CN102876376A - Method for improving hydrogenation production of gasoline and diesel oil by coal tar - Google Patents
Method for improving hydrogenation production of gasoline and diesel oil by coal tar Download PDFInfo
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- CN102876376A CN102876376A CN2012103648661A CN201210364866A CN102876376A CN 102876376 A CN102876376 A CN 102876376A CN 2012103648661 A CN2012103648661 A CN 2012103648661A CN 201210364866 A CN201210364866 A CN 201210364866A CN 102876376 A CN102876376 A CN 102876376A
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Abstract
The invention discloses a method for improving hydrogenation production of gasoline and diesel oil by coal tar, and belongs to the fields of coal chemical industry and energy technology. The invention is characterized in that the method comprises the following steps: distilling coal tar for separation to obtain light oil (360 DEG C) and heavy oil (360 DEG C), performing delayed coking of the heavy oil, mixing with the light oil, adding the mixed oil into a reaction distillation tower for catalytic cracking and fractionation, introducing the oil gas after catalytic cracking into a hydrogenation reaction tower for hydrorefining, distilling the reaction product to obtain high-quality distillate of gasoline and diesel oil. A catalytic distillation catalyst and a sulfide catalyst used in the invention are prepared by appropriate carriers and active components through a liquid phase method, wherein the appropriate carriers and active components are selected base on the composition and performance of the coal tar. The method of the invention is simple in process, high in catalyst activity and selectivity, low in residual charcoal, and high in gasoline and diesel oil yield, provides a new approach for the utilization of coal tar, and has good economic benefits and industrial application prospects.
Description
Technical field
The invention belongs to energy technology and field of environment protection, relate to a kind of method that coal tar hydrogenating is produced petrol and diesel oil that improves.
Background technology
In the Coal Chemical Industry process, coal tar is as one of staple product of coking industry, and its output accounts for 3% ~ 4% of shove charge coal, and it forms very complicated, produces about 15.00 Mt per year.Can be divided into coal-tar heavy oil according to dry distillation of coal temperature difference, coal-tar middle oil and coalite tar, three's composition and different in kind, its processing and utilization method is different.At present, the part coal-tar heavy oil be used for to extract outside the Chemicals, in the major part/and coalite tar and a small amount of coal-tar heavy oil be used as fuel and carry out extensive burning.Because contain a large amount of ring texture compound and more sulphur, the nitrogen compounds such as aromatic series in the coal tar, fire row is emitted a large amount of sulfur-bearing nitrogenous compounds, and environment is caused serious pollution, the environmental protection energy of advocating energetically with Present Global runs in the opposite direction.Produce the product of clear energy sources and alternative petrochemical complex with coal tar, such as diesel oil, gasoline, aviation kerosene, liquefied petroleum gas (LPG) etc., can be combined with the energy, Chemical Engineering Technology, form coal---the integrated new industry of derived energy chemical, be important development direction from now on, this alleviates environmental pollution that fire coal causes, reduces China the dependence of Imported oil is all had great significance for China.
Along with the continuous increase of coal tar output, the processing of the cleaning of coal tar and effective the utilization become more and more important.According to chemical constitution and the character of coal tar, our develop coal tar fractional distillation-delayed coking-catalytic distillation-hydrogenation upgrading-air distillation new technology of producing petrol and diesel oil.Coal tar distillation is separated into lightweight oil and mink cell focus, the catalytic distillation cracking on the catalytic distillation catalyzer of the delayed coking of mink cell focus and lightweight oil, adjust the cut ratio of petrol and diesel oil, reduce the gum level in the cut, then hydrofining on sulfide catalyst, reduce the sulphur nitrogen content in the oil product, regulate acid number, the gained distillate obtains high-quality gasoline and diesel oil etc. through distillation again.The delayed coking of mink cell focus has reduced the carbon residue amount.Producing without the three wastes in air distillation or catalytic distillation-hydrofining-air distillation, is a process green, recycling.Following known technology all comes with some shortcomings:
Chinese patent, application number: 201210149833.5, a kind of method of utilizing coal tar to produce petrol and diesel oil, gas and residue that its process produces are more, and the productive rate of petrol and diesel oil is low.
