CN103789026A - Processing method for coal tar fluidized bed hydrogenation of heterogeneous catalyst - Google Patents
Processing method for coal tar fluidized bed hydrogenation of heterogeneous catalyst Download PDFInfo
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Abstract
The invention relates to a processing method for coal tar fluidized bed hydrogenation of a heterogeneous catalyst. The method comprises the following four steps: pretreating coal tar raw materials; distilling and separating; carrying out fluidized bed hydrogenation and cracking on heavy fractions of coal tar; and upgrading and processing. According to the method, a fluidized bed reactor is used for carrying out a hydrogenation and cracking reaction so that the problem that partial temperatures are not uniformly distributed can be effectively reduced and avoided; the liquid-solid separation of the catalyst in the reactor can be realized so that the abrasion of a pipeline is reduced; meanwhile, a solid catalyst deposition area of the fluidized bed reactor is relatively enlarged and the separation effect of the catalyst is improved.
Description
Technical field
The invention belongs to coal chemical technology, particularly a kind of processing method of coal tar boiling bed hydrogenation of heterogeneous catalyst.
Background technology
Along with the variation of petroleum products demand structure in the day by day in short supply and world wide of China's hydrocarbon resources, market maintains sustained and rapid growth to the demand of light-weight fuel oil and the demand of heavy fuel oil (HFO) is reduced rapidly, and the deep processing technology of coal tar has become the emphasis of petroleum refining industry's exploitation.Conventional coal tar hydrogenating technology conventionally adopt fixed-bed reactor and
suspended-bed reactoralthough fixed-bed reactor cost is low, also there is the coking and the heat-obtaining problem that are difficult to overcome; In addition, want to make full use of the reaction compartment of fixed-bed reactor, many loading catalysts of need trying one's best, could improve the processing power of device, and in fixed-bed reactor, the amount of fill of catalyzer is conditional, and there is regeneration problem in catalyzer; When the main drawback of suspended-bed reactor is mobile in reactor and pipeline containing solid reactant flow, can cause more serious wearing and tearing to reactor and pipeline.And in delay coking process, a part of stock oil becomes coke, reduce raw material availability.
CN101250433A has introduced a kind of fixed bed hydrogenation reactor, and its weak point is in feed coal tar, to need to add coke inhibitor, to slow down coal tar coking reaction at high temperature, has increased the cost of the raw material coal tar hydrocracking course of processing.CN201010217358.1 provides a kind of coal tar suspension bed hydrogenation method, its weak point is that the heavy oil viscosity in the normal end in this technique is large, boiling point is high, no matter be to adopt filtering separation or centrifugation or underpressure distillation to separate, higher organic materials is contained in capital in catalyst residue, and separation costs is higher.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of processing method of coal tar boiling bed hydrogenation of heterogeneous catalyst, the method is used ebullated bed reactor to carry out hydrocracking reaction, can effectively reduce or remit the problem of local temperature skewness, and can realize the liquid-solid separation of catalyzer in reactor, and the solid catalyst negative area of ebullated bed reactor can be increased relatively, improve the separating effect of catalyzer.
For achieving the above object, the processing method of the coal tar boiling bed hydrogenation of heterogeneous catalyst of the present invention is to carry out according to the following steps:
(1) coal tar raw material pre-treatment
First adopt heating to leave standstill evaporation and ultracentrifuge processed coal tar raw material, adopt again batch still evaporation or tube furnace evaporation or electro-dewatering desalting and dewatering, then the method that adopts solvent extraction and settleability whizzer to combine, or adopt the method for super three-phase centrifugation to remove mechanical impurity;
(2) fractionation by distillation
To make respectively and be less than 260 ℃, 260～370 ℃ and be greater than 370 ℃ of three cuts by distillation through pretreated coal tar raw material, the cut that coal tar is less than to 260 ℃ carries out phenol removal, obtain dephenolize oil and crude phenols, wherein gained crude phenols further make phenolic compound;
(3) the boiling bed hydrogenation cracking of coal tar heavy cut
first prepare boiling-bed catalyst slurry oil, get the heavy distillate that is greater than 370 ℃ obtaining in coal tar boiling bed hydrogenation catalyst, vulcanizing agent, turning oil and step (2), send into together in the catalyst slurry preparation facilities with whipping device, under normal pressure, at 60～180 ℃ of temperature, mix, obtain boiling bed hydrogenation cracking catalyst slurry oil;
the boiling bed hydrogenation cracking of heavy ends, enters ebullated bed reactor by oil-catalyst slurry from the position more than beds of ebullated bed; Being greater than of obtaining in step (2) entered to boiling bed hydrogenation reactor from reactor bottom after the heavy distillate of 370 ℃ or full distillate oil mix with hydrogen and carry out cracking; Boiling bed hydrogenation reactor reaction effluent obtains liquid-phase mixing logistics and hydrogen-rich gas after separator separates; Hydrogen-rich gas continues reaction as recycle hydrogen; Liquid phase mixture flows to into atmospheric fractional tower, and tower top obtains being less than 370 ℃ of light ends oil, obtains being greater than 370 ℃ of heavy oil of the normal end at the bottom of tower, and heavy oil of the normal end is recycled directly to and in boiling bed hydrogenation reactor, carries out hydrocracking reaction as turning oil; The regeneration from discharge the bottom of boiling bed hydrogenation reactor of reacted catalyzer;
(4) upgrading processing
The boiling point that the benzoline of 260～370 ℃ that cutting in step (2) is obtained and step (3) obtain is less than the light ends oil of 370 ℃ and carries out upgrading processing, be less than the stock oil that 260 ℃ of dephenolize oil are processed as distillate upgrading together, processing oil fuel and industrial chemicals.
