Catalyst for oxidising oil purification gas condensate and oil fractions from mercaptan and method for its producing

FIELD: chemistry.

SUBSTANCE: invention covers the catalyst of purification of oil, gas condensate and oil fractions from mercaptan, namely to catalyst of oxidising sweetening of the specified products. The description of the new catalyst of oxidising alkali-free oil sweetening and the method for its producing are provided, which contains 1-5% of derivative transitional metal and 95-99% of layer aluminium silicate produced by application of cuprous chloride from ammonia containing water or water-alcohol solution on aluminum silicate from groups of illite or layer silicates.

EFFECT: improved catalyst for oxidising oil purification is produced.

2 cl, 2 tbl, 5 ex

 

The invention relates to catalysts for oil refining, gas condensate and oil fractions from mercaptans, particularly to catalysts of oxidative demercaptanization of these products. Removal of odorous, toxic and having corrosion activity of mercaptans is a necessary condition for the use of oil fractions as fuel or in the manufacture of chemical products. Currently, two approaches are used for the sweetening of petroleum products. The first of them is carrying out Hydrotreating (exhaustive catalytic hydrogenation) followed by conversion of the resulting hydrogen sulfide into elemental sulfur. This approach provides almost complete removal of sulfur from processed foods and is the most common. At the same time it is very expensive due to the use of expensive catalysts, which lifetime is limited and mnogostadiinost technologies, including catalytic hydrogenation, partial combustion of the hydrogen sulfide, the catalytic oxidation of hydrogen sulfide with sulfur dioxide (Claus process) and, finally, the direct catalytic oxidation of residual hydrogen sulfide in the so-called tails Claus process. So widespread is another method of removing mercaptans - oxidative demercaptanization (ODM) - catalytic oxidation with the formation of n is toxic and do not have a strong odor of organic disulfides:

2RSH+1/2O2→RSSR+H2About

Typically the oxidation is carried out with oxygen or air at room or elevated temperature in the presence of a homogeneous or heterogeneous catalyst based on a transition metal. Widespread, in particular, the so-called MEROX process developed by UOP. In the Tengiz oil field (Kazakhstan) implemented a similar process SSM-LCA-1, developed sue the VNIIUS (Russia, Kazan). At the same time, modern methods of SSM is not free from drawbacks, in particular, with the use of aqueous alkali, requiring a large number of sewage treatment and other complicating factors. The development of improved methods ODM remains an urgent task.

The number of known catalysts ODM, active only in the presence of aqueous alkali, in most of these catalytic compositions of the assumption of cobalt phthalocyanine (for example, European patent No. 394571, the Federal Republic of Germany patent No. 3008284 and others). Catalysts of this type provide a sufficiently complete removal of mercaptans. Their common disadvantage is the complexity of the technology associated with the need for a large number of additional operations - division of water-hydrocarbon mixtures, sewage treatment, etc. does Not solve the problem and use together with ftlot the Anino cobalt solid alkali (patent USSR No. 359786). In this case, the alkali gradually washed out of the catalyst, the water formed during the oxidation of mercaptans. In addition, this catalytic composition is hygroscopic and dangerous to handle.

Closer to the proposed technical solution are catalysts alkali free SSM.

Known catalyst ODM carried out by oxidation of the mercaptans oxygen chelate complex of the transition metal with bi-, tri - or tetradentate ligand containing at least one amide group (French patent 2573087)). Specific use of substituted 2-(alkyl(aryl, alkylaryl))-aminocarboxylic and other more complex compounds. As metal may be Co, Fe, Cu, Ni, Mn. The disadvantage is the low stability of the catalyst and the use for the manufacture of expensive and scarce components.

Known catalyst ODM obtained by processing the ion exchange resin copper salts (patent UK 167017). The disadvantage of the catalyst is small, the duration of continuous operation (1 volume of catalyst cleans without regeneration only from 40 to 400 volumes of petroleum products). An additional disadvantage is the complexity of regeneration, accompanied by the formation of waste water, and high temperature processing (recommended 90°).

Also known catalysts OD is - complexes of copper with tetracentron or tetracenomycin (French patent 2591610). Catalysts provide a high degree of purification, however, their practical use is unlikely because of the extreme high cost and scarcity of components.

Closest to the proposed decision is contained in European patent 0252853. According to the patent for the treatment of oil fractions in a stationary layer is proposed catalyst containing 0.05-5% chelate complex compounds of metal (according to the text, use porphyrinates and phthalocyanines, mainly cobalt), 5-35% of the pyrolysis of coal and 60-90% of an inorganic matrix is silica or aluminosilicate (including kaolin, montmorillonite, and so on). The disadvantage of this method is the complexity of the technology of preparation of the catalyst, due to the use of expensive components in the catalyst (phthalocyanines and porfirista) and the need to conduct the process with his participation at high pressure (up to 30 ATM, the recommended value is 10 ATM).

