Catalyst hydroperiod and how hydroperiod of crude oil with its use

 

(57) Abstract:

The invention relates to catalysts and methods of hydroperiod of crude oil. Catalyst hydroperiod oil raw material containing the oxide of cobalt and/or Nickel oxide, molybdenum trioxide, aluminum oxide, characterized in that it further contains a phosphate of aluminum and iron phosphate when the mass ratio of aluminum phosphate to phosphate from 3 to 10, and magnesium phosphate in the following ratio, wt.%:

The oxide of cobalt and/or Nickel oxide - 2 - 5

The molybdenum trioxide - 10 - 15

The aluminum phosphate - 1,5 - 10

Iron phosphate is 0.5 - 1

The magnesium phosphate, and 0.1 - 1

- Aluminum oxide - the rest is up to 100%

Hydroperiod of crude oil at a temperature of 300 to 420oC, pressure of 2.0 - 10.0 MPa, the space velocity of the raw material is 1.0 - 10.0 h-1, the ratio of N2/raw 100-1000 nm3/m3using this catalyst can improve gidroobesserivaniya, diasterous, dearomatized and demetallizing the efficiency of the process compared with the known catalysts. 2 C. p. F.-ly, 4 PL.

The invention relates to catalysts hydroperiod of crude oil and Rivonia and dearomatization diesel fractions, hydrodesulphurization unit, demetallization and diazotoluene vacuum distillates.

Known [1] alumonickelsilicate (AHM) and aluminoborosilicate (AKM) catalysts hydroperiod of crude oil. Such catalysts contain 2 to 5 wt.% CoO or NiO, 10-15 wt.% MoO3and - Al2O3. Hydrogenating metals is administered either by impregnation of the calcined granules media, or in catalyst mass and mixing, followed by drying at 100-120oC and calcination at 500-550oC granules of the catalyst.

In the hydrofining process of middle distillates, as well as mixtures of middle distillates gasoline fractions at a pressure of 3.0 to 3.5 MPa, a temperature of 350-380oC, space velocity of the feedstock 2-2,5 h-1these catalysts to reduce the sulfur content from 10000-13000 ppm up to 1500-2000 ppm, and the iodine value of from 5 to 10 g iodine/100 g 2-3 g of iodine/100 g [2].

These known catalysts have the following disadvantages: 1) when the diesel Hydrotreating of distillates to reduce the sulphur content of less than 0.10 wt.% need cutting to reduce the volumetric rate and raise the temperature of the process, which reduces the service life of the catalyst and limits the possibility of production of ekologichnost it is impossible to reduce the content in diesel distillates aromatic hydrocarbons up to 20 vol.% even more active in this process AHM-catalyst.

These problems are partially solve the Hydrotreating catalysts, containing in its composition P2O5[3]. The catalyst contains up to 5 wt.% P2O5in alumnirelations matrix (NiO 2-4%, MoO310-14%, Al2O3- else). The active catalyst in the Hydrotreating process of the vacuum distillate at a temperature of 360oC, a pressure of 5 MPa, the space velocity of the feedstock is not less than 1 h-1.

Closest to the proposed technical solution is the catalyst for Hydrotreating petroleum fractions containing (wt.%) 3,5-4,4 NiO, 13,5 or 14.8 MoO3, 2,0-4,0 P2O5the rest up to 100% Al2O3[4], as well as the way hydroperiod carried out at a temperature of 260-360oC, a pressure of 1.05 ceiling of 5.60 MPa, the space velocity of the raw material of 0.1-10 h-1, the ratio of H2/raw 35,6-1780 nm3/m3in the presence of AHM sulfide catalysts in the form [5].

The catalyst used for Hydrotreating gasoline and diesel fractions. When the Hydrotreating gasoline fraction 91-185oC with a sulfur content of 0.03 wt. % at a temperature of 320oC, a pressure of 2.0 MPa, the space velocity of the raw material 5 h-1the ratio of circulation of hydrogen containing gas 100 nm3/m3rolled what uranium sulfur and 1.0 wt.% at a temperature of 360oC, a pressure of 2.5 MPa, the space velocity of the raw material 6 h-1the residual sulfur content is 0.09-0.10 wt.%. The disadvantage of this catalyst is the impossibility of obtaining it in standard conditions of Hydrotreating environmentally friendly diesel fuels, as well as insufficient dearomatizing activity of the catalyst.

