CN101649220B - Method for simultaneously producing liquid fuel and asphalt paving materials by coprocessing coal and heavy oil - Google Patents
Method for simultaneously producing liquid fuel and asphalt paving materials by coprocessing coal and heavy oil Download PDFInfo
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- CN101649220B CN101649220B CN 200910075453 CN200910075453A CN101649220B CN 101649220 B CN101649220 B CN 101649220B CN 200910075453 CN200910075453 CN 200910075453 CN 200910075453 A CN200910075453 A CN 200910075453A CN 101649220 B CN101649220 B CN 101649220B
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Abstract
The invention relates to a method for simultaneously producing liquid fuel and asphalt paving materials by coprocessing coal and heavy oil. The method comprises the following steps: mixing coal dust, catalyst and heavy oil to prepare pulp; preheating and entering a reactor to carry out reaction; separating reaction products to separate gaseous substance, light oil, water and heavy mixture; extracting hydrogen from the separated gaseous substance through pressure swing adsorption; returning the purified hydrogen to the reactor to be used circularly, and using the remaining gas as fuel after purification; carrying out oil-water separation on the separated light oil and water to obtain the light oil and the water; leading the heavy mixture into a distilling tower to obtain coarse oil and tower bottom product through distillation separation; mixing the coarse oil and the light oil to obtain liquid fuels of gasoline, kerosene, diesel fuel, fuel oil, and the like through upgrading process; and processing the tower bottom product to get the asphalt paving materials. The invention has the advantage that under the moderate process condition, the liquid fuel and asphalt paving materials can be produced simultaneously.
Description
Technical field
The invention belongs to a kind of method of producing simultaneously liquid fuel and pitch class pavior by coal and heavy oil co-processing.
Background technology
Liquid fuel is present most important energy and material in the world, is the requisite of society, the guarantee of social civilization.Liquid fuel is mainly derived from from underground mining oil out.Oil distribution on earth is also inhomogeneous, and China is oil-poor country.
Pitch is the binder commonly used of paving the way, and its objective is building stones are bonded together.Bitumen for road use is mainly derived from oil.Pitch is as consolidating material, stand the effect of the climatic factor such as high temperature, low temperature, Atmospheric precipitation and heavy load, requires to have that enough cohesiveness, weather resistance and high temperature do not trickle, the characteristics of not embrittlement of low temperature.Special Road (heavy traffic road such as advanced road, bridge, airfield runway and the temperature difference differ larger atrocious weather highway section) needs to use high performance modified bitumen.The Trinida lake pitch is a kind of high-quality properties-correcting agent for asphalt modification.But because it derives from specific pitch lake, import price is higher than the high-quality heavy traffic paving asphalt.
Utilize prior art to make liquid fuel (direct and indirect liquefaction, the dry distillation of coal etc. such as coal) from coal, also can make bitumen for road use and performance and the similar properties-correcting agent of Trinida lake pitch (Chinese invention patent ZL99107872.1 and ZL02158702.7) from coal.
Direct coal liquefaction technology is the process that coal is transformed into liquid fuel (being designated hereinafter simply as oil) under high temperature, high hydrogen pressure condition.In order to obtain higher oily productive rate, improve hydrogen utilization ratio, except higher temperature and hydrogen pressure, also need use the circulating solvent of pre-hydrogenation, expensive catalyzer, multistage operator scheme.Caused the problem that once investment is high, process cost is high of DCL/Direct coal liquefaction.
Kerosene co-processing liquefaction technology is based on a coal liquefaction technology of conventional direct coal liquefaction technology development.With coal and petroleum residual oil co-processing, produce oil.If used residual oil has good hydrogen supply capacity, coal and residual oil have good synergistic effect under liquefaction temperature, and kerosene co-processing liquefaction technology is better than conventional direct coal liquefaction technology to a certain extent.If but used residual oil does not have good hydrogen supply capacity, not only can not improve oily productive rate, also can reduce oily productive rate (China Mining University's journal, 2003, Vol.32, No.1,48-52).
