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INVENTION
Patent of the Russian Federation RU2141503
METHOD OF PRODUCTION OF LOW-FORGED PETROLEUM PRODUCTS
The name of the inventor: VN Kasterin; Kasterin K.V.
The name of the patent owner: Kasterin Vladimir Nikolaevich
Address for correspondence: 103001, Moscow, B.Patriarshy per 8, ap. 42, Kasterinu VN.
Date of commencement of the patent:
Use: petrochemistry. Essence: petroleum distillates are subjected to catalytic hydrodewaxing in the presence of a catalyst containing high-silica zeolite, hydrogenating components, a binder. The dewaxed product is stabilized to obtain the dewaxed catalyst, the desired product. The initial petroleum distillate is subjected to catalytic hydrodewaxing in a mixture with a stabilized dewaxed distillate, the desired product taken in an amount of 5-95% by weight of the original distillate. Preferably, the catalytic hydrodewaxing is subjected to an initial distillate in a mixture with a stabilized dewaxed catalyst, the desired product and additionally a straight-run gasoline fraction of HK-62 ° C, in an amount of up to 10% by weight of the mixture. Catalytic hydrodewaxing is carried out at a temperature of 280-420 ° C, a pressure of 3-10 MPa, a hydrogen-containing gas: raw material ratio of 200-1500 nm 3 / m 3 . The technical result is that the method allows to increase the regeneration cycle of the catalyst operation, improve the quality of the target product, and increase its yield.
DESCRIPTION OF THE INVENTION
The invention relates to oil refining, in particular to methods for producing low-hardening oils, hydraulic fluids, diesel, aviation fuels and other types of low-hardening petroleum products.
Processes for preparing low-hardening products using hydrocracking processes of hydrocarbon feedstocks in which the hydrocracking product is subjected to separation and distillation with recycling of the distillate products to be mixed with the feedstock are known. Thus, in the method of Pat. US 3,617,508, 71, a distillation residue is sent for recirculation, in the process according to the patent. US 3,775,297, 71, aimed at simultaneous production of gasoline and naphthenic lubricating oils, the distillate gas oil and residual fractions are recycled.
Disadvantages of these methods consist in the complexity of the technological schemes associated in the first method with the need to wash the hydrocracking product with water and drying the hydrogen-containing gas, in the second, using a special pre-treatment of the cracking catalyst. In addition, recycling in this case solves the problem of increasing the conversion of raw materials, and the conversion of high-boiling hydrocarbons belonging to different classes. At the same time, recirculation leads to an increase in the concentration of high-boiling hydrocarbons in the hydrocracking reactor, which entails stricter process conditions, a decrease in the regeneration period of the catalyst.
At present, the most effective methods for obtaining low-hardening petroleum products are processes using the catalytic hydrodewaxing of petroleum feedstocks using catalysts based on high-silica zeolites.
There are known methods for producing low-hardening petroleum products, carried out in several stages using a catalytic hydrodewaxing step carried out in the presence of a catalyst based on high-silica zeolites. For example, a combination of hydrocracking and catalytic hydrodewaxing steps is known (European application EP 0189648, 86) for the production of rocket and distillate fuels, a combination of hydrotreating steps, catalytic hydrodewaxing and hydrotreating (RU 2047648, 95) to produce an insulating oil component; Combination of alternating hydrotreatment processes and catalytic hydrodewaxing in one reactor (RU 2034903, 95); A combination of hydrocracking steps, catalytic hydrodewaxing, post-treatment (WO 97/18278, 97).
All these methods are characterized by multi-stage.
Processes for the preparation of low-hardening petroleum products by catalytic hydrodewaxing using catalysts based on high-silica zeolites are known, conducted in a single step in which the catalysts used have a certain characteristic (EP 0279180, 88, international application WO 91/15120.91).
Closer to the process described is a method for producing low-hardening petroleum products by catalytic hydrodewaxing of petroleum distillates in the presence of a catalyst containing a mixed multivalent form of the high-silica zeolite, hydrogenating components, a binder at a temperature of 260-380 ° C, a pressure of 4-5 MPa, 6 h -1 , hydrogen: feedstock ratio of 500: 1500 (RU 2109792, 98).
The disadvantage of the method lies in the insufficiently long inter-regeneration cycle of the catalyst operation, the reduced yield of the target product, and in limited opportunities to achieve the low-temperature properties of petroleum products required by the relevant specifications.
The object of the invention is to increase the inter-regeneration cycle of the catalyst operation, improve the quality of the target product, and increase the yield of the desired product.
