CN115651703B - Method for preparing low-sulfur marine fuel oil base oil from coal tar - Google Patents
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Abstract
The invention discloses a method for preparing low-sulfur marine fuel oil base oil from coal tar, and relates to the preparation of low-sulfur marine fuel oil base oil from reprocessing and utilization of coal tar at low cost. The invention is coupled with the traditional fixed bed and slurry bed reactor through the liquid phase spraying device to respectively form new liquid phase spraying hydrogenation reactors, and then coal tar is used as raw materials to respectively hydrogenate light and heavy components of the coal tar under the cooperation of the special slurry bed catalyst capable of directionally adsorbing asphaltenes to prepare the low-sulfur marine fuel oil base oil. The invention is characterized in that firstly, the new reactor can obviously improve the hydrodesulfurization reaction efficiency, reduce the reaction severity, prolong the device operation period and lower the processing cost of the marine oil with low sulfur, and secondly, the coal tar contains more macromolecular polycyclic aromatic hydrocarbon, thereby improving the unit heat value of the marine fuel oil and improving the fuel economy.
Description
Technical Field
The invention relates to the technical field of heavy oil reprocessing, in particular to a method for preparing low-sulfur marine fuel oil base oil from coal tar.
Background
Coal tar is a liquid product obtained in the carbonization and gasification processes of coal, and has extremely complex composition, and can divide coal tar into three types according to different carbonization temperatures: low temperature coal tar (400-600 ℃), medium temperature coal tar (600-800 ℃) and high temperature coal tar (800-1000 ℃). The organic compound mainly takes a macromolecular aromatic ring structure as a main component, and consists of alkane, aromatic hydrocarbon, colloid and asphaltene, and simultaneously contains various oxygen, sulfur, nitrogen, metal and other heterocyclic rings.
The coal tar is rich in various chemicals with high added value, and the traditional direct combustion utilization not only can pollute the environment, but also can waste the chemicals with high added value in the coal tar, so that the processing quality utilization of the coal tar is very necessary. The method for preparing fuel oil (or other oil products) by processing coal tar has many mature processes and methods at home and abroad, mainly distillation and hydrogenation. The prepared fuel oil (or other oil products) mainly comprises naphtha, gasoline, aviation kerosene, diesel oil, marine fuel oil and the like.
Patent publication No. CN 102719271A discloses a method for preparing diesel oil from high-temperature coal tar, which comprises the steps of refining coal tar, mixing a catalyst, carrying out autoclave hydrogenation, and fractionating the obtained liquid product to obtain the diesel oil. However, the method uses diesel oil as a main product, which means that the sulfur and nitrogen content in the coal tar is required to be reduced to a lower value, the operation cost is relatively high, and the yield of the diesel oil is not too high.
Patent publication No. CN 104479739A discloses a method for producing fuel oil by hydrogenating high-temperature coal tar distillate, which comprises the steps of firstly fractionating high-temperature coal tar to obtain light distillate as a raw material, then hydrofining to obtain a product, and then fractionating to obtain the finished oil with different distillate sections. The method has the problems that the utilization rate of the coal tar is too low, the whole fraction of the coal tar cannot be directly treated, and the waste of coal tar resources is caused.
Patent publication No. CN 101781575A discloses a method for preparing high clean fuel oil from medium and low temperature coal tar, which is to mix an organic solvent with the coal tar to divide the coal tar into light fuel oil and heavy fuel oil. But the heavy fuel oil obtained by the method has higher impurity content.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for preparing low-sulfur marine fuel oil base oil from coal tar, which couples a fixed bed, a slurry bed reactor and a liquid phase spraying technology and uses a slurry bed catalyst in a matching way so as to furthest utilize coal tar resources to prepare various low-sulfur marine fuel oil base oils, and simultaneously achieve the purposes of reducing reaction severity and prolonging the running period of a device.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for preparing low-sulfur marine fuel oil base oil from coal tar comprises the following steps of;
step a, coal tar 1 passes through a fractionating tower 3 to obtain first light distillate 5 and heavy distillate 6;
step b, mixing the first light distillate 5 with new hydrogen 2, entering a liquid-phase spraying fixed bed hydrogenation reactor 11, sequentially contacting a protective agent and a hydrogenation refining agent for hydrogenation refining reaction, and removing sulfur, nitrogen and metal heteroatoms in the first light distillate 5;
step c, the reaction product obtained by the refining reaction enters a first separation device 12, first recycle hydrogen 13 returns to the inlet of a liquid-phase spraying fixed bed hydrogenation reactor 11, and the liquid product is fractionated to obtain naphtha 14 and low-sulfur fraction type marine fuel oil base oil 15;
step d, mixing the heavy distillate 6 with a slurry bed hydrogenation catalyst and new hydrogen 2, and feeding the mixture into a liquid phase spray slurry bed hydrogenation reactor 7 for hydro-thermal cracking reaction;
and e, the reaction product obtained in the step d enters a second separation device 8, second recycle hydrogen 9 returns to the inlet of a liquid-phase spraying slurry bed hydrogenation reactor 7, the liquid product is fractionated, the obtained second light distillate 10 is mixed with the first light distillate 5 in the step a and enters a liquid-phase spraying fixed bed hydrogenation reactor 11, and the heavy fraction is directly used as low-sulfur residue type marine fuel oil base oil 16.