Chinese patent, publication number: CN 1097210A, introduce the method that coalite tar is produced diesel oil in utilizing, its operation is many, needs a large amount of pickling and alkali cleaning, and it is many to produce waste liquid, and environmental pollution is serious, and the product quality that obtains is low.
Chinese patent, publication number: CN 1064882A, introduce a kind of method of producing diesel oil with coalite tar, its process will adopt vitriol oil washing, and the waste water of generation causes serious environmental pollution, and can only be for the trans-utilization of coalite tar.
Chinese patent, publication number: CN 101235298A, introduce a kind of processing method with preparing substitutive diesel oil from coal tar, it adopts stirred-tank reactor, can't operate continuously, the product performance that obtain are poor, and product yield is low.
Chinese patent, publication number: CN 1706917A, introduce technique and catalyzer thereof from preparing diesel from coal tar, its operation is more, and is more loaded down with trivial details, and can only produce diesel oil distillate.
Summary of the invention
The invention provides a kind of method of coal tar hydrogenating upgrading.Take resource rational utilization and environment protection as purpose; there is more drawback for coal tar technique; environmental pollution is serious; added value is low; the problems such as the petrol and diesel oil productive rate is low organically combine the utilization of realization tar resource by catalytic distillation, delayed coking and hydrofining, change into high added value; productive rate is high, the petrol and diesel oil that meets the demands.In addition, waste residue and the combustion gas of comprehensive utilization process itself make the energy-conservation and environmental protection of production process, have avoided secondary pollution.Through distillation, delayed coking, catalytic distillation, air distillation is passed through in the hydrogenation upgrading again, cuts into 150 ℃ of gasoline (＜150 ℃) and diesel oil (〉 according to recovered temperature with coal tar in the present invention).The present invention improved the transformation efficiency of balanced reaction and consecutive reaction selectivity, energy-conservation of consumption reduction, prolonged catalyst life, carbon residue amount decrease, the petrol and diesel oil productive rate is high, flow process is simple and reduce investment outlay.
Technical scheme of the present invention is as follows:
Coal tar raw material among the present invention comprises coal-tar heavy oil, and wherein one or two or more kinds of coal-tar middle oil and coalite tar mixed as raw material.
The method is that just coal tar is divided into lightweight oil (＜360 after distillation
oC) and mink cell focus (〉 360
oC), be mixed into reactive distillation column with lightweight oil after the delayed coking of mink cell focus and carry out catalytic pyrolysis and fractionation.The delay coke main purpose is that the mink cell focus with high carbon residue is converted into lightweight oil.Mix the injection still kettle with lightweight oil with obtaining oil gas after the delayed coking of mink cell focus, adopt the waste residue and the combustion gas that produce in the coal tar conversion process to heat, the still kettle temperature is controlled between 250 ~ 500 ℃.When the still kettle heating arrived 250 ℃, the oil gas that distills entered in the reaction fractionating tower that molecular sieve/aluminium oxide catalyst is housed and reacts and rectifying.Molecular sieve/aluminium oxide catalyst, wherein molecular sieve comprises ZSM-5, ZSM-48, y-type zeolite, mordenite and β zeolite or their mixture, molecular sieve content is 0.5 ~ 95wt%.The ratio of reactive distillation column bed diameter and the particle diameter of preformed catalyst is greater than 10, and the Main Function of catalyzer is selective splitting macromole and as the filler of distillation tower, is used for separating of reaction product and product cut.Enter to mix by the interchanger heating with hydrogen by feedstock pump through the oil gas of catalytic distillation and enter hydrofining reactor, hydrofining.The feeding temperature of control hydrofining reactor is 280 ~ 360
oC; Hydrogen partial pressure 5 ~ 15 MPa, volume space velocity 0.3 ~ 4.0 h
-1With hydrogen to oil volume ratio be 300 ~ 1200:1; Hydrobon catalyst is the SiO with two mesopore composite structures
2, Al
2O
3, TiO
2Be carrier Deng oxide compound, take one or two or more kinds mixture of the metallic sulfide of nickel, cobalt, molybdenum, tungsten as activeconstituents.Distillate after the hydrofining distills through normal pressure, cuts into 150 ℃ of gasoline (＜150 ℃) and diesel oil (〉 according to recovered temperature).