This object is achieved by the described method for producing low-hardening petroleum products by catalytic hydrodewaxing of petroleum distillates in the presence of a catalyst containing high silica zeolite, hydrogenating components, a binder in which the catalytic hydrodewaxing is subjected to a feed distillate in a mixture with a stabilized dewaxed catalyst, the desired product, in an amount of 5-95mas. % Of the original distillate. Preferably, the catalytic hydrodewaxing is subjected to an initial distillate in a mixture with a stabilized dewaxed catalyst, the desired product and additionally a straight-run gasoline fraction of HK-62 ° C, taken up to 10 mas. % Of the mixture. Preferably, the catalytic hydrodewaxing is also carried out at a temperature of 280-420 ° C, a pressure of 3-10 MPa, a hydrogen-containing gas: raw material ratio of 200-1500 nm 3 / m 3 .
The distinctive features are that the catalytic hydrodewaxing is subjected to the initial distillate in a mixture with the stabilized dewaxed catalyst, the desired product taken in the above amount, and under the preferred process conditions.
The method described is as follows. The oil distillate is mixed with a hydrogen-containing gas in a hydrogen-containing gas: raw material ratio of 200-1500 Nm 3 / m 3 , heated to a temperature of 280-420 ° C and at a pressure of 3-10 MPa is fed to a reactor containing a catalyst containing high silica zeolite, hydrogenating components, binder , On which selective cracking of n-alkanes, which degrade the low-temperature properties of petroleum fractions, is carried out. The resulting catalyst is stabilized sequentially by separating the gaseous products from the liquid phase and distilling the liquid phase by means of which the low-boiling fractions are separated from the desired ones, achieving the fractional composition, flash point and other quality parameters that limit the content of low-boiling fractions in the desired products with the appropriate normative and technical documents. The resulting stabilized dewaxed catalyst, the desired product is partially recycled for mixing with the feed distillate and catalytic hydrodewaxing, is subjected to the initial distillate in a mixture with a stabilized dewaxed catalyst, the desired product taken in an amount of 5-95mas. % Of the original distillate. The remainder of the desired product is sent to the product park for mixing with various additives and other commodity components. Hydrodewaxing of petroleum fractions is characterized by exceptional selectivity due to the nature of catalysts used in the process, including high silica zeolites, such as pentasil-type zeolites, which have a sieve action and selectivity with respect to n-paraffin conversion. In this dewaxing process, the catalyst plays the role of the separating device, selectively adsorbing and then converting the n-paraffins. Recycling of a part of the target product to the dewaxing process allows to reduce the concentration of n-paraffins in the feedstock, which makes it possible to carry out the process in a more "soft" regime, which creates conditions for increasing the selectivity of the process-increasing the yield of the target product.
Using recirculation of the stabilized target product of the hydrodewaxing process allows reducing the content of n-alkane hydrocarbons in the feed to the reactor, so the degree of conversion required is reduced.
Due to the "milder" process conditions, in order to achieve the desired conversion of n-alkane hydrocarbons, all other conditions being equal, the required process temperature is lower in the described process than in the case of the known process, or at the same process temperatures, the bulk feed rate of the process is higher.
Using milder conditions of the process, an increase in the regeneration cycle of the catalyst operation is achieved, and the course of side reactions of cracking of iso-alkane hydrocarbons decreases, thereby increasing the yield of the desired product. Under equal conditions for hydrodewaxing, the low-temperature properties of the product obtained by the described method are much higher than those known, which makes it possible to obtain products of a new, better quality. The process of catalytic hydrodewaxing is accompanied by the formation of a certain amount of hydrocarbon gases, as well as light gasoline fractions that reduce the yield of the target products and are by-products of the process, which, depending on the general technological scheme of oil refining, and market requirements may be undesirable. To reduce the formation of such hydrocarbons, i.e., to increase the yield of the desired catalytic hydrodewaxing products, the initial distillate is mixed in a mixture with a stabilized dewaxed catalyst, the desired product and additionally a straight-run gasoline fraction of NK-62 ° C, taken up to 10 mas. % Of the mixture. The fraction of NK-62 o C is a mixture of mainly hydrocarbons with the number of carbon atoms of 5 and 6, is characterized by a low octane number and additional processing is required to improve its anti-knock properties.
The described method allows, together with an increase in the yield of the desired product, to improve also the antiknock properties of the resulting gasoline fractions due to the conversion of n-paraffin hydrocarbons contained in the fraction of NK-62 ° C in isomerization-cracking reactions.
Example 1
Catalytic hydrodewaxing is subjected to a straight-run hydrotreated kerosene fraction of 180-270 ° C containing 42.96 mas. % N-alkane hydrocarbons and having a crystallization start temperature of -29 ° C, on a catalyst containing, %: Zeolite type ZSM-5-67, NiO-4 and AL2O3, the balance at 4 MPa, 380 ° C, a feed rate of 4.5 h -1 and a hydrogen-containing gas / feed ratio of 300 nm 3 / m 3 .
The conditions of the process and the results obtained are shown in the table.
