CN106701186A - Method used for processing high temperature coal tar - Google Patents
Method used for processing high temperature coal tar Download PDFInfo
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- CN106701186A CN106701186A CN201510769120.2A CN201510769120A CN106701186A CN 106701186 A CN106701186 A CN 106701186A CN 201510769120 A CN201510769120 A CN 201510769120A CN 106701186 A CN106701186 A CN 106701186A
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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
- C10G69/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one other conversion process
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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
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/04—Diesel oil
Abstract
The invention provides a method used for processing high temperature coal tar. The method comprises following steps: high temperature coal tar is mixed with solvent naphtha, an obtained mixture is delivered into a demetalization reactor, the mixture is reacted with a filling material, an obtained effluent is delivered into a water washing tower to contact with fresh water, an obtained mixed material is delivered into a dehydrating tower, metal-free high temperature coal tar and water are obtained via separation, the metal-free high temperature coal tar is delivered into a boiling-bed reactor for hydrogenation reaction, an obtained reaction effluent is subjected to flash evaporation dehydration fractionation so as to obtain a light fraction and a heavy fraction, the light fraction is delivered into a fixed bed reactor for hydrogenation reaction, an obtained reaction product is subjected to separation so as to obtain gas, naphtha, and diesel oil, all of the heavy fraction is recycled back to the boiling-bed reactor for circular process, or a part of the heavy fraction is recycled back to the boiling-bed reactor, and the rest heavy fraction is discharged. The method is capable of removing metal in high temperature coal tar at mild conditions, and delaying metal inactivation of catalysts in hydrogenation reactors and increasing of bed pressure drop.
Description
Technical field
The invention belongs to field of coal tar deep processing, and in particular to high temperature coal-tar low temperature, low cost, fast eliminating metal simultaneously carry out the process of hydrotreating.
Background technology
Black or dark brown viscous liquid with pungent odour that coal tar is generated when being coal destructive distillation,Abbreviation tar,It is different according to heating final temperature,Coal tar low three kinds of coal tar high in being divided into,Wherein 500 DEG C -600 DEG C of coalite tar,700 DEG C -900 DEG C of medium temperature coal tar,900 DEG C -1100 DEG C of high temperature coal-tar,Its processing temperature is different,The composition and property of correspondence coal tar have very big difference,Especially high temperature coal-tar property is the most inferior,Middle coalite tar and high temperature coal-tar are two kinds of completely different tar,Composition without,Water content is different,Also difference is very big for tenor,High temperature coal-tar is a kind of material of dark oil,There is special odor,Compared with middle coalite tar,High temperature coal-tar density is big,Carbon residue is high,Condensed-nuclei aromatics content is high,Especially with colloid,The heavy constituent content such as asphalitine is high,Tenor is high.Containing 10% ~ 30% moisture content in high temperature coal-tar, and the state of Water-In-Oil is presented.Coalite tar processing method is not appropriate for processing high temperature coal-tar in, it is necessary to find new process route and process conditions.
As economic development and light-weight fuel oil demand constantly increase, coal tar hydrogenating production light-weight fuel oil is increasingly obtained the favor of tar producer, middle coalite tar hydrogenation production light Fuel oil tech is relatively ripe, in the industry cycle promotes more.But middle coalite tar and high temperature coal-tar are two kinds of completely different tar, nature difference is very big, it is relatively fewer that high temperature coal-tar is hydrogenated with industrialized device at present, it is reported that industrialized device has 100,000 tons of industrialized units of Qitaihe Baotailong Coal Chemical Industry Co., Ltd. at present, it uses high temperature coal-tar back-end crop technology, by the removing of the colloid in coal tar, asphalitine and mechanical admixture, light component is carried out into hydrotreating, in addition, not yet document report has industrialized plant running.Cause high temperature coal-tar to fail extensive industrialized reason and constitute much relations with its property, wherein one of reason is that high temperature coal-tar heavy constituent content is high, especially colloid, the condensed-nuclei aromatics content such as asphalitine is high, and wherein corresponding Fe, Ca, the tenors such as Na are especially high, in using traditional fixed bed hydrogenation processing procedure, these metals can be deposited in catalyst surface or bed space after being removed, catalyst is caused to inactivate or bed pressure drop rising, especially Hydrodemetalation catalyst superficial metal deposition amount is big, catalyst deactivation rate and pressure drop rise speed especially cause device shortening service cycle soon.
