CN1205303C - Method of making hydrogen containing gas using lignite and peat - Google Patents

Method of making hydrogen containing gas using lignite and peat Download PDF

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Publication number
CN1205303C
CN1205303C CN 03145689 CN03145689A CN1205303C CN 1205303 C CN1205303 C CN 1205303C CN 03145689 CN03145689 CN 03145689 CN 03145689 A CN03145689 A CN 03145689A CN 1205303 C CN1205303 C CN 1205303C
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brown coal
peat
reaction
water
hydrogen
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CN1475432A (en
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毕继诚
程乐明
任辉
张�荣
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Shanxi Institute of Coal Chemistry of CAS
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Shanxi Institute of Coal Chemistry of CAS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The present invention relates to a method for preparing hydrogen containing gas by brown coal and peat. Pulverized brown coal or peat, additives and water are added to a high pressure reactor; after the reaction temperature achieves 350 to 700 DEG C and the reaction pressure achieves 16 to 40MPas at the temperature rise rate of 10 to 15 DEG C /min in nitrogen atmosphere, the mixture in the high pressure reactor reacts for 5 to 60 minutes and is cooled to the room temperature; gas and liquid products are separated, and the separated gas is gas containing hydrogen. The present invention has the advantages of low energy consumption, no environmental pollution, rapid reaction speed, short stay time and simple technology.