By method production of the present invention obtain gasoline fraction (＜150 ℃〉yield 10 ~ 25%, octane value is 75 ~ 85, density 0.70 ~ 0.76g/cm
3, can be used as the blend component of gasoline.The yield of diesel oil distillate (150 ~ 360 ℃) is 70 ~ 85%, and cetane value is 45, density 0.83 ~ 0.86g/cm
3, condensation point is lower than-20 ℃, can be used as low-coagulation diesel oil No. 10.Combustion gas and cinder productive rate are not higher than 10%.
The mode of operate continuously, flexible operation, easy are adopted in distillation of the present invention, delayed coking, catalytic distillation, hydrofining and air distillation.
The present invention adopts air distillation, delayed coking to combine with the gas phase catalysis cracking process, and the combustion gas and the cinder that take full advantage of process have reduced energy consumption; Improve the transformation efficiency of balanced reaction by air distillation, delayed coking and reaction rectification technique, improved the selectivity of reaction, prolonged the Hydrobon catalyst life-span, reduced simultaneously catalyst levels; Elder generation's fractionation repeated hydrogenation carries out desulfurization removing nitric, reduces gum level, has reduced the hydrogen consumption; Product yield is high, wide scope of material.
Description of drawings
Fig. 1 is process flow diagram of the present invention.
Among the figure: 1 atmospheric distillation tower; 2 catalytic distillation towers; 3 delayed coking drums, 4 hydrofining reaction towers; 5 distillation towers.
Embodiment
Be described in detail specific embodiments of the invention below in conjunction with technical scheme and accompanying drawing.
Embodiment 1: coal tar is divided into lightweight oil (＜360 after distillation
oC) and mink cell focus (＜360
oC).Following table 1 is seen air distillation material balance test-results
| Raw material | Lightweight oil (＜360 ℃) | Mink cell focus (＜360 ℃) | |
| Quality/g | 2000 | 900 | 1100 |
| Percentage ratio/% | 45 | 55 |
Embodiment 2: mink cell focus (＜360
oC) obtain light-end products after the delayed coking.Following table 2 is seen delayed coking material balance test-results
| Raw material | Light-end products | Coke | |
| Quality/g | 1100 | 825 | 275 |
| Percentage ratio/% | 75% | 25% |
Embodiment 3: the gas phase catalysis cracking of coal tar on molecular sieve/aluminium oxide catalyst.Inject the reaction fractionating tower that molecular sieve/aluminium oxide catalyst is housed and carry out catalytic distillation mixing with lightweight oil after the delayed coking of mink cell focus, catalyzer is comprised of the aluminum oxide that contains 35%ZSM-48 and 15% mordenite, obtain the columnar product of 2.0-3.0 mm by molding bonded, length 3-8 mm, bulk density 0.65-0.80 g/mL, intensity is greater than 40 N/mm.Adopt the waste residue and the combustion gas that produce in the coal tar conversion process to heat, agent-oil ratio is controlled between the 1-20.The combustion gas that produces is used for the heating of distillation tower.Following table 2 is seen catalytic distillation material balance test-results
| Raw material | Water content | The cracked oil quality | The catalyzer adsorptive capacity | Carbon residue | Gas+loss | |
| Quality/g | 1800 | 27 | 1485 | 108 | 90 | 81 |
| Percentage ratio/% | 1.5 | 82.5 | 6.0 | 5.5 | 4.5 |
Following table 3 is seen the catalytic distillation oil property
Embodiment 4: load-type nickel molybdenum sulphide catalyzer is Hydrobon catalyst.Carrier adopts SiO
2-Al
2O
3, specific surface area is at 200-400 m
2/ g, pore volume is at 0.5-2.0 cm
3/ g, the most probable pore size distribution is at 2-4 nm and 10-15nm.Nickel molybdenum sulphide precursor adopts nickelous nitrate or nickel acetate and ammonium thiomolybdate.Adopt equi-volume impregnating to prepare load-type nickel molybdenum sulphide catalyzer through dipping-drying-steps such as roasting.Following table 3 sees that reaction process condition and product form.
