CN1219852C - Method for continuous conversion of low-rank coal in subcritical water or supercritical water - Google Patents
Method for continuous conversion of low-rank coal in subcritical water or supercritical water Download PDFInfo
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- CN1219852C CN1219852C CN 200310109657 CN200310109657A CN1219852C CN 1219852 C CN1219852 C CN 1219852C CN 200310109657 CN200310109657 CN 200310109657 CN 200310109657 A CN200310109657 A CN 200310109657A CN 1219852 C CN1219852 C CN 1219852C
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Abstract
The present invention relates to a method for continuously converting low-order coal in subcritical water or supercritical water. The present invention is used for preparing coal water slurry or a mixture of coal water slurry and alkaline metal and/or oxides or hydroxides of alkaline earth metal. The present invention guarantees the continuous high-pressure conveyance of the coal water slurry, and the coal water slurry is added in a reaction system. Then, the present invention utilizes the peculiar property of the supercritical water, and the low-order coal is effectively extracted and pyrolyzed, and is converted into gas products, liquid products and solid products. The present invention has the advantage that the present invention has no need of drying, and has no discharge of harmful gases, the water can be cyclically used, the technology is favorable to environments, the technology process is simple, and the present invention is favorable to the industrial continuous production technology.
Description
Technical field:
The invention belongs to a kind of method for transformation of low-rank coal, relate in particular to a kind ofly under inferior, condition of supercritical water, low-rank coal is converted into continuously the method for liquid fuel, high heating value gas and active carbocoal.
Background technology:
Low-rank coal is peatification and the lower coal of degree of coalification in the coal-forming process.Brown coal are coals that thermal value is 3500-4000 kilocalorie/kilogram, no adhesion, fugitive constituent height, moisture is big in the low-rank coal.The brown coal reserves of China reach 1,260 hundred million tons, account for 14% of national coal total reserves.Peat is by water, the flammable humatite that mineral substance and organic three parts are formed, and moisture content is big.The peat resource total reserves of China reaches 4,700,000,000 tons, is a kind of important potential energy source.Brown coal and peat are because moisture content is big, and calorific value is low, and easy-weathering and spontaneous combustion should not be transported for long-distance; Directly efficiency of combustion is low, contaminate environment.Therefore; how can be as soon as possible low-rank coal such as brown coal and peat be processed into the efficient height, be convenient to transport the clean fuel of storage, this is for utilizing the low-rank coal resource rationally and effectively; solving unevenness between supply and demand and protect atmosphere to exempt from pollution, all is a very urgent problem.
In order to reduce the brown coal water content, the outstanding button history of A is at CN85100817A, 1987 (exsiccant complete assemblys that are used for the high-moisture brown coal) and Friedrich B Bie Er Fil moral spy are at CN1157846A, 1997 (being used for reducing the method for former brown coal water content, equipment and press) proposed the apparatus and method of dry brown coal respectively.Obviously this soil that has increased extra equipment and investment and taken for the brown coal utilization.
Matsumura etc. (Fuel 78 (1999) 1049-1056) have provided use hydrocarbon or alcohol (for example benzene, toluene, dimethylbenzene, tetraline pyridine, tetraline, normal hexane, methyl alcohol, butanols) carry out supercritical extraction to coal as supercutical fluid research.It is big that but these organic solvents have toxicity, price height, and stable inadequately in extraction process, be easy to participate in reaction and cause solvent loss and can not high-temperature operation etc. shortcoming.Therefore, the report that does not still have practical application.
(Ind.Eng.Chem.Res.39:4040-4053 such as Antal, 2000) report biomass experiments of continuous gasification hydrogen manufacturing under the condition of supercritical water in the reactor of 6.22 millimeters of internal diameters such as W-Gum, yam starch, xylogen, Microcrystalline Cellulose, glycerine, glucose and sawdust, but do not related to the coal solid organic matters.