In any case but pursuing high oily yield must be take severe condition (430-470 ℃, 15-30MPa) as cost.Nonetheless, the products distribution scope of current optimization technique is (in dry ash-free basis charging raw coal): oily productive rate about 55%, aquatic products rate about 10%, residue productive rate about 30%, gas productive rate about 10%.
The H/C atomic ratio of coal is about 0.2-1, and the H/C atomic ratio of oil is about 1.6-2.0.This is to be determined by the condensed aromatics structure of coal and the alkane structure of oil.Become alkane or naphthenic hydrocarbon structure must need harsh reaction conditions the condensed aromatics structural transformation of coal.
But the petroleum residual oil simple process that derives from intermediate base and cycloalkyl is used for paving the way, and just can be used for paving the way but the residual oil that derives from paraffinic crude needs special process to process.Mainly be due to the difference on the chemical structure.The used pitch of paving the way, its chemical structure need comprise certain aromatic hydrocarbons and hydrogenation of aromatics structure.
Summary of the invention
The purpose of this invention is to provide a kind of under mild conditions co-processing coal and heavy oil, the method for producing simultaneously liquid fuel and pitch class pavior.
Present method organically combines the coal of " the poor hydrogen of rich aromatization " and the heavy oil of " the rich hydrogen of poor aromatization ", with the coal partial liquefaction.By regulating the co-processing process condition, oil and slag that the co-processing process is produced are the purpose product altogether, can greatly reduce the severity of DCL/Direct coal liquefaction process, also will reduce gas productive rate and hydrogen consumption simultaneously.Improve the DCL/Direct coal liquefaction economy from once investment, process cost and three aspects of product utilization.
The present invention includes following steps:
(1) coal dust, catalyzer and heavy oil mixed pulp;
(2) after the coal oil mixture preheating, enter reactor and react;
(3) reaction product is separated, and isolates gaseous substance, lightweight oil and water, and the heavy mixture, isolated gaseous substance is carried hydrogen by pressure-variable adsorption, and the hydrogen of purification turns back in the reactor and recycles, and remaining gas is used as fuel after purifying; Isolated lightweight oil and water carry out oily water separation, obtain lightweight oil and water;
(4) the heavy mixture enters distillation tower, obtains thick oil and bottom product through fractionation by distillation;
(5) slightly oil and lightweight oil mix, and can get gasoline, kerosene, diesel oil, fuel wet goods liquid fuel through upgrading processing;
(6) bottom product is treated, gets pitch class pavior.
Aforesaid coal is bituminous coal, brown coal.Heavy oil is normal/vacuum residuum, catalytically cracked oil, gelatin liquefaction heavy oil.
Catalyzer is the DCL/Direct coal liquefaction custom catalysts as mentioned above, and abandoning property of cheapness catalyzer such as red mud, Natural pyrite, metallurgical flying dust, high ferro coal gangue or FeSO are arranged
4Deng, Mo base hydrogenation catalyst is such as molybdenum ash MoO
3Or moly-sulfide etc., Ni-Mo base hydrogenation catalyst is such as Ni-Mo/Al
2O
3), ultra-fine high-dispersion iron catalyst.
Ultra-fine high-dispersion iron catalyst is by being prepared as follows the method preparation as mentioned above:
Method one:
With a certain amount of FeSO
4Saturated solution joins in the coal dust, stirs; (2) a certain amount of sodium sulphite saturated solution or urea saturated solution are joined in the above-mentioned coal dust, stir, make coal sample; (3) with coal sample vacuum-drying 5 hours under 80-120 ℃ of temperature, make the ultra-fine high-dispersion iron catalyst that is supported on the coal sample.(preparation method sees first three step in the ZL98102883.7 claim 1 particularly.)
