CN105296002A - Method for producing fuel oils by hydrogenation after coal tar cleaning and phenol extraction and system thereof - Google Patents
Method for producing fuel oils by hydrogenation after coal tar cleaning and phenol extraction and system thereof Download PDFInfo
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Abstract
The invention relates to a method for producing fuel oils by hydrogenation after coal tar cleaning and phenol extraction and a system thereof. According to the technical scheme, coal tar is sent into a distillation column to separate a phenol-rich fraction and other fractions; dephenolized oil obtained after cleaning and phenol extraction of the phenol-rich fraction is used as solvent naphtha to be mixed with a catalyst and a vulcanizing agent, and the mixture is vulcanized to prepare catalyst slurry; the other fractions and the catalyst slurry are mixed and the mixture is sent into a slurry-bed hydrocracking reactor to undergo a hydrocracking reaction; reactants obtained after the hydrocracking reaction are then sent into a separation system to separate hydrogen-rich gas, light oil and tail oil containing a catalyst; the light oil is sent into a fixed-bed hydrogenation reactor to undergo a hydrofining reaction; and reactants obtained after the hydrofining reaction are sent into a fractionating tower to separate gaseous hydrocarbon, a gasoline fraction and a diesel fraction. The technology of the invention is simple; utilization rate of raw materials is high; the system is environmentally friendly, has low production cost and operating cost and is simple to maintain; service life of a catalyst is prolonged; and product yield is high.
Description
Technical field
The present invention relates to a kind of production method and system of fuel oil, a kind of coal tar cleans and puies forward the method and system that phenol back end hydrogenation produces fuel oil specifically.
Background technology
Along with rapid economic development, grow with each passing day for the demand of light-end products in market, the effective way that coal tar hydrogenating is its lighting and cleans, and is also the main probing direction that coal tar processing utilizes.Coal tar is the by product of coal coking, destructive distillation and gasification.Full fraction of coal tar is different from crude oil or heavy oil, and it forms complexity, and aromatic hydrocarbons, resin and asphalt content are relatively high, and particularly oxygen level is at about 8wt%.Wherein oxygen mainly exists with the form of phenols and furfuran compound, and phenolic compound is one of basic raw material of chemical industry, and added value is higher.Traditional coal tar processing route mainly contains two kinds, and one is chemical industry route, although extraction yield can reach more than 95%, often processes 1 ton needs nearly 0.2 ton of consumption alkali containing phenol raw material, produces a large amount of reluctant phenolic wastewater simultaneously.And another kind of route is hydrogenation route, coal tar after hydrogenation except can removing in coal tar the heteroatoms (as metal, sulphur, nitrogen and oxygen etc.) of the overwhelming majority, in hydrogenation process, also can there is the reactions such as macromole cracking, aromatic hydrocarbons open loop are saturated, olefin saturated, finally can produce clean light-end products.For hydrogenation route, also form kinds of processes and supporting catalyzer at present.
CN1351130A discloses a kind of method of producing diesel by utilizing coal tar, in this patent with in coal tar lower than the lighting end of 370 DEG C for raw material obtains diesel product through fixed bed hydrogenation is refining, catalyzer used is Hydrobon catalyst and dearomatization catalyst.The lighting end be mainly applicable in coal tar of this technique, can not process full fraction of coal tar, particularly last running.Full fraction of coal tar or last running resin and asphalt content high, fixed-bed reactor be difficult to processing; Secondly contain micron-sized coal dust in full cut or last running, these micron-sized coal dusts are once will soon cause the obstruction of beds after entering fixed-bed reactor.In addition, enter in the lighting end of fixed bed and be rich in phenols, phenols directly enters hydrofining section will produce water after hydrogenation reaction, and water has disadvantageous effect for life-span of hydrogenation catalyst and activity, and adds hydrogen consumption.CN101240191A discloses a kind of method of producing lightweight fuel oil by coal tar heavy fractioning hydrogenation, and the method adopts fixed bed hydrogenation to refine-hydrocracking-hydro-upgrading combination process.Although this technique can process the last running in coal tar, but technical process is complicated, except the reactor that needs three kinds of difference in functionalitys and catalyzer, separation system is set up to discharge the water formed in hydrogenation process, to avoid causing disadvantageous effect to hydrocracking catalyst after also needing hydrofining reaction.Above two kinds of techniques all adopt fixed-bed process, therefore also have corresponding requirements for coal tar raw material, and the solid impurity (as coal dust, ash grade) that raw material goes after having to pass through repeatedly pre-treatment could charging.CN1766058A discloses a kind of coal tar and entirely heats up in a steamer floating bed hydrocracking technique, and its catalyzer is water-soluble homogeneous catalyst.Compare fixed bed hydrogenation, suspension bed hydrogenation process can process the inferior raw material containing impurity, and maximizedly can utilize raw material production light-end products.But full fraction of coal tar hydrogenation can change the phenolic compound of high added value in tar into hydro carbons and water, reduce added value on the one hand; Increase hydrogen consumption on the other hand, the existence of water simultaneously also can reduce the activity of catalyzer and the corrosion of life-span and increase equipment and pipeline.In addition, this technique uses water-soluble phosphorus nikel molybdate, and the dispersed sulfur system of this kind of catalyzer is huge, and equipment is complicated, and energy consumption is high.
