CN108300504B - Method for improving quality of heavy oil and yield of light oil - Google Patents
Method for improving quality of heavy oil and yield of light oil Download PDFInfo
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- 239000003921 oil Substances 0.000 title claims abstract description 70
- 239000000295 fuel oil Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 29
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- 238000002407 reforming Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000001833 catalytic reforming Methods 0.000 claims description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 239000011280 coal tar Substances 0.000 claims description 3
- 238000000629 steam reforming Methods 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 10
- 238000005336 cracking Methods 0.000 abstract description 8
- 230000008878 coupling Effects 0.000 abstract description 6
- 238000010168 coupling process Methods 0.000 abstract description 6
- 238000005859 coupling reaction Methods 0.000 abstract description 6
- 230000006872 improvement Effects 0.000 abstract description 6
- 230000009467 reduction Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 27
- 239000011269 tar Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- 239000003245 coal Substances 0.000 description 13
- 239000007789 gas Substances 0.000 description 12
- 238000011065 in-situ storage Methods 0.000 description 10
- 238000000197 pyrolysis Methods 0.000 description 9
- 238000004523 catalytic cracking Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000006057 reforming reaction Methods 0.000 description 3
- 239000012494 Quartz wool Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- KDRIEERWEFJUSB-UHFFFAOYSA-N carbon dioxide;methane Chemical compound C.O=C=O KDRIEERWEFJUSB-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G29/00—Refining of hydrocarbon oils, in the absence of hydrogen, with other chemicals
- C10G29/02—Non-metals
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/70—Catalyst aspects
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/06—Gasoil
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for improving the quality of heavy oil and the yield of light oil, belonging to the technical field of energy and chemical industry. The method utilizes the characteristic that a Ni-based catalyst simultaneously catalyzes methane reforming and heavy oil cracking, and methane-rich gas and heavy oil (or heavy oil-rich oil products) simultaneously react on the Ni-based catalyst, so that coupling upgrading is realized, and the aims of simultaneously improving the light oil content and the light oil yield are fulfilled. The method solves the problems of obvious reduction of the oil yield, limited improvement of the light oil yield and the like in the traditional heavy oil lightening process, has important significance for improving the quality of heavy oil and solving the problems of system blockage and the like caused by high content of heavy components, and also provides a new way for comprehensive utilization of methane.
Description
Technical Field
The invention relates to a method for improving the quality of heavy oil and the yield of light oil and application thereof, belonging to the technical field of energy.
Background
Heavy oil has the characteristics of high viscosity, difficult volatilization and the like, so that the problems of low catalyst activity, easy inactivation and the like caused by easy system blockage or catalyst surface covering exist in the processing and utilization process. Pyrolysis is one of important ways for realizing graded conversion, cleaning and efficient utilization of coal, and can obtain high-calorific-value semicoke and coal tar rich in various chemicals besides clean coal gas. However, one of the major problems with the low temperature pyrolysis process is that the heavy components (boiling point greater than 360 ℃) of the tar are produced in high content, typically accounting for more than 50% of the tar composition, and these heavy components cause a series of problems in downstream equipment and operations. Such as condensation at the tube walls and filters, resulting in plugging, fouling and corrosion of the tubing or equipment; the mixture of the pyrolysis dust and the gas-liquid separation unit is blocked and the oil-dust separation is difficult, the long-term operation stability of the system is affected, and the industrial application of the pyrolysis technology is hindered. In order to realize the lightening of tar, researchers use Ni or carbon materials as catalysts to carry out tar catalytic cracking in an inert atmosphere, so that the content of the light tar is increased, but the total yield of the tar is obviously reduced while the tar is lightened, and the yield of the light tar is not obviously increased or is only increased. Chinese patent CN103773425A discloses a method for processing heavy oil, which discloses that heavy oil participates in a contact cracking reaction unit, takes inferior heavy oil as a raw material, utilizes nickel metal deposited on a contact agent in the inferior heavy oil and CO generated by gasifying the inferior heavy oil and then entering a conversion unit2Catalytically reacting the gas with a methane-rich gas in a dry reforming unit with a Ni-containing regenerated contact agent to form CO and H2However, this method is carried out with CO and H2The mixed gas is used as atmosphere to carry out heavy oil cracking; the active substance generated by methane can not be directly coupled with the radical formed by heavy oil cracking in situ, so as to achieve the purpose of improving the yield of light oil products and the total yield of tar. Therefore, there is a need in the art for an efficient and simple method for improving heavy oil quality and light oil yield.
Disclosure of Invention
Aiming at the existing problems, the invention provides a method for improving the quality of heavy oil and the yield of light oil (quality improvement for short) by utilizing the characteristic that a Ni-based catalyst can simultaneously catalyze the cracking of heavy oil and the catalytic reforming of methane. In the quality-improving reaction device, the methane catalytic reforming and the heavy oil catalytic cracking are coupled in situ on the Ni-based catalyst, so that the aims of improving the content and the yield of the light oil product are fulfilled.
