CN100395181C - Method of preparing active carbon using brown coal in supercritical water - Google Patents
Method of preparing active carbon using brown coal in supercritical water Download PDFInfo
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- CN100395181C CN100395181C CNB2006100481990A CN200610048199A CN100395181C CN 100395181 C CN100395181 C CN 100395181C CN B2006100481990 A CNB2006100481990 A CN B2006100481990A CN 200610048199 A CN200610048199 A CN 200610048199A CN 100395181 C CN100395181 C CN 100395181C
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Abstract
The process of preparing active carbon with brown coal in supercritical water includes filling brown coal into filter and setting in reactor, heating to 500-700 deg.c, pumping in water preheated to 300-650 deg.c into the reactor in the rate of 8000-12000 kg/sq m.hr, raising pressure to 22-40MPa to react for 0.5-3 hr, taking out solid reaction product and soaking in HCl solution of 3-10 vol% at 60-100 deg.c for 10-40, and drying to obtain the active carbon product. The process can utilize brown coal with high water content directly, and has the advantages of lower reaction temperature, short reaction period and no need of pre-treating ash content in brown coal.
Description
Technical field
The invention belongs to a kind of brown coal and produce the method for activated carbon, relate in particular to a kind of method that in the supercritical water medium, prepares activated carbon by one step of brown coal.
Background technology
The brown coal reserves of China reach 1,260 hundred million tons, account for 14% of national coal total reserves, its principal feature be contain that water gaging height, calorific value are low, easy-weathering and spontaneous combustion.The utilization ratio of brown coal is all lower in coal firing boiler and coal gasification course, and major cause is that it must be through the drying process of high energy consumption.In order to reduce the brown coal water content, CN85100817A (the exsiccant complete assembly 1987 that is used for the high-moisture brown coal) and CN1157846A (being used for reducing the method 1997 of former brown coal water content) have proposed the apparatus and method of dry brown coal, obviously this soil that has increased extra equipment, invests and taken for the brown coal utilization respectively.
Active carbon material is the carbon materials with Different Pore Structures, is widely used in other fields such as purification, support of the catalyst, gas storage material and medicine.The brown coal degree of coalification is lower, is one of important source material of producing in mesopore activity carbon.In the coal-based activated carbon process of the conventional system of industry at present:
1. require the feed coal ash content lower or usually, and be difficult to the SiO that removes in the coal through deliming process in advance
2Need consume a large amount of pharmaceutical chemicalss such as hydrofluoric acid in mineral substance;
2. must be to the high brown coal of water content through drying process in advance;
3. must remove volatile matter and heteroatomss such as O, H, S in the coal through carbonization process, generally about 600-900 ℃, its main purpose is to form the carbonized material with certain pore texture and physical strength by pyrolytic reaction to temperature of reaction.The initial hole that forms during charing is bigger, by decolorizing carbon and tar filling or sealing, causes that specific surface area is very little, absorption property is poor;
4. must could obtain the active carbon material of hole prosperity through the inner generation in semicoke surface and the carbon hole oxidizing reaction of reactivation process after charing, usually gas such as water vapour, carbonic acid gas and the oxygen etc. with oxidisability react with the carbon generating gasification, temperature is generally about 800-1100 ℃, purpose is by gasification reaction the blind hole on semicoke surface to be opened, and, make the semicoke specific surface increase in the inner further generation of macropore pore-creating reaction.
Can find out that by above factor there is problems such as being suitable for coal narrow range, process complexity, energy consumption height in industrial conventional activated carbon preparation technology.
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 state of this moment is called supercritical water.Physicochemical properties of supercritical water is between gaseous state and liquid water, and its character is easy to regulate by changing reaction conditions; Supercritical water is better to the solubleness of organism and gas molecule, and to the solubleness of inorganics far below liquid water but greater than the water at atmospheric pressure steam under the uniform temp; Also to have viscosity low for supercritical water in addition, the characteristics that diffustivity is good.
Yang Junbing etc. (CN 1107025C) have reported that the phenolic resin carbonized material activates the result who produces activated carbon in supercritical water, but do not relate to raw materials such as coal or coal tar.Salvador F. etc. are at US6239067, EP0974553 (A1) and ES2155746 (A1) have proposed to utilize supercritical water and supercritical co as activator charing Jiao to be carried out activatory notion flow process and device, but do not have further embodiment report, it relates generally to semicoke or the lower coal of volatile content is carried out the process that priming reaction prepares activated carbon in supercritical water.