Active metal in described step (3) in catalyzer is one or more in nickel, cobalt, molybdenum, tungsten, chromium and iron; Carrier is one or more in aluminum oxide, silicon oxide, aluminium oxide-silicon oxide, titanium oxide.
Described catalyzer comprises by oxide weight per-cent: nickel or cobalt 0.1%～10%, molybdenum or tungsten 0.5%～25%.
Described catalyzer is extrudate or spherical.
Described granules of catalyst diameter (spherical diameter or bar shaped diameter) is 0.04～2.0 mm, and specific surface area is 50～350 m
2/ g.
Vulcanizing agent described in described step (3) is the material that can generate hydrogen sulfide under reaction conditions.
Described vulcanizing agent is sulphur or dimethyl thioether.
The solids concn of described oil-catalyst slurry is 15～50 wt%.
Hydrocracking reaction temperature in described step (3) is 300～550 ℃, reaction pressure 10～25 MPa, and air speed is 0.1～10 h
-1, hydrogen to oil volume ratio is 200～2000 ︰ 1.
Advantage of the present invention is:
1, use ebullated bed reactor to carry out hydrocracking reaction, can effectively reduce or remit the problem of local temperature skewness.
2, can realize the liquid-solid separation of catalyzer in reactor, thereby reduce the wearing and tearing of pipeline.
3, the solid catalyst negative area of ebullated bed reactor can be increased relatively, improve the separating effect of catalyzer.
Embodiment
The technical process of the coal tar boiling bed hydrogenation of heterogeneous catalyst of the present invention is:
(1) the first incoming stock oily pretreatment unit of stock oil dewaters and de-solid impurity processing, and pretreated purification stock oil (pretreated coal tar) is sent into fractionation by distillation unit.
(2) be cut into and be less than 260 ℃, 260～370 ℃ and be greater than 370 ℃ of three cuts by distillation through pretreated stock oil, the cut that coal tar is less than to 260 ℃ carries out phenol removal, obtain dephenolize oil and crude phenols, wherein crude phenols can further be refined and obtain phenolic compound.Wherein the cut cutting temperature of fractionation by distillation can be selected flexibly according to the needs of actual production and operation.Especially, if coal tar raw material oil is heavier or viscosity is too high, can not carry out fractionation by distillation, directly carry out boiling bed hydrogenation cracking.
(3) heavy distillate, coal tar boiling bed hydrogenation catalyst, vulcanizing agent and turning oil that small portion step (2) being obtained is greater than 370 ℃, join together in the catalyst slurry preparation facilities with whipping device, under normal pressure, at 60～180 ℃ of temperature, mix, obtain boiling bed hydrogenation cracking catalyst slurry oil, the solids concn of described oil-catalyst slurry can be 15～50 wt%.
Described catalyzer is the hydrotreating catalyst of this area routine, wherein the active metal of catalyzer be nickel, cobalt, molybdenum or tungsten etc. one or more.As catalyzer composition can comprise by weight percentage: nickel or cobalt are that 0.1%～10%(calculates by its oxide compound), molybdenum or tungsten are that 0.5%～25%(calculates by its oxide compound), carrier can be aluminum oxide, silicon oxide, aluminium oxide-silicon oxide, titanium oxide etc. one or more.Catalyzer is extrudate or spherical.Granules of catalyst diameter (spherical diameter or bar shaped diameter) is 0.04～2.0 mm, and specific surface area is 50～350 m
2/ g.