(colleges and universities' chemical engineering journal 15 (1) 40-44,2001 such as Lv Xiuyang; Agricultural mechanical journal 32 (3) 27-30,2001) proposed the working procedure of the two charging systems of double pump and pump and air-operated solenoid valve door, the solid waste of having reported biomass such as Mierocrystalline cellulose, residue from beans after making, rice husk, xylogen is the development of decomposer and test overview continuously in super, near-critical water.This unit temp can reach 600 ℃, pressure 40MPa, the residence time, concentration of slurry can reach 10wt% at 24 seconds-15 minutes, Maximum Supply Quantity be 2.4 liters/time.Though Guo Liejin etc. are at CN1375447A, 2002 have proposed the continuous supercritical water gasification hydrogen-producing method and apparatus of organic solid-state material.But this patent is emphasized organic solid-state materials such as biomass, only reported that Xylo-Mucine (CMC) is an additive, use glucose solution (0.1-0.8M), glucose solution+basic additive, lower concentration sawdust+CMC (sawdust concentration 2.0wt%, CMC1wt%) example, whole patent do not relate to this organic solid-state thing of coal.Lv Xiuyang and Guo Liejin all adopt the two charging systems of double pump, alternately switch by valve, realize biomass by hydrolyzation and device for producing hydrogen continuously feeding generally, and this realizes that on large-scale plant its difficulty is sizable.
Summary of the invention:
The purpose of this invention is to provide a kind of eco-friendly, under the condition of inferior, supercritical water, be converted into liquid fuel continuously by low-rank coal, the method for high heating value gas and active carbocoal.
To achieve these goals, the technological line that the present invention adopts is: at first prepare finite concentration and can keep the certain hour coal grain can settled coal water slurry or the oxide compound of coal water slurry and basic metal and/or alkaline-earth metal or the mixture of oxyhydroxide, the continuous high-pressure delivery of assurance coal water slurry.Because reaction medium itself is a water, therefore, the preparation coal water slurry can be used the high low-rank coal of water content, directly pulverizes and mixes with water without drying, adds reactive system.Utilize the peculiar property of supercritical water then, with low-rank coal extract effectively, pyrolysis, be converted into three kinds of useful products of gas, liquid, solid.Specifically, the inventive method comprises the steps:
(1) granularity is the coal water slurry that obtains 10-40wt% after the low-rank coal coal dust of 60-150 micron and water fully stir, and coal water slurry is boosted to 17-40MPa, and be preheating to 120-350 ℃;
(2) water is boosted to 17-40MPa, and be preheated to 400-700 ℃;
(3) with the coal water slurry after the preheating and water under the promotion of uniform pressure, weight ratio by water and coal is 1-10: 1, the flow rate of water is with 3.0-6.0 kilogram/time, the flow rate of coal water slurry enters reactor with 3.0-4.5 kilogram/time, water and coal water slurry mixture reach the subcritical of water or supercritical state 360-650 ℃ and 17-40Mpa in the reactor, stop in the reactor to transform in 10 seconds-3 minutes;
(4) reaction product enters the solid separating tank of gas-liquid, isolating solid product is discharged at the bottom of by jar, gas, liquid product enter knockout drum, gaseous product is discharged by the gas-liquid separation tank top, product liquid enters gun barrel, the liquid phase oil product is taken out by the oily water separation tank top, and water is then discharged by the oily water separation pot bottom, recycles.
The oxide compound or the oxyhydroxide that can also add alkali metal hydroxide and/or alkaline-earth metal in the reactor in (3) step are as catalyzer or CO
2Absorption agent promotes low-rank coal to transform, and generates more hydrogen-rich gas, fixing sulfide in gas phase simultaneously, and the weight ratio of its adding is a low-rank coal: the oxide compound of alkali metal hydroxide and/or alkaline-earth metal or oxyhydroxide=1: 0.5-2
Aforesaid alkali-metal oxyhydroxide is KOH or NaOH.
The oxide compound of aforesaid alkaline-earth metal or oxyhydroxide are Ca (OH)
2, CaO, Mg (OH)
2Or MgO.
The low-rank coal granularity is preferably in the 73-80 micron as mentioned above.
The weight ratio that enters reactor water and coal as mentioned above is preferably in 5-10: 1.
The residence time was preferably 10 seconds-2 minutes in the reactor as mentioned above.
The pressure of reactor is preferably in 24.5-30MPa as mentioned above.
Characteristics of the present invention
Drying-free can directly use the high low-rank coal of water content, as brown coal and peat;
The pyrolysis of low-rank coal, extraction and hydrogenation can carry out in a reactor;
No noxious gas emission, water can be recycled, and technology is environmentally friendly;
Speed of response is fast, and the residence time is short;
Change operational condition, can control the ratio of gas, liquid, solid product;
Technological process is simple, helps the industrialization continuous production processes and realizes.
Embodiment:
Fig. 1 is a schematic flow sheet of the present invention.
