CN104449865A - Method for improving catalytic coal gasification activity and catalyst recovery rate - Google Patents
Method for improving catalytic coal gasification activity and catalyst recovery rate Download PDFInfo
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- CN104449865A CN104449865A CN201410548041.4A CN201410548041A CN104449865A CN 104449865 A CN104449865 A CN 104449865A CN 201410548041 A CN201410548041 A CN 201410548041A CN 104449865 A CN104449865 A CN 104449865A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
- C10J3/46—Gasification of granular or pulverulent flues in suspension
- C10J3/54—Gasification of granular or pulverulent fuels by the Winkler technique, i.e. by fluidisation
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
- C10J2300/0913—Carbonaceous raw material
- C10J2300/093—Coal
- C10J2300/0936—Coal fines for producing producer gas
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
- C10J2300/0983—Additives
- C10J2300/0986—Catalysts
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
- C10J2300/00—Details of gasification processes
- C10J2300/16—Integration of gasification processes with another plant or parts within the plant
- C10J2300/1625—Integration of gasification processes with another plant or parts within the plant with solids treatment
- C10J2300/1628—Ash post-treatment
- C10J2300/1631—Ash recycling
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention discloses a method for improving catalytic activity and catalyst water washing recovery rate. The method comprises the following steps: by taking high-ash-content coal as a raw material, carrying out HCl-HF-HCl de-ashing treatment on raw coal; adding a potassium carbonate catalyst to coal after acid de-ashing for dipping load according to the volume ratio of the coal after acid de-ashing to a K2CO3 solution being 1 to 1, wherein the adding amount of the catalyst potassium carbonate is 2-10wt%; gasifying the prepared catalyst-loaded sample in a high-pressure fluidized bed, wherein the gasification reaction temperature is 650-750 DEG C, the reaction pressure is 3-4MPa, the standing time is 1-3 hours, and the condition is steam atmosphere; washing gasified residue with water of which the water-slag volume ratio is 3-5 times at 60-80 DEG C for 20-30 minutes, and recycling the catalyst washing water. The method disclosed by the invention has the advantages of being simple and practical, and capable of meeting application of high-ash-content coal in the catalytic gasification process.
Description
Technical field
The present invention relates to a kind of method improving catalytic coal gasifaction activity and catalyst recovery yield.
Background technology
Gasification is the main method realizing Coal Clean and efficiency utilization, is most important and one of the gordian technique the most widely of development Modern Coal-based Chemical.The catalytic gasification of coal is a kind of advanced gasification process reducing temperature of reaction, improve speed of reaction, improve gas composition.The catalytic gasification of coal carries out under the state being solid at coal, the powder of catalyzer and coal mixes according to a certain percentage equably, the catalyzer of coal surface arrangement, by corroding fluting effect, makes coal and vaporized chemical contact better to reach to obtain at a lower temperature compared with high reaction rate and the object of direct synthetic natural gas.In quickening coal gasification speed, improve charcoal percent conversion, in same gasification rate decline low reaction temperatures, reduce energy expenditure and realize the aspects such as gasification product directional trend there is superiority.
The low-temperature catalysis gasification of coal was once the study hotspot of Coal Chemical Industry scholar when oil crisis in last century.In the interpolation catalyzer such as alkali, alkaline-earth metal situation, coal can 650 DEG C-750 DEG C rapid generating gasification reactions, have that gasification efficiency is high, facility investment is little, without the need to making oxygen by air separation, and outside heat-conducting mode can be utilized to carry out the advantages such as steam gasification.Exxon company of the U.S. once built catalytic gasification pilot scale gasification installation at the beginning of the eighties, was regarded as representational catalysis gasification technique.
According to result of study in the past, K
2cO
3it is catalyzer best in coal gasification course, but, due to the existence of clay mineral in the material of colliery, generate the potassium aluminum silicate of inertia with catalytic gasification sylvite catalyzer used, reduce catalytic effect significantly, particularly silicon, coal that aluminium content is high are totally unfavorable to catalytic gasification; And potassium aluminum silicate is water insoluble, causes catalyst recovery difficulty, be difficult to recycle; Cause high cost and lack competitiveness, catalytic gasification fails to promote and industrial application in the coal conversion process developed in 20th century, studies carefully inactivation and loss that its major cause is just catalyzer.The reaction of this inactivation is as follows:
K
2CO
3+2SiO
2·Al
2O
3·2H
2O→2KAlSiO
4+2H
2O+CO
2
The effect that correlative study reports catalyzer and coal ash causes catalyst deactivation and catalyst recovery difficulty.The people such as Giacomo Bruno have studied K
2cO
3respectively with quartz, illite, kaolinite three kinds of minals at steam atmosphere, pressure is 3.6MPa temperature of reaction is 973K, and the residence time is the characteristic of reacted residue under the environment of 3 hours.Result shows, the rate of recovery of potassium after hot water wash of reacting in rear three kinds of residues is respectively: 100%, 44% and 52%, and K is described
2cO
3with illite, kaolinite mineral there occurs reaction, generates the material not easily washed.
