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Method for simply synthesizing gamma-Al2O3 and use thereof in ethanol dehydration

A simple, aluminum alkoxide technology, applied in chemical instruments and methods, hydrocarbon production from oxygen-containing organic compounds, organic chemistry, etc., can solve problems such as complex processes or devices, difficult to remove, wide pore distribution, etc., to achieve good activity and The effect of selectivity, good activity and selectivity, uniform pore size distribution

Inactive Publication Date: 2011-04-27
CHINA PETROCHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the difference in preparation methods, the alumina carrier used in industry often has a wide range of pore distribution, which has an adverse effect on the transmission of reaction materials and the selection of reaction products.
[0004] The preparation methods of alumina are mainly divided into the following types: the first is the acid method, that is, the neutralization reaction of aluminum salt and alkali, the raw materials used are aluminum trichloride, ammonia water, etc., a hydrogenation method disclosed in patent ZL94107295.9 The preparation method of the catalyst carrier, which prepares activated alumina after neutralizing the acidic aqueous solution containing aluminum ions and the alkaline aqueous solution containing or not containing aluminum ions; the patent CN03101176. Ammonium oxalate or ammonium citrate, etc. are used as raw materials, heated and concentrated to form aluminum hydroxide precipitate, dried and heated to decompose and remove the NH in it 4 Cl, the obtained solid powder is converted into γ-Al by roasting at 400-800°C for 3-6 hours 2 o 3 , which saves the process of filtration and washing, but the chlorine ions are introduced into the raw materials used, so that the product purity is not high, and it will also have an adverse effect on the ethanol dehydration reaction
[0005] The second is the alkaline method, that is, the neutralization reaction of aluminate and acid. The aluminates used are mainly sodium metaaluminate and potassium metaaluminate, and the acids used include nitric acid, sulfuric acid, hydrochloric acid and carbon dioxide. CN98110593. 9 discloses a method for preparing activated alumina using metaaluminate-carbon dioxide as a raw material, which is the alkaline method, but when the pH value is controlled below 9.5, fraidonite (NaAl(OH) 2 CO 3 ), insoluble in water and difficult to remove, although the pH value can be controlled below 9.5 in the disclosed method of CN02120772.0, it needs to control the gelling temperature and residence time to ensure that no franitonite is produced, and the device is complicated
[0008] Summarizing the methods proposed before, most of the preparation steps are many, the cycle is long, the process or device is complicated, the preparation process is demanding, and if it is not handled properly, Na + 、K + and SO 4 2- , Cl - etc., making the catalyst purity not high, thus affecting its catalytic ethanol dehydration performance

Method used

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  • Method for simply synthesizing gamma-Al2O3 and use thereof in ethanol dehydration
  • Method for simply synthesizing gamma-Al2O3 and use thereof in ethanol dehydration
  • Method for simply synthesizing gamma-Al2O3 and use thereof in ethanol dehydration

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Experimental program
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Effect test

Embodiment 1

[0033] Weigh 36.75g Al(NO 3 ) 3 9H 2 O, set the volume to 250ml, make a 0.6mol / L solution, use 6mol / L urea aqueous solution as precipitant, add Al(NO 3 )3 9H 2 In O solution, adjust the pH to 8-9. After the precipitation is completed, the slurry is stirred at room temperature for 0.5 h, filtered, and the filter cake is dried overnight at 120 ° C, and then calcined in a muffle furnace at 600 ° C for 4 h to obtain γ- al 2 o 3 . 30~50 mesh γ-Al 2 o 3 1.5g of catalyst is loaded into the constant temperature section of the fixed-bed reactor, and the rest is filled with quartz sand. -1 N 2 The bed temperature was raised to 350°C under the air flow rate, and then the 92wt% ethanol solution was added for 0.6h -1 The mass space velocity is injected into the system, and the generated gas and liquid are sampled and analyzed. The results are shown in Table 1.

Embodiment 2

[0035] Weigh 91.88g of aluminum isopropoxide, set the volume to 250ml, make a 1.5mol / L solution, stir at room temperature and add 5mol / L precipitant NH 3 ·H 2 O solution, adjust PH=8~9, after the precipitation is completed, stir the slurry at room temperature for 1h, filter, wash until pH=7, dry the filter cake at 120°C overnight, then place it in a 600°C muffle furnace for calcination for 4h , to get γ-Al 2 o 3 . 30~50 mesh γ-Al 2 o 3 1.5g of catalyst is loaded into the constant temperature section of the fixed-bed reactor, and the rest is filled with quartz sand. -1 N 2 The bed temperature was raised to 380°C under the gas flow rate, and then the 92wt% ethanol solution was added for 1.2h -1 The mass space velocity is injected into the system, and the generated gas and liquid are sampled and analyzed. The results are shown in Table 1.

Embodiment 3

[0037] Weigh 36.75g Al(NO 3 ) 3 9H 2 O, dilute to 250ml, make a 0.6mol / L solution, and use 6mol / L NH 3 ·H 2 O is a precipitant, adding Al(NO 3 ) 3 9H 2 In the O solution, adjust the pH to 8-9. After the precipitation is completed, the slurry is stirred at room temperature for 2 hours, filtered, and the filter cake is dried at 120°C overnight, and then calcined in a muffle furnace at 600°C for 6 hours to obtain γ-Al 2 o 3 . 30~50 mesh γ-Al 2 o 3 1.5g of catalyst is loaded into the constant temperature section of the fixed-bed reactor, and the rest is filled with quartz sand. -1 N 2 The bed temperature was raised to 400°C under the air flow rate, and then the 92wt% ethanol solution was added for 5h -1 The mass space velocity is injected into the system, and the generated gas and liquid are sampled and analyzed. The results are shown in Table 1.

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Abstract

The invention discloses a method for simply synthesizing Gamma-Al2O3, and application thereof in ethanol dehydration. The method for synthesizing Gamma-Al2O3 comprises the steps that aluminum salt and de-ionized water are prepared into a 0.5mol / L to 1.5mol / L solution; while stirring, a precipitating agent solution is added into an aluminum salt solution in a dropwise manner till the pH value of the aluminum salt solution is 7 to 9; then the solution is stirred at room temperature for 0.5h to 2h, and the precipitate is filtered and dried at the constant temperature of 80 DEG C to 120 DEG C for 6 hours to 12 hours and then ground; and powder obtained by grinding is calcined at the temperature of 450 DEG C to 700 DEG C for 2 hours to 6 hours. The catalyst of the invention has simple preparation with little time consumption, high purity as well as narrow and uniform pore diameter distribution, being beneficial to the transportation of reaction materials and the selection of reaction products; and the catalyst has good activity and selectivity for preparing ethylene by ethanol dehydration.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a simple and rapid synthesis of γ-Al 2 o 3 method, and the γ-Al 2 o 3 Application of catalytic ethanol dehydration to ethylene. Background technique [0002] Ethylene is the most important basic raw material in the petrochemical industry, and it is also the chemical with the largest output in the world. The development level of the ethylene industry represents the overall development level of a country's petrochemical industry. In industry, it is mainly used to synthesize polyethylene, ethylbenzene, ethylene oxide, dichloroethane, oligomers, etc. In addition, ethylene also has important applications in medicine and agriculture. Utilizing renewable biomass resources to produce ethanol and further dehydrating it into ethylene, that is, the development of bio-ethylene technology, has become an important content of the petroleum substitution strategy and a current rese...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/30C07C1/24C07C11/04B01J21/04
CPCY02P20/52
Inventor 黄和李慧胡燚苏国东成源海胡耀池索红波
Owner CHINA PETROCHEMICAL CORP
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