Patent CN1676583A describes a kind of high temperature coal tar hydrocracking technique, wherein high temperature coal tar introduces heating furnace and mixes with hydrogen, enter hydrofining reactor after mixing, again hydrofining reactor is returned to through the hydrogen isolated into high-pressure separator that exchanges heat through circulating hydrogen compressor, generation oil enters low pressure separator, enter deoxidation tower after low point of fuel oil of sub-department, enter fractionating column after further taking off fuel gas, gasoline is obtained after fractionation, diesel oil and lubricating oil, tail oil enter hydrocracking reactor.A large amount of metals of content etc. are easily caused the component that catalyst inactivation and bed pressure drop rise in high temperature coal tar in this patent, directly processed using traditional hydrofining reactor in the case where not anticipated to raw material, catalyst deactivation rate can be caused to accelerate and bed pressure drop rising, then cause device shortening service cycle.
Patent CN200610105277.6 describes a kind of power plant's purification method of coal tar, needs to prepare miscella in the method, adds demulsifier, then heats, and it is de- to respectively enter one-level electricity, and the step such as two grades of electricity are de- and three-level electricity is de-, step is relative complex and relatively costly.
The content of the invention
It is big for tenor in current high temperature coal-tar, carry out the shortcoming that catalyst for demetalation metal deposition capability is big in hydrogenation reactor, deactivation rate is fast during hydrogenation reaction, the present invention provides a kind of high temperature coal-tar processing method, the existence form and actual tests result of metal in the coal tar that Binding experiment research finds, metal in high temperature coal-tar is removed under relaxing process conditions, purification coal tar raw material, slow down metal inactivation and the rising of bed pressure drop of catalyst in hydrogenation reactor, for high temperature coal-tar provides a kind of feasible hydrotreating method.
Found by studying, the existence form of metal has very big difference with the existence form of metal in traditional residual oil in high temperature coal-tar, metal is mainly the metals such as Ni, V in residual oil, and many presence in the form of porphyrin metal complex, due in the heavy constituent colloid and asphalitine that are embedded in residual oil these metals more, it is necessary in the presence of catalyst and hydrogen high temperature removal；And the metal in high temperature coal-tar is mainly with the presence of the metal oxide forms such as Fe, Ca, Na, Ni, V tenor are little, this formed process is relevant, coal steam needs Water spray to cool down during High T-emperature Carbonization, the salt such as Ca, Mg in water can enter in coal tar, while having substantial amounts of coal ash, furnace wall breakage thing and some mineral matters during the dry distillation of coal（Calcite, albite）Deng doping wherein, these materials can carry substantial amounts of alkaline metal oxide（CaO, Na2O、MgO、Fe2O3）Into in high temperature coal-tar, in high temperature coal-tar storage simultaneously and transportation, enter coal tar because the reasons such as corrosive pipeline also result in the part metals ion such as Fe, as the above analysis, metal in high temperature coal-tar is with the presence of being greatly with mineral form, so if it is clearly contretemps to be applied on coal tar metal removal using traditional demetallated mode of residual oil again.But contain 10% ~ 30% moisture, and the state that Water-In-Oil is presented more due to high temperature coal-tar, there is a certain degree of emulsification, find to be difficult to be demulsified coal tar and remove metal therein using the general demulsifier of tradition in process of the test.
