CN108728174B - Catalyst recovery method for coal catalytic gasification reaction - Google Patents
Catalyst recovery method for coal catalytic gasification reaction Download PDFInfo
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- CN108728174B CN108728174B CN201710266391.5A CN201710266391A CN108728174B CN 108728174 B CN108728174 B CN 108728174B CN 201710266391 A CN201710266391 A CN 201710266391A CN 108728174 B CN108728174 B CN 108728174B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 38
- 238000002309 gasification Methods 0.000 title claims abstract description 36
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 31
- 239000003245 coal Substances 0.000 title claims abstract description 27
- 238000011084 recovery Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000003513 alkali Substances 0.000 claims abstract description 32
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 14
- 238000010521 absorption reaction Methods 0.000 claims abstract description 8
- 238000004090 dissolution Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 5
- 230000029087 digestion Effects 0.000 claims abstract description 4
- 238000002955 isolation Methods 0.000 claims abstract description 4
- 238000010791 quenching Methods 0.000 claims abstract description 4
- 230000000171 quenching effect Effects 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 16
- 239000011736 potassium bicarbonate Substances 0.000 claims description 8
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 8
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- ZCZLQYAECBEUBH-UHFFFAOYSA-L calcium;octadec-9-enoate Chemical compound [Ca+2].CCCCCCCCC=CCCCCCCCC([O-])=O.CCCCCCCCC=CCCCCCCCC([O-])=O ZCZLQYAECBEUBH-UHFFFAOYSA-L 0.000 claims description 4
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 3
- 229960005147 calcium acetate Drugs 0.000 claims description 3
- 239000001639 calcium acetate Substances 0.000 claims description 3
- 235000011092 calcium acetate Nutrition 0.000 claims description 3
- 239000004227 calcium gluconate Substances 0.000 claims description 3
- 229960004494 calcium gluconate Drugs 0.000 claims description 3
- 235000013927 calcium gluconate Nutrition 0.000 claims description 3
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 229940095643 calcium hydroxide Drugs 0.000 claims description 2
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 229940087373 calcium oxide Drugs 0.000 claims description 2
- 235000012255 calcium oxide Nutrition 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 5
- 239000012670 alkaline solution Substances 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 16
- 239000002893 slag Substances 0.000 abstract description 14
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052700 potassium Inorganic materials 0.000 abstract description 11
- 239000011591 potassium Substances 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000007788 liquid Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- 238000005303 weighing Methods 0.000 description 6
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 150000001340 alkali metals Chemical class 0.000 description 4
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 3
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 229910018516 Al—O Inorganic materials 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- SXQXMCWCWVCFPC-UHFFFAOYSA-N aluminum;potassium;dioxido(oxo)silane Chemical compound [Al+3].[K+].[O-][Si]([O-])=O.[O-][Si]([O-])=O SXQXMCWCWVCFPC-UHFFFAOYSA-N 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 229910052909 inorganic silicate Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- DHCDFWKWKRSZHF-UHFFFAOYSA-N sulfurothioic S-acid Chemical compound OS(O)(=O)=S DHCDFWKWKRSZHF-UHFFFAOYSA-N 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- 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
- C10J3/72—Other features
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
A catalyst recovery method for coal catalytic gasification reaction. The method comprises three steps of pretreatment of catalytic gasification residues, alkali dissolution and alkali washing absorption. (1) After quenching the catalytic gasification residues, collecting and grinding the catalytic gasification residues under the condition of air isolation; (2) adding an alkali solution into the material prepared in the step (1) for alkali dissolution; (3) and (3) adding an alkali solution into the material prepared in the step (2) to perform alkali washing absorption digestion reaction. Washing and centrifuging the product of (3) for multiple times, and extracting a separation solution. The patent develops a technology for recovering the catalyst by ventilating and alkali washing, and test results show that when the water-slag ratio is 2, the total potassium recovery rate reaches 98.8 percent. The method for recovering the catalyst has the advantages of simple process, environmental protection, low energy consumption and high recovery rate.
Description
Technical Field
The invention relates to a method for recovering a catalyst for catalytic coal gasification reaction, and belongs to the technical field of catalytic coal conversion.