Method two:
With the saturated solution of sulfur-containing anion with contain in a kind of adding coal dust in the saturated solution of iron ion and stir, make A, another kind of solution is added among the A stir again, can make the ultra-fine high-dispersion iron catalyst that is supported on the coal sample after the drying.(preparation method sees ZL 98118156.2 the first steps particularly)
Method three:
(1) in the ammoniacal liquor of high-speed stirring, disposable impouring iron salt solutions, preparation Fe (OH)
3Or Fe (OH)
2With the FeOOH precipitation, reaction end pH value is controlled to be 8-13; (2) by the centrifugal above-mentioned reaction product of supercentrifuge, obtain the iron-based hydrogel; (3) in high speed dispersor, iron-based hydrogel and an amount of coal dust and liquefaction solvent are mixed together dispersion, obtain being supported on the ultra-fine high-dispersion iron catalyst on the coal sample.(specifically seeing ZL 99103015.X)
The weight ratio of coal and heavy oil is with the metering of dry coal base as mentioned above, coal: heavy oil=2-10: 10, and the weight ratio of catalyzer and coal is with the metering of dry coal base, catalyzer: coal=0.01-50: 100.
Preheating temperature is lower 60-150 ℃ than temperature of reaction as mentioned above.
Aforesaid reaction conditions is: temperature of reaction is 300-450 ℃, and reaction pressure is 5-20MPa, and the reaction times is 0.5-2 hour.
Reactor can adopt conventional DCL/Direct coal liquefaction reactor as mentioned above, such as the forced-circulation boiling bed bioreactor in tubular reactor, U.S. CTSL and the HRI technique in German IGOR and the Japanese NEDOL technique, the pump circulation suspended-bed reactor in the Chinese Shenhua technique.
Pressure Swing Adsorption hydrogen operational condition is pressure 0.3-4MPa, temperature 30-50 ℃ as mentioned above.
Conventional sulfur removal technology is adopted in aforesaid gas sweetening, washes method, crystallization sulphur method such as pure amine absorption process, liquid-phase oxidation reduction method, copper.
Single-stage or stage separator are adopted in aforesaid separation, such as high-temperature separator, middle temperature separator or low-temperature separator.The separating unit inlet temperature is that 250-450 ℃, pressure are 5-20MPa.
Distillation tower is atmospheric distillation tower or vacuum still as mentioned above, and the atmospheric distillation tower service temperature is that 300-360 ℃, pressure are 0.1-0.2MPa, and the vacuum still service temperature is that 320-400 ℃, pressure are 0.001-0.02MPa.
Mixed upgrading processing is hydrofining, hydrocracking or reforming process from the thick oil of distillation tower with from the lightweight oil of water-and-oil separator as mentioned above.
The as mentioned above processing of base product product, comprise solvent extraction (specifically seeing ZL99107872.1) or pulverize (specifically seeing ZL02158702.7, ZL200610012547.9) getting pitch class pavior, pitch class pavior comprises pitch and asphalt modifier.
The invention has the advantages that:
1. this patent organically combines the coal of " the poor hydrogen of rich aromatization " and the heavy oil of " the rich hydrogen of poor aromatization ", produces simultaneously liquid fuel and pitch class pavior by direct coal liquefaction technology or kerosene co-processing technology;
2. can reduce the reaction severity, reduce factory and once invest and the prolonged operation expense;
3. can reduce the hydrogenation degree of depth, need not solvent cycle; Heavy component directly utilizes, and need not hydrotreatment, has greatly simplified technical process, easy handling.
Description of drawings
Fig. 1 is process flow sheet of the present invention
Embodiment
Embodiment 1
Coal/catalytically cracked oil=2/3 (wt, dry coal base), red mud are as catalyzer, and add-on is 3% (wt, dry coal base).Said mixture is preheated to 310 ℃ through preheater, and in the forced-circulation boiling bed bioreactor, reaction is 1 hour under 380-400 ℃, 10MPa hydrogen pressure condition.
Reaction product is separated under 350 ℃ of high-temperature separators, 10MPa condition, and the high-temperature separator top product enters under 200 ℃ of low-temperature separator, the 3MPa condition and is separated into gas-liquid two-phase.Gaseous substance through eight tower pressure-swing absorption apparatuss at 2.12MPa, purifying hydrogen of hydrogen under 35 ℃ of conditions, isolated hydrogen turns back in the reactor and recycles, remaining gas behind pure amine absorption process desulfurizing and purifying as fuel.Low-temperature separator bottom liquid product obtains lightweight oil through condensation, oily water separation.The high-temperature separator bottoms enters vacuum still.Under 350 ℃, 0.007MPa operational condition, obtain thick oil.