The present invention is aimed at improving hypoaesthesia activity of the catalyst hydroperiod, it dearomatizing activity in the processing of diesel fractions, and diasterous and demetallizing activity in the case of processing gas oil fractions.

Applying the catalyst hydroperiod, contain an oxide of cobalt and/or Nickel, molybdenum trioxide, aluminum oxide, which further comprises a phosphate of aluminum and iron phosphate when the mass ratio of aluminum phosphate to phosphate from 3 to 10, and magnesium phosphate in the following ratio, wt.%:

The oxide of cobalt and/or Nickel oxide - 2 - 5

The molybdenum trioxide - 10 - 15

The aluminum phosphate - 1,5 - 10

Iron phosphate is 0.5 - 1

The magnesium phosphate, and 0.1 - 1

- aluminum oxide - the Rest is up to 100%

The catalyst of this composition may the and, space velocity of the raw material is 1.0 - 10.0 h-1, the ratio of H2/ raw 100 - 1000 nm3/m3.

As raw materials can be used straight-run gasoline fractions with sulfur contents of up to 6000 ppm diesel fraction with a sulfur content of up to 13,000 ppm, as well as vacuum distillates 350 - 540oC. the sulfur Content in products Hydrotreating gasoline fractions on the catalyst is not more than 0.05 ppm (degree hydrodesulphurization unit not less of 99.98%), diesel fractions less than 500 ppm (degree hydrodesulphurization unit not less 95,8%), vacuum gas oil is less than 750 ppm (degree hydrodesulphurization unit not less 95,8%). The content of aromatic hydrocarbons in diesel fractions decreases from 25 - 28 vol.% to less than 17% vol. (the degree of dearomatization less than 39%).

The observed effect of increasing hypoaesthesia activity, hydrogenating activity towards aromatic hydrocarbons, as well as diasterous and demetallizing the activity of the catalyst in the case of processing gas oil fractions due to the introduction of the AKM and AHM - catalysts instead of phosphorus oxide together phosphates of aluminum and iron in a certain ratio, and magnesium phosphate.

Example 1. To 85,85 g (dry substance) of aluminum hydroxide Al(OH)3add 1.5 g of aluminum phosphate AlPO4, 0.5 g of iron phosphate FePO (4and 0.1 g of magnesium phosphate Mg3(PO4)2. The mixture is suspended for 2 h at 80 - 90oC, then peptizing nitric acid and the resulting mass is stirred for 2 h at 50 - 60oC. Then the mass zamalchivaut ammonia to pH 6 to 8, dried to a moisture content of 55 to 60 wt.%, cooled to room temperature and molded into extrudates with a diameter of 2 to 3 mm and a length of 10 - 15 mm extrudates provalivajut on the air 24 h, dried for 6 h at 120oC and calcined at 500oC for 4 h Then the granules impregnated with the moisture absorption by a solution of nitrate of cobalt and paramolybdate ammonium in 14% ammonia solution with the aim of applying granules 2 g of CoO and 10 g MoO3. The obtained pellets of the catalyst is dried at 120oC for 6 h and calcined at 400oC for 4 hours Polsat aluminum - 1,5

Iron phosphate - 0,5

The magnesium phosphate - 0,1

- aluminum oxide - the Rest is up to 100%

Example 2. The catalyst prepared according to example 1, but take 68,0 g (dry substance) of aluminum hydroxide, 10 g of aluminum phosphate, 1 g of magnesium phosphate. Granules applied 5 g CoO and 15 g MoO3. Obtain 100 g of a catalyst of the following composition, wt.%:

The cobalt oxide - 5

The molybdenum trioxide - 15

The aluminum phosphate - 10

Iron phosphate - 1

The magnesium phosphate - 1

-aluminum oxide - the Rest is up to 100%

Example 3. The catalyst prepared according to example 1, but take 79,25 g (dry substance) of aluminum hydroxide, 3.5 g of aluminum phosphate, 0.75 g of iron phosphate, 0.5 g of magnesium phosphate. Granules applied 3.5 g CoO and 12.5 g of molybdenum trioxide MoO3. Obtain 100 g of a catalyst of the following composition wt%:

