Preparation method of ethyl tert butyl ether

A technology of ethyl tert-butyl ether and ethanol, which is used in ether preparation, chemical instruments and methods, and unsaturated compound addition to prepare ether, etc., can solve the problems of difficult separation, easy loss of particles, and high reactivity, and achieve reactivity High performance, good stability and high catalyst activity

Active Publication Date: 2015-07-22
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0017] Aiming at the deficiencies in the prior art, the present invention provides a method for preparing ethyl tert-butyl ether (ETBE) through etherification and / or intermolecular dehydration with isobutylene and ethanol aqueous solution, which is characterized in that it uses cesium phosphotungstate acid salt (C S2.5 h 0.5 PW 12 o 40 ) As a catalyst, it overcomes the typical heteropolyacid phosphotungstic acid and its salt cesium phosphotungstic acid catalyst, which is easy to lose during use and the particles are too small, which makes separation difficult and difficult to use in fixed bed reactors. Disadvantages, continuous production is realized on a fixed bed reactor, high reactivity, easy recovery, and reusable

Method used

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Examples

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Effect test

preparation example Construction

[0025]The preparation method of the acid salt catalyst of the loaded cesium phosphotungstate used in the present invention comprises the following contents:

[0026] (1) Take the silica gel carrier and prepare cesium carbonate solution and phosphotungstic acid solution;

[0027] (2) Impregnating the silica gel carrier with cesium carbonate solution, then drying and roasting;

[0028] (3) The material obtained in step (2) is impregnated with phosphotungstic acid solution, then dried and calcined to obtain the final catalyst.

[0029] In the above catalyst preparation method of the present invention, the silica gel carrier can use common commercially available products, and can also be prepared according to conventional methods in the art. The amount of solute in cesium carbonate (cesium 133) solution and phosphotungstic acid solution is determined according to the amount of active components required by the final catalyst.

[0030] In the catalyst preparation method of the pr...

Embodiment 1

[0033] The acid salt of cesium phosphotungstate (C S2.5 h 0.5 PW 12 o 40 ) catalyst preparation method:

[0034] Using a two-step equal-volume impregnation method, take an appropriate amount of cesium carbonate (C S2 CO 3 ) was dissolved in deionized water, the carrier silica gel was immersed in the above solution, the sample was dried at 120°C, and baked at 350°C for 5 hours.

[0035] Quantitative phosphotungstic acid (H 3 PW 12 o 40 ) was dissolved in deionized water, and the above calcined sample was immersed in phosphotungstic acid solution, dried at 120°C, and calcined at 450°C for 4 hours to obtain catalyst A.

[0036] After XRD analysis, the active component of catalyst A is the acid salt of cesium phosphotungstate (C S2.5 h 0.5 PW 12 o 40 ), the content of active components in the catalyst is 38% by weight.

[0037] Change the amount of cesium carbonate and phosphotungstic acid, and keep other conditions unchanged, to obtain catalyst B, the mass content of...

Embodiment 2~15

[0039] The acid formula (C S2.5 h 0.5 PW 12 o 40 ) catalyst, used for the reaction of ethanol (or ethanol aqueous solution) and isobutene to prepare ethyl tert-butyl ether. The reaction is carried out in a Φ18mm×1200mm stainless steel fixed-bed reactor, and 30ml of the above-mentioned catalyst is loaded in the reactor, and the reaction The top and bottom of the reactor are respectively filled with quartz sand with a diameter of Φ0.5mm ~ 1.2mm. After the reactor is installed, it is replaced with nitrogen three times, and the airtight test is passed. The isobutylene, ethanol or ethanol aqueous solution is sent into the pre-reactor with a metering pump. heater. Examples 2-8 use catalyst A, and examples 9-15 use catalyst B. The reaction conditions and reaction results are shown in Table 1.

[0040] Table 1 Reaction conditions and reaction results of Examples 2-15.

[0041] serial number Raw material ethanol content / % Reaction pressure / MPa Reaction temperature / ...

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Abstract

The invention provides a preparation method of ethyl tert butyl ether. With isobutylene and ethanol as reaction raw materials and supported caesium phosphotungstate acidic salt as a catalyst, the ethyl tert butyl ether is prepared under the reaction conditions that liquid hourly volume space velocity of isobutylene is 0.5-5.0 / h, mole ratio of the ethanol to the isobutylene is (1.0-10.0):1, reaction temperature is 90-200 DEG C and reaction pressure is 2.0-6.0MPa. The preparation method provided by the invention adopts the supported caesium phosphotungstate acidic salt as the catalyst, the defect that the typical heteropolyacid phosphotungstic acid and caesium phosphotungstate acidic salt thereof are easy to run away in a using process, are difficult to separate as particles are too small and are difficult to be used on a fixed bed reactor is overcome, continuous production by virtue of a fixed bed is realized, reaction activity is high, the supported caesium phosphotungstate acidic salt is easy to recycle and can be repeatedly used, and a reaction process operation is easy, so that the preparation method provided by the invention is a new environment-friendly process.

Description

technical field [0001] The invention provides a method for synthesizing ethyl tert-butyl ether (ETBE) with isobutene and ethanol aqueous solution through etherification and / or intermolecular dehydration. 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/04C07C41/06B01J27/188
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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