Described vulcanizing agent can generate for sulphur or dimethyl thioether etc. the material of hydrogen sulfide under reaction conditions.
(4) oil-catalyst slurry is sent into ebullated bed reactor from the position more than beds of ebullated bed; Heavy distillate or the full distillate oil of 370 ℃ of being greater than that step (2) is obtained mixes from reactor bottom and enters boiling bed hydrogenation reactor with hydrogen.At reaction pressure 10～25 MPa, temperature of reaction is 300～550 ℃, and air speed is 0.1～10 h
-1, hydrogen to oil volume ratio is 200～2000 ︰ 1.Boiling bed hydrogenation reactor reaction effluent obtains liquid-phase mixing logistics and hydrogen-rich gas after separator separates; Hydrogen-rich gas continues reaction as recycle hydrogen; Liquid phase mixture flows to into atmospheric fractional tower, and tower top obtains being less than 370 ℃ of light ends oil, obtains being greater than 370 ℃ of heavy oil of the normal end at the bottom of tower, and heavy oil of the normal end is recycled directly to and in boiling bed hydrogenation reactor, carries out hydrocracking reaction as turning oil; The regeneration from discharge the bottom of boiling bed hydrogenation reactor of reacted a part of catalyzer.
(5) boiling point that the benzoline of 260～370 ℃ step (2) cutting being obtained and step (4) obtain is less than the light ends oil of 370 ℃ and carries out upgrading processing, be less than the stock oil that 260 ℃ of dephenolize oil are processed as distillate upgrading together, processing oil fuel and industrial chemicals.
For further illustrating the solution of the present invention and effect, enumerate following examples, but protection scope of the present invention is not limited to the following example.
Embodiment 1
Take a kind of coalite tar as raw material, through dewatering after solid impurity pre-treatment, be cut into and be less than 260 ℃, 260～370 ℃ and be greater than 370 ℃ of three cuts through distillation, the cut that coal tar is less than to 260 ℃ carries out phenol removal, obtains dephenolize oil and crude phenols; The heavy distillate that is greater than 370 ℃ is boiling bed hydrogenation cracking stock oil, enters ebullated bed reactor and carries out hydrocracking reaction; Boiling bed hydrogenation reactor reaction effluent obtains liquid-phase mixing logistics and hydrogen-rich gas after separator separates; Hydrogen-rich gas continues reaction as recycle hydrogen; Liquid phase mixture flows to into atmospheric fractional tower, and tower top obtains being less than 370 ℃ of light ends oil, obtains being greater than 370 ℃ of heavy oil of the normal end at the bottom of tower, and heavy oil of the normal end is recycled directly to and in boiling bed hydrogenation reactor, carries out hydrocracking reaction as turning oil; The regeneration from discharge the bottom of boiling bed hydrogenation reactor of reacted a part of catalyzer.The benzoline of 260～370 ℃ and atmospheric fractional tower tower top light ends oil that distillation cutting is obtained carry out hydrogenation upgrading processing, are less than 260 ℃ of dephenolize oil together as the stock oil of distillate upgrading processing, produce light-end products oil.Feed coal tar character is in table 1, and each technique unit technological condition is in table 2, and light-end products oil main character is in table 3.
Test is to carry out on the boiling bed hydrogenation testing apparatus of 0.1 ton/day, and hydrocracking unit adopts two ebullated bed reactor series connection, and deep hydrofinishing unit adopts two fixed-bed reactor series connection.
Embodiment 2
Take coalite tar in one as raw material, through dewatering after solid impurity pre-treatment, be cut into and be less than 230 ℃ and be greater than 230 ℃ of three cuts through distillation, the cut that coal tar is less than to 230 ℃ carries out phenol removal, obtains dephenolize oil and crude phenols; The heavy distillate that is greater than 230 ℃ is boiling bed hydrogenation cracking stock oil, enters ebullated bed reactor and carries out hydrocracking reaction; Boiling bed hydrogenation reactor reaction effluent obtains liquid-phase mixing logistics and hydrogen-rich gas after separator separates; Hydrogen-rich gas continues reaction as recycle hydrogen; Liquid phase mixture flows to into atmospheric fractional tower, and tower top obtains being less than 370 ℃ of light ends oil, obtains being greater than 370 ℃ of heavy oil of the normal end at the bottom of tower, and heavy oil of the normal end is recycled directly to and in boiling bed hydrogenation reactor, carries out hydrocracking reaction as turning oil; The regeneration from discharge the bottom of boiling bed hydrogenation reactor of reacted a part of catalyzer.Atmospheric fractional tower tower top light ends oil is carried out to hydrogenation upgrading processing, be less than 230 ℃ of dephenolize oil together as the stock oil of distillate upgrading processing, produce light-end products oil.Feed coal tar character is in table 1, and each technique unit technological condition is in table 2, and light-end products oil main character is in table 3.