Summary of the invention
Produce the problem of coal-based activated carbon at industrial routine, the purpose of this invention is to provide a kind of method for preparing activated carbon by brown coal through one step of supercritical water reaction.
The present invention utilizes the good diffustivity of supercritical water and to organic solvability, treasury is got, pyrolysis and gasification react on one, makes charing-priming reaction finish in same reactor, generates the high-ratio surface activated carbon; In addition, also can be by changing conditions such as temperature of reaction, pressure, the pore structure and the absorption property thereof of control activated carbon.Compare with the inert atmosphere charing, supercritical water can be penetrated into extraction elementary product of pyrolysis and micromolecular compound in the micropore of coal, promotes in the coal volatile matter and S, O etc. are heteroatomic removes; Tar, gas molecule that pyrolysis simultaneously produces are soluble in supercritical water and are taken out of, make that also condensation reaction is difficult to take place, and the hole on semicoke surface is open state.With water at atmospheric pressure steam activation reacting phase ratio, the supercritical water molecule is easy to enter the coal tar depths, priming reaction takes place in depths in semicoke surface and carbon hole simultaneously, promotes micropore to generate and raising priming reaction speed, can generate activated carbon products behind diluted acid wash section ash content.
In addition, also can add alkali metal hydroxide and/or alkaline earth metal oxide in reactive system, alkali metal hydroxide and/or alkaline earth metal hydroxides catalyzer to reach the carrying out of catalytic activation reaction, reduce the purpose of activation temperature.Supercritical water can carry catalyzer and arrive inside, carbon hole, thus might make priming reaction in the depths in carbon hole more effective carrying out, significantly improve the pore volume and the specific surface of activated carbon.Simultaneously, ash content in the feed coal can react with the alkali metal hydroxide that is added, alkaline earth metal oxide or alkaline earth metal hydroxides as quartz, pyrite and clay etc., forming solvend when diluted acid erase residual catalyzer is subsequently removed, this has just reduced the ash oontent in the product, thereby reduced requirement, avoided the pre-deliming operation of feed coal coal ash.
Specifically, the inventive method comprises the steps:
(1) at first with ash oontent at 1-22%, granularity is at pack into strainer and place reactor of the brown coal of 0.075-1mm;
(2) reactor is heated to 500-700 ℃;
(3) with temperature 300-650 ℃ preheating water with 8000-12000kg/hm
2Flow pump into reactor, and rising reaction pressure makes water in the reactor reach 500-700 ℃ of the supercritical state temperature of reaction and the reaction pressure 22-40MPa of water, brown coal stop in reactor and transformed in 0.5-3 hour;
(4) Fan Ying gas, liquid product obtain gaseous product after gas-liquid separation, and product liquid obtains oil product after oily water separation, and the water after the separation can recycle;
(5) the reaction solid product takes out from reactor, joins temperature at 60-100 ℃, and concentration was flooded 10-40 minute in the HCl of 3-10vol%, obtained activated carbon products after the drying.
In the strainer in (1) step, also can add the mixture of alkali metal hydroxide, alkaline earth metal oxide, alkaline earth metal hydroxides, alkali metal hydroxide and alkaline earth metal oxide or the mixture of alkali metal hydroxide and alkaline earth metal hydroxides, and mix with brown coal, the weight percent of itself and brown coal is 3-30%.
The alkali metal hydroxide that is added is KOH or NaOH as mentioned above.
The alkaline earth metal oxide CaO or the MgO that are added as mentioned above.
The alkaline earth metal hydroxides that is added is Ca (OH) as mentioned above
2Or Mg (OH)
2
The brown coal ash oontent of reaction use is preferably in 1-20% as mentioned above.
The brown coal granularity of reaction use is preferably in 0.2-0.5mm as mentioned above.
Temperature of reaction is preferably in 600-700 ℃ as mentioned above.
The residence time is preferably 0.5-2 hour in the reactor as mentioned above.
The pressure of reactor is preferably in 22-35MPa as mentioned above.
The 5-20% that is preferably of the weight percent of the mixture of the mixture of alkali metal hydroxide, alkaline earth metal oxide, alkaline earth metal hydroxides, alkali metal hydroxide and alkaline earth metal oxide or alkali metal hydroxide and alkaline earth metal hydroxides and brown coal as mentioned above.
The concentration of HCl is preferably in 5-8vol% as mentioned above.