Summary of the invention
The object of the invention is to solve the problems of the technologies described above, there is provided that a kind of technique is simple, raw material availability is high, environmentally friendly, production cost and running cost is low, it is simple to safeguard, improve catalyzer work-ing life, product yield is high, guarantee system long-term stability is run coal tar cleans and puies forward the method that phenol back end hydrogenation produces fuel oil.
The present invention also provides the system of the preparing fuel oil with coal oil hydrogenation product that a kind of system for aforesaid method is simple, reliable, equipment investment cost is low.
The inventive method comprises the following steps:
(1) coal tar is sent into distillation tower normal pressure and isolate rich phenol cut and other cut, described rich phenol cut enters clean phenol system of putting forward to carry out clean phenol of carrying and obtains the dephenolize oil of phenol content lower than 3.5wt%, and dephenolize oil is sent into catalyst slurry batch can and made catalyst pulp as solvent oil with catalyzer and vulcanizing agent mixing sulfuration;
(2) sulfuration is carried out after the mixing of catalyzer raw material, solvent and vulcanizing agent, the condition of sulfuration is: hydrogen to oil volume ratio (under mark condition): 400-600, temperature 230 DEG C of sulfuration 3-5h, sulfuration 3-5h at 320 DEG C, hydrogen pressure 3-6MPa, vulcanizing agent is dimethyl disulfide.Catalyst pulp after sulfuration completes mixes with other cut obtained in step (1) to send under hydrogen in slurry bed system hydrocracking reactor exists and carries out hydrocracking reaction, and the reactant obtained is sent into thermal separation systematic position and gone out hydrogen-rich gas, lightweight oil and the tail oil containing catalyzer;
(3) lightweight oil obtained in step (2) is sent into fixed bed hydrogenation reactor and carry out hydrofining reaction, the reactant obtained is sent into separation column and is isolated petroleum naphtha and diesel oil.In described step (1), described vulcanizing agent catalyzer, urge the mixing quality of vulcanizing agent and dephenolize oil than being 1:(2-5): (4-7).
In described step (2), catalyzer (with active ingredient oxide basis) is 0.5-5:100 with the mixing quality ratio of other cut, is more preferably 1-3:100.
In described step (2), the temperature of reaction controlling described slurry hydrocracking reactor is 330-480 DEG C, reaction pressure: 12-20MPa, and volume space velocity is 0.1-3.0h
-1, hydrogen to oil volume ratio (under mark condition) is: 1000-2000.
In described step (3), isolated described hydrogen-rich gas can be used as and fills in hydrogen feeding slurry bed system hydrocracking reactor.
In described step (2), the tail oil containing catalyzer loops back slurry bed system hydrocracking reactor in whole or in part and participates in reaction.
In described step (3), control the temperature of reaction 300-400 DEG C of described fixed bed hydrogenation reactor, reaction pressure 6-12MPa, volume space velocity: 0.1-3.0h
-1, hydrogen to oil volume ratio is 400-1200.