Test is to carry out on the boiling bed hydrogenation testing apparatus of 0.1 ton/day, and hydrocracking unit adopts two ebullated bed reactor series connection, and deep hydrofinishing unit adopts two fixed-bed reactor series connection.
Embodiment 3
Take a kind of coal-tar heavy oil as raw material, through dewatering after solid impurity pre-treatment, because feed coal tar is heavier and viscosity is larger, feed coal tar after pretreatment directly enters boiling bed hydrogenation reactor and carries out hydrocracking reaction, and reaction effluent obtains liquid-phase mixing logistics and hydrogen-rich gas after separator separates; Hydrogen-rich gas continues reaction as recycle hydrogen; Liquid phase mixture flows to into atmospheric fractional tower, and tower top obtains being less than 370 ℃ of light ends oil, obtains being greater than 370 ℃ of heavy oil of the normal end at the bottom of tower, and heavy oil of the normal end is recycled directly to and in boiling bed hydrogenation reactor, carries out hydrocracking reaction as turning oil; The regeneration from discharge the bottom of boiling bed hydrogenation reactor of reacted a part of catalyzer.Atmospheric fractional tower tower top light ends oil is carried out to hydrogenation upgrading processing, produce light-end products oil.Feed coal tar character is in table 1.Each technique unit technological condition is in table 2, and light-end products oil main character is in table 3.
Test is to carry out on the boiling bed hydrogenation testing apparatus of 0.1 ton/day, and hydrocracking unit adopts two ebullated bed reactor series connection, and deep hydrofinishing unit adopts two fixed-bed reactor series connection.
Table 1 embodiment 1～3 coal tar raw material oil nature
Table 2 embodiment 1～3 hydrocracking and hydrofining unit technological condition
The main character of table 3 embodiment 1～3 light-end products oil
Can find out from the data of table 3, the light-end products oil that the present invention obtains all reaches or approaches national high-grade fuel oil standard.
The above, only better embodiment of the present invention, not the present invention is done to any pro forma restriction, the equivalent variations embodiment that any technician makes the technology contents of above-mentioned announcement, in every case be the content that does not depart from technical solution of the present invention, any simple modification, equivalent variations and the modification above-described embodiment done according to technical spirit of the present invention, all still belong in the scope of technical solution of the present invention.
Claims (9)
1. a processing method for the coal tar boiling bed hydrogenation of heterogeneous catalyst, is characterized in that: it comprises the following steps:
(1) coal tar raw material is carried out to pre-treatment
First adopt heating to leave standstill evaporation and ultracentrifuge processed coal tar raw material, adopt again batch still evaporation or tube furnace evaporation or electro-dewatering desalting and dewatering, then the method that adopts solvent extraction and settleability whizzer to combine, or adopt the method for super three-phase centrifugation to remove mechanical impurity;
(2) fractionation by distillation
To make respectively and be less than 260 ℃, 260～370 ℃ and be greater than 370 ℃ of three cuts by distillation through pretreated coal tar raw material, the cut that coal tar is less than to 260 ℃ carries out phenol removal, obtain dephenolize oil and crude phenols, wherein gained crude phenols further make phenolic compound;
(3) the boiling bed hydrogenation cracking of coal tar heavy cut
1. first prepare boiling-bed catalyst slurry oil, get the heavy distillate that is greater than 370 ℃ obtaining in coal tar boiling bed hydrogenation catalyst, vulcanizing agent, turning oil and step (2), send into together in the catalyst slurry preparation facilities with whipping device, under normal pressure, at 60～180 ℃ of temperature, mix, obtain boiling bed hydrogenation cracking catalyst slurry oil;
2. the boiling bed hydrogenation cracking of heavy ends, enters ebullated bed reactor by oil-catalyst slurry from the position more than beds of ebullated bed; Being greater than of obtaining in step (2) entered to boiling bed hydrogenation reactor from reactor bottom after the heavy distillate of 370 ℃ or full distillate oil mix with hydrogen and carry out cracking; Boiling bed hydrogenation reactor reaction effluent obtains liquid-phase mixing logistics and hydrogen-rich gas after separator separates; Hydrogen-rich gas continues reaction as recycle hydrogen; Liquid phase mixture flows to into atmospheric fractional tower, and tower top obtains being less than 370 ℃ of light ends oil, obtains being greater than 370 ℃ of heavy oil of the normal end at the bottom of tower, and heavy oil of the normal end is recycled directly to and in boiling bed hydrogenation reactor, carries out hydrocracking reaction as turning oil; The regeneration from discharge the bottom of boiling bed hydrogenation reactor of reacted catalyzer;
(4) upgrading processing
The boiling point that the benzoline of 260～370 ℃ that cutting in step (2) is obtained and step (3) obtain is less than the light ends oil of 370 ℃ and carries out upgrading processing, be less than the stock oil that 260 ℃ of dephenolize oil are processed as distillate upgrading together, processing oil fuel and industrial chemicals.