1. water pot 2. coal water slurry basins 3. water pumps 4. coal water slurry pumps 5. water preheaters 6. coal water slurry preheaters 7. reactors 8. system pressure variable valve 9. gas-liquids are consolidated separating tank 10. knockout drums 11. under meters 12. gun barrels 13. flow control valves 14. water pump inlet valves 15. coal water slurry inlet valves 16. coal water slurry outlet valves 17. coal water slurry exhaust-valves 18. electronic scaless
The little dragon's pool brown coal powder of water content 14.8% is broken to 74 microns coal water slurry that are made into 24.8wt% with water to be placed in the basin 2.When beginning experiment, the inlet valve 15 of boiling water coal slurry pump 4, the power switch of boiling water coal slurry pump 4 starts coal water slurry pump 4, regulate flow to 4.5 kilogram/time, coal water slurry boosts to 24.5MPa through coal water slurry pump 4; The inlet valve 14 of boiling water pump 3 closes system's outlet valve 8, starts water pump 3, regulate pump capacity to 6.0 kilogram/time, water boosts to 24.5MPa via water pump 3, is preheated to 520 ℃ by water preheater 5.The weight ratio of water and coal is about 9: 1.After treating system's each point temperature, pressure-stabilisation, when coal water slurry pump discharge pressure and system pressure 24.5MPa balance, boiling water coal slurry pump discharge valve 16, be heated to 120 ℃ by coal water slurry preheater 6, beginning is to system feeding, Reactor inlet and temperature out reach 410 ℃ of temperature of reaction, the pressure 24.5MPa of setting, and reaction picks up counting.15 seconds residence time, the slurries amount is weighed by electronic scales 18 and is drawn between the reaction period.It is even that circulating tank 2 is in whipped state maintenance coal slurry in the reaction process.Reaction product enters the solid separating tank 9 of gas-liquid through system pressure variable valve 8, realize that the gas-liquid fluid separates with solid product, solid product is discharged at the bottom of by jar, the gas-liquid fluid product enters carries out gas-liquid separation in the knockout drum 10, gaseous product is discharged by knockout drum 10 tops, by wet flow indicator 11 meterings.Product liquid enters gun barrel 12, and the liquid phase oil product is taken out by gun barrel 12 tops, and water then is expelled to water pot 1 by gun barrel 12 bottoms and recycles.Reaction result sees Table 1.
When needs add basic metal or alkaline earth metal oxide or oxyhydroxide, then in coal water slurry basin 2, add coal/oxide compound or coal/required additive of oxyhydroxide proportioning, and stir at basin 2.All the other operations are identical with embodiment 1.When the peat of the Huachuan of use water content 10.32%, except that the raw material difference, the preparation of raw slurry is identical with brown coal, and all the other operations are also identical with embodiment 1.Table 1 is except that listing embodiment 1, and the reaction result of the embodiment under different material and the differential responses condition is also listed in table 1.
Table 1
| Embodiment | Temperature ℃ | Pressure Mpa | The second residence time | Coal-water fluid concentration wt% | Coal powder size μ m | Preheating temperature ℃ | Flow rate, kilogram/time | Water/coal slurry weight ratio | Productive rate % | Gas composition % | ||||||||
| Coal slurry | Water | Coal slurry | Water | Gas | Oil | Residual Jiao | CH 4 | C 2-6 | H 2 | CO | CO 2 | |||||||
| 1 | 410 | 24.5 | 15 | 24.8 | 74 | 120 | 520 | 4.5 | 6.0 | 8.41 | 23.4 | 7.0 | 67.7 | 4.10 | 1. 44 | 5.93 | 4.67 | 83.01 |
| 2 | 365 | 17.0 | 60 | 24.8 | 74 | 120 | 400 | 4.2 | 5.1 | 7.93 | 15.1 | 6.4 | 79.7 | 0.35 | 0.31 | 0.50 | 2.27 | 96.58 |
| 3 | 420 | 34.5 | 30 | 35.0 | 104 | 130 | 625 | 4.5 | 5.5 | 5.35 | 27.5 | 7.7 | 66.9 | 4.39 | 1.62 | 5.87 | 1.31 | 86.81 |
| 4 | 430 | 38.5 | 60 | 15.8 | 142 | 150 | 650 | 4.5 | 3.0 | 8.80 | 28.6 | 6.5 | 64.7 | 4.78 | 1.98 | 7.04 | 4.30 | 81.90 |
| 5 | 540 | 30.0 | 120 | 18.0 | 74 | 250 | 680 | 3.0 | 3.0 | 10.0 | 38.4 | 5.5 | 56.1 | 5.85 | 2.10 | 6.99 | 2.50 | 82.56 |
| 6* | 650 | 38.5 | 15 | 20.0 | 74 | 350 | 690 | 4.0 | 4.5 | 9.60 | 89.8 | 2.4 | 25.7 | 38.0 | 6.58 | 55.0 | 0.00 | 0.40 |
| 7** | 600 | 26.0 | 90 | 25.0 | 74 | 350 | 650 | 4.0 | 4.0 | 7.0 | 79.2 | 11.8 | 9.1 | 34.0 | 18.5 | 41.6 | 0.45 | 5.42 |
Note: RTD: the residence time; * coal/CaO=1 (weight ratio); * Huachuan peat, water content 10.32%, peat/CaO=1.67 (weight ratio).