Present system comprises the distillation tower, slurry bed system hydrocracking reactor, thermal separation system, fixed bed hydrogenation reactor and the separation column that connect successively, wherein, described distillation tower top exit is put forward phenol system be connected with catalyst slurry batch can entrance through clean, and described catalyst slurry batch can exports and is connected with the entrance of slurry bed system hydrocracking reactor.
The outlet at bottom of described thermal separation system is respectively with the entrance of slurry bed system hydrocracking reactor be out-of-bounds connected.
For the problem of depositing in background technology, contriver considers to adopt distillation tower will cut out rich phenol cut and other cut by distillation, cutting temperature can adjust according to raw material practical situation between 150-300 DEG C, preferred cutting temperature temperature is 170-260 DEG C, isolated rich phenol composition obtains dephenolize oil through clean carrying after phenol systematic position goes out crude phenols, carry out clean carry phenol can extract to greatest extent added value in coal tar higher containing phenolic compound, significantly reduce the discharge of phenolic wastewater in technique simultaneously, reduce environmental pollution, crude phenols can obtain crude phenols byproduct further, refine and obtain smart phenolic product.For clean carry phenol after the dephenolize oil that obtains, contriver finds, when in dephenolize oil, phenol content is lower than 3.5wt%, can be used as solvent oil add in catalyst slurry batch can with catalyzer, vulcanizing agent carries out being mixed and made into catalyst mix slurry, dephenolize oil is substituted conventional solvent oil Kaolinite Preparation of Catalyst mixed slurry and has some benefit following: (1) inherently stems from coal tar raw material due to dephenolize oil, there is not the compatibility issues of oil product, therefore the catalyst mix slurry prepared for raw material with it better can mix with distilling other cut be partitioned into, the dispersion of better promoting catalyst in other cut.(2) because the phenols in dephenolize oil is substantially removed, dephenolize oil can not cause disadvantageous effect to the activity of catalyzer or life-span.(3) phenol technique is put forward by clean, dephenolize oil replace solvents oil is made to enter system, save production cost, farthest utilize raw material, split by distillation and clean and carry phenol, phenol in coal tar is removed in advance, in subsequent technique material, phenol content significantly reduces the generation that can reduce waste water in hydrogenation process, thus avoid disadvantageous effect is caused to fixed bed hydrogenation reactor inner catalyst, solve the various problems that in technique, side reaction generation water brings, also reduce the consumption of hydrogen.(4) added value of phenol products itself is high, and particularly the high middle coalite tar containing phenols, can improve the economic return of whole technique; Simultaneously due to the extraction of phenols, reduce the hydrogen consumption of follow-up hydrogenation system.
The described clean method carrying phenol can adopt existing environment amenable various coal tar to put forward phenol technology, if the patent No. is CN201410080517.6, the clean phenol technique of carrying that denomination of invention is the separation method of phenolic compound and nitrogenous compound " in the coal tar ", its technique is simple, environmentally friendly, do not produce phenolic wastewater, can Fast synchronization removes phenols chemical combination and nitrogenous compound, removal effect is good.
Catalyzer in described catalyst mix slurry can use molybdenum base, iron-based, the catalyzer of Ni-based or complex class, described vulcanizing agent can use sulphur, dithiocarbonic anhydride, one or more in dimethyl thioether, in the present invention, owing to using dephenolize oil as solvent oil, reduce the compatibility issues of different oil product, make the dispersiveness of catalyzer better, and then improve the work-ing life of catalytic effect and catalyzer, therefore vulcanizing agent catalyzer, urge the mixing quality of vulcanizing agent and dephenolize oil than being 1:(2-5): (4-7), catalyzer (with active ingredient oxide basis) is 0.5-5:100 with the mixing quality ratio of other cut, more be preferably 1-3:100.
Beneficial effect:
1) introducing is clean puies forward phenol technique, and what the added value to greatest extent in extraction coal tar was higher contains phenolic compound, significantly reduces the discharge of phenolic wastewater simultaneously, minimizing environmental pollution.In addition, due to the extraction containing phenolic compound, can reduce hydrogen consumption in later stage hydrogenation process, the water produced after simultaneously also can reducing phenols hydrogenation is on catalyst activity and the impact in life-span.Dephenolize oil belongs to light oil raw material and can directly enter in system as solvent oil use, reduces production cost.