The people such as Lothar Kuhn have selected the coal sample having carried out being rich in sial and carry out interpolation K
2cO
3the research of catalytic gasification, result shows, the mineral containing potassium in residue are kaliophylite (KAlSiO
4) and potassium aluminosilicate (K (Al, the Fe) SiO of iron content
4).
K. the coal that the people such as Formella have studied different coal ash content adds the rate of catalysis reaction after catalyzer.Result shows, when coal ash content is 30.1%, coal that the catalyzer of interpolation 17.1% could be 18.8% with ash content is needed to add the catalytic rate of the catalyzer of 9.9% suitable, under catalytic gasification environment, catalyzer and coal ash generate aluminosilicate mineral, the generation of these mineral makes the effective constituent of catalyzer reduce, and reduces the catalytic efficiency of catalyzer.
Domestic East China University of Science is also studied the interaction of catalyzer and minerals in coal.The steam catalytic gasification of salt of wormwood to coal is have studied in fixed-bed reactor, investigate the interaction of potassium and 10 kinds of minerals in coal, result shows, in coal steam gasification process, potassium carbonate catalyst and minerals in coal interact the compound being formed and be insoluble in water.When in pit ash, calcium contents is less, in the amount gentle ashing slag that potassium catalyzer and mineral substance react, aluminium content is linear, i.e. K:A1=1:1.The amount of potassium and mineral substance reaction affects the katalysis of potassium catalyzer.
Summary of the invention
Instant invention overcomes above-mentioned technical deficiency part, its object is to provide a kind of method improving catalyst activity and catalyst recovery yield in catalysis gasification technique, the method is simple and practical, meets the application of coal at catalysis gasification technique of high ash oontent.
Above-mentioned purpose of the present invention is achieved through the following technical solutions.
Improve a method for catalytic activity and the catalyzer washing rate of recovery, comprise the steps:
(1) it with the coal of high ash oontent for raw material, the process of HCl-HF-HCl deliming is carried out to raw coal, step and the processing condition of detailed deliming process are shown in Chen Haokan. the research of sulphur transition rule in pyrolysis and hydropyrolysis process. and Shanxi Inst. of Coal Chemistry, Chinese Academy of Sciences, 1998;
(2) by the coal after sour deliming and K
2cO
3solution is 1:1 by volume, the coal after sour deliming is added potassium carbonate catalyst and carries out dip loading, and the addition of catalyzer salt of wormwood is 2-10wt%(mass percent);
(3) sample of the supported catalyst prepared gasifies in high pressure fluidized-bed, gasification reaction temperature 650 DEG C-750 DEG C, reaction pressure 3-4 MPa, and the residence time is 1-3h, steam atmosphere;
(4) residue after gasification is 3-5 times of water through grain slag volume ratio, at 60-80 DEG C, after washing 20-30 min, is recycled by catalyst detergent Water Sproading.
Mineral substance in ash content of coal often exists with inert condition, and particularly on-catalytic composition is as SiO
2, burnt hole can be blocked, reduce the contact area of vaporized chemical and carbon, hinder the carrying out of gasification reaction.Deliming process is stripped of the part coal ash of blocking hole, part blind hole is opened, can produces new vesicular structure.The generation of new vesicular structure, can increase the specific surface area of coal tar, improves the useful area that vaporized chemical contacts with carbon, reaction rate accelerates.Along with the carrying out of catalytic gasification, the coal of non-deliming, ash can form large shell, blocking duct.Thus, deliming coal tar is burnt relative to raw coal, has higher gasification reactivity.On the other hand, after deliming, the content of coal CLAY MINERALS AND THEIR SIGNIFICANCE reduces, and the degree of catalyzer and these substance reactions reduces, and improves the washing rate of recovery of catalyzer.
The present invention has the following advantages:
(1) be stripped of the ash content in coal, the catalyzer making interpolation a small amount of has very high catalytic activity.
(2) improve the washing rate of recovery of catalyzer.
(3) subject range of coal in catalysis gasification technique is expanded.
(4) the present invention can be widely used in the independent gasification of coal, biomass (comprising rubbish etc.) etc. or the common gasification of burning and coal and biomass and catalytic gasification.
Embodiment:
The present invention is described in detail as follows in conjunction with the embodiments:
Comparative example 1
(1) king family's tower raw coal is in fluidized-bed, temperature of reaction 750 DEG C, reaction pressure 3.5MPa, and the residence time is 3h, gasifies under steam atmosphere, and efficiency of carbon conversion is 51.6%.