The HCl solution temperature is preferably in 80-90 ℃ as mentioned above, the best 20-30min of dipping time.
Characteristics of the present invention:
1. drying-free can directly use the high brown coal of water content;
2. the charing of brown coal, reactivation process can be carried out in a reactor;
3. to compare temperature low with conventional activated carbon activating process, and the reaction times is short;
4. the ash content in the brown coal raw material need not pre-treatment;
5. the entire reaction sealing is carried out, and hot water can be recycled, and technology is environmentally friendly;
6. technological process is simple, and the gas-liquid product is convenient to separate and reclaim;
7. heteroatomic removing such as S, N in the promotion coal.
Description of drawings
Fig. 1 is that brown coal of the present invention transform preparation activated carbon device synoptic diagram as shown in the figure in supercritical water, the 1st, and water pot, the 2nd, the high-pressure pump inlet valve, the 3rd. high-pressure pump, the 4th, water preheater, the 5th, reactor, the 6th, back pressure valve, the 7th, water cooler, the 8th, strainer, the 9th, knockout drum, the 10th. gun barrel.
Embodiment
In order to guarantee that brown coal do not take out of with supercritical water, with pack into strainer and place reactor of a certain amount of raw material; Water directly pumps into reactive system by high-pressure pump; The flow of water is regulated by high-pressure pump, and determines through rotating speed-flux modification curve; Reactor adopts large power, electrically process furnace direct heating, armoured thermocouple is housed respectively in outlet, inlet and the center of reactor measures feed temperature, and reactor also is provided with the armoured thermocouple of assaying reaction wall temperature, with control reaction temperature.The gauge measurement reaction pressure is equipped with in Reactor inlet and outlet respectively.See embodiment 1 in conjunction with Fig. 1 concrete operations.
Embodiment 1
It is stand-by in the water tank 1 that distilled water is packed into.The little dragon's pool brown coal powder of ash content 10.9% is broken to pack into strainer 8 and place reactor 5, N of 0.2-0.5mm
2Replacement(metathesis)reaction system excluding air.By electrical heater reactor 5 is elevated to 650 ℃ of temperature of reaction.During the experiment beginning, drive high-pressure pump inlet valve 2, start water pump 3, regulate flow to 10000kg/ (hm
2), water is preheated to 500 ℃ by water preheater 4, closes back pressure valve 6 and boosts to 25MPa by high-pressure pump 4, and reaction 60min and regulate back pressure valve 6 to keep reaction pressures be 25MPa picks up counting.The gas-liquid product is carried by supercritical water and leaves reactor 5, enters knockout drum and separates and carry out gas-liquid separation in 9 after 7 coolings of back pressure valve 6 step-downs and water cooler, and gaseous product is discharged by knockout drum 9 tops, by wet flow indicator metering sampling analysis also.Product liquid enters gun barrel 10, and oil product is taken out by gun barrel 10 tops, and water then is expelled to water pot 1 by gun barrel 10 bottoms and recycles.Reaction is closed preheater 4 and reactor 5 heating power supplies after finishing, and pumps into cold water by high-pressure pump 3 temperature of reactor is reduced to below 300 ℃, stops high-pressure pump 3 and powered-down.The solid product of reaction is taken out from reactor, remove wherein ash content with temperature at 80 ℃ 6vol%HCl solution impregnation activated carbon 30min then, filter back 105 ℃ of dry 3h and obtain activated carbon products, the activated carbon results of property sees Table 1.
The little dragon's pool brown coal powder of ash content 10.9% is broken to pack into strainer 8 and place reactor 5, N of 0.2-0.5mm
2Replacement(metathesis)reaction system excluding air.By electrical heater reactor 5 is elevated to 700 ℃ of temperature of reaction.Regulate discharge to 8000kg/ (hm
2), preheater is with about water preheat to 650 ℃.Close back pressure valve 6 and boost to 22.1MPa by high-pressure pump 4, reaction 50min picks up counting.Solid product with reaction after reaction finishes takes out from reactor, removes wherein ash content with temperature at 95 ℃ 10vol%HCl solution impregnation activated carbon 10min then, and all the other operations are identical with embodiment 1.The activated carbon results of property sees Table 1.