2) solvent oil of the oil of the dephenolize after carrying phenol as Kaolinite Preparation of Catalyst slurry is cleaned in employing, because dephenolize oil inherently stems from coal tar raw material, there is not the compatibility issues of oil product, mix can better disperse in coal tar by promoting catalyst with coal tar be therefore called slurry with catalyst preparing after.Again because the phenols in dephenolize oil substantially removes, disadvantageous effect can not be caused to the activity of catalyzer or life-span.
3) adopt slurry bed system hydrocracking and fixed bed hydrogenation combination process, substantially increase the adaptability of raw material, also improve the handiness of operation.Slurry bed system hydrocracking also can process the coal tar that solid content is higher and carbon residue is higher, and passable the supplementing online and get rid of outward of catalyzer, thus ensure that reactor can long-term operation.Meanwhile, adopt tail oil circulation technology, improve the utilization ratio of raw material.And fixed bed hydrogenation both can slough the heteroatomss such as most of sulphur, nitrogen, oxygen and metal in raw material, improved the quality of oil product; Can be worth with improve diesel oil distillate 16 by hydrogenation aromatics-removing again, obtain the oil product of high-quality.
4) present invention process is simple, raw material availability is high, environmentally friendly, production cost and running cost is low, it is simple to safeguard, improve catalyzer work-ing life, the system long-term stability of guarantee is run, environmentally friendly, system is simple and reliable, easy maintenance, product and byproduct yield high, there is wide market application foreground.
Accompanying drawing explanation
Fig. 1 is present invention process schema and system diagram.
Wherein, 1-catalyzer raw material; 2-catalyst premixing and vulcanizing boiler; 3-coal tar; 4-distillation tower; 5-slurry bed system hydrocracking reactor; 6-is clean puies forward phenol system; 7-thermal separation system; 8-fixed bed hydrogenation reactor; 9-separation column; 10-hydrocarbon gas; 11-gasoline fraction; 12-diesel oil distillate; 13-residual oil; The outer whipping oil of 14-; 15-crude phenols; 16-hydrogen.
Embodiment
System embodiment:
The top exit of distillation tower 4 is connected with the clean entrance putting forward phenol system 6, the described clean oil phase outlet putting forward phenol system 6 is connected with the entrance of catalyst slurry batch can 2, the outlet at bottom of described distillation tower 4 is all connected with the entrance of slurry bed system hydrocracking reactor 5 with the outlet of catalyst slurry batch can 2, the outlet of described slurry bed system hydrocracking reactor 5 connects thermal separation system, pneumatic outlet is arranged at described thermal separation system 7 top, middle part has oil phase to export, bottom has tail oil to export, described oil phase outlet is connected and fixed bed hydroprocessing reactor 8 and separation column 9 successively, the tail oil outlet of described thermal separation system 7 is respectively with the entrance of slurry bed system hydrocracking reactor be out-of-bounds connected.
Process example:
(1) feed coal tar 3 is sent into distillation tower 4 and isolate rich phenol cut and other cut, distillation temperature is 150-300 DEG C, and pressure is normal pressure.Described rich phenol cut enters clean phenol system 6 (this system adopts the patent No. to be that the processing method of CN201410080517.6 is carried out) of putting forward to carry out clean phenol of carrying and obtains dephenolize oil and crude phenols 15, dephenolize oil is sent into catalyst slurry batch can 2 and is mixed and made into catalyst pulp as solvent oil and catalyzer and vulcanizing agent, described vulcanizing agent catalyzer, urges the mixing quality of vulcanizing agent and dephenolize oil than being 1:(2-5): (4-7).