2. the processing method of the coal tar boiling bed hydrogenation of heterogeneous catalyst as claimed in claim 1, is characterized in that: the hydrocracking reaction temperature in described step (3) is 300～550 ℃, reaction pressure 10～25 MPa, and air speed is 0.1～10 h
-1, hydrogen to oil volume ratio is 200～2000 ︰ 1.
3. the processing method of the coal tar boiling bed hydrogenation of heterogeneous catalyst as claimed in claim 1, is characterized in that: the solids concn of described oil-catalyst slurry is 15～50 wt%.
4. the processing method of the coal tar boiling bed hydrogenation of heterogeneous catalyst as claimed in claim 1, is characterized in that: the active metal in described step (3) in catalyzer is one or more in nickel, cobalt, molybdenum, tungsten, chromium and iron; Carrier is one or more in aluminum oxide, silicon oxide, aluminium oxide-silicon oxide, titanium oxide.
5. the processing method of the coal tar boiling bed hydrogenation of the heterogeneous catalyst as described in claim 1 or 4, is characterized in that: described catalyzer comprises by oxide weight per-cent: nickel or cobalt 0.1%～10%, molybdenum or tungsten 0.5%～25%.
6. the processing method of the coal tar boiling bed hydrogenation of the heterogeneous catalyst as described in claim 1 or 4, is characterized in that: described catalyzer is extrudate or spherical.
7. the processing method of the coal tar boiling bed hydrogenation of the heterogeneous catalyst as described in claim 1 or 4, is characterized in that: described granules of catalyst diameter (spherical diameter or bar shaped diameter) is 0.04～2.0 mm, and specific surface area is 50～350 m
2/ g.
8. the processing method of the coal tar boiling bed hydrogenation of heterogeneous catalyst as claimed in claim 1, is characterized in that: vulcanizing agent described in described step (3) is the material that can generate hydrogen sulfide under reaction conditions.
9. the processing method of the coal tar boiling bed hydrogenation of the heterogeneous catalyst as described in claim 1 or 8, is characterized in that: described vulcanizing agent is sulphur or dimethyl thioether.
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Cited By (6)
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| CN105296002A (en) * | 2015-11-17 | 2016-02-03 | 中国五环工程有限公司 | Method for producing fuel oils by hydrogenation after coal tar cleaning and phenol extraction and system thereof |
| CN106701159A (en) * | 2016-11-30 | 2017-05-24 | 胜帮科技股份有限公司 | Fluidized bed hydrogenation system and method of high solid content coal tar |
| CN111876196A (en) * | 2020-08-03 | 2020-11-03 | 新疆宣力环保能源有限公司 | Coal tar hydrogenation method and system |
| CN114433118A (en) * | 2020-10-30 | 2022-05-06 | 中国科学院宁波材料技术与工程研究所 | Fluidized bed hydrogenation catalyst and processing method of coal tar whole fraction |
| CN114437824A (en) * | 2020-10-30 | 2022-05-06 | 中国科学院宁波材料技术与工程研究所 | Method for producing clean fuel from coal tar whole fraction |
| CN114958425A (en) * | 2022-01-10 | 2022-08-30 | 新疆宣力环保能源股份有限公司 | Coal tar hydrogenation process using coal tar residue |
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| CN114958425A (en) * | 2022-01-10 | 2022-08-30 | 新疆宣力环保能源股份有限公司 | Coal tar hydrogenation process using coal tar residue |
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Application publication date: 20140514 |