The cobalt oxide is 3.5

The molybdenum trioxide is 12.5

The aluminum phosphate - 3,5

Iron phosphate - 0,75

The magnesium phosphate - 0,5

-aluminum oxide - the Rest is up to 100%

Example 4 (the prototype). To 80,5 g (A. with.in.) aluminum hydroxide is added an aqueous solution of orthophosphoric acid (H3PO4, containing 3.5 g of P2P5. The mixture was thoroughly stirred at 80-90oC, then a lot zamalchivaut and the diameter of 2-3 mm and a length of 10-15 mm Then the catalyst prepared according to example 3. Obtain 100 g of a catalyst of the following composition, wt.%:

The cobalt oxide is 3.5

The molybdenum trioxide is 12.5

Perioxide phosphorus - 3,5

-aluminum oxide - the Rest is up to 100 %

Example 5 (for comparison). The catalyst prepared according to example 3, but the aluminum phosphate is added. Obtain 100 g of a catalyst of the following composition, wt. %:

The cobalt oxide is 3.5

The molybdenum trioxide is 12.5

Iron phosphate - 0,75

The magnesium phosphate - 0,5

-aluminum oxide - the Rest is up to 100 %

Example 6 (comparison). The catalyst prepared according to example 3, but the phosphate is added. Obtain 100 g of a catalyst of the following composition, wt.%:

The cobalt oxide is 3.5

The molybdenum trioxide is 12.5

The aluminum phosphate - 3,5

The magnesium phosphate - 0,5

-aluminum oxide - the Rest is up to 100 %

Example 7 (for comparison). The catalyst prepared according to example 3, but the magnesium phosphate is added. Obtain 100 g of a catalyst of the following composition, wt.%:

The cobalt oxide is 3.5

The molybdenum trioxide is 12.5

The aluminum phosphate - 3,5

Iron phosphate - 0,75

-aluminum oxide - the Rest is up to 100 %

Example 8 (comparison). The catalyst prepared according to example 3, but the phosphates of aluminum and iron is not added. Get 100 g to the s - 0,5

-aluminum oxide - the Rest is up to 100 %

Example 9 (for comparison). The catalyst prepared according to example 3, but the phosphates of iron and magnesium is not added. Obtain 100 g of a catalyst of the following composition, wt.%:

The cobalt oxide is 3.5

The molybdenum trioxide is 12.5

The aluminum phosphate - 3,5

-aluminum oxide - the Rest is up to 100 %

Example 10 (for comparison). The catalyst prepared according to example 3, but the phosphates of aluminum and magnesium is not added. Obtain 100 g of a catalyst of the following composition, wt.%:

The cobalt oxide is 3.5

The molybdenum trioxide is 12.5

Iron phosphate - 0,75

-aluminum oxide - the Rest is up to 100 %

Examples 11-20. The catalysts in examples 11-20 are prepared analogously to examples 1-10, but instead of CoO on the catalyst impregnation put the same amount of NiO.

Example 21. The catalyst prepared according to example 3, but instead of 1.75 g of CoO on the catalyst is applied to 1.75 g of NiO. Obtain 100 g of a catalyst of the following composition, wt.%:

The cobalt oxide is 1.75

Nickel oxide is 1.75

The molybdenum trioxide is 12.5

The aluminum phosphate - 3,5

Iron phosphate - 0,75

The magnesium phosphate - 0,5

-aluminum oxide - the Rest is up to 100 %

In table. 1 shows the chemical compositions of the samples of the catalysts prepared according to examples 1-21.

Temper, prepared according to examples 1-21, in the process of hydroperiod this raw material.

The catalysts prepared according to examples 1-10, tested in the Hydrotreating gasoline having the following characteristics:

sulfur content, ppm - 300

the octane number by the motor method, the points - 65

iodine value, g iodine per 100 g of gasoline - 1-2

the induction period, min - 900

density, kg/m3- 760

fractional composition, oC

N. K. - 40

10% - 60

50% - 110

90% - 160

98% - 170

Test conditions: temperature 300oC, a pressure of 2 MPa, the volumetric feed rate of the raw material 5 h-1the ratio of H2/raw 100 nm3/m3. Catalyst loading 100 cm3. Before testing on all raw materials, all the catalysts were sliderule diesel fuel with a sulfur content of 1.05 wt.% at a temperature of 360oC, a pressure of 5 MPa, a space velocity of diesel fuel 2 h-1and the ratio of H2/raw materials 500 nm3/m3within 24 hours the Results are given in table. 2.

As can be seen from the table. 2, the catalysts prepared according to the invention, have the best gidroobesserivaniya properties than the sample prepared according to prototypical according to the invention, have the worst gidroobesserivaniya properties. Also less activity possesses a specimen prepared according to the prototype, that is, containing in its composition of P2O5.

