The method of hydrogenation of the olefin fractions c6-c20

 

Usage: petrochemistry. Carry out the hydrogenation of olefin fractions With6-C20obtained in the oligomerization of olefins in the liquid phase in one or more parallel and/or sequential reactors with stationary katalysatoren on Nickel-containing catalyst hydrogen-containing gas at elevated temperature and pressure with the return of up to 90 wt.% hydrogenated feed is separated into the original fraction olefins. The fraction of olefins and hydrogen-containing gas is fed into the lower part of the reactor by ozonation hydrogen-containing gas through a fraction of the olefins, the temperature hydrogen-containing gas does not exceed 20oC. Technical result: increased conversion of the hydrogenation process. 2 C.p. f-crystals, 3 tab., 6 Il.

The invention relates to the petrochemical industry, to obtain saturated oligomers of olefins that can be used as solvents, or high-octane vysokotochnoye additives in fuel, components, lubricants and so on.

Famous article, A. Huseynova, describing the process of hydrogenation of propylene oligomers (G. A. Huseynov. The study of the process of hydrogenation of propylene oligomers with the aim of gaining the process of hydrogenation of propylene oligomers at various industrial catalysts.

But in the described method, hydrogenation on Nickel-containing catalyst at temperatures as low as 165oSince there is a partial destruction of the oligomer, decreases the viscosity of the product. Further, the temperature of hydrogenation contributing to a deterioration of destruction.

A method of obtaining saturated oligomers (Application EP 989106, IPC C 07 C 9/00, publ. 29.03.2000 g), including the state of oligomerization With3-C5olefins on postinoculation catalyst with subsequent hydrogenation of at least part of the flow of oligomers containing paraffins and olefins, hydrogenation catalyst, such as Ni/Al2O3with the formation of saturated oligomers; returning at least part of the flow of saturated oligomers in the oligomerization zone.

The disadvantage of this method is recycling the saturated oligomers in the oligomerization zone, which causes additional costs for the recycling of the reaction product, and not a high conversion of the hydrogenation process.

The known method of gas-phase hydrogenation of olefins on the catalyst (Application Germany 19719833, IPC C 07 C 5/03, publ. 19.11.98). Gas-phase hydrogenation of liquid mixtures containing more than 50% With6-C20-olefins, carried out with hydrogen or speciously with temperature above the boiling olefins at a pressure of injection of the catalyst, containing Nickel and silicon, with 30-50oWith 0.2-2 MPa.

The disadvantage of this method is the need of overheating olefins to a temperature exceeding the temperature of its boiling point, which leads to increased energy consumption, and high enough conversion of the hydrogenation process.

The closest in technical essence is a method for isoparaffin hydrocarbon solvent (Patent Poland 153558, IPC C 07 C 5/03, publ. 31.10.91) by catalytic hydrogenation of the fraction of oligomers of propylene with 423-523 To, a pressure of 1-3 MPa and space velocity of the raw material of 0.2-2 h-1(based on catalyst) hydrogen gas (H2more than about 90. %) with a flow rate of 100-500 liters per 1 l of raw materials. Used in the hydrogenation catalyst with a content of 40-50% metallic Nickel, 0.5 to 1.0% zinc oxide and 0.5 to 1.0% barium oxide, deposited on a natural silicate or a mixture of silicon oxide, treated with nitric acid. Hydrogenation of oligomers of propylene is carried out in several stages (for example, in a flow reactor) with a return to 90% of the finished product in raw materials and/or in the reactor.

The disadvantage of this method is not sufficiently high conversion of the hydrogenation process.

The objective of the proposed izobretatele oligomerization of olefins.

To solve this problem is proposed a method of hydrogenation of the olefin fractions With6-C20obtained in the oligomerization of olefins carried out in the liquid phase in the flow reactor at a Nickel catalyst the hydrogen-containing gas at elevated temperature and pressure with the return of up to 90 wt. % hydrogenated feed is separated into the original fraction olefins, and the fraction of olefins and hydrogen-containing gas is fed into the lower part of the reactor by ozonation hydrogen-containing gas through a fraction of the olefins, the temperature hydrogen-containing gas does not exceed 20oWith and hydrogenation is carried out in one or more parallel and/or sequential reactors with a stationary catalyst.