Description

A kind of brown coal and peat are produced the method for hydrogen-containing gas
Technical field:
The invention belongs to a kind of brown coal and peat and produce the method for hydrogen-containing gas, relate in particular to a kind ofly at the supercritical water state with add under the condition of alkaline-earth metal, produce the method for hydrogen-containing gas by brown coal and peat.
Background technology:
Brown coal are coals that thermal value is 3500-4000 kilocalorie/kilogram, no adhesion, fugitive constituent height, moisture is big. 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 easily differentiation and spontaneous combustion should not be transported for long-distance; Directly burning, then efficient is low, contaminate environment.Therefore how can change brown coal and Properties of Peat as soon as possible; be processed into the efficient height, be convenient to the clean fuel that transports and store, this utilizes coal and peat resource for rational and effective; solving unevenness between supply and demand and protect atmosphere to exempt from pollution, all is a very urgent problem.
Hydrogen is the clean fuel that can store, transport, and its product is a water when carrying out energy transformation, can really realize the zero release of pollutent.Particularly be good economic outlook and the environment-friendly advantage that the high efficiency etc. of the fuel cell of fuel is brought, promote people to carry out the research of carbonaceous material hydrogen manufacturing with hydrogen.Hatano (EP1001002,2002) has proposed to utilize the part of fuel burning, and the CaO thermolysis is by carbonaceous organic material hydrogen manufacturing.The Olsvik of Norwegian (WO0018681,2000) has proposed the patent of natural G﹠W reformation hydrogen production.Germany Karlsruhe (DE19955150,2001) uses supercritical water and hydrocarbon and/or alcohol using the hydrogen that the production fuel cell is used under the catalyzer condition.(Ind.Eng.Chem.Res such as Antal, 2000,39:4040-4053) reported that humidogene material with wood chip/W-Gum is at 963K, under the supercritical water state of 28MPa, use gac to be catalyzer, can obtain the organic H2 57% of 2.18 liters/gram, the hydrogen-rich gas of CO2 33%, the carbon gasification rate reaches 97wt% in the biomass.Minowa and co-worker thereof ((Renewable Energy, 1999,16:1114) find to use the reduced nickel catalyzer in the hot pressurized water of 623K and 18MPa, fibrin gasification also can obtain hydrogen-rich gas.Lee ancestor English disclosed (CN1085522) utilizes sun power to produce hydrogen from biomass and water, and temperature of reaction is decomposed under the condition of normal pressure in 200-1000 ℃ of scope, and the gas mixture that liquid hydrocarbon generates through catalytic cracking obtains the hydrogen of higher degree after purifying treatment.Guo Liejin etc. are at CN1375447A, and 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, is additive with the Xylo-Mucine, when using sawdust as raw material, and hydrogen 21-30.5% only in the gaseous product, and carbonic acid gas reaches 50.4-63.8%.Whole patent does not relate to this organic solid-state thing of coal.In order to obtain purity higher H 2, the CO2 product gas that contains 33-63% in the above-mentioned report needs to separate, and this has just increased the complexity of technology.
In order to reduce the brown coal water content, the outstanding button history of A has proposed the apparatus and method of dry brown coal respectively at CN1157846A (being used to reduce the method for former brown coal water content, equipment and press) CN85100817A (the exsiccant complete assembly that is used for the high-moisture brown coal) and Friedrich B Bie Er Fil moral spy.Obviously this soil that has increased extra equipment and investment and taken for the brown coal utilization.
Summary of the invention
The objective of the invention is to provide a kind of environmental friendliness, technology is simple, cost is low, is produced the method for hydrogen-containing gas under the condition of supercritical water by the gasification of brown coal and peat.
When critical temperature Tc (374.2 ℃) that is higher than it respectively when the temperature T and the pressure P of water and emergent pressure Pc (22.1MPa), the water of this moment is called supercritical water (SCW).Supercritical water has stronger penetrating power, dissolving power and extracting and separating ability.Supercritical water is to the insoluble characteristic of inorganics of grading of the ash in organic high-solvency and the coal, makes solvation and the diffusion in SCW promptly of organism that the brown coal pyrolysis produces, dilution, makes condensation or the reaction of knot charcoal be difficult to take place, and easily and ash separation.Brown coal and peat swelling, dissolving in supercritical water form small-particle and are dispersed in the supercritical water, produce homogeneous phase or intend the homogeneous mixture, help homogeneous reaction fast.Because the diffusibility of supercritical water, the internal structure that is easy to enter coal and peat, thereby the residue of gained is porous material, has good activity and absorption property.
