Process method for preparing ethyl tert-butyl ether

A technology of ethyl tert-butyl ether and process method, which is applied in the direction of preparation of ether by addition of unsaturated compounds, ether preparation, chemical instruments and methods, etc., can solve the problems of activity reduction, poor stability, dissolution loss, etc., and achieve conversion rate High performance, good stability and easy operation

Active Publication Date: 2013-04-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage at present is the low activity
[0016] The heteropolyacid catalyst itself has low activity and poor stability, which limits its application
The lack of stability of heteropolyacid catalysts is mainly manifested in poor thermal stability, water solubility and alcohol solubility.
The thermal stability of heteropoly acid is not good, and it will slowly decompose at higher temperature, resulting in the loss of active components, and then the activity decreases; the alcohol solubility of heteropoly acid, in the reaction system containing alcohol, heteropoly acid will be dissolved and lost , thereby reducing the activity of

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0026] In the preparation process of the above-mentioned aluminum-based composite oxide, the reaction time is 2h-20h, preferably 4h-16h, most preferably 6h-12h. The drying temperature is 90°C-150°C, preferably 100°C-140°C, most preferably 110°C-130°C. The drying time is 4h-24h, preferably 6h-16h, most preferably 10h-12h. The calcination temperature is 400°C-800°C, preferably 450°C-700°C, most preferably 500°C-600°C. The calcination time is 8h-24h, preferably 8h-14h, most preferably 8h-12h.

[0027] The formed aluminum-based composite oxide support is impregnated in a heteropolyacid solution according to a conventional impregnation method. The immersion time is 4h-24h, preferably 4h-12h, most preferably 6h-12h. The impregnation is dried at 100°C-180°C for 4h-12h, preferably at 100°C-160°C for 6h-12h, most preferably at 100°C-120°C for 6h-8h. The impregnation is calcined at 250°C-550°C for 6h-24h, preferably at 300°C-500°C for 6h-12h, most preferably at 350°C-450°C for 8h-12...

Embodiment 1

[0030] A certain amount of aluminum nitrate and a certain amount of magnesium nitrate are prepared into an aqueous solution a, and deionized water and a certain amount of potassium hydroxide are used to prepare an aqueous solution b, and the solution b is added dropwise to a under normal temperature and stirring, and the reaction After 6 hours, a white paste precipitate was obtained, which was washed, filtered, and dried at 120°C for 10 hours, then extruded according to a conventional method, and then calcined at 500°C for 8 hours to obtain a magnesium-aluminum composite oxide carrier.

[0031] Dissolve phosphomolybdic acid in deionized water, immerse the above-mentioned shaped and roasted catalyst carrier in the heteropoly solution for 12 hours, dry the impregnated material at 110°C for 12 hours, and roast at 350°C for 8 hours to obtain the catalyst. The catalyst composition is shown in Table 1.

[0032] The etherification of isobutene and ethanol is carried out in a Φ18mm×12...

Embodiment 2

[0034] Other conditions are the same as in Example 1, except that the consumption of magnesium nitrate and phosphomolybdic acid is changed, the catalyst composition is shown in Table 1, and the reaction results are shown in Table 2.

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PUM

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Abstract

The invention provides a process method for preparing ethyl tert-butyl ether. The process method comprises the following steps of: taking isobutene and ethanol as raw materials, and using a heteropoly acid/aluminum-based complex oxide catalyst, wherein the heteropoly acid/aluminum-based complex oxide catalyst takes a complex oxide as a carrier and takes heteropoly acid as an active component, the complex oxide is one or more of aluminum-based complex oxides in MgO-Al2O3, TiO2-Al2O3 and ZrO2-Al2O3, and the heteropoly acid is one or more of phosphotungstic acid, silicotungstic acid, arsenotungstic acid, germanotungtic acid, phosphomolybdic acid, silicomolybdic acid, arsenomolybdic acid, germanomolybdic acid and the like. According to the process method provided by the invention, the catalyst adopting the aluminum-based complex oxide to load the heteropoly acid is adopted, so that the shortcomings of inactivation of the catalyst and reduced conversion rate, which are caused by easiness in damaging the Keggin structure of the heteropoly acid of the heteropoly acid catalyst, easiness in loss of acid amount and difficulty in separation, can be overcome.

Description

technical field [0001] The invention provides a process suitable for preparing ethyl tert-butyl ether (ETBE) through the etherification reaction of hydrocarbons and alcohols. technical background [0002] As gasoline additives, ethyl tert-butyl ether (ETBE) and methyl tert-butyl ether (MTBE) have a good blending effect, good chemical stability, can be miscible with hydrocarbon fuels in any proportion, and have excellent shock resistance performance. Moreover, the addition of ETBE and MTBE can reduce the emission of harmful gases such as CO and air pollution. Compared with MTBE, ETBE has a higher octane number and a lower vapor pressure. Therefore, gasoline added with ETBE can meet the requirements for use in hot and dry areas. At the same time, because the leakage of MTBE will cause certain water pollution problems, there is a tendency to limit its use. As one of the substitutes of MTBE, ETBE began to receive people's attention. [0003] The production process of ETBE is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/04C07C41/06B01J31/26B01J31/38
Inventor 霍稳周乔凯吕清林刘野李花伊田丹魏晓霞
Owner CHINA PETROLEUM & CHEM CORP
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