Example 2
Catalytic hydrodewaxing was subjected to the kerosene fraction of Example 1 under the conditions of Example 1 (except for the process temperature). The product obtained is stabilized, namely, it is subjected to separation and distillation to obtain a stabilized dewaxed catalyst, the desired product (kerosene), and the kerosene fraction is then subjected to catalytic dewaxing in a mixture with stabilized dewaxed catalyst, the desired product, taken in varying amounts, at temperatures providing the product with The same temperature of the onset of crystallization as in the known method.
The conditions of the process and the results obtained are shown in the table.
Example 3
Catalytic hydrodewaxing is subjected to a straight-run diesel fraction of 180-350 ° C containing 40.52 mas. % N-alkane hydrocarbons and having a pour point of -6 ° C. in a mixture with a stable dewaxed catalyst-the desired product (diesel fuel) on the catalyst of example 1 at a pressure of 5 MPa, 330 ° C., a feed rate of 2.5 hours - 1 , the ratio of hydrogen-containing gas / feed is 400 nm 3 / m 3 . Received diesel fuel with a yield of 79 mas. %, Having a pour point of -26 o C, which does not meet the requirements of GOST for winter diesel fuel.
Example 4
Catalytic hydrodewaxing is subjected to the diesel fraction of Example 3 in a mixture with a stabilized dewaxed catalyst, the desired product (diesel fuel), taken in an amount of 35 wt. % Of the original distillate under the conditions of Example 3. A diesel fuel was obtained in a yield of 79.1mg. %, Having a pour point of -37 o C, which meets the requirements of GOST for winter diesel fuel.
Example 5
Catalytic hydrodewaxing is subjected to a fraction of 240-420 ° C of a transformer oil (hydrocracking product) containing 26 mas. % Of n-alkane hydrocarbons and having a pour point of + 15 ° C, in admixture with a stabilized dewaxed catalyst, the desired product (transformer oil base), with a final 30 mA content. % The process is carried out on a catalyst containing, %: NiO - 3.0, MoO 3 - 8.0; Zeolite type ZSM-5 - 60; Al 2 O 3 is the rest. Process conditions: pressure 4.0 MPa, temperature 320 ° C, feed rate 2.7 h -1 , hydrogen-containing gas / feed ratio 1000 nm 3 / m 3 . A transformer oil base is obtained with a yield of 84.6%, with a pour point of -48 ° C (at the desired pour point of -45 ° C).
Example 6
A hydraulic oil fraction of 220-320 ° C containing 7% by weight aromatic hydrocarbons in a mixture with a stabilized dewaxed catalyst, the desired product (hydraulic oil base), taken in an amount of 20 mas. %, Is subjected to dewaxing on a catalyst containing, by weight, %: NiO 4.0, WO 3 9.0; Zeolite type ZSM-5 - 72; Al 2 O 3 is the rest. Process conditions: pressure 5.5 MPa, temperature 285 ° C, feed rate 2.2 h -1 , hydrogen-containing gas / feed ratio 950. The obtained product, the hydraulic oil base, has a pour point of -81 ° C and meets the existing requirements On this indicator of quality.
Example 7
Catalytic hydrodewaxing is subjected to a transformer oil fraction according to Example 5 and under the conditions of Example 5. The difference is that a mixture of a fraction of a transformer oil, a stable dewaxed catalyst, the desired product, and additionally a straight-run fraction of NK-62 ° C (octane number 60 by a motor method) , Taken in an amount of 3ml. % Of the mixture. A transformer oil base is obtained with a yield of 84.95 wt. And a temperature of -48 ° C. The resulting gasoline fraction NK -180 ° C (yield 9.8% by weight of the mixture) has an octane number of 80 by the motor method.
Example 8
Catalytic hydrodewaxing is subjected to a diesel fraction according to Example 3 and under the conditions of Example 4 in a mixture with a stabilized dewaxed catalyst, the desired product (diesel fuel) and additionally a straight fraction PC-62, the amount of which is 9 mass. % Per mixture. A diesel fuel is obtained with a yield of 80.4 mas. %, Having a pour point of -37 ° C.
CLAIM
1. A process for the preparation of low-hardening petroleum products by catalytic hydrodewaxing of petroleum distillates in the presence of a catalyst containing a high-silica zeolite, hydrogenating components, binder, at elevated temperature and pressure, characterized in that the initial distillate is subjected to catalytic hydrodewaxing in a mixture with a stabilized dewaxed catalyst, the desired product In an amount of 5 to 95% by weight of the original distillate.
2. A process according to claim 1, characterized in that the catalytic hydrodewaxing is subjected to an initial distillate in a mixture with a stabilized dewaxed catalyst, the desired product and additionally a straight-run gasoline fraction of HK-62 ° C, in an amount of up to 10% by weight of the mixture.
3. A method according to claim 1, characterized in that the catalytic dewaxing is carried out at a temperature of 280-420 ° C, a pressure of 3-10 MPa, a hydrogen-containing gas: raw material ratio of 200-1500 nm 3 / m 3 .
print version
Date of publication 07.04.2007gg
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