To achieve these goals, press the weight ratio 2-10 of water and brown coal or peat: 1, the weight ratio 0-0.1 of additive and coal or peat: 1 ratio, with brown coal or the peat of pulverizing, additive and water add in the high-pressure reactor, under nitrogen atmosphere, temperature rise rate with 10-15 ℃/min makes temperature of reaction reach 350-700 ℃, after reaction pressure reaches 16-40MPa, reacted 5-60 minute, be cooled to room temperature, the gas-liquid product separates, isolated gas is hydrogen-containing gas, and the liquid phase oil aqueous emulsion extracts with tetrahydrofuran (THF) and carries out oily water separation, and isolated tetrahydrofuran (THF) solvend adds anhydrous Na 2SO 4Remove minor amount of water wherein, the tetrahydrofuran (THF) extraction oil evaporates and 0.02MPa under the 60-70 ℃ of condition through at normal pressure, after the vacuum-drying, obtains oil product under the 30-50 ℃ of condition, and isolated water can be recycled.
Aforesaid brown coal water content is at 8-25%;
The general granularity of the granularity of aforesaid brown coal is preferably in 0.25-0.40mm at 0.15-0.40mm
Aforesaid additive is to separate the calcium oxide that obtains by divided calcium carbonate.Also the available hydrogen potassium oxide is as additive.
As mentioned above, temperature of reaction of the present invention generally is facing of water to separate temperature and determine to be equal to or greater than, and the suitable temperature of reaction of brown coal is in 600-700 ℃ of scope.The temperature of reaction that peat suits is in 450-550 ℃ of scope.
As mentioned above, reaction pressure is to determine with the emergent pressure that is equal to or greater than water.The operating pressure that requirement and the admissible service temperature of quickening according to reaction, particularly reactor materials used allows, suitable reaction pressure scope is at 25-35MPa.
As mentioned above, water and brown coal or peat weight ratio are to determine with the throughput of brown coal transformation efficiency and unit reaction volume and the stabilized with mixture of water and brown coal or peat.The scope of the suitable water and the weight ratio of brown coal or peat is at 4-6: 1.
As mentioned above, the reaction times is to determine with the throughput and the gasification degree of brown coal or peat transformation efficiency and unit reaction volume, and the suitable reaction times was at 5-30 minute.
The liquid phase oil aqueous emulsion carries out oily water separation with the tetrahydrofuran (THF) extraction as mentioned above, and is better for separating effect, also can add the NaCl breakdown of emulsion.
Characteristics of the present invention
1. drying-free can directly use the brown coal (peat) of high moisture content, and energy consumption is low;
2. gasification reaction, water gas shift reaction and the CO2 that carries out brown coal (peat) in reactor fixes;
3. there is not noxious gas emission, the environmentally friendly technology that water can be recycled;
4. speed of response is fast, and the residence time is short;
5. change operational condition can be controlled the gas-liquid ratio of product admittedly;
6. helping continuous production processes realizes.
Embodiment
Embodiment 1
Water content 14.8% little dragon's pool brown coal powder is broken to 0.25-0.40mm, press the weight ratio 5: 1 and the CaO of water and brown coal: the weight ratio of coal 0.1: 1, brown coal, calcium oxide and the water of pulverizing is added in the high-pressure reactor, under nitrogen atmosphere, make temperature of reaction reach 550 ℃ of the temperature of reaction of setting with the temperature rise rate of 15 ℃/min, after reaction pressure reaches 33Mpa, reaction picks up counting. react after 5 minutes, stop heating, shift out reactor, force air cooling to room temperature.The gas-liquid product separates.Gaseous product adopts the saturated aqueous common salt draining to get the gas method and gets the gas metering and carry out permanent gases and hydrocarbon gas stratographic analysis.The liquid phase oil aqueous emulsion is with tetrahydrofuran (THF) extraction carrying out oily water separation, and is better for separating effect, adds the NaCl breakdown of emulsion.Isolated tetrahydrofuran (THF) solvend adds anhydrous Na 2SO 4Remove minor amount of water wherein, the tetrahydrofuran (THF) extraction oil evaporates and 0.2 normal atmosphere under the 60-70 ℃ of condition through at normal pressure, after the vacuum-drying, obtains oil product under the 30-50 ℃ of condition.Solid residue is weighed.Isolated water can be recycled.Reaction result sees Table 1.
Embodiment 2
Water content 14.8% little dragon's pool brown coal powder is broken to 0.25-0.40mm, press the weight ratio 5: 1 of water and brown coal, brown coal, the water pulverized are added in the high-pressure reactor, under nitrogen atmosphere, make temperature of reaction reach 550 ℃ of the temperature of reaction of setting with the temperature rise rate of 10 ℃/min, after reaction pressure reached 32Mpa, reaction picked up counting.React after 5 minutes, stop heating, shift out reactor, force air cooling to room temperature.Gas dosing analysis subsequently is all identical with embodiment 1 with oily water separation.Reaction result sees Table 1.
Embodiment 3
Little dragon's pool brown coal, water content 14.8%.Brown coal powder is broken to 0.25-0.40mm, press the weight ratio 4: 1 of water and brown coal, brown coal, the water pulverized are added in the high-pressure reactor, under nitrogen atmosphere, make temperature of reaction reach 600 ℃ of the temperature of reaction of setting with the temperature rise rate of 12.5 ℃/min, after reaction pressure reached 29.5Mpa, reaction picked up counting.React after 5 minutes, stop heating, shift out reactor, force air cooling to room temperature.Gas dosing analysis subsequently is all identical with embodiment 1 with oily water separation.Reaction result sees Table 1.
Embodiment 4