The same table shows the results of comparative tests of the catalysts prepared according to examples 3 and 4 (prototype) in various environments. From the presented data shows that all the proposed technological range of the inventive catalyst has the best gidroobesserivaniya properties compared with the prototype.

The samples made in examples 11-21, tested in the straight diesel Hydrotreating distillate and vacuum gas oil West Siberian oil 350-540oC. Loading catalysts 100 cm3.

Straight-run distillate diesel fuel has the following characteristics:

sulfur content, ppm - 12000

density, kg/m3- 843

iodine value, g iodine per 100 g of fuel - 1-3

the content of aromatic hydrocarbons, vol.% - 28

fractional composition,oC

N. K. - 190

10% - 240

30% - 265

50% - 290

90% - 350

96% - 365

Vacuum gas oil has the following characteristics: contains sulfur 18000 ppm; the content of total azote test: at the hydrofining straight-run distillate diesel fuel temperature 340oC, a pressure of 4 MPa, the volumetric feed rate 3 h-1the ratio of H2/raw material 300 nm3/m3; when the Hydrotreating of vacuum gas oil: temperature 340oC, a pressure of 5 MPa, the volumetric feed rate of the raw material 1 h-1the ratio of H2/raw materials 500 nm3/m3.

In table. 3 shows the test results of samples of the catalysts in the process of hydroperiod prjamogonnogo diesel distillate. In table. 4 shows the results of tests of samples of the catalysts in the process of hydroperiod vacuum gasoil. In these tables the results of comparative tests of the catalysts prepared according to examples 3 and 4 (prototype), in different technological conditions.

Analysis of the data table. 3 shows that the inventive catalyst has the best compared to the prototype and catalysts comparison gidroobesserivaniya properties in the process of hydroperiod straight diesel distillate, as well as the best dearomatization properties in this process: the degree hydrodesulphurization unit increases to 91.6 % for the prototype to 95.8 - 96,3 % of the catalyst according to the invention, and the degree of dearomatization from 17.9 % in the prototype to 39,3-46.4 % of the proposed catalyst is July with the prototype and comparison samples gidroobesserivaniya, diastereomer and demetallization properties in the hydrofining process vacuum gazala: degree of desulfurization increases from 93.9 % in prototype to 95.8-96,2 % of the catalyst according to the invention; degree of diazotoluene with 61,5 % to 73,1-76,9 %; degree of demetallization from 86 % to 90 %. While coking ability of the product is reduced from 0.15 % prototype 0.10-0,11 % of the catalyst according to the invention.

The analysis of table. 2-4 shows that the claimed catalyst effective in the process of hydroperiod of crude oil (straight-run gasoline and diesel fraction, a vacuum gas oil) in the following technological conditions; temperature 300-420oC, a pressure of 2.0-10.0 MPa, the volumetric feed rate is 1.0-10.0 h-1the ratio of H2/raw 100-1000 nm3/m3.

1. Catalyst hydroperiod oil raw material containing the oxide of cobalt and/or Nickel oxide, molybdenum trioxide, aluminum oxide, characterized in that it further contains a phosphate of aluminum and iron phosphate when the mass ratio of aluminum phosphate to phosphate 3 - 10, as well as magnesium phosphate at the following content, wt.%:

The oxide of cobalt and/or Nickel oxide - 2 - 5

The molybdenum trioxide - 10 - 15

100%

2. How hydroperiod of crude oil at elevated temperature and pressure, space velocity of the raw material is 1.0 - 10.0 h-1, the ratio of N2/raw 100 - 1000 nm3/m3in the presence of a catalyst comprising the oxides of cobalt and/or Nickel oxide, molybdenum trioxide, aluminum oxide, characterized in that the catalyst additionally contains aluminum phosphate and iron phosphate when the mass ratio of aluminum phosphate to phosphate 3 - 10, as well as magnesium phosphate at the following content, wt.%:

The oxide of cobalt and/or Nickel oxide - 2 - 5

The molybdenum trioxide - 10 - 15

The aluminum phosphate - 1,5 - 10

Iron phosphate is 0.5 - 1

The magnesium phosphate, and 0.1 - 1

-Aluminum oxide - the Rest is up to 100%

and hydroperiod carried out at a temperature of 300 to 420oC, pressure of 2.0 - 10.0 MPa.

 

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