Based on above-mentioned discovery, the present invention provides a kind of high temperature coal-tar processing method, and methods described includes following content：
（1）The filler that high temperature coal-tar merges after preheated to 150~250 DEG C into filling in demetalization processor, with demetalization processor with oil miscible solvent is fully contacted and is reacted；
（2）Step（1）The reaction effluent for obtaining enters water scrubber, is fully contacted with fresh water, the metal inorganic substance for coming is dissociateed in reaction effluent and is dissolved into water；
（3）Step（2）The mixture for obtaining enters dehydrating tower, carries out water-oil separating, obtains removing the high temperature coal-tar and water after metal；
（4）Step（3）The high temperature coal-tar for obtaining carries out hydrogenation reaction after mixing with hydrogen into fluidized bed reactor, and reaction effluent obtains light component and heavy constituent by after flash-evaporation dehydration, being fractionated into；
（5）Step（4）Isolated light component enters fixed bed reactors after mixing with hydrogen, and hydrogenation reaction is carried out in the presence of a catalyst, and gas, naphtha and diesel oil are obtained after product is separated；
（6）Step（4）Isolated heavy constituent all returns to fluidized bed reactor circular treatment, or part returns to fluidized bed reactor, and device is thrown away outside remainder.
In the inventive method, the high temperature coal-tar is the high temperature coal-tar obtained through destructive distillation or coking for heating final temperature more than 900 DEG C, and the boiling range of the high temperature coal-tar is 120 DEG C ~ 650 DEG C.
In the inventive method, the boiling range of the solvent naphtha is 65~450 DEG C, preferably 120~400 DEG C, more preferably 150~320 DEG C, in the composition of the solvent naphtha, alkane and naphthene content are 70~90%, can be specifically one or several the mixtures in hydrofining diesel oil, hydrofinishing naphtha, hydrofinishing washing oil, hydrofinishing light oil, hydrofinishing carbolic oil.
In the inventive method, step（1）Described in the mass ratio of solvent naphtha and high temperature coal-tar be 1:20~1:3, preferably 1:10~1:5.
In the inventive method, the step（1）In can also add auxiliary agent, the auxiliary agent is alcohols material, can be monohydric alcohol or polyalcohol, preferably monohydric alcohol, can be specifically one or more in methyl alcohol, ethanol, isopropanol, sec-butyl alcohol.
In the inventive method, the promoter addition is the 1/10000~1/100 of raw material weight of oil；It is preferred that 1/1000~1/150.
In the inventive method, the filler of filling can be one or several in ceramic ring, quartz sand, activated carbon, diatomite, silica, aluminum oxide, zeolite, preferably ceramic ring, diatomite, activated carbon and silica in the demetalization reactor；The aperture of the filler is 200nm~50 μm, preferably 300nm~10 μm.
In the inventive method, 2~5 layers of filling of filler point in the demetalization reactor, it is preferred that dividing 3~4 layers of filling, and along Flow of Goods and Materials direction filler aperture from large to small, also from large to small, the pore size difference of adjacent two layers filler is 50 nm~1000 nm to bed voidage, to those skilled in the art simultaneously, when dividing multilayer filling filler, the ratio of multilayer filler is that those skilled in the art can determine by existing knowledge.
In the inventive method, the demetalization reactor can be two and be arranged in parallel, and when wherein one reactor reaches processing limit, switch another demetalization reactor.
In the inventive method, the filler of filling is different from traditional Hydrodemetalation catalyst in demetalization reactor, and filler herein has very strong appearance dirt and interception capacity, but does not have catalysis activity substantially；When therefore can avoid traditional catalyst for demetalation because of high-temperature hydrogenation caused by aromatic hydrocarbons polycondensation the problems such as catalyst coking.
In the inventive method, step（4）Middle light component and heavy constituent cutting temperature are 320 DEG C~400 DEG C, preferably 340 DEG C~360 DEG C, the cutting temperature of weight component can be suitably adjusted according to feedstock property and ebullating bed reactor area temperature rise situation.
In the inventive method, step（4）Described in the reaction condition of fluidized bed reactor be：300 DEG C~400 DEG C of reaction temperature, preferably 340 DEG C~380 DEG C, 8~18MPa of reaction pressure, preferably 10~16MPa, 0.2~8.0h of volume space velocity-1, preferably 0.4~4.0h-1, hydrogen to oil volume ratio 100:1~1500:1, preferably 600:1~1200:1.