(2) raw coal is pulverized, adopt granularity be less than 0.096mm(-160 order) coal sample 50g, add the hydrochloric acid 200ml of 5M, heat 2 hours in the water bath with thermostatic control of 55-60 DEG C, stirred once every 10 minutes, subsequently coal sample is filtered, be transferred in plastic beaker, add the hydrofluoric acid of 200ml, heat as stated above, dissolve, filter, then coal sample is transferred in beaker, add concentrated hydrochloric acid 200ml, repeat heating in water bath operation, the coal sample of HCl treatment is filtered, carefully wash with the distilled water of heat, until use AgNO
3solution detects in filtrate to be existed without Cl ion, obtained de-ash coal.
(3) step (2) is prepared sample in fluidized-bed, temperature of reaction 750 DEG C, reaction pressure 3.5MPa, the residence time is 3h, gasifies under steam atmosphere, and efficiency of carbon conversion is 81.1%.
Embodiment 1
(1) king family's tower coal sample and K
2cO
3catalyst solution carries out dip loading for 1:1 by volume, makes K in supported catalyst king family tower coal sample
2cO
3catalyst loadings is 2wt%.
(2) raw coal is pulverized, adopt granularity be less than 0.096mm(-160 order) coal sample 50g, add the hydrochloric acid 200ml of 5M, heat 2 hours in the water bath with thermostatic control of 55-60 DEG C, stirred once every 10 minutes, subsequently coal sample is filtered, be transferred in plastic beaker, add the hydrofluoric acid of 200ml, heat as stated above, dissolve, filter, then coal sample is transferred in beaker, add concentrated hydrochloric acid 200ml, repeat heating in water bath operation, the coal sample of HCl treatment is filtered, carefully wash with the distilled water of heat, until use AgNO
3solution detects in filtrate to be existed without Cl ion, obtained de-ash coal.
(3) step (2) is prepared sample and K
2cO
3catalyst solution carries out dip loading for 1:1 by volume, makes K in supported catalyst king family tower coal sample
2cO
3catalyst loadings is 2wt%.
(4) step (1) is prepared sample in fluidized-bed, temperature of reaction 750 DEG C, reaction pressure 4MPa, the residence time is 1h, gasifies under steam atmosphere, and efficiency of carbon conversion is 63.6%.
(5) step (3) is prepared sample in fluidized-bed, temperature of reaction 750 DEG C, reaction pressure 4MPa, the residence time is 1h, gasifies under steam atmosphere, and efficiency of carbon conversion is 86%.
(6) residue after step (4) being gasified is 3 times through grain slag volume ratio, and at 60 DEG C, after washing 20min, catalyst recovery yield is 32.6%.
(7) residue after step (5) being gasified is 3 times through grain slag volume ratio, and at 60 DEG C, the washing 20min rear catalyst rate of recovery is 51.9%.
Embodiment 2
(1) king family's tower coal sample and K
2cO
3catalyst solution carries out dip loading for 1:1 by volume, makes K in supported catalyst king family tower coal sample
2cO
3catalyst loadings is 5wt%.
(2) raw coal is pulverized, adopt granularity be less than 0.096mm(-160 order) coal sample 50g, add the hydrochloric acid 200ml of 5M, heat 2 hours in the water bath with thermostatic control of 55-60 DEG C, stirred once every 10 minutes, subsequently coal sample is filtered, be transferred in plastic beaker, add the hydrofluoric acid of 200ml, heat as stated above, dissolve, filter, then coal sample is transferred in beaker, add concentrated hydrochloric acid 200ml, repeat heating in water bath operation, the coal sample of HCl treatment is filtered, carefully wash with the distilled water of heat, until use AgNO
3solution detects in filtrate to be existed without Cl ion, obtained de-ash coal.
(3) step (2) is prepared sample and K
2cO
3catalyst solution carries out dip loading for 1:1 by volume, makes K in supported catalyst king family tower coal sample
2cO
3catalyst loadings is 5wt%.
(4) step (1) is prepared sample in fluidized-bed, temperature of reaction 700 DEG C, reaction pressure 3.5MPa, the residence time is 2h, gasifies under steam atmosphere, and efficiency of carbon conversion is 80.6%.
(5) step (3) is prepared sample in fluidized-bed, temperature of reaction 700 DEG C, reaction pressure 3.5MPa, the residence time is 2h, gasifies under steam atmosphere, and efficiency of carbon conversion is 90.3%.
(6) residue after step (4) being gasified is 4 times through grain slag volume ratio, and at 70 DEG C, after washing 25min, catalyst recovery yield is 53.8%.