Little dragon's pool brown coal, water content 14.8%.Brown coal powder is broken to 0.25-0.40mm, press the weight ratio 6: 1 and the CaO of water and brown coal: the weight ratio of coal 0.5: 1, brown coal, calcium oxide and the water of pulverizing is added in the high-pressure reactor, under nitrogen atmosphere, make temperature of reaction reach 600 ℃ of the temperature of reaction of setting with the temperature rise rate of 15 ℃/min, after reaction pressure reached 28Mpa, reaction picked up counting.React after 5 minutes, stop heating, shift out reactor, force air cooling to room temperature.Gas dosing analysis subsequently is all identical with embodiment 1 with oily water separation.Reaction result sees Table 1.
Embodiment 5
Little dragon's pool brown coal, water content 14.8%.Brown coal powder is broken to 0.25-0.40mm, press the weight ratio 4: 1 and the CaO of water and brown coal: the weight ratio of coal 0.2: 1, brown coal, calcium oxide and the water of pulverizing is added in the high-pressure reactor, under nitrogen atmosphere, make temperature of reaction reach 600 ℃ of the temperature of reaction of setting with the temperature rise rate of 15 ℃/min, after reaction pressure reached 28Mpa, reaction picked up counting.React after 5 minutes, stop heating, shift out reactor, force air cooling to room temperature.Gas dosing analysis subsequently is all identical with embodiment 1 with oily water separation.Reaction result sees Table 1.
Embodiment 6
Little dragon's pool brown coal, water content 14.8%.Brown coal powder is broken to 0.25-0.40mm, press the weight ratio 4: 1 and the CaO of water and brown coal: the weight ratio of coal 1: 1, brown coal, calcium oxide and the water of pulverizing is added in the high-pressure reactor, under nitrogen atmosphere, make temperature of reaction reach 650 ℃ of the temperature of reaction of setting with the temperature rise rate of 15 ℃/min, after reaction pressure reached 33Mpa, reaction picked up counting.React after 15 minutes, stop heating, shift out reactor, force air cooling to room temperature.Gas dosing analysis subsequently is all identical with embodiment 1 with oily water separation. and reaction result sees Table 1.
Embodiment 7
Little dragon's pool brown coal, water content 14.8%.Brown coal powder is broken to 0.25-0.40mm, press the weight ratio 6: 1 and the KOH of water and brown coal: the weight ratio of coal 0.04: 1, brown coal, KOH and the water of pulverizing is added in the high-pressure reactor, under nitrogen atmosphere, make temperature of reaction reach 400 ℃ of the temperature of reaction of setting with the temperature rise rate of 15 ℃/min, after reaction pressure reached 24Mpa, reaction picked up counting.React after 5 minutes, stop heating, shift out reactor, force air cooling to room temperature.Gas dosing analysis subsequently is all identical with embodiment 1 with oily water separation.Reaction result sees Table 1.
Embodiment 8
Huo Lin river brown coal, water content 8.8%.Brown coal powder is broken to 0.25-0.40mm, presses the weight ratio 6: 1 of water and brown coal, brown coal, the water of pulverizing is added in the high-pressure reactor, under nitrogen atmosphere, make temperature of reaction reach 400 ℃ of the temperature of reaction of setting with the temperature rise rate of 15 ℃/min, after reaction pressure reached 24Mpa, reaction picked up counting.React after 5 minutes, stop heating, shift out reactor, force air cooling to room temperature.Gas dosing analysis subsequently is all identical with embodiment 1 with oily water separation.Reaction result sees Table 1.
Embodiment 9
Huachuan peat, water content 10.32%.Peat dust is broken to 0.25-0.40mm, press the weight ratio 6: 1 and the CaO of water and peat: the weight ratio of coal 0.6: 1, peat, calcium oxide and the water of pulverizing is added in the high-pressure reactor, under nitrogen atmosphere, make temperature of reaction reach 500 ℃ of the temperature of reaction of setting with the temperature rise rate of 15 ℃/min, after reaction pressure reached 33.5Mpa, reaction picked up counting.To react after 30 minutes, stop heating, shift out reactor, force air cooling to room temperature. gas dosing analysis subsequently is all identical with embodiment 1 with oily water separation.Reaction result sees Table 1.
Comparative Examples 10
Little dragon's pool brown coal, water content 14.8%.Brown coal powder is broken to 0.25-0.40mm, and the brown coal of pulverizing add in the high-pressure reactor, under nitrogen atmosphere, make temperature of reaction reach 400 ℃ of the temperature of reaction of setting with the temperature rise rate of 15 ℃/min, and after reaction pressure reached 24Mpa, reaction picked up counting.React after 5 minutes, stop heating, shift out reactor, force air cooling to room temperature.Gas dosing analysis subsequently is all identical with embodiment 1 with oily water separation.Reaction result sees Table 1.
The reaction result of table 1 embodiment
Embodiment Temperature Pressure Stop Water/coal The CaO/ coal Productive rate (%), daf Gas yield Gas composition (%)
K MPa Time, divide Weight ratio Weight ratio Gas Oil Residual Jiao Milliliter/gram daf CH 4 C 2-6 H 2 CO CO 2
1 823 33 60 5 0.1 41.9 3.4 48.2 329.2 34.0 6.7 13.2 0.0 47.2
2 823 32 30 5 0 41.6 3.7 49.9 314.1 28.0 6.5 16.4 0.0 49.1
3 873 29.5 5 4 0 45.5 3.8 47.2 356.6 31.5 7.2 13.5 0.5 47.4
4 873 28 5 6 0.5 59.5 2.3 43.9 313.1 37.3 8.2 46.1 0.6 7.8
5 873 28 5 4 0.2 39.9 3.6 47.9 294.5 49.2 8.4 18.7 0.0 23.6
6 923 33 15 4 1 97.9 1.7 23.5 518.0 38.9 5.2 55.6 0.0 0.4
7 873 30.5 5 4 0.04* 52.9 3.6 42.7 466.6 30.8 7.2 21.6 0.6 39.9
8 823 27 5 4 0 43.8 2.5 45.1 396.2 32.3 6.0 22.3 0.5 38.9
9 773 33.5 30 6** 0.6 70.0 19.7 7.2 508.0 21.5 30.3 48.2 0.0 0.05
10 773 2.1 5 - - 28.6 5.0 64.7 184.2 24.3 7.4 12.4 1.6 54.3
Note: daf-moisture-and-ash-free basis * KOH/ coal * * water/peat