The liquid phase spraying fixed bed hydrogenation reactor 11 and the liquid phase spraying slurry bed hydrogenation reactor 7 are internally provided with liquid phase spraying devices, each liquid phase spraying device comprises a conical pipe and a firing pin, the outer wall of the large opening end of the conical pipe is tangential with the inner wall of the reactor, the small opening end is vertically opposite to the firing pin welded on the inner wall of the reactor, a certain distance exists, and the inner diameter of the small opening end is the same as the outer diameter of the firing pin. When the oil-gas mixture enters the reactor, the oil-gas mixture is emitted from the small opening end of the conical pipe through the conical opening to be changed in diameter, and is impacted on the firing pin, the gas-liquid mixture is highly dispersed again, the gas-liquid contact area is increased, hydrogen is more easily dissolved in oil, the hydrogenation reaction effect is enhanced, the severity of hydrogenation operation conditions is reduced, and meanwhile, the low-sulfur fuel oil base oil is obtained.
The particle size of the slurry bed hydrogenation catalyst is 50-80 mu m, the carrier is carbon black, the macroporous structure cannot be more than 15%, the mesoporous structure is not less than 60%, and the specific surface area is 700-900m 2 Between/g, the active metal loading is between 3 and 7 percent, and asphaltenes can be directionally adsorbed.
The slurry bed hydrogenation catalyst is one or a mixture of organic sulfonic acid Ni and organic sulfonic acid Fe, can be directionally adsorbed on coal tar asphaltene, has a metal content of 6.1-6.6%, has a function of directionally adsorbing asphaltene in the coal tar, inhibits the generation of coking, prolongs the operation period of the reactor, and realizes high-conversion-rate long-period operation of the slurry bed under the low-pressure condition under the combined action of the slurry bed catalyst and a liquid-phase spraying technology.
The coal tar 1 comprises high-temperature coal tar, medium-low-temperature coal tar and mixed oil thereof, wherein the proportion of the mixed oil is that of the high-temperature coal tar: the medium-low temperature coal tar is 6:4 to 7:3.
The temperature of the fractionating tower 3 in the step a is 380-400 ℃.
The step b is performed with hydrofining reaction, the reaction temperature is 335-345 ℃, the pressure is 8-9MPa, the hydrogen-oil ratio is 700:1-800:1, and the airspeed is 0.5-1.0 h -1 。
The step d is carried out the hydro-thermal cracking reaction, the reaction temperature is 450-460 ℃, the pressure is 10-12MPa, the hydrogen-oil ratio is 1200:1-1500:1, and the airspeed is 0.5-1.5 h -1 。
The liquid product of step e is fractionated at 380 ℃.
The main functions of the liquid-phase spraying fixed bed hydrogenation reactor 11 and the liquid-phase spraying slurry bed hydrogenation reactor 7 are to reduce the reaction pressure, and the reaction temperature, the hydrogen-oil ratio and the airspeed must be regulated and controlled in the above operation conditions while the reaction pressure is reduced, so that the normal operation of the two reactors can be realized.
The method takes coal tar as a raw material to prepare the base oil of the marine fuel oil.
The product prepared by the method is various low-sulfur marine fuel oil base oils, wherein the sulfur content of the distillate type low-sulfur marine fuel oil base oil is less than 0.3, and the sulfur content of the residue type marine fuel oil base oil is less than 1%.