The hydrogenation product supplied in original fraction olefins may contain unreacted hydrogen.

Possible fractional flow of hydrogen containing gas into the reactor hydrogenation 30-50% of the total number of hydrogen containing gas is served in the middle part of the reactor, 50-70% in the lower part of the reactor.

The process of hydrogenation using a hydrogen-containing gas, the temperature of which does not exceed 20oWith, in several catalytic zones allows the hut is the combination of all features allows you to achieve the desired result.

Hydrogenation of the olefin fractions With6-C20obtained in the oligomerization of olefins, e.g. ethylene and propylene, can be electrolytic hydrogen or hydrogen-containing gas, for example, metabodrene fraction from ethylene production following composition,%: hydrogen - 90,0-99,0; methane - 1,0-10,0; moisture - 1.0 ppm, or another hydrogen-containing fraction.

The hydrogenation can be carried out in one reactor, with several catalytic zones, divided inert material, or in reactors, connected in series or parallel-sequentially (i.e., two reactors arranged in parallel, and both of them the product stream is served in the third reactor, and so on). Between catalytic zones possible additional cooling. The process of hydrogenation is carried out at a temperature of 60-300oC and a pressure of 0.2 to 4.0 MPa.

Perhaps the original fraction olefins fed to the hydrogenation, be diluted with a solvent. As the solvent used recycle the product of hydrogenation, nefras, hexane or a mixture thereof.

All of the above is illustrated by the following examples.

Example 1 Raw - hexene (propylene dimers) is mixed with a hydrogenation product containing neproreagirovavshimi two layers of catalyst Nickel on kieselguhr (TU 38-101396-89). Between the layers is filled with the catalyst carrier T-8 (TU 480-1-406-79). At the same time in the reactor serves the hydrogen-containing gas with a temperature not exceeding 20oWith ethylene production following composition,%: hydrogen - 95,2; methane - 4,8; oxygen - OTS.; nitrogen - OTS.; moisture - 1.0 ppm (Fig.1).

The process of hydrogenation is carried out at a temperature of 70oC, 0.5 MPa, the space velocity of the raw materials 1,0 h-1. The ratio of raw materials: hydrogen withstand equal to 1:120.%. The hydrogen-containing gas is fed into the lower part of the reactor by ozonation hydrogen-containing gas through the original fraction. The product of hydrogenation - hexane is cooled and collected in a receiver and analyzed by gas chromatography using a chromatograph "Crystal 2000", on silica column Packed with the sorbent CE-30. The indicator "bromine number" define standard bromate-bromanil method. 90 wt.% hydrogenated feed is cut back to the original fraction is fed to the hydrogenation.

Obtained during the hydrogenation product can be used as a solvent in the manufacture of synthetic rubbers, as an additive in fuel.

The results of the experiment are presented in table.1.

Example 2 the Experience carried out in the conditions of example 1, but Bogorodsk the middle part of the reactor (Fig.2).

The results of the experiment are presented in table.1.

Example 3 the Experience carried out in the conditions of example 1, but the hydrogenation serves HEXEN-1 (trimer of ethylene, THE 38-602-09-28-91) in solvent hexane (50 wt.% hexene-1 and 50 wt.% hexane). The hydrogenation is conducted electrolytic hydrogen. Hydrogen is fed to the hydrogenation of fractional - 50% of the total taken of hydrogen is served in the lower part of the reactor, 50% in the middle part of the reactor (Fig. 2).

30 wt.% hydrogenated feed is cut back to the original fraction is fed to the hydrogenation.

Obtained during the hydrogenation product can be used as a solvent in the manufacture of synthetic rubbers, as an additive in fuel.

The results of the experiment are presented in table.1.

Example 4 the Experience carried out in the conditions of example 1, but the hydrogenation serves HEXEN-1 (trimer of ethylene TU 38-602-09-28-91) in a solvent containing 50 wt.% nefras 65/75 and 50 wt.% section of hydrogenated feed - hexane (50 wt.% hexene-1 and 50 wt.% solvent).

The hydrogenation is carried out in two serially connected reactors with intermediate cooling of the product between the reactors (Fig.3). 30 wt.% hydrogenated feed is cut back to the original fraction is fed to the hydrogenation.

The results of the experiment are presented in table.1.