Claims (8)
1. the method that low-rank coal transforms in subcritical or supercritical water continuously is characterized in that comprising the steps:
(1) granularity is the coal water slurry that obtains 10-40wt% after the low-rank coal coal dust of 60-150 micron and water fully stir, and coal water slurry is boosted to 17-40MPa, and be preheating to 120-350 ℃;
(2) water is boosted to 17-40MPa, and be preheated to 400-700 ℃;
(3) with the coal water slurry after the preheating and water under the promotion of uniform pressure, weight ratio by water and coal is 1-10: 1, the flow rate of water is with 3.0-6.0 kilogram/time, the flow rate of coal water slurry enters reactor with 3.0-4.5 kilogram/time, water and coal water slurry mixture reach the subcritical of water or supercritical state 360-650 ℃ and 17-40Mpa in the reactor, stop in the reactor to transform in 10 seconds-3 minutes;
(4) reaction product enters the solid separating tank of gas-liquid, isolating solid product is discharged at the bottom of by jar, gas, liquid product enter knockout drum, gaseous product is discharged by the gas-liquid separation tank top, product liquid enters gun barrel, the liquid phase oil product is taken out by the oily water separation tank top, and water is then discharged by the oily water separation pot bottom, recycles.
2. the method that a kind of low-rank coal as claimed in claim 1 transforms in subcritical or supercritical water continuously, it is characterized in that can also adding in the reactor in (3) step the oxide compound or the oxyhydroxide of alkali metal hydroxide and/or alkaline-earth metal, the weight ratio of its adding is a low-rank coal: the oxide compound of alkali metal hydroxide and/or alkaline-earth metal or oxyhydroxide=1: 0.5-2.
3. the method that a kind of low-rank coal as claimed in claim 2 transforms in subcritical or supercritical water continuously is characterized in that described alkali-metal oxyhydroxide is KOH or NaOH.
4. the method that a kind of low-rank coal as claimed in claim 2 transforms in subcritical or supercritical water continuously is characterized in that the oxide compound of described alkaline-earth metal or oxyhydroxide are Ca (OH)
2, CaO, Mg (OH)
2Or MgO.
5. the method that a kind of low-rank coal as claimed in claim 1 or 2 transforms in subcritical or supercritical water continuously is characterized in that described low-rank coal granularity is at the 73-80 micron.
6. the method that a kind of low-rank coal as claimed in claim 1 or 2 transforms continuously in subcritical or supercritical water is characterized in that the described weight ratio that enters reactor water and coal is at 5-10: 1.
7. the method that a kind of low-rank coal as claimed in claim 1 or 2 transforms in subcritical or supercritical water continuously is characterized in that the residence time is 10 seconds-2 minutes in the described reactor.
8. the method that a kind of low-rank coal as claimed in claim 1 or 2 transforms in subcritical or supercritical water continuously, the pressure that it is characterized in that described reactor is at 24.5-30MPa.
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-
2003
- 2003-11-11 CN CN 200310109657 patent/CN1219852C/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010069146A1 (en) * | 2008-12-19 | 2010-06-24 | 新奥科技发展有限公司 | Coal processing method by using characteristic of sub-critical and supercritical water |
| CN102333464A (en) * | 2009-07-29 | 2012-01-25 | 朴寅植 | Midsole pad for women's shoes that distributes pressure applied onto the sole of the foot, and midsole and shoe having same |
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