The technical scheme adopted by the invention is as follows: methane-rich gas for catalytic reforming of methane and oil products rich in heavy oil components enter from the inlet of a reaction device, coupling upgrading is carried out on a Ni-based catalyst with Ni content of 0.1-30 wt.% at the temperature of 400-900 ℃, and the upgraded oil products are cooled by a cold trap and then collected. The content of light components (the boiling point is less than 360 ℃) in the oil product is obtained after simulated distillation analysis.
Further, the heavy oil upgrading reaction device is one of a fixed bed, a fluidized bed, an entrained flow bed or a moving bed.
The reaction temperature is 500-750 ℃.
The catalytic reforming of methane according to the invention comprises carbon dioxide reforming of methane, steam reforming of methane or partial oxidation of methane.
Further, the heavy oil is one or more of coal in-situ pyrolysis tar, coal tar or atmospheric residue.
Further, the Ni content in the Ni-based catalyst is 1-20 wt.%.
The invention has the beneficial effects that: the characteristics that the Ni-based catalyst can catalyze methane reforming and heavy oil cracking at the same time are utilized, and the hydrogen-rich active free radicals generated in the methane reforming process are utilized to stabilize the free radicals generated in the heavy oil catalytic cracking process, so that the content of the light oil product and the yield of the light oil product are improved. The method solves the problems of obvious reduction of the total oil yield and limited improvement of the light oil yield caused by the improvement of the H/C atomic ratio under the condition of no external hydrogen in the traditional heavy oil lightening process, has important significance for solving the industrial application of system blockage caused by heavy oil, improvement of the oil quality and the like at present, and provides a new way for the comprehensive utilization of methane.
Drawings
FIG. 1 is a schematic diagram of the improvement of heavy oil quality and light oil yield;
FIG. 2 is a schematic view of a fixed bed reactor used in examples and comparative examples;
FIG. 3 is a graph comparing the oil yield, light oil content and yield of example 1 and comparative examples 1, 2 and 3;
FIG. 4 is a graph showing the oil yield, light oil content and yield of example 2 and comparative examples 1, 2 and 3;
FIG. 5 is a graph showing the oil yield, light oil content and yield of example 3 and comparative examples 1, 2 and 3;
FIG. 6 is a graph showing the oil yield, light oil content and yield of example 4.
Detailed Description
The present process is further illustrated by the following various specific examples, which are not intended to limit the invention, but rather the invention is more fully understood by those of ordinary skill in the art without limiting in any way.
The test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
FIG. 1 shows a method for improving heavy oil quality and light oil yield, which comprises the steps of entering and mixing methane-rich gas for methane catalytic reforming and oil products rich in heavy oil components from the inlet of a reaction device, carrying out coupling upgrading on a Ni-based catalyst with Ni content of 0.1-30 wt.% at 900 ℃ under 400-. The light oil content in the oil product is obtained after simulated distillation analysis.
In the preferred embodiment of the method, the oil product rich in heavy oil components is unchanneled coal pyrolysis tar, the in-situ generation and upgrading process is carried out in a stainless steel tube fixed bed reactor (figure 2) with the inner diameter of 14mm and the length of 290mm, the reactor is of a vertical two-layer structure, coal, quartz wool, a Ni-based catalyst and quartz wool are sequentially placed from top to bottom, a gas inlet is formed in the top of the reactor, and an outlet is formed in the bottom of the reactor.
The pyrolysis oil yield and light oil yield (dry ashless basis) were calculated as follows:
light oil yield-oil product yield x light oil content
Wherein, WOil productIs the quality of the oil product; w0Respectively the coal sample mass; a. theadIs ash in the coal; madIs the moisture in the coal.
Example 1
300mL/min methane-rich gas (CH) for catalytic reforming of methane4：120mL/min、CO2：120mL/min、N2: 60mL/min) from the upper section of the reactor, mixing with 5g of tar pyrolyzed in situ from non-ditch coal at 650 ℃, and adding Ni/Al with Ni content of 10 wt%2O3And carrying out coupling upgrading on the catalyst. The upgraded oil is cooled by a cold trap at the temperature of-20 ℃ and then collected. Wherein, Ni/Al2O3The catalyst dosage is 1g, the reaction temperature is 650 ℃, and the reaction time is 40 min. FIG. 3 is a comparison of oil yield, light oil content and yield for example 1 and comparative examples 1 to 3. It can be found that the light oil content and yield are higher than those of the comparative example by adopting the methane carbon dioxide catalytic reforming and heavy oil catalytic cracking coupled upgrading method. The light oil content is increased from 55 wt.% to 76 wt.% after coupling upgrading; the yield of light oil is improved from 6.6 wt.% to 7.4 wt.%, and is improved by 12%. This difference is mainly due to the Ni/Al ratio in the methane-rich atmosphere2O3The catalyst not only can catalyze the cracking of heavy oil, but also can catalyze the reforming reaction of methane and carbon dioxide, and active hydrogen-rich radicals generated by the reforming reaction of methane can be combined with radicals generated by the cracking of heavy oil, so that more radicals generated by the heavy oil can be stabilized to form light oil instead of gas. Therefore, the light oil content and the yield in the upgrading process of coupling methane catalytic reforming and heavy oil catalytic cracking are obviously improved.