Thick oil and lightweight oil mix, and obtain gasoline, diesel oil, kerosene and fuel wet goods liquid fuel through hydrofining.
The base product product is crushed to below 5 microns, namely gets road asphalt modifier.
Embodiment 2
Moly-sulfide is added as catalyzer in coal/catalytically cracked oil=1/1 (wt, dry coal base), and add-on is 0.05% (wt, dry coal base).Said mixture is preheated to 300 ℃ through preheater, and in tubular reactor, reaction is 1 hour under 390 ℃, 11MPa hydrogen pressure condition.
Reaction product is separated under 330 ℃ of high-temperature separators, 11MPa condition, the separator top product through eight tower pressure-swing absorption apparatuss at 3.85MPa, purifying hydrogen of hydrogen under 40 ℃ of conditions, isolated hydrogen turns back in the reactor and recycles, and remaining gas is used as fuel behind liquid-phase oxidation reduction method desulfurizing and purifying.Liquid and solid matter enter 320 ℃ of temperature,, pressure 0.016MPa flashing tower, overhead product obtains lightweight oil through condensation, oily water separation.Bottom product through atmospheric distillation tower under 350 ℃, 0.138MPa operational condition and vacuum still under 350 ℃, 0.008MPa operational condition, obtain thick oil.
Thick oil and lightweight oil mix, and obtain gasoline, diesel oil, kerosene and fuel wet goods liquid fuel through hydrocracking.
The underpressure distillation bottom product is crushed to below 5 microns, namely gets road asphalt modifier.
Embodiment 3
Coal/long residuum=3/5 (wt, the dry coal base), ultra-fine high-dispersion iron catalyst preparation method is: the saturated solution of 7g ferrous sulfate joins in the 100g coal sample, stir, then the saturated solution that adds 3.5g sodium sulphite, and the rear 80 ℃ of lower vacuum-dryings 5 hours that stir, make the ultra-fine high-dispersion iron catalyst that is supported on the coal sample.The add-on of ultra-fine high-dispersion iron catalyst is 20% (wt, dry coal base).Said mixture is preheated to 330 ℃ through preheater, and in the pump circulation suspended-bed reactor, reaction is 1.5 hours under 400 ℃, 8-10MPa hydrogen pressure condition.
Reaction product is separated under 360 ℃ of high-temperature separators, 8-10MPa condition, and the high-temperature separator top product enters under 210 ℃ of low-temperature separator, the 3-4MPa condition and is separated into gas-liquid two-phase.Gaseous substance through eight tower pressure-swing absorption apparatuss at 2.9MPa, 38 ℃ of lower purifying hydrogen of hydrogen, isolated hydrogen turns back in the reactor and recycles, remaining gas behind pure amine absorption process desulfurizing and purifying as fuel.Low-temperature separator bottom liquid product obtains lightweight oil through condensation, oily water separation.The high-temperature separator bottoms enters vacuum still, under 360 ℃, 0.008MPa operational condition, obtains thick oil.
Thick oil and lightweight oil mix, and obtain gasoline, diesel oil, kerosene and fuel wet goods liquid fuel through hydrocracking.
The base product product is through the toluene extracting, and extract is removed light component through distillation, and the residue heavy component is the pitch that can satisfy AH90# asphalt for high-grade highway standard.
Embodiment 4
Ni-Mo/Al is added in coal/vacuum residuum=1/3 (wt, dry coal base)
2O
3As catalyzer, add-on is 0.03% (wt, dry coal base).Said mixture is preheated to 320 ℃ through preheater, and in tubular reactor, reaction is 1 hour under 400 ℃, 8MPa hydrogen pressure condition.
Reaction product is separated under 360 ℃ of high-temperature separators, 8MPa condition, and the high-temperature separator top product enters under 220 ℃ of low-temperature separator, the 4MPa condition and is separated into gas-liquid two-phase.Gaseous substance through eight tower pressure-swing absorption apparatuss at 3.57MPa, 42 ℃ of lower purifying hydrogen of hydrogen, isolated hydrogen turns back in the reactor and recycles, remaining gas behind pure amine absorption process desulfurizing and purifying as fuel.Low-temperature separator bottom liquid product obtains lightweight oil through condensation, oily water separation.The high-temperature separator bottoms enters vacuum still, under 380 ℃, 0.01MPa operational condition, obtains thick oil.