The invention has the beneficial effects that:
the invention has the advantages that the coal tar is used as raw material to prepare the base oil of the marine fuel oil, the coal resource is reasonably utilized, and the liquid phase spraying technology is coupled with the fixed bed and slurry bed technology, so that the severity of the reaction condition is reduced, the raw material conversion rate is high, and the desulfurization rate is high. Compared with fuel oil such as gasoline, diesel oil and the like, the marine fuel oil has lower index requirements, reduces the operation cost, and the sulfur content of the obtained two marine fuel oil base oils basically accords with the new index of the global marine fuel oil sulfur content in 2020, proposed by the world shipping organization (IMO).
Drawings
Fig. 1 is a technical process flow chart of the present invention.
Fig. 2 is a schematic view of a liquid-phase spraying apparatus according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
a. The coal tar 1 passes through a fractionating tower 3 with the temperature of 380 ℃ to obtain first light distillate 5 and heavy distillate 6;
b. mixing the first light distillate 5 in the step a with new hydrogen 2, and feeding into a liquid-phase spraying fixed bed hydrogenation reactor 11 for refining reaction, wherein the catalyst used in the refining reaction is Ni-Mo/Al 2 O 3 Protective agent and Ni-Mo/Al 2 O 3 Hydrofining agent, reaction temperature is 335 ℃, pressure is 6MPa, hydrogen-oil ratio is 700:1, space velocity is 0.5h -1 ；
c. The reaction product obtained by the refining reaction enters a first separation device 12, first recycle hydrogen 13 returns to the inlet of a liquid-phase spraying fixed bed hydrogenation reactor 11, and the liquid product is fractionated to obtain naphtha 14 and low-sulfur fraction type marine fuel oil base oil 15;
d. the heavy distillate oil 6 obtained through the step a is carried with slurry bed hydrogenation catalyst and new hydrogen 2 to be mixed and enter a liquid phase spray slurry bed hydrogenation reactor 7 to carry out hydro-thermal cracking reaction, wherein the catalyst is nickel-iron series active carbon catalyst, the reaction temperature is 450 ℃, the pressure is 10MPa, the hydrogen-oil ratio is 1200:1, and the space velocity is 0.5h -1 ；
e. And d, the reaction product obtained in the step a enters a second separation device 8, second recycle hydrogen 9 returns to the inlet of a liquid-phase spraying slurry bed hydrogenation reactor 7, the liquid product is fractionated at 380 ℃, the obtained second light distillate 10 is mixed with the first light distillate 5 in the step a and enters a liquid-phase spraying fixed bed hydrogenation reactor 11, and the heavy fraction is directly used as low-sulfur residue type marine fuel oil base oil 16.
The coal tar is medium-low temperature coal tar. The basic properties of the distillate type and residue type marine fuel oil obtained in this example are shown in Table 1 and Table 2. As can be seen from Table 2, the sulfur content value and the main indexes of flash point, density, carbon residue, ash content, moisture and the like of the two marine fuel oil base oils all meet national standards, and the viscosity value is basically close to the national standards.
Basic properties of Low temperature coal tar in Table 1
TABLE 2 essential oil base Properties of distillate and residue type marine fuel oils
Example 2
In the embodiment, in the step a, the coal tar enters a fractionating tower 3 with the temperature of 380 ℃ for fractionating; in the step b, the obtained first light distillate 5 and new hydrogen 2 are mixed and enter a liquid-phase spraying fixed bed hydrogenation reactor 11 for refining reaction, and the reaction conditions are as follows: the temperature is 335 ℃, the pressure is 8MPa, the hydrogen-oil ratio is 800:1, and the airspeed is 1.5h -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step d, the heavy distillate oil 6 obtained in the step a is mixed with a slurry bed hydrogenation catalyst and new hydrogen 2 and enters a liquid phase spray slurry bed hydrogenation reactor 7 to carry out hydro-thermal cracking reaction, wherein the reaction conditions are as follows: the temperature is 460 ℃, the pressure is 12MPa, the hydrogen-oil ratio is 1200:1, and the airspeed is 1h -1 . Other conditions were the same as in example 1, and distillate-type and residue-type marine fuel oil base oils were produced, the basic properties of which are shown in Table 3. As can be seen from Table 3, the sulfur content value, the carbon residue, the density, the ash content, the water content and other main indexes of the two marine fuel oil base oils all meet the national standard, and the flash point and the viscosity value are basically close to the national standard.