Example 2
The difference between this example and example 1 is: Ni/Al2O3The Ni content in the catalyst was 5 wt.%. The oil yield, light oil content and yield before and after the catalyst conversion to light weight are shown in FIG. 4. Compared with comparative examples 1-3, the light oil content and yield are further improved, wherein the light oil content can reach 81%. The light oil yield is 8.3%, and is relatively improved by 26%.
Example 3
The difference between this example and example 2 is: the carrier of the Ni-based catalyst is made of coal-based active carbon instead of Al2O3Ni loading of 5 wt.%, reaction atmosphere of 300mL/min methane-rich gas (CH)4：120mL/min、CO2：120mL/min、N2: 60 mL/min). As can be seen from fig. 5, the Ni-based catalyst supported on activated carbon also significantly improved the light oil content and yield, and the oil yield was not significantly reduced as compared to comparative example 3. Compared with comparative examples 1 to 3, the light oil content was as high as 97%. The light oil yield is 9.8%, and is improved by nearly 50%.
Example 4
The difference between this example and example 3 is: the methane-rich gas is (CH)4: 120mL/min, water vapor: 120mL/min, N2: 60mL/min), 5% Ni/activated carbon as catalyst. As shown in fig. 6, it was found that the light oil content and yield can be also significantly improved by combining steam reforming of methane with in situ catalytic cracking of heavy component-rich tar. The light oil content at 650 ℃ was 91%, the light oil yield was 9.3%, demonstrating the effectiveness of the process for increasing the light oil content and yield.
Comparative example 1
300mL/min N2Entering from the upper section of the reactor, mixing with 5g of tar pyrolyzed in situ without ditch coal, escaping from the outlet of the reactor under the action of no catalyst, cooling by a cold trap at the temperature of minus 20 ℃ and collecting. Wherein, the in-situ pyrolysis temperature of the unjoined ditch coal is 650 ℃ and the time is 40 min. The heavy oil content in the oil was 45%.
Comparative example 2
The differences from comparative example 1 are: 300mL/min methane-rich gas (CH) for catalytic reforming of methane4：120mL/min、CO2：120mL/min、N2: 60mL/min) instead of N2. As can be seen from fig. 2, when there is no Ni-based catalyst, since the methane-rich gas cannot undergo the reforming reaction, the oil yield, light oil content and yield are similar to those under a nitrogen atmosphere, and weight reduction is not achieved.
Comparative example 3
The differences from comparative example 1 are: 300mL/min N2Entering from the upper section of the reactor, mixing with 5g of tar pyrolyzed in situ without ditch coal at 650 ℃, and then adding 10 wt.% of Ni/Al2O3Quality-improving reaction is carried out under the action of the catalyst, and the quality-improved product escapes from an outlet and is collected after being cooled by a cold trap at the temperature of minus 20 ℃. Wherein the dosage of the catalyst is 1g, the reaction temperature is 650 ℃, and the reaction time is 40 min.
The results in FIG. 3 show that, in the nitrogen atmosphere, the yield of oil products is significantly reduced (23%) after the in-situ catalytic cracking of the direct pyrolysis tar without the waste coal by the Ni-based catalyst, and although the light oil content is increased from 55% to 69%, the light oil yield is slightly reduced.
The above description is only for the purpose of creating a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (5)
1. A method for improving the quality of heavy oil and the yield of light oil is characterized in that methane-rich gas for catalytic reforming of methane enters from an inlet of a reaction device, is mixed with heavy oil at the temperature of 400-900 ℃, then is coupled and upgraded on a Ni-based catalyst with the Ni content of 0.1-30 wt.%, and the upgraded heavy oil is cooled by a cold trap and then is collected; the heavy oil is one or more of coal tar and atmospheric residue.
2. The method of claim 1, wherein the reaction device is one of a fixed bed, a fluidized bed, an entrained flow bed, or a moving bed.
3. The method as claimed in claim 1, wherein the reaction temperature is 500-750 ℃.
4. The method of claim 1, wherein the catalytic reforming of methane comprises carbon dioxide reforming of methane, steam reforming of methane, or partial oxidation of methane.
5. The method of claim 1, wherein the Ni content of the Ni-based catalyst is 1 ~ 20 wt.%.
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| CN103773425B (en) * | 2012-10-24 | 2016-01-20 | 中国石油化工股份有限公司 | A kind of working method of heavy oil |
| CN105176577B (en) * | 2015-08-19 | 2016-11-30 | 中石化炼化工程（集团）股份有限公司 | A kind of heavy hydrocarbon adds the method for methane |
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