The little dragon's pool brown coal powder of ash content 10.9% is broken to pack into strainer 8 and place reactor 5, N of 0.5-1mm
2Replacement(metathesis)reaction system excluding air.By electrical heater reactor 5 is elevated to 500 ℃ of temperature of reaction.Regulate discharge to 12000kg/ (hm
2), water is preheated to 300 ℃ by water preheater 4, closes back pressure valve 6 and boosts to reaction pressure 40MPa by high-pressure pump 4, and reaction 180min picks up counting.Solid product with reaction after reaction finishes takes out from reactor, removes wherein ash content with temperature at 60 ℃ 3vol%HCl solution impregnation activated carbon 40min then, and all the other operations are identical with embodiment 1.The results are shown in Table 1.
Embodiment 4
To be crushed to the little dragon's pool brown coal of the ash content 10.9% of 0.2-0.5mm, with catalyzer be that 10% ratio is made into mixture according to potassium hydroxide and brown coal weight percent, add in the strainer 8.All the other operations are identical with embodiment 1.The results are shown in Table 1.
To be crushed to the little dragon's pool brown coal of the ash content 10.9% of 0.2-0.5mm, with catalyzer be that 3% ratio is made into mixture according to potassium hydroxide and brown coal weight percent, add in the strainer 8.By electrical heater reactor 5 is elevated to 600 ℃ of temperature of reaction.Water is preheated to 500 ℃ by water preheater 4, closes back pressure valve 6 and boosts to reaction pressure 25MPa by high-pressure pump 4, and reaction 60min picks up counting.All the other operations are identical with embodiment 1.The results are shown in Table 1.
Embodiment 6
To be crushed to the little dragon's pool brown coal of the ash content 10.9% of 0.075-0.2mm, with catalyzer be that 10% ratio is made into mixture according to calcium oxide/brown coal weight percent, add in the strainer 8.By electrical heater reactor 5 is elevated to 650 ℃ of temperature of reaction.Water is preheated to 500 ℃ by water preheater 4, boosts to reaction pressure 22.5MPa, and reaction 90min picks up counting.All the other operations are identical with embodiment 1, the results are shown in Table 1.
Embodiment 7
To be crushed to the Huo Lin river brown coal of the ash content 21.6% of 0.075-0.2mm, with catalyzer be 1 to 1.8 according to potassium hydroxide and calcium hydroxide weight ratio, catalyst weight and brown coal weight ratio are that 28% ratio is made into mixture, add in the strainer 8.By electrical heater reactor 5 is elevated to 700 ℃ of temperature of reaction.Water is preheated to 600 ℃ by water preheater 4, boosts to reaction pressure 28MPa, and reaction 30min and regulate back pressure valve 6 to keep reaction pressures be 28MPa picks up counting.All the other operations are identical with embodiment 1.The results are shown in Table 1.
The result shows that brown coal can a step generate the high-ratio surface activated carbon in supercritical water, and by changing the purpose that reaction conditions such as temperature of reaction, pressure and interpolation catalyzer can reach control punch structure and specific surface generation.In addition, add behind the catalyzer activated carbon essential substance such as SiO in the ash content in the coal after diluted acid cleans
2, CaO, Fe
2O
3, Al
2O
3, the MgO decreasing ratio can be higher than 90%.This method might form industrial technology, can reduce process energy consumption and activated carbon cost.
Table 1. embodiment gained activated carbon is analyzed
Claims (10)
1. brown coal prepare the method for activated carbon in supercritical water, it is characterized in that comprising the steps:
(1) at first with ash oontent at 1-22%, granularity is at pack into strainer and place reactor of the brown coal of 0.075-1mm;
(2) reactor is heated to 500-700 ℃;
(3) with temperature 300-650 ℃ preheating water with 8000-12000kg/hm
2Flow pump into reactor, and rising reaction pressure makes water in the reactor reach 500-700 ℃ of the supercritical state temperature of reaction and the reaction pressure 22-40MPa of water, brown coal stop in reactor and transformed in 0.5-3 hour;
(4) Fan Ying gas, liquid product obtain gaseous product after gas-liquid separation, and product liquid obtains oil product after oily water separation, and the water after the separation can recycle;
(5) the reaction solid product takes out from reactor, joins temperature at 60-100 ℃, and concentration was flooded 10-40 minute in the HCl of 3-10vol%, obtained activated carbon products after the drying.
2. a kind of brown coal as claimed in claim 1 prepare the method for activated carbon in supercritical water, it is characterized in that described brown coal ash oontent at 1-20%, and granularity is at 0.2-0.5mm.