TABLE 3 essential properties of distillate and residue marine fuel oils
Example 3
In the embodiment, in the step a, the coal tar enters a fractionating tower 3 with the temperature of 400 ℃ for fractionating; in the step b, the obtained first light distillate 5 and new hydrogen 2 are mixed and enter a liquid-phase spraying fixed bed hydrogenation reactor 11 for refining reaction, and the reaction conditions are as follows: the temperature is 345 ℃, the pressure is 9MPa, the hydrogen-oil ratio is 800:1, and the airspeed is 1.0h -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step d, the heavy distillate oil 6 obtained in the step a is mixed with a slurry bed hydrogenation catalyst and new hydrogen 2 and enters a liquid phase spray slurry bed hydrogenation reactor 7 to carry out hydro-thermal cracking reaction, wherein the reaction conditions are as follows: the temperature is 460 ℃, the pressure is 12MPa, the hydrogen-oil ratio is 1500:1, and the airspeed is 0.5h -1 . Other conditionsAs in example 1, distillate and residue type base oils for marine fuel oils were produced, the basic properties of which are shown in table 4. As can be seen from Table 4, the sulfur content value, the carbon residue, the density, the ash content, the water content and other main indexes of the two marine fuel oil base oils all meet the national standard, and the flash point and the viscosity value are basically close to the national standard.
TABLE 4 essential properties of distillate and residue marine fuel oils
Example 4
In the embodiment, in the step a, high-temperature coal tar is taken as a raw material and enters a fractionating tower 3 with the temperature of 400 ℃ for fractionating; in the step b, the obtained first light distillate 5 and new hydrogen 2 are mixed and enter a liquid-phase spraying fixed bed hydrogenation reactor 11 for refining reaction, and the reaction conditions are as follows: the temperature is 345 ℃, the pressure is 8MPa, the hydrogen-oil ratio is 800:1, and the airspeed is 0.5h -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step d, the heavy distillate oil 6 obtained in the step a is mixed with a slurry bed hydrogenation catalyst and new hydrogen 2 and enters a liquid phase spray slurry bed hydrogenation reactor 7 to carry out hydro-thermal cracking reaction, wherein the reaction conditions are as follows: the temperature is 455 ℃, the pressure is 11MPa, the hydrogen-oil ratio is 1500:1, and the airspeed is 1.0h -1 . Other conditions were the same as in example 1, and distillate-type and residue-type marine fuel oil base oils were produced, the basic properties of which are shown in Table 5. As can be seen from Table 5, the sulfur content value, the carbon residue, the density, the ash content, the moisture and other main indexes of the two marine fuel oil base oils all meet the national standard, and the flash point and the viscosity value are basically close to the national standard.
TABLE 5 essential oil base Properties of distillate and residue marine fuel oils
Example 5
In the embodiment, in the step a, high-temperature, medium-temperature and low-temperature coal tar is taken as a mixed raw material to enter a fractionating tower 3 with the temperature of 380 ℃ for fractionating; in the step b, the obtained first light distillate 5 and new hydrogen 2 are mixed and enter a liquid-phase spraying fixed bed hydrogenation reactor 11 for refining reaction, and the reaction conditions are as follows: the temperature is 340 ℃, the pressure is 9MPa, the hydrogen-oil ratio is 800:1, and the airspeed is 1.0h -1 The method comprises the steps of carrying out a first treatment on the surface of the In the step d, the heavy distillate oil 6 obtained in the step a is mixed with a slurry bed hydrogenation catalyst and new hydrogen 2 and enters a liquid phase spray slurry bed hydrogenation reactor 7 to carry out hydro-thermal cracking reaction, wherein the reaction conditions are as follows: the temperature is 460 ℃, the pressure is 11MPa, the hydrogen-oil ratio is 1300:1, and the airspeed is 0.75h -1 . Other conditions were the same as in example 1, and distillate-type and residue-type marine fuel oil base oils were produced, the basic properties of which are shown in Table 6. As can be seen from Table 6, the sulfur content value, the carbon residue, the density, the ash content, the water content and other main indexes of the two marine fuel oil base oils all meet the national standard, and the flash point and the viscosity value are basically close to the national standard.