In the inventive method, step（5）Described in the operating condition of fixed bed reactors be：240~380 DEG C of reaction temperature, preferably 280~340 DEG C, 3~18MPa of reaction pressure, preferably 8~16MPa, 0.1~4.0h of volume space velocity-1, preferably 0.4~2.0h-1, hydrogen to oil volume ratio 100:1~1500:1, preferably 500:1~1300:1
In the inventive method, fixed bed reactors filling Hydrobon catalyst, generally with silicon-containing alumina or aluminum oxide as carrier, with group VIB and/or group VIII metal as active metal component, the preferred molybdenum of group VIB and/or tungsten, the VIIIth preferred cobalt of race or/and nickel.In described Hydrobon catalyst, group VIII metal content is calculated as 2wt% ~ 12wt% with oxide, and group VIB tenor is calculated as 5wt% ~ 25wt% with oxide.The Hydrobon catalyst can be prepared by prior art, it is also possible to select business Hydrobon catalyst.FDS-4A, 481-3, FH-40 that business Hydrobon catalyst such as Fushun Petrochemical Research Institute develops etc..
In the inventive method, catalyst in described fluidized bed reactor is the hydrofinishing microspheric catalyst of the water resistant developed for coal tar, with group VIB and group VIII metal as active metal component, the wherein preferred molybdenum of group VIB and/or tungsten, the preferred cobalt of group VIII metal or/and nickel, metal active constituent is cobalt, nickel, molybdenum, one or more in tungsten, auxiliary agent can be contained in catalyst for refining, such as K, P, Mg, one or more in Zr and Ca, group VIII metal content is calculated as 3wt% ~ 10wt% with oxide, group VIB tenor is calculated as 6wt% ~ 30wt% with oxide.
In the inventive method, the gas-liquid separator and fractionating column are current commercial plants conventional and be separation equipment well-known to those skilled in the art.
Compared with prior art, the inventive method has the following advantages that：
1st, in the inventive method, it is found that the metal in high temperature coal-tar exists with inorganic salt form, metal impurities therein can be removed under the relative operating condition for relaxing using the inventive method, it is to avoid problem of the conventional method using hydrogenation high temperature removal high cost.
2nd, the inventive method operates the metal in removing coal tar at a lower temperature, and easy polycondensation causes the problem that catalyst is inactivated at high temperature can to avoid the unsaturated hydrocarbons such as alkadienes in coal tar.
3rd, in the inventive method, the demetalization processor inner stuffing is without carried metal, and aperture is big, retention and holds that dirty ability is strong, cost less than the carried metal in conventional method catalyst for demetalation, while being capable of the metallic salt that removes of effectively catching.
4th, in the inventive method, it is used as precipitating reagent by using solvent naphtha, the colloidal stability of system can be destroyed by adding solvent naphtha, on the one hand the viscous force between original component is reduced, on the other hand the heavy constituents such as the asphalitine in Jiao He centers are parsed, the components precipitates such as the toluene insolubles and mechanical admixture that are most suspended in system at last get off, and simultaneous overwhelming majority precipitated metal gets off.
5th, in the inventive method, it is similar to the oxygenatedchemicals aldehydes matter property in coal tar because alcohols material contains hydroxyl after adding auxiliary agent alcohols material, can reach and dissolve each other, the metal inorganic salt hydrophily come so is dissociateed in coal tar strong, have part metals and be dissolved into alcohols first, and in dehydrating tower, alcohols is miscible with water, and alcohol-water mixture does not dissolve each other with coal tar raw material, such alcohols carries salt and enters in water, and realization extracts metal inorganic salt from coal tar.