Background
Coal accounts for 79% of world energy reserves and is the most abundant fossil energy. Among the coal utilization technologies, the coal gasification technology is the basis and key for clean and efficient utilization and conversion of coal. The coal catalytic gasification technology is a representative technology of a novel coal gasification technology, coal and a catalyst are uniformly mixed according to a certain proportion, and the catalyst dispersed on the surface of the coal better contacts with a gasification agent through erosion slotting action, so that the gas-solid reaction rate is accelerated.
The U.S. Exxon company established a catalytic gasification unit of 1t/d scale in the 70 s of the 20 th century and conducted a great deal of process research. In recent years, GPE company in the United states successfully copies 1t/d test on the basis of Exxon technology, perfects partial technology and develops 'blue gas' (blue gas) for producing SNG by catalytic gasificationTM) Technology ", a commercial demonstration project (" May-Flowery "project) was built in Boston, USA. The technology has the advantages of low water consumption ratio, high heat efficiency and good environmental protection benefit. The technology is popularized and contacted with the domestic Tang group and the universal group. GPE in patent US2009/0165382a1 proposes a set of catalyst recovery schemes: after quenching and water washing, the catalyst semi-coke is in contact reaction with alkali metal hydroxide, and the product is further reacted with CO2Contact reaction to remove residual CO2And after the generated gas is separated from the generated gas, carrying out slag-liquid separation to obtain a catalyst solution. Washing the slag with water to obtain a dilute solution containing a small amount of catalyst; alkali metal hydroxide contact reaction and CO2The purpose of the contact reaction is to convert the insoluble salt into the soluble salt and dissolve and recover the soluble salt.
Much research has been carried out in the aspects of coal catalytic gasification and catalyst recovery in China. The Xinao energy company develops a pilot test research of a coal catalytic gasification technology of 300t/d, adopts a scheme of multi-section fluidized bed (pyrolysis section, catalytic gasification section and combustion gasification section) for fractional gasification and ash fusion slag removal, and is suitable for different coal types. By washing with water (soluble K)+Easy to dissolve in water) + hydrothermal digestion (converting insoluble potassium salt to soluble K+With the aid of basic substances Ca (OH)2Can make the KAlSiO difficult to be compatible4Formation of more insoluble Ca3Al2SiO4(OH)8Simultaneously, KOH is released; ) And recovering the catalyst, wherein the recovery rate of the catalyst is 92-93%. The complete process technology of a large-scale coal catalytic gasification device is developed by combining a tripod project at present. In addition, some colleges and research institutions such as east China university, Zhejiang university, Shanxi coal chemical institute have literature and patent reports, but most of them stay in the laboratory.
Common coal gasification catalysts are alkali metals, alkaline earth metals, transition metals and the like, wherein hydroxides and carbonates of alkali metals are accepted as the monomer catalysts with the highest efficiency. Compared with direct coal gasification, the catalytic coal gasification technology has obvious advantages, but the catalytic coal gasification has not been industrialized so far, mainly because a large amount of alkaline substances are remained in the slag after catalytic gasification, and the direct discharge of alkaline ash slag causes serious pollution to the environment, and more importantly, the high catalyst cost causes the catalytic gasification technology to lose economic benefits.
In conclusion, the alkali metal catalyst has large load, easy inactivation, high catalyst cost, immature recovery process, pollution of alkali-containing ash, no economic benefit of the alkali metal coal catalytic gasification technology and other factors, and restricts the large-scale popularization of coal catalytic gasification.
Disclosure of Invention
The purpose of the invention is as follows: the invention provides a catalyst recovery method for catalytic coal gasification reaction, and can provide a catalyst recovery method with simple process, environmental protection, low energy consumption and high recovery rate
The technical scheme is as follows: the invention provides a catalyst recovery method for coal catalytic gasification reaction, which comprises the steps of pretreatment of catalytic gasification residues, alkali dissolution and alkali washing absorption, and is characterized by comprising the following steps:
step 1): after quenching the catalytic gasification residues, collecting and grinding the catalytic gasification residues under the condition of air isolation;
step 2): adding an alkali solution into the material prepared in the step 1) for alkali dissolution;
step 3): adding an alkali solution into the material prepared in the step 2) for alkali washing absorption to generate a digestion reaction.
Step 4): washing and centrifuging the product obtained in the step 3) for multiple times, and extracting the separated liquid.
Typically, the collecting and grinding atmosphere is N2The particle size of the residue after grinding is 0.250 to 0.425 mm.