As shown in Table 3, oil distillate is on load-type nickel molybdenum sulphide catalyzer 340
oMore than the C, 8MPa hydrofining has effectively removed sulphur nitrogen, greatly reduces colloid, shows that load-type nickel molybdenum sulphide catalyzer has well to remove the heteroatoms ability, the product water-white that obtains, free from extraneous odour, the petrol and diesel oil mixture that quality is high.
Embodiment 3: the product introduction atmospheric distillation tower after 3 times hydrofining of example condition cuts into 150 ℃ of gasoline (＜150 ℃) and diesel oil (〉 according to recovered temperature).Lower 4 tables are seen vapour, diesel oil character
| Gasoline | Diesel oil | |
| Density/gcm-1 | 0.72 | 0.85 |
| S content/ng/ μ L | 34 | 20 |
| N content/ng/ μ L | <1 | <3 |
| Colloid mg/ |
2 | 20 |
| Acid number/mgKOH/100mL | <1 | 3.5 |
| Other | Color: water-white octane value: 75 | Color: yellowish cetane value: 45 |
As shown in Table 4, oil distillate obtains the petrol and diesel oil distillate through atmospheric distillation.The product free from extraneous odour that obtains, the gasoline that quality is high and diesel oil.
Embodiment 4: the catalytic distillation distillate is raw material, on embodiment 1,2,3 the basis in 8.0MPa and 340
oC carries out stability experiment, and following table 5 is seen the reaction process condition of operation in 1000 hours and obtained at last product property.
| Gasoline | Diesel oil | |
| Density/gcm-1 | 0.72 | 0.85 |
| S content/ng/ μ L | 36 | 24 |
| N content/ng/ μ L | <1 | <3 |
| Colloid mg/ |
3 | 21 |
| Acid number/mgKOH/100mL | <1 | 3.5 |
| Other | Color: water-white octane value: 75 | Color: yellowish cetane value: 45 |
1000 hours experimental result as shown in Table 5, load-type nickel molybdenum sulphide catalyzer shows satisfactory stability, without phenomenons such as coking and deactivations, compare substantially constantly containing with beginning test of sulphur and nitrogen in the resulting petrol and diesel oil product of air distillation, reaches 3 mg100mL for gasoline gum content
-1, also be reduced to 21mg100mL for the diesel oil gum level
-1, the vapour that obtains in addition, diesel oil free from extraneous odour have good stability, and quality is high, meets national petrol and diesel oil standard.The above results shows that technology of the present invention can transform coal tar efficiently to petrol and diesel oil, realizes the tar resource utilization.
Claims (5)
1. one kind is improved the method that coal tar hydrogenating is produced petrol and diesel oil, and coal tar is divided into lightweight oil (＜360 after distillation
oC) and mink cell focus (〉 360
oC), be mixed into reactive distillation column with lightweight oil after the delayed coking of mink cell focus and carry out catalytic pyrolysis and fractionation, the oil gas behind the catalytic pyrolysis enters the hydrogenation reaction tower, hydrofining, and reaction product obtains high-quality gasoline and diesel oil distillate oil through distillation again; Be further characterized in that: the oil gas after the delayed coking of mink cell focus injects still kettle with lightweight oil, adopts the waste residue and the combustion gas that produce in the coal tar conversion process to heat, and the still kettle temperature is controlled at 250 ~ 500 ℃; The oil gas that distills enters and carries out catalytic cracking reaction and rectifying in the reaction fractionating tower that molecular sieve/aluminium oxide catalyst is housed; Lightweight oil behind the catalytic pyrolysis enters the hydrofining reaction tower through the interchanger heating, hydrofining, and reaction product obtains high-quality gasoline and diesel oil distillate oil through distillation again; 280 ~ 360 ℃ of feeding temperatures, hydrogen partial pressure 4 ~ 15 MPa, volume space velocity 0.3 ~ 4.0 h
-1, hydrogen to oil volume ratio is 300 ~ 1200:1;
Employed molecular sieve/the aluminium oxide catalyst of reaction distillation, wherein the molecular sieve molecular sieve comprises ZSM-5, ZSM-48, y-type zeolite, mordenite and β zeolite or their mixture, molecular sieve content is 0.5-95wt%;
Hydrobon catalyst is the loading type sulfide catalyst, and carrier is the oxide carrier with two mesopore composite structures.