6th, using fluidized bed reactor and correspondence catalyst treatment coal tar, the heat discharged during coal tar hydrogenating can effectively be disperseed, it is to avoid focus occurs, and helps to realize that reactor temperature is homogeneous, beneficial to reaction；Boiling-bed catalyst is in the bed pressure drop that aromatic hydrocarbons material reaction green coke high is caused can be avoided to rise problem under back-mixing state simultaneously.
Specific embodiment
Technical scheme is further illustrated below by specific embodiment, but is not limited to the embodiment.
The high temperature coal-tar raw material and solvent oil nature that the embodiment of the present invention is used are listed in table 1 respectively, and demetalization processor process conditions are shown in Table 2.Ceramic ring, diatomite, four kinds of fillers of activated carbon and silica are loaded in direction respectively from top to bottom in the demetalization processor, the aperture of four kinds of fillers is followed successively by 5 ~ 10 μm, 1 ~ 3 μm, 500nm ~ 900nm, 300 ~ 500nm, the admission space ratio of four kinds of fillers is 30:25:25:20, naphtha and diesel fuel mixtures that flux oil is obtained for hydrotreating.
The catalyst of filling is the hydrofinishing microspheric catalyst of the water resistant developed for coal tar in the fluidized bed reactor, with group VIB as active metal component, wherein preferred molybdenum and/or tungsten, auxiliary agent can be contained in catalyst for refining, such as one or more in K, P, Mg, Zr and Ca, group VIB tenor is calculated as 6wt% ~ 30wt% with oxide.Catalyst in reactor reserve is 60%；
Fixed bed reactors load Hydrobon catalyst, with aluminum oxide as carrier, with group VIB as active metal component, and preferably molybdenum and/or tungsten.In described Hydrobon catalyst, group VIB tenor is calculated as 5wt% ~ 25wt% with oxide.The Hydrobon catalyst is the FH-40 catalyst that Fushun Petrochemical Research Institute develops.
The coal tar of table 1 and dilution oil nature
Embodiment 1
Test raw material is high temperature coal-tar described in table 1, and solvent naphtha and auxiliary agent are added in demetalization processing procedure, and auxiliary agent is ethanol, and concrete technology condition is shown in Table 2, and reaction result is shown in Table 3, table 4 and table 5.
Embodiment 2
Test raw material is high temperature coal-tar described in table 1, and solvent naphtha and auxiliary agent are added in demetalization processing procedure, and auxiliary agent is ethanol, and concrete technology condition is shown in Table 2, and reaction result is shown in Table 3, table 4 and table 5.
Embodiment 3
Test raw material is middle coalite tar described in table 1, and solvent naphtha is added in demetalization processing procedure, and concrete technology condition is shown in Table 2, and reaction result is shown in Table 3, table 4 and table 5.
Embodiment 4
Test raw material is high temperature coal-tar described in table 1, and solvent naphtha is added in demetalization processing procedure, but is added without auxiliary agent, and concrete technology condition is shown in Table 2, and reaction result is shown in Table 3, table 4 and table 5.
Comparative example 1
It is raw material that comparative example 1 uses high temperature coal-tar, but solvent naphtha and auxiliary agent are added without in processing procedure, still use conventional methods and processed, for ease of comparing, HDM treatment is carried out to the raw material using ebullated bed-fixed bed group technology and traditional catalyst for demetalation, reaction condition is that temperature is 280, and hydrogen dividing potential drop is 15MPa, hydrogen to oil volume ratio is 900, and volume space velocity is 0.5h-1, ebullated bed and fixed bed point hydrogenation conditions are shown in Table 2, and result of the test is shown in Table 3.