Thick oil and lightweight oil mix, and obtain gasoline, diesel oil, kerosene and fuel wet goods liquid fuel through hydroforming.
The underpressure distillation bottom product is through the trieline extracting, and extract is removed light component through distillation, and the residue heavy component is the pitch that can satisfy AH90# asphalt for high-grade highway standard.
Embodiment 5
Coal/gelatin liquefaction heavy oil=1/3 (wt, dry coal base) adds FeSO
4As catalyzer, add-on is 2% (wt, dry coal base).Said mixture is preheated to 300 ℃ through preheater, and in tubular reactor, reaction is 1 hour under 380 ℃, 12MPa hydrogen pressure condition.
Reaction product is separated under 320 ℃ of high-temperature separators, 10MPa condition, the separator top product through eight tower pressure-swing absorption apparatuss at 3.97MPa, purifying hydrogen of hydrogen under 45 ℃ of conditions, isolated hydrogen turns back in the reactor and recycles, and remaining gas is used as fuel behind liquid-phase oxidation reduction method desulfurizing and purifying.Liquid and solid matter enter 340 ℃ of temperature,, pressure 0.012MPa flashing tower, overhead product obtains lightweight oil through condensation, oily water separation.Bottom product through atmospheric distillation tower under 360 ℃, 0.127MPa operational condition and vacuum still under 360 ℃, 0.009MPa operational condition, obtain thick oil.
Thick oil and lightweight oil mix, and obtain gasoline, diesel oil, kerosene and fuel wet goods liquid fuel through hydroforming.
The underpressure distillation bottom product is crushed to below 100 orders, namely gets road asphalt modifier.
Claims (12)
1. a coal and the heavy oil co-processing method of producing simultaneously liquid fuel and pitch class pavior is characterized in that comprising the steps:
(1) coal dust, catalyzer and heavy oil mixed pulp;
The weight ratio of its coal and heavy oil is with the metering of dry coal base, coal: heavy oil=2-10: 10, and the weight ratio of catalyzer and coal is with the metering of dry coal base, catalyzer: coal=0.01-50: 100;
(2) after the coal oil mixture preheating, enter reactor and react;
Its preheating temperature is lower 60-150 ℃ than temperature of reaction; Its temperature of reaction is 300-450 ℃, and reaction pressure is 5-20MPa, and the reaction times is 0.5-2 hour;
(3) reaction product is separated, and isolates gaseous substance, lightweight oil and water, and the heavy mixture, isolated gaseous substance is carried hydrogen by pressure-variable adsorption, and the hydrogen of purification turns back in the reactor and recycles, and remaining gas is used as fuel after purifying; Isolated lightweight oil and water carry out oily water separation, obtain lightweight oil and water; Wherein: the inlet temperature of separating unit is that 250-450 ℃, pressure are 5-20MPa; It is pressure 0.3-4MPa, temperature 30-50 ℃ that pressure-variable adsorption is put forward the hydrogen operational condition;
(4) the heavy mixture enters distillation tower, obtains thick oil and bottom product through fractionation by distillation;
Its distillation tower is atmospheric distillation tower or vacuum still, and the atmospheric distillation tower service temperature is that 300-360 ℃, pressure are 0.1-0.2MPa, and the vacuum still service temperature is that 320-400 ℃, pressure are 0.001-0.02MPa;
(5) slightly oil and lightweight oil mix, and process to get gasoline, kerosene, diesel oil, oil fuel liquid fuel through upgrading;
(6) bottom product is treated, gets pitch class pavior;
Described catalyzer is red mud, Natural pyrite, metallurgical flying dust, high ferro coal gangue, FeSO
4, Mo base hydrogenation catalyst, Ni-Mo base hydrogenation catalyst or ultra-fine high-dispersion iron catalyst.