3. a kind of brown coal as claimed in claim 1 prepare the method for activated carbon in supercritical water, it is characterized in that described temperature of reaction is 600-700 ℃, and reaction pressure is 22-35MPa.
4. a kind of brown coal as claimed in claim 1 prepare the method for activated carbon in supercritical water, it is characterized in that the residence time is 0.5-2 hour in the described reactor.
5. a kind of brown coal as claimed in claim 1 prepare the method for activated carbon in supercritical water, the concentration that it is characterized in that HCl as mentioned above is at 5-8vol%, and the HCl solution temperature is at 80-90 ℃, and dipping time is 20-30 minute.
6. the method that in supercritical water, prepares activated carbon as each described a kind of brown coal of claim 1-5, it is characterized in that also adding the mixture of alkali metal hydroxide, alkaline earth metal oxide, alkaline earth metal hydroxides, alkali metal hydroxide and alkaline earth metal oxide or the mixture catalyzer of alkali metal hydroxide and alkaline earth metal hydroxides in described (1) strainer that goes on foot, and mix with brown coal, the weight percent of itself and brown coal is 3-30%.
7. a kind of brown coal as claimed in claim 6 prepare the method for activated carbon in supercritical water, it is characterized in that described alkali metal hydroxide is KOH or NaOH.
8. a kind of brown coal as claimed in claim 6 prepare the method for activated carbon in supercritical water, it is characterized in that described institute alkaline earth metal oxide is CaO or MgO.
9. a kind of brown coal as claimed in claim 6 prepare the method for activated carbon in supercritical water, it is characterized in that described alkaline earth metal hydroxides is Ca (OH)
2Or Mg (OH)
2
10. a kind of brown coal as claimed in claim 6 prepare the method for activated carbon in supercritical water, the 5-20% that the weight percent that it is characterized in that the mixture catalyzer of the mixture of described alkali metal hydroxide, alkaline earth metal oxide, alkaline earth metal hydroxides, alkali metal hydroxide and alkaline earth metal oxide or alkali metal hydroxide and alkaline earth metal hydroxides and brown coal is.
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| CN101928605A (en) * | 2010-08-17 | 2010-12-29 | 新奥科技发展有限公司 | Method for processing slurry-like residual carbon |
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| CN104628062B (en) * | 2015-02-04 | 2017-04-26 | 西安交通大学 | Method for gasifying unsymmetrical dimethylhydrazine waste liquor through supercritical water |
| CN105349183B (en) * | 2015-11-06 | 2017-11-17 | 中国科学院山西煤炭化学研究所 | The method and apparatus that coal conversion in supercritical water prepares activated carbon by-product combustion gas simultaneously and tar |
| CN105439144A (en) * | 2015-11-18 | 2016-03-30 | 福建翔丰华新能源材料有限公司 | Method for preparing high-performance activated carbon |
| CN109761233A (en) * | 2019-03-05 | 2019-05-17 | 太原科技大学 | The method and apparatus that a kind of overcritical or subcritical water processing distillers ' grains prepare active carbon |
| CN110451508B (en) * | 2019-08-12 | 2021-06-04 | 新疆同力和环材科技有限公司 | Preparation method of coal-based mesoporous activated carbon |
| CN110523378B (en) * | 2019-09-16 | 2022-05-10 | 安徽工业大学 | Application of cyanobacteria mud in algae-water separation station in preparation of biomass activated carbon and in tail water algal toxin adsorption |
| CN112299410B (en) * | 2020-10-26 | 2022-06-24 | 山西国重工程科技有限公司 | High-purity and high-conductivity porous carbon and preparation method thereof |
| CN115228398B (en) * | 2022-06-28 | 2023-09-26 | 同方工业有限公司 | Continuous extraction preparation method and device for coal-based organic micro-nanospheres |
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| CN1086791A (en) * | 1992-11-10 | 1994-05-18 | 昆明煤炭科学研究所 | A kind of manufacture method of high quality brown coal base active carbon |
| US6239067B1 (en) * | 1998-07-23 | 2001-05-29 | Universidad De Salamanca | Process and apparatus for the production of activated carbon |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086791A (en) * | 1992-11-10 | 1994-05-18 | 昆明煤炭科学研究所 | A kind of manufacture method of high quality brown coal base active carbon |
| US6239067B1 (en) * | 1998-07-23 | 2001-05-29 | Universidad De Salamanca | Process and apparatus for the production of activated carbon |
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