2. method according to claim 1 is further characterized in that: described Hydrobon catalyst is one or two or more kinds of metallic sulfide of nickel, cobalt, molybdenum, tungsten.
3. method according to claim 1 and 2, be further characterized in that: described oxide compound with two mesopore composite structures is SiO
2, Al
2O
3Or TiO
2
4. according to the method for claim 1 or 2 described a kind of coal tar hydrogenating upgradings, be further characterized in that: coal tar is one or two or more kinds mixing in high temperature tar, middle temperature tar, the semi coking tar.
5. according to the method for a kind of coal tar hydrogenating upgrading claimed in claim 3, be further characterized in that: coal tar is one or two or more kinds mixing in high temperature tar, middle temperature tar, the semi coking tar.
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|---|---|---|---|
| CN2012103648661A CN102876376A (en) | 2012-09-27 | 2012-09-27 | Method for improving hydrogenation production of gasoline and diesel oil by coal tar |
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|---|---|---|---|
| CN2012103648661A CN102876376A (en) | 2012-09-27 | 2012-09-27 | Method for improving hydrogenation production of gasoline and diesel oil by coal tar |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103289740A (en) * | 2013-01-23 | 2013-09-11 | 大连理工大学 | Method for preparing clean fuel oil from coal tar |
| CN104449844A (en) * | 2013-09-17 | 2015-03-25 | 安徽实华工程技术股份有限公司 | Delayed coking process for coal tar |
| CN108102703A (en) * | 2016-11-24 | 2018-06-01 | 中国石油化工股份有限公司 | A kind of processing and treating method of catalytic diesel oil |
| CN110538660A (en) * | 2018-05-29 | 2019-12-06 | 中国石油化工股份有限公司 | Catalyst for hydrofining of cracked tar |
| CN115786002A (en) * | 2022-06-28 | 2023-03-14 | 中国海洋石油集团有限公司 | Method for producing diesel oil by coal tar hydrogenation treatment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1880411A (en) * | 2006-03-04 | 2006-12-20 | 荆门市金吉化工有限公司 | Process for preparing fuel oil by using coal tar |
| CN102676219A (en) * | 2012-05-15 | 2012-09-19 | 大连理工大学 | Method for utilizing coal tar to produce gasoline and diesel |
-
2012
- 2012-09-27 CN CN2012103648661A patent/CN102876376A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1880411A (en) * | 2006-03-04 | 2006-12-20 | 荆门市金吉化工有限公司 | Process for preparing fuel oil by using coal tar |
| CN102676219A (en) * | 2012-05-15 | 2012-09-19 | 大连理工大学 | Method for utilizing coal tar to produce gasoline and diesel |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103289740A (en) * | 2013-01-23 | 2013-09-11 | 大连理工大学 | Method for preparing clean fuel oil from coal tar |
| CN104449844A (en) * | 2013-09-17 | 2015-03-25 | 安徽实华工程技术股份有限公司 | Delayed coking process for coal tar |
| CN108102703A (en) * | 2016-11-24 | 2018-06-01 | 中国石油化工股份有限公司 | A kind of processing and treating method of catalytic diesel oil |
| CN108102703B (en) * | 2016-11-24 | 2020-06-09 | 中国石油化工股份有限公司 | Processing method of catalytic diesel oil |
| CN110538660A (en) * | 2018-05-29 | 2019-12-06 | 中国石油化工股份有限公司 | Catalyst for hydrofining of cracked tar |
| CN110538660B (en) * | 2018-05-29 | 2021-11-30 | 中国石油化工股份有限公司 | Catalyst for hydrofining of cracked tar |
| CN115786002A (en) * | 2022-06-28 | 2023-03-14 | 中国海洋石油集团有限公司 | Method for producing diesel oil by coal tar hydrogenation treatment |
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Application publication date: 20130116 |