Claims (8)

1. brown coal and peat are produced the method for hydrogen-containing gas, it is characterized in that comprising the steps: weight ratio 2-10: 1 by water and brown coal or peat, the weight ratio 0.04-0.1 of additive and brown coal or peat: 1 ratio, with grinding particle size at the brown coal of 0.15-0.40mm or grinding particle size at 0.25-0.40mm peat, additive and water add in the high-pressure reactor, under nitrogen atmosphere, temperature rise rate with 10-15 ℃/min makes temperature of reaction reach 350-700 ℃, after reaction pressure reaches 16-40Mpa, reacted 5-60 minute, be cooled to room temperature, the gas-liquid product separates, isolated gas is hydrogen-containing gas, the liquid phase oil aqueous emulsion extracts with tetrahydrofuran (THF) and carries out oily water separation, and isolated tetrahydrofuran (THF) solvend adds anhydrous Na 2SO 4Remove minor amount of water wherein, the tetrahydrofuran (THF) extraction oil evaporates and 0.02MPa under the 60-70 ℃ of condition through at normal pressure, after the vacuum-drying, obtains oil product under the 30-50 ℃ of condition, and isolated water can be recycled; Wherein additive is to separate calcium oxide or the potassium hydroxide that obtains by divided calcium carbonate.
2. a kind of brown coal as claimed in claim 1 and peat are produced the method for hydrogen-containing gas, it is characterized in that described liquid phase oil aqueous emulsion also adds the NaCl breakdown of emulsion when carrying out oily water separation with the tetrahydrofuran (THF) extraction.
3. a kind of brown coal as claimed in claim 1 or 2 and peat are produced the method for hydrogen-containing gas, it is characterized in that described brown coal water content is at 8-25%.
4. a kind of brown coal as claimed in claim 1 or 2 and peat are produced the method for hydrogen-containing gas, and the granularity that it is characterized in that described brown coal is at 0.25-0.40mm.
5. a kind of brown coal as claimed in claim 1 or 2 and peat are produced the method for hydrogen-containing gas, and the temperature of reaction that it is characterized in that described brown coal is in 600-700 ℃ of scope, and the temperature of reaction of peat is in 450-550 ℃ of scope.
6. a kind of brown coal as claimed in claim 1 or 2 and peat are produced the method for hydrogen-containing gas, it is characterized in that described reaction pressure is at 25-35Mpa.
7. a kind of brown coal as claimed in claim 1 or 2 and peat are produced the method for hydrogen-containing gas, and the scope of weight ratio that it is characterized in that described water and brown coal or peat is at 4-6: 1.
8. a kind of brown coal as claimed in claim 1 or 2 and peat are produced the method for hydrogen-containing gas, it is characterized in that the described reaction times was at 5-30 minute.
CN 03145689 2003-07-11 2003-07-11 Method of making hydrogen containing gas using lignite and peat Expired - Lifetime CN1205303C (en)

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CN1205303C true CN1205303C (en) 2005-06-08

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CN111676037A (en) * 2020-06-05 2020-09-18 瀜矿环保科技(上海)有限公司 System for biomass preparation hydrogen and biochar based on steel slag extract

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