2. a kind of coal as claimed in claim 1 and heavy oil co-processing are produced the method for liquid fuel and pitch class pavior simultaneously, it is characterized in that described coal dust is bituminous coal or brown coal.
3. a kind of coal as claimed in claim 1 and heavy oil co-processing are produced the method for liquid fuel and pitch class pavior simultaneously, it is characterized in that described heavy oil is long residuum, vacuum residuum, catalytically cracked oil or gelatin liquefaction heavy oil.
4. a kind of coal as claimed in claim 1 and heavy oil co-processing are produced the method for liquid fuel and pitch class pavior simultaneously, it is characterized in that described Mo base hydrogenation catalyst is molybdenum ash MoO
3Or moly-sulfide.
5. a kind of coal as claimed in claim 1 and heavy oil co-processing are produced the method for liquid fuel and pitch class pavior simultaneously, it is characterized in that described Ni-Mo base hydrogenation catalyst is Ni-Mo/Al
2O
3
6. a kind of coal as claimed in claim 1 and heavy oil co-processing are produced the method for liquid fuel and pitch class pavior simultaneously, it is characterized in that described ultra-fine high-dispersion iron catalyst is by being prepared as follows the method preparation:
Method one:
(1) with a certain amount of FeSO
4Saturated solution joins in the coal dust, stirs;
(2) a certain amount of sodium sulphite saturated solution or urea saturated solution are joined in the above-mentioned coal dust, stir, make coal sample;
(3) with coal sample vacuum-drying 5 hours under 80-120 ℃ of temperature, make the ultra-fine high-dispersion iron catalyst that is supported on the coal sample;
Method two:
With the saturated solution of sulfur-containing anion with contain in a kind of adding coal dust in the saturated solution of iron ion and stir, make A, another kind of solution is added among the A stir again, can make the ultra-fine high-dispersion iron catalyst that is supported on the coal sample after the drying;
Method three:
(1) in the ammoniacal liquor of high-speed stirring, disposable impouring iron salt solutions, preparation Fe (OH)
3Or Fe (OH)
2With the FeOOH precipitation, reaction end pH value is controlled to be 8-13;
(2) by the centrifugal above-mentioned reaction product of supercentrifuge, obtain the iron-based hydrogel;
(3) in high speed dispersor, iron-based hydrogel and an amount of coal dust and liquefaction solvent are mixed together dispersion, obtain being supported on the ultra-fine high-dispersion iron catalyst on the coal sample.
7. a kind of coal as claimed in claim 1 and heavy oil co-processing are produced the method for liquid fuel and pitch class pavior simultaneously, it is characterized in that described reactor adopts forced-circulation boiling bed bioreactor in tubular reactor, U.S. CTSL and the HRI technique in German IGOR, the Japanese NEDOL technique or the pump circulation suspended-bed reactor in the Chinese Shenhua technique.
8. a kind of coal as claimed in claim 1 and heavy oil co-processing are produced the method for liquid fuel and pitch class pavior simultaneously, it is characterized in that described gas sweetening adopts pure amine absorption process, liquid-phase oxidation reduction method, copper to wash method or crystallization sulphur method.
9. a kind of coal as claimed in claim 1 and heavy oil co-processing are produced the method for liquid fuel and pitch class pavior simultaneously, it is characterized in that single-stage or stage separator are adopted in the separation of described step (3).
10. a kind of coal as claimed in claim 1 and heavy oil co-processing are produced the method for liquid fuel and pitch class pavior simultaneously, it is characterized in that described separator is high-temperature separator, middle temperature separator or low-temperature separator.
11. a kind of coal as claimed in claim 1 and heavy oil co-processing are produced the method for liquid fuel and pitch class pavior simultaneously, it is characterized in that described thick oil from distillation tower and are hydrofining, hydrocracking or reforming process from the mixed upgrading of the lightweight oil of water-and-oil separator processing.
12. a kind of coal as claimed in claim 1 and heavy oil co-processing are produced the method for liquid fuel and pitch class pavior simultaneously, what it is characterized in that described base product product is treated to solvent extraction or pulverizing.
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