(2) sulfuration Kaolinite Preparation of Catalyst slurry is carried out after the mixing of catalyzer raw material, solvent and vulcanizing agent, the condition of sulfuration is: hydrogen to oil volume ratio (under mark condition): 400-600, temperature 230 DEG C of sulfuration 3-5h, sulfuration 3-5h at 320 DEG C, hydrogen pressure 3-6MPa, vulcanizing agent is dimethyl disulfide.Sulfuration completes the catalyst pulp obtained and mixes with other cut obtained in step (1) and send into hydrogen 16 in slurry bed system hydrocracking reactor 5 and carry out hydrocracking reaction under existing, catalyzer (with active ingredient oxide basis) is 0.5-5:100 with the mixing quality ratio of other cut, is more preferably 1-3:100.The temperature of reaction controlling described slurry hydrocracking reactor 5 is 330-480 DEG C, reaction pressure: 12-20MPa, and volume space velocity is 0.1-2.0h
-1hydrogen to oil volume ratio is: 1000-2000, the reactant obtained sends into thermal separation system 7, and (working pressure scope is: normal pressure-25MPa, operating temperature range is: 200-480 DEG C) isolate hydrogen-rich gas, lightweight oil and the tail oil containing catalyzer, hydrogen-rich gas can be used as hydrogen and sends in slurry bed system hydrocracking reactor 5 and catalyst premixing and vulcanizing boiler 2, tail oil component loops overfall state bed hydroprocessing cracking case 5 containing catalyzer participates in reaction, and rest part is outer whipping oil 14.
(3) lightweight oil obtained in step (2) is sent into fixed bed hydrogenation reactor 8 and carry out the further Arene removal of hydrofining reaction, remove the heteroatomss such as sulphur, nitrogen, oxygen and metal, control the temperature of reaction 300-400 DEG C of described fixed bed hydrogenation reactor 8, reaction pressure 6-12MPa, volume space velocity 0.1-3.0h
-1, hydrogen to oil volume ratio is 400-1200.The reactant obtained is sent into separation column 9 and is isolated hydrocarbon gas 10, gasoline fraction 11, diesel oil distillate 12 and residual oil 13.
Select a kind of typical middle coalite tar as test raw material below, through dewatering and desalting with after removing the process such as mechanical impurity, the character of coal tar raw material is as table 1:
The character of table 1 coal tar raw material
Embodiment processing condition are as shown in table 2, and product slates is as shown in table 3.The catalyzer that wherein slurry bed system hydrocracking reactor 5 uses is heterogeneous composite catalyst, wherein aluminum oxide 24wt%, ferric oxide 50wt%, nickel oxide 6wt%, molybdenum oxide 20wt%, and particle diameter is 5-100 μm; What fill in fixed bed hydrogenation reaction 8 is Hydrobon catalyst, and its composition and character are: molybdenum oxide 20wt%, nickel oxide 8wt%, carrier is gama-alumina.The pore volume of catalyzer is 0.5cm
3/ g, specific surface area is 180m
2/ g.
Table 2 embodiment 1,2, the processing condition of 3,4
Table 3 products therefrom yield distribution
Claims (9)
1. coal tar cleans and puies forward the method that phenol back end hydrogenation produces fuel oil, it is characterized in that, comprises the following steps:
(1) coal tar is sent into distillation tower normal pressure and isolate rich phenol cut and other cut, described rich phenol cut enters clean phenol system of putting forward to carry out clean phenol of carrying and obtains the dephenolize oil of phenol content lower than 3.5wt%, and dephenolize oil is sent into catalyst slurry batch can and made catalyst pulp as solvent oil with catalyzer and vulcanizing agent mixing sulfuration;
(2) mixed with other cut obtained in step (1) to send under hydrogen in slurry bed system hydrocracking reactor exists by catalyst pulp and carry out hydrocracking reaction, the reactant obtained is sent into thermal separation systematic position and is gone out hydrogen-rich gas, lightweight oil and the tail oil containing catalyzer;
(3) lightweight oil obtained in step (2) is sent into fixed bed hydrogenation reactor and carry out hydrofining reaction, the reactant obtained is sent into separation column and is isolated petroleum naphtha and diesel oil.
2. coal tar as claimed in claim 1 cleans and puies forward the method that phenol back end hydrogenation produces fuel oil, it is characterized in that, in described step (1), the mixing quality of described vulcanizing agent, catalyzer and dephenolize oil is than being 1:(2-5): (4-7).
3. coal tar as claimed in claim 1 cleans and puies forward the method that phenol back end hydrogenation produces fuel oil, it is characterized in that, in described step (2), catalyzer (with active ingredient oxide basis) is 0.5-5:100 with the mixing quality ratio of other cut.
4. the coal tar as described in claim 1 or 3 cleans puies forward the method that phenol back end hydrogenation produces fuel oil, it is characterized in that, in described step (2), control the temperature of reaction of described slurry hydrocracking reactor: 330-480 DEG C, reaction pressure: 10-20MPa, volume space velocity is 0.1-3.0h
-1, hydrogen to oil volume ratio is: 1000-2000.