Example 5 the Experience of the wire is wt.% nefras 65/75 and 50 wt.% section of hydrogenated feed - hexane.

The hydrogenation is carried out in two parallel reactors (Fig.4), the hydrogen-containing gas is fed into the lower part of the reactor. 50% hydrogenated feed is cut back to the original fraction is fed to the hydrogenation.

Obtained during the hydrogenation product can be used as a solvent in the manufacture of synthetic rubbers, as an additive in fuel.

The results of the experiment are presented in table.1.

Example 6 the Experience carried out in the conditions of example 1, but the hydrogenation serves HEXEN-1 (trimer of ethylene TU 38-602-09-28-91) and hydrogenation is carried out in three reactors, two of which operate in parallel, with subsequent cooling of the intermediate product and its delivery in the third reactor (Fig.5). 5% hydrogenated feed is cut back to the original fraction is fed to the hydrogenation.

Obtained during the hydrogenation product can be used as a solvent in the manufacture of synthetic rubbers, as an additive in fuel.

The results of the experiment are presented in table.1.

Example 7 the Experience carried out in the conditions of example 6, but the hydrogenation serves fraction C12olefins (tetramer propylene, THE 38-101260-77). 90% of the hydrogenated feed is cut back to the original fraction is fed to the hydrogenation.

Hydrogenation hydrogenation process, the product can be used as a solvent in the manufacture of synthetic rubbers, as an additive in the fuel in the production of synthetic oils.

The results of the experiment are presented in table.2.

Example 8 the Experience carried out in the conditions of example 1, but the hydrogenation serves fraction of olefins With20(propylene pentamers THAT 2411-020-05766801-94) in hexane (10 wt. % fraction of olefins With20and 90 wt.% hexane) and the hydrogenation is carried out in four reactors, two of which are parallel to the obtained intermediate product is cooled and served in the third and then the fourth reactor (Fig.6). 30% hydrogenated feed is cut back to the original fraction is fed to the hydrogenation.

Obtained during the hydrogenation product can be used as a solvent in the manufacture of synthetic rubbers, as an additive in the fuel in the production of synthetic oils.

The results of the experiment are presented in table.3.

As can be seen from the presented examples, the proposed method allows for the hydrogenation of olefin fractions C6-C20with high conversion and get the products that are used as solvents, high-octane fuel additives, bases for light oils.

Claims

1. The method of hydrogenation of the olefin fractions With6-C20With and hydrogenation is carried out in one or more parallel and/or sequential reactors with a stationary catalyst.

2. The method of hydrogenation of the olefin fractions With6-C20under item 1, characterized in that the initial fraction of olefins serves hydrogenation product containing unreacted hydrogen.

3. The method of hydrogenation of the olefin fractions With6-C20on PP.1 and 2, characterized in that the hydrogen-containing gas is fed to the hydrogenation of fractional 50-70% of the total number of hydrogen containing gas is served in the lower part of the reactor, 30-50% in the middle part of the reactor.

 

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FIELD: regeneration of heat and extraction of impurities.

SUBSTANCE: the invention is pertaining to the method of regeneration of heat and extraction of impurities from the area of the heat-producing reaction in the fluidized flow, conducted for conversion into light olefins of oxygenates present in the flow of the oxygenate (oxygen-containing) raw. raw. The offered method includes the new system of a two-stage quick chilling intended for extraction at the first stage of water from the outgoing from the reactor flow and regeneration of heat of this flow for the purpose, at least, of the partial evaporation of the raw flow due to indirect heat-exchange between the oxygenated raw and the flow of the upper product of the first stage or the flow of recirculation of the first stage. The flow of purification being withdrawn from the first stage, contains the large share of impurities and the high-boiling oxygenates. In the second stage besides conduct extraction of water from the products flow containing light olefins, and produce the flow of the purified water, which requires only the minimum evaporation of the water for production of the water flow of the high degree purification. The method allows to concentrate the impurities in a rather small flow and ensures the significant saving of power and money resources at production of a flow of the vaporous raw guided into the area of realization of the heat-exchange reaction in the fluidized flow.

EFFECT: the invention ensures concentration of the impurities in a rather small flow and the significant saving of power and money at production of the flow of the vaporous raw directed into the area of realization of the heat-exchange reaction in the fluidized flow.

19 cl, 3 tbl, 4 dwg, 5 ex

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