The demetalization processor of table 2 and ebullated bed-fixed bed hydrogenation reactor reaction condition
Metal removal effect contrast under the conditions of the different disposal of table 3
The different material of table 4 is hydrogenated to the contrast of naphtha property
The different material of table 5 is hydrogenated to the contrast of diesel oil property
Claims (15)
1. a kind of high temperature coal-tar processing method, methods described includes following content：
（1）The filler that high temperature coal-tar merges after preheated to 150~250 DEG C into filling in demetalization processor, with demetalization processor with oil miscible solvent is fully contacted and is reacted；
（2）Step（1）The reaction effluent for obtaining enters water scrubber, is fully contacted with fresh water, the metal inorganic substance for coming is dissociateed in reaction effluent and is dissolved into water；
（3）Step（2）The mixture for obtaining enters dehydrating tower, carries out water-oil separating, obtains removing the high temperature coal-tar and water after metal；
（4）Step（3）The high temperature coal-tar for obtaining carries out hydrogenation reaction after mixing with hydrogen into fluidized bed reactor, and reaction effluent obtains light component and heavy constituent by after flash-evaporation dehydration, being fractionated into；
（5）Step（4）Isolated light component enters fixed bed reactors after mixing with hydrogen, and hydrogenation reaction is carried out in the presence of a catalyst, and gas, naphtha and diesel oil are obtained after product is separated；
（6）Step（4）Isolated heavy constituent all returns to fluidized bed reactor circular treatment, or part returns to fluidized bed reactor, and device is thrown away outside remainder.
2. in accordance with the method for claim 1, it is characterised in that：The boiling range of the high temperature coal-tar is 120 DEG C ~ 650 DEG C.
3. in accordance with the method for claim 1, it is characterised in that：The boiling range of the solvent naphtha is 65~450 DEG C.
4. according to the method described in claim 1 or 2, it is characterised in that：The solvent naphtha is one or several in hydrofining diesel oil, hydrofinishing naphtha, hydrofinishing washing oil, hydrofinishing light oil, hydrofinishing carbolic oil.
5. in accordance with the method for claim 1, it is characterised in that：Step（1）Described in the mass ratio of solvent naphtha and high temperature coal-tar be 1:20~1:3.
6. in accordance with the method for claim 1, it is characterised in that：Step（1）Middle addition auxiliary agent, the auxiliary agent is alcohols material.
7. in accordance with the method for claim 6, it is characterised in that：The alcohols material is monohydric alcohol or polyalcohol, specifically one or more in methyl alcohol, ethanol, isopropanol, sec-butyl alcohol.
8. in accordance with the method for claim 1, it is characterised in that：The promoter addition is the 1/10000~1/100 of raw material weight of oil.
9. in accordance with the method for claim 1, it is characterised in that：The filler of filling is one or several in ceramic ring, quartz sand, activated carbon, diatomite, silica, aluminum oxide, zeolite in the demetalization reactor.
10. in accordance with the method for claim 1, it is characterised in that：The aperture of the filler is 200nm~50 μm.
11. in accordance with the method for claim 1, it is characterised in that：2~5 layers of filling of filler in the demetalization reactor point, and along Flow of Goods and Materials direction filler aperture from large to small, while bed voidage is also from large to small.
12. in accordance with the method for claim 11, it is characterised in that：The pore size difference of the adjacent two layers filler is 50 nm~1000 nm.
13. in accordance with the method for claim 1, it is characterised in that：Step（4）Middle light component and heavy constituent cutting temperature are 320 DEG C~400 DEG C.
14. in accordance with the method for claim 1, it is characterised in that：Step（4）Described in the reaction condition of fluidized bed reactor be：300 DEG C~400 DEG C of reaction temperature, preferably 340 DEG C~380 DEG C, 8~18MPa of reaction pressure, preferably 10~16MPa, 0.2~8.0h of volume space velocity-1, preferably 0.4~4.0h-1, hydrogen to oil volume ratio 100:1~1500:1, preferably 600:1~1200:1.
15. in accordance with the method for claim 1, it is characterised in that：Step（5）Described in the operating condition of fixed bed reactors be：240~380 DEG C of reaction temperature, preferably 280~340 DEG C, 3~18MPa of reaction pressure, preferably 8~16MPa, 0.1~4.0h of volume space velocity-1, preferably 0.4~2.0h-1, hydrogen to oil volume ratio 100:1~1500:1, preferably 500:1~1300:1.
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| CN106701186B (en) | 2018-03-16 |
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