Unexpectedly been found that a catalyst containing 1-5% chloride copper (I) or copper (II) and 99.5 to 95% of the silicate from the group of hydrolog or layered silicates and received by application of an alcohol or water-alcohol solution containing ammonia in an amount of 5 to 25 wt.%, shows high activity in the ODM in the absence of alkali p and normal pressure in the temperature range 15-75° C. as alcohol may be used aliphatic alcohol C1-C5branched or unbranched, or aminoplast, such as monoethanolamine. Thanks to the invention eliminates the need for expensive phtalocyanine derivatives and process at high pressure. The goal is not achieved, if not met at least one of the above conditions, for example:

- if instead of chloride of copper using a different salt (nitrate, sulfate, stearate, etc.);

- if the media is used aluminosilicate, not belonging to the specified mineral groups (e.g., Muscovite), silica gel, etc.;

- if the application is made in the absence of ammonia from aqueous or alcohol solution of chloride of copper.

Thus, the subject invention is a new catalyst for oxidative alkali free sweetening of oil, gas condensate or oil fractions above composition obtained by the application of chloride of copper from ammonia-water or water-alcohol solution, and how to obtain it.

The invention is illustrated in examples 1-2. Comparative examples 3-5 illustrate the impossibility of achieving the objectives in the case of deviations of the catalyst defined in the formula of the present invention.

Example 1.

Preparation of catalyst

To 10 g of expanded vermiculite, washed twice with hydrochloric acid, add with stirring, 20 ml of 5% aqueous solution of chloride of copper (II)containing 9.5 wt.% of ammonia. The resulting mass is stirred at 50°C for 2 hours, and the sharp weakening of the staining solution. Then the mass is cooled, the catalyst is filtered off and washed twice with an excess of 96% ethanol and dried at 100°C in vacuum for 6 hours. Get the catalyst A. the Analysis shows the concentration of copper in the catalyst 3.5 wt.%. Similarly receive catalysts B-E. the Structure and parameters of the process of preparation of the catalyst is summarized in table 1.

Table 1
The catalysts of oxidative demercaptanization of petroleum fractions
Catalystthe content in the initial solution*, wt.%the content in the catalyst, %
wateralcoholammoniaCuthe aluminosilicate
And-- Ethanol 90.59.53.596.5 vermiculite
B40Ethanol 3525 2.597.5 vermiculite
* * *15Methanol 8051.099.0 vermiculite
G50Isopropanol 44.06.02.597.5 vermiculite
D30Isoamyl alcohol 65.05.0,2.7.97.3 montmorillonite
E10Ethanol 50153.097.0 vermiculite
Monoethanolamine 25
* - excluding chloride copper
** - used CuCl

Example 2.

Testing is carried out in the reactor column type with a height of 15 cm and a diameter of 1.1 cm catalyst Loading And 40, Through a bed of the catalyst at room temperature and normal pressure flow kerosene with the original content of mercaptan sulfur 0.03% (total sulfur content of 0.22%) with a bulk velocity 8 hour-1. Experience occurs within 140 hours. In the beginning of the experiment the content of mercaptan sulfur output is 0.0004% (4 ppm)after 140 hours of 0.001% (10 ppm). Thus, the dissolved oxygen in these conditions is s enough to achieve satisfactory cleaning from mercaptans. Similarly conduct experiments with catalysts B-E. the results of the experiments are presented in table 2. You can see that all the catalysts in accordance with the invention also provide a sufficiently high quality.

25
Table 2
The results of experiments on the sweetening of oil, petroleum fractions and gas
CatalystThe cleaned oilFeed rate, h-1Temperature, °The content of mercaptan sulfur, ppm
In the sourceOutput after 140 hours of work
Andkerosene82230010
Bkerosene8403006
Bthe condensate62533010
Bcrude oil67545010
Inkerosene62530012
Gkerosene1230010
Dkerosene4.5253008
Ekerosene12253006
Ethe condensate8253308

Below are the results of the comparative experiments, showing the impossibility of achieving the goal without using the entire set of techniques proposed in the invention.

Example 3.

The process is conducted as in example 2, but the preparation of the catalyst used instead of expanded vermiculite processed similarly the mineral Muscovite. Through 10 hours after the start of the content of mercaptan sulfur in the reactor exit is 50 ppm, kerosene acquires a bluish colour, which signifies the washing away of metal from the catalyst.

Example 4.

The process is conducted as in example 2, but instead of copper chloride in the preparation of the catalyst used sulphate of copper (II). After 50 hours of operation the concentration of mercaptan sulfur in the reactor exit is 40 ppm, 10 h 220 ppm.

Example 5.

The process is conducted as in example 2, but the preparation of the catalyst using an aqueous solution of chloride of copper, not containing ammonia. 50 the speakers work, the concentration of mercaptan sulfur output is 25 ppm, over 140 hours 90 ppm.

1. Catalyst for oxidative demercaptanization oil containing 1-5% of a derivative of a transition metal and 95-99% of layered silicate structure, characterized in that as the derivative of the transition metal is used chloride of copper (I) or copper (II)associated in a complex with ammonia, and the silicate mineral group hydrolog or layered silicates, and the application of chloride of copper is produced from an alcohol or water-alcohol solution.

2. The method of preparation of the catalyst according to claim 1, characterized in that the catalyst is obtained by applying the chloride copper containing ammonia or alcohol or water-alcohol solution, the alcohol use aliphatic linear or branched alcohol C1-C5and/or aminoplast, and the concentration of ammonia is 5-25 wt.%.



 

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