TABLE 6 essential oil base Properties of distillate and residue marine fuel oils
Claims (2)
1. The method for preparing the low-sulfur marine fuel oil base oil from the coal tar is characterized by comprising the following steps of;
step a, the coal tar (1) is subjected to a fractionating tower (3) to obtain first light distillate (5) and heavy distillate (6);
step b, mixing the first light distillate (5) with new hydrogen (2), entering a liquid-phase spraying fixed bed hydrogenation reactor (11), sequentially contacting a protective agent and a hydrogenation refining agent for carrying out hydrogenation refining reaction, and removing sulfur, nitrogen and metal heteroatoms in the first light distillate (5);
c, enabling a reaction product obtained by the refining reaction to enter a first separation device (12), returning first circulating hydrogen (13) to an inlet of a liquid-phase spraying fixed bed hydrogenation reactor (11), and fractionating the liquid product to obtain naphtha (14) and low-sulfur fraction type marine fuel oil base oil (15);
step d, mixing the heavy distillate oil (6) with a slurry bed hydrogenation catalyst and new hydrogen (2) and then entering a liquid phase spraying slurry bed hydrogenation reactor (7) for hydro-thermal cracking reaction;
step e, the reaction product obtained in the step d enters a second separation device (8), second circulating hydrogen (9) returns to the inlet of a liquid-phase spraying slurry bed hydrogenation reactor (7), the liquid product is fractionated, the obtained second light distillate oil (10) and the first light distillate oil (5) in the step a are mixed and enter a liquid-phase spraying fixed bed hydrogenation reactor (11), and the heavy distillate is directly used as low-sulfur residue type marine fuel oil base oil (16);
the liquid phase spraying fixed bed hydrogenation reactor (11) and the liquid phase spraying slurry bed hydrogenation reactor (7) are internally provided with a liquid phase spraying device, the liquid phase spraying device comprises a conical pipe and a firing pin, the outer wall of the large opening end of the conical pipe is tangential to the inner wall of the reactor, the small opening end is vertically opposite to the firing pin welded on the inner wall of the reactor, a certain distance exists, the inner diameter of the small opening end is the same as the outer diameter of the firing pin, when an oil-gas mixture enters the reactor, is ejected from the small opening end of the conical pipe through the diameter change of the conical opening, and is impacted on the firing pin, the gas-liquid mixture is highly dispersed again, and meanwhile, the low-sulfur fuel oil base oil is obtained;
the particle size of the slurry bed hydrogenation catalyst is 50-80 mu m, the carrier is carbon black, the macroporous structure cannot be more than 15%, the mesoporous structure is not less than 60%, and the specific surface area is 700-900m 2 Between/g;
the active metal is one or a mixture of organic sulfonic acid Ni and organic sulfonic acid Fe, can be directionally adsorbed on the coal tar asphaltene, and has the active metal load content of 6.1-6.6%;
the temperature of the fractionating tower (3) in the step a is 380-400 ℃;
and b, carrying out hydrofining reaction at 335-345 ℃, 8-9MPa, 700:1-800:1 hydrogen-oil ratio and 0 airspeed.5～1.0h -1 ；
The step d is carried out the hydro-thermal cracking reaction, the reaction temperature is 450-460 ℃, the pressure is 10-12MPa, the hydrogen-oil ratio is 1200:1-1500:1, and the airspeed is 0.5-1.5 h -1 ；
Said step e liquid product is fractionated at 380 ℃;
the catalyst used in the refining reaction is a Ni-Mo/Al2O3 protective agent and a Ni-Mo/Al2O3 hydrogenation refining agent.
2. The method for preparing the low-sulfur marine fuel oil base oil from the coal tar according to claim 1, wherein the coal tar (1) comprises high-temperature coal tar, medium-low-temperature coal tar and mixed oil thereof, and the ratio of the mixed oil is that of the high-temperature coal tar: the medium-low temperature coal tar is 6:4 to 7:3.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103695031A (en) * | 2013-12-27 | 2014-04-02 | 成都博晟能源科技有限公司 | Method for producing diesel oil and bunker fuel blend component from coal tar |
| CN109705909A (en) * | 2017-10-25 | 2019-05-03 | 中国石油化工股份有限公司 | By the method for coal tar production bunker fuel oil |
| CN112980484A (en) * | 2021-03-01 | 2021-06-18 | 内蒙古晟源科技有限公司 | Method for producing special marine heavy fuel oil by using coal tar as raw material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103695031A (en) * | 2013-12-27 | 2014-04-02 | 成都博晟能源科技有限公司 | Method for producing diesel oil and bunker fuel blend component from coal tar |
| CN109705909A (en) * | 2017-10-25 | 2019-05-03 | 中国石油化工股份有限公司 | By the method for coal tar production bunker fuel oil |
| CN112980484A (en) * | 2021-03-01 | 2021-06-18 | 内蒙古晟源科技有限公司 | Method for producing special marine heavy fuel oil by using coal tar as raw material |
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