Method of obtaining tertiary ethyl butyl ether

Method for the preparation of tertiary alkyl ethers; ₇ LOG US # * -._____________________________________________

9W / mo, c

Summary

Preparation process tritotagoy alkylether of from iso-olefins and aliphatic-economic aklodles presence of catalyst DPO THY form sulfonated styrene-tdivinylovenzoliou resins, characterized in that tdson the reaction forming the tertiary alkyl ether, dsou and d separating the tertiary alkyl ether of from hydrocarbons and their · Associations that do not accompany it, It is carried out on a flat disk fractionator and in which some of the disks are equipped with catalyst beads suitable for it. of the ether is derived from ter-alkyl ether, while the ether obtained is purely, substantially, removed from the base.

Method for the preparation of tertiary alkyl ethers

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This invention relates to a process for the preparation of tertiary alkyl ethers of isoolefins and aliphatic aldehydes.

Especially. The invention relates to the preparation of methyl tert-butyl ether or methyl tert-amyl ether from isobutylene and methanol or isoamylene or carimethahydrate respectively.

The following description will be omitted for the sake of simplification. in the preparation of methyl-tert-butyl ether, but the method is also fully applicable to the preparation of all other tert-alkyl ethers, provided that the differences between the boiling points of the ingredients and the products are of the same order of magnitude.

Methyl-tert-butyl ether (MTBX) is prepared, according to the known technique, by equilibrium reaction, which is generally contained in varying percentages of hydrocarbon fractions 0_a, with methane in the presence of a suitable catalyst, which yields sulfonated styrene-divylbenzene resins, at a temperature which may range from the usual temperature up to about 10 ° C.

In practice, isobutane is not available on an industrial scale and therefore will not be referred to the above case of hydrocarbon fraction containing isobutane

The reaction is a two-way reaction and when either the amount of methanol used approaches the stoichiometric, or the conversion of the bovine is 90% or more at temperatures that give a reasonable reaction rate.

When greater conversions are required, excess methanol should be used and this should be separated from the reaction and recycled in the event that conversions are reached at approximately greater than 95 ° C. the reaction must be separated and the residual mixture undergoes a second reaction step, and again, under almost stoichiometric conditions it allows conversion of about 99%.

* However, there is a problem that this work is indispensable to evaporators.^y two reactors used '

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Cy stamped, two nipples ^AH , KH

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6tis of distillation so as to increase the investment and operating costs. ^?The most up-to-date technique (Eurobian Patent published June 19, 1980, no. 8860) indicates a method for overcoming the above-mentioned problems with the supply of a mixture containing isobutene and methanol containing methanol also to distillation, so as to form MTBE and separate MTBE from CL components at the same time.

However, the method described in the foregoing patent has a number of serious disadvantages associated with the fact that the catalyst will act or refill the distillation column and thereby meet specific requirements. For this reason it is used in bag-forming bags, which leaves plenty of room for the vapor and liquid passages, but it is difficult, however, to prepare and place them in the bag.

The method described in the aforementioned European patent also has the disadvantage that the continuous phase in the interior of the column is represented by the gas phase, while the dispersed phase is either the liquid phase, the inertial phase, or the driving phase. practically in the gas phase.

These guides also have the potential to form significant amounts of dimers because there is a lack of alcohol in the gas phase.

It has now been found, surprisingly surprisingly, that all the aforementioned disadvantages can be avoided by the realization of the reaction which leads to the formation of a terminal alkylation (MTBE) by both In a single fractional distillation apparatus in which some disks are provided with catalyst beds in the form of styrofoam-stearoyl-dibutyl sulfide resin-based pellets, suitable for all.

* The method according to the present invention comprises: feeding the ydrogonanthrakonj load containing equal-olefinr, to fractional distillation column in which certain ^ DPA discs are provided with beds of catalyst apoteloumefou DPA resins soulfonomefou styrene-divinylbenzene and separated or DPA Group fractionation trays or DPA d wealth discs fractionation; feed, of alcodel, single, near the top of the column, preferably above the last catalytic bed and partial disks (between 4 and 8) below where refueling is performed; reaction of iso-olefin with alcodine on the disks which are supplied which are immersed in the liquid containing the alcohol and through which it passes, the vapor bubbles and the separation of the ether produced from the other components in the fractionation trays and in the like ether, and as a top product the hydrocarbons being fed and possibly an alkodel in the form of azeotrope with the hydrocarbons being fed. &lt;- /

The method according to the present invention in the case of MTBE, comprising: supplying water to the water;

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- 3 cargo containing isobutene in a fractional distillation column, in which some of the discs are provided with catalyst beds, which are free of styrene sulfonyl dioxide fractionation trays; or simple fractionation trays; near the top of the column and preferably above the catalytic bed and between 4 and 8 disks below where the isobutene is refluxed or refluxed with methanol as well as methanol. and those which are immersed in methanol containing methanol and through which the bubbles of steam pass through and separate the MTBE produced from the other components in the mixture; to obtain substantially pure MTBE bottom and hydrocarbon peaks, the various isobutene and methanol adducts in an amount analogous to azeotropic.

The process according to the present invention comprises a pressure of between 500 and 1000 KPa.

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The hydrocarbon load containing the iso-olefin is fed to the columns according to the discs according to the invention in such a way that at least two disks containing catalytic cathodes are present on top of each other. This is the power supply. The vapors produced by the braids in the fractional distillation column pass through the bubbles through the catalytic beds, which are preferably not less than three, and either methanol and isobutyric acid or hydrogen sulfide.

the catalyst is in the form of beads between 0.5 and 1 mm in diameter, and the thickness of each catalyst bed is in the order of 1 meter.

The condenser present in each disc comprising the catalyst flows into the lower distillation disc from one or more conventional barriers, and the catalyst is always immersed in the condenser.

The catalyst is held in each tray by the fact that it contains a lattice at least at the base and top of the bed, thereby preventing it from escaping.

The invention will be more pronounced with the appendix design which represents a non-limiting embodiment thereof.

The reference number I indicates the fractional distillation disks and the integers 2 a d, a fractional distillation disc containing catalytic cyclin 3 or which is retained by the lattice 4 and 5, respectively. passing through the catalytic bed. The fog follows the upper path showing arrow 7.-A non-limiting embodiment of the method according to the invention is described below. -&gt; /. Zf-W

Example

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Manufacture of a distillation column with sections of tubes with flanges 10 cm in diameter and 100 cm in length, and containing six distilled bubble distillation trays (two biscuits per disc).

* The column is manufactured by swapping parts of tubes filled with a catalyst and parts containing six trays to obtain a total of half portions above the feed and two portions below the feed. The column is fed with 2 KGR / H 0 ^. containing 50% of isobutene.

1: 1 reflux is maintained and 575 g of methanol is fed with reflux. The operating pressure is 800 ° C and the operating temperature is 60 -50 ° C. The top product consists of 1035 ORs containing 30 GR of methanol and 5 GR of equimolar. As a bottom product, 154-0 GR MTBE is obtained practically pure.