5. coal tar as claimed in claim 1 cleans and puies forward the method that phenol back end hydrogenation produces fuel oil, it is characterized in that, in described step (3), isolated described hydrogen-rich gas can be used as and fills in hydrogen feeding slurry bed system hydrocracking reactor.
6. coal tar as claimed in claim 1 cleans and puies forward the method that phenol back end hydrogenation produces fuel oil, it is characterized in that, in described step (2), the tail oil containing catalyzer loops back slurry bed system hydrocracking reactor in whole or in part and participates in reaction.
7. the coal tar as described in claim 1 or 5 or 6 cleans puies forward the method that phenol back end hydrogenation produces fuel oil, it is characterized in that, in described step (3), control the temperature of reaction 300-400 DEG C of described fixed bed hydrogenation reactor, reaction pressure 6-12MPa, volume space velocity: 0.1-3.0h
-1, hydrogen to oil volume ratio: 400-1200.
8. the system of preparing fuel oil with coal oil hydrogenation product, it is characterized in that, comprise the distillation tower, slurry bed system hydrocracking reactor, thermal separation system, fixed bed hydrogenation reactor and the separation column that connect successively, wherein, described distillation tower top exit is put forward phenol system be connected with catalyst slurry batch can entrance through clean, and described catalyst slurry batch can exports and is connected with the entrance of slurry bed system hydrocracking reactor.
9. the system of preparing fuel oil with coal oil hydrogenation product as claimed in claim 8, is characterized in that, the outlet at bottom of described thermal separation system is respectively with the entrance of slurry bed system hydrocracking reactor be out-of-bounds connected.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106987267A (en) * | 2017-04-14 | 2017-07-28 | 太原理工大学 | A kind of hydrocracking unit and technique |
| CN108300511A (en) * | 2018-03-13 | 2018-07-20 | 中国五环工程有限公司 | Middle coalite tar two-stage hydrogenation treatment process and its system |
| CN113337308A (en) * | 2021-05-26 | 2021-09-03 | 洛阳瑞华新能源技术发展有限公司 | Multi-element dispersant slurry of heavy oil suspension bed hydrogenation catalyst |
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| CN103789026A (en) * | 2014-01-29 | 2014-05-14 | 河南龙成煤高效技术应用有限公司 | Processing method for coal tar fluidized bed hydrogenation of heterogeneous catalyst |
| US20150136660A1 (en) * | 2013-11-19 | 2015-05-21 | Uop Llc | Process for removing a contaminant from coal tar |
| CN205313469U (en) * | 2015-11-17 | 2016-06-15 | 中国五环工程有限公司 | System for coal tar hydrogenation for production fuel oil |
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Patent Citations (3)
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| US20150136660A1 (en) * | 2013-11-19 | 2015-05-21 | Uop Llc | Process for removing a contaminant from coal tar |
| CN103789026A (en) * | 2014-01-29 | 2014-05-14 | 河南龙成煤高效技术应用有限公司 | Processing method for coal tar fluidized bed hydrogenation of heterogeneous catalyst |
| CN205313469U (en) * | 2015-11-17 | 2016-06-15 | 中国五环工程有限公司 | System for coal tar hydrogenation for production fuel oil |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106987267A (en) * | 2017-04-14 | 2017-07-28 | 太原理工大学 | A kind of hydrocracking unit and technique |
| CN106987267B (en) * | 2017-04-14 | 2018-11-09 | 太原理工大学 | A kind of hydrocracking unit and technique |
| CN108300511A (en) * | 2018-03-13 | 2018-07-20 | 中国五环工程有限公司 | Middle coalite tar two-stage hydrogenation treatment process and its system |
| CN108300511B (en) * | 2018-03-13 | 2023-12-15 | 中国五环工程有限公司 | Two-stage hydrotreating process and system for medium-low temperature coal tar |
| CN113337308A (en) * | 2021-05-26 | 2021-09-03 | 洛阳瑞华新能源技术发展有限公司 | Multi-element dispersant slurry of heavy oil suspension bed hydrogenation catalyst |
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