygenation multifunctional catalyst. The efficient organic sulfur hydrolysis and deoxygenation multifunctional catalyst provided by the invention has the advantages of high conversion ratio, good thermal stability and long service life.

Description

technical field [0001] The invention belongs to an organic sulfur hydrolysis conversion catalyst, in particular to a preparation method and application of an organic sulfur hydrolysis conversion and deoxidation catalyst in feed gas. [0002] technical background [0003] Gases such as coal-based synthesis gas, coke oven gas, natural gas and smelting dry gas contain a large amount of organic sulfides. When used in industrial production, organic sulfides may lead to the deactivation of subsequent synthesis catalysts, resulting in a decline in industrial yield. Therefore, in the conversion and utilization or discharge process of the above-mentioned gases, the organic sulfur in the gas must be converted and removed to meet the environmental protection requirements of the subsequent synthesis or discharge. The sulfur in the feed gas is usually more than 90% H 2 S, the content of organic sulfur is generally less than 10%, and organic sulfides are mainly COS, CS 2 And a small amo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J32/00B01J21/06B01J27/135B01J23/78B01J23/34B01J23/89B01J23/887B01J37/02B01J37/03B01J37/08B01J37/34B01D53/86B01D53/48C10K1/00C10K1/34C10L3/10
CPCB01D53/48B01D53/86B01D53/8603B01D53/8606B01J21/066B01J23/002B01J23/34B01J23/78B01J23/8873B01J23/8877B01J23/8993B01J27/135B01J37/0205B01J37/0207B01J37/0213B01J37/036B01J37/088B01J37/343B01J37/349B01J2523/00C10K1/002C10K1/004C10K1/34C10L3/101C10L3/103B01J2523/31B01J2523/47B01J2523/48B01J2523/13B01J2523/17B01J2523/842B01J2523/3706B01J2523/3712B01J2523/55B01J2523/72B01J2523/25B01J2523/68B01J2523/828B01J2523/847B01J2523/22B01J2523/27B01J2523/845
Inventor 丁晶晶吴伟杨丽萍陈井凤于慧芳牛玉杰
Owner 江苏天东新材料科技有限公司
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