(7) residue after step (5) being gasified is 4 times through grain slag volume ratio, and at 70 DEG C, after washing 25min, catalyst recovery yield is 79.8%.
Embodiment 3
(1) king family's tower coal sample and K
2cO
3catalyst solution carries out dip loading for 1:1 by volume, makes K in supported catalyst king family tower coal sample
2cO
3catalyst loadings is 10wt%.
(2) raw coal is pulverized, adopt granularity be less than 0.096mm(-160 order) coal sample 50g, add the hydrochloric acid 200ml of 5M, heat 2 hours in the water bath with thermostatic control of 55-60 DEG C, stirred once every 10 minutes, subsequently coal sample is filtered, be transferred in plastic beaker, add the hydrofluoric acid of 200ml, heat as stated above, dissolve, filter, then coal sample is transferred in beaker, add concentrated hydrochloric acid 200ml, repeat heating in water bath operation, the coal sample of HCl treatment is filtered, carefully wash with the distilled water of heat, until use AgNO
3solution detects in filtrate to be existed without Cl ion, obtained de-ash coal.
(3) step (2) is prepared sample and K
2cO
3catalyst solution carries out dip loading for 1:1 by volume, makes K in supported catalyst king family tower coal sample
2cO
3catalyst loadings is 10wt%.
(4) step (1) is prepared sample in fluidized-bed, temperature of reaction 650 DEG C, reaction pressure 3MPa, the residence time is 3h, gasifies under steam atmosphere, and efficiency of carbon conversion is 90.1%.
(5) step (3) is prepared sample in fluidized-bed, temperature of reaction 650 DEG C, reaction pressure 3MPa, the residence time is 3h, gasifies under steam atmosphere, and efficiency of carbon conversion is 93.3%.
(6) residue after step (4) being gasified is 5 times through grain slag volume ratio, and at 80 DEG C, after washing 30min, catalyst recovery yield is 65.8%.
(7) residue after step (5) being gasified is 5 times through grain slag volume ratio, and at 80 DEG C, after washing 30min, catalyst recovery yield is 89.6%.
Be more than preferred embodiment of the present invention, the unsubstantiality that every technical solution of the present invention is done improves, and when the function produced does not exceed the scope of technical solution of the present invention, all belongs to protection scope of the present invention.
Claims (1)
1. improve a method for catalytic coal gasifaction activity and catalyst recovery yield, it is characterized in that comprising the steps:
(1) it is with the coal of high ash oontent for raw material, carries out the process of HCl-HF-HCl deliming to raw coal;
(2) by the coal after sour deliming and K
2cO
3solution is 1:1 by volume, the coal after sour deliming is added potassium carbonate catalyst and carries out dip loading, and the addition of catalyzer salt of wormwood is 2-10wt%;
(3) sample of the supported catalyst prepared gasifies in high pressure fluidized-bed, gasification reaction temperature 650 DEG C-750 DEG C, reaction pressure 3-4 MPa, and the residence time is 1-3h, steam atmosphere;
(4) residue after gasification is 3-5 times of water through grain slag volume ratio, at 60-80 DEG C, after washing 20-30 min, is recycled by catalyst detergent Water Sproading.
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Cited By (15)
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CN105567330A (en) * | 2015-12-17 | 2016-05-11 | 新奥科技发展有限公司 | Catalytic gasification method of high-ash-content anthracite |
CN106064100A (en) * | 2016-05-31 | 2016-11-02 | 新奥科技发展有限公司 | A kind of processing method of base metal catalysts washing recovered liquid |
CN106064099A (en) * | 2016-05-31 | 2016-11-02 | 新奥科技发展有限公司 | The recovery method of insolubility base metal catalysts in a kind of catalytic gasification lime-ash |
CN106590762A (en) * | 2015-10-15 | 2017-04-26 | 中国石油化工股份有限公司 | Method for improving performance of catalyst in catalytic coal gasification by using composite additive |
CN106590748A (en) * | 2016-12-22 | 2017-04-26 | 中国科学院山西煤炭化学研究所 | Catalytic pyrolysis and gasification method for leather waste |
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CN106635175A (en) * | 2016-12-22 | 2017-05-10 | 中国科学院山西煤炭化学研究所 | Catalytic gasification method for petroleum coke |
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CN110624581A (en) * | 2018-06-25 | 2019-12-31 | 中国石油化工股份有限公司 | Method for recovering coal gasification catalyst |
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CN106064100B (en) * | 2016-05-31 | 2018-07-13 | 新奥科技发展有限公司 | A kind of processing method of base metal catalysts washing recovered liquid |
CN106064100A (en) * | 2016-05-31 | 2016-11-02 | 新奥科技发展有限公司 | A kind of processing method of base metal catalysts washing recovered liquid |
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