The alkali liquor in the step 2) is KHCO3The pH is controlled at7~9。
The atmosphere for dissolving the alkali in the step 2) is CO2The temperature is 80-150 ℃, the pressure is 1.2-2.5 MPa, the stirring speed is 200-800 r/min, and the time is 20-60 min.
The alkali liquor in the step 3) is organic calcium salt or inorganic calcium salt, preferably one or more than two of calcium hydroxide, calcium oxide, calcium gluconate, calcium acetate and calcium oleate.
The alkali dissolving atmosphere in the step 3) is N2Or air, the temperature is 150-220 ℃, the pressure is 1.5-2.5 MPa, the stirring speed is 200-800 r/min, and the time is 1-4 h.
The invention has the following effects:
1. green and environment-friendly, and simple process. The catalyst is collected and ground under the condition of air isolation, potassium sulfide in residues is reduced from being oxidized into various inert substances without catalytic activity, such as sulfide, thiosulfate, sulfate and the like after being exposed to air, the collection of sulfur is reduced, and meanwhile, water consumption is reduced in the process of absorbing alkali solution and alkali washing.
2. The recovery rate is improved, the pH value is controlled during alkaline dissolution, the concentration of silicon in the residue is reduced, the generation of silicide without catalytic activity is inhibited, and CO is introduced2Removing the potassium aluminosilicate without catalytic activity so that the potassium exists in the form of soluble potassium salt; alkali washing absorption takes alkali as a dissolving agent, and KAlSiO which is a slightly soluble salt4The bond between Al-O and Si-O is broken, and the difficult-to-dissolve potassium salt is converted into soluble potassium salt, so that the recovery rate of the active component is improved. Test results show that when the mass ratio of the grain slag is 2, the total potassium recovery rate reaches 98.8 percent.
3. The alkali dissolving process supplements the unrecoverable active ingredients, and prepares for the subsequent cyclic utilization of the catalyst, and the process is simple.
Detailed Description
The process of the present invention is described in detail below with reference to examples, but the examples are only illustrative and are not intended to limit the scope of the present invention.
Example 1
In N2Weighing 1g of catalyst residue under the atmosphere, grinding to 60-100 meshes, and adding KHCO3Catalyst residues treated by solution additionIn the slag, PH is 9, introducing CO into the reaction kettle2The temperature is 150 ℃, the pressure is 1.2MPa, the stirring speed is 300r/min, and the time is 20 min. Then adding the calcium hydroxide solution into a reaction kettle, wherein the mass ratio of the alkaline residue is 8:1, and the atmosphere is N2The temperature is 220 ℃, the pressure is 2.5MPa, the stirring speed is 300r/min, and the time is 4 h. The product was then washed with water 3 times and centrifuged, and the separated liquid was extracted. The mass ratio of the grain slag is 14:1, and the total potassium recovery rate is 96.8 percent
Example 2
In N2Weighing 1g of catalyst residue under the atmosphere, grinding to 60-100 meshes, and adding KHCO3Adding the solution into the treated catalyst residue, adjusting the pH to 8, introducing CO into a reaction kettle2The temperature is 150 ℃, the pressure is 1.2MPa, the stirring speed is 300r/min, and the time is 30 min. Then adding the calcium hydroxide solution into a reaction kettle, wherein the mass ratio of the alkaline residue is 4:1, and the atmosphere is N2The temperature is 220 ℃, the pressure is 2MPa, the stirring speed is 400 r/min, and the time is 2 h. The product was then washed with water 3 times and centrifuged, and the separated liquid was extracted. The mass ratio of the grain slag is 6:1, and the total potassium recovery rate is 97.2 percent
Example 3
In N2Weighing 1g of catalyst residue under the atmosphere, grinding to 60-100 meshes, and adding KHCO3Adding the solution into the treated catalyst residue, adjusting the pH to 8, introducing CO into a reaction kettle2The temperature is 150 ℃, the pressure is 1.2MPa, the stirring speed is 300r/min, and the time is 30 min. Then adding the calcium oleate solution into a reaction kettle, wherein the mass ratio of the alkaline residue is 2:1, the atmosphere is air, the temperature is 160 ℃, the pressure is 2MPa, the stirring speed is 400 r/min, and the time is 2 h. The product was then washed with water 3 times and centrifuged, and the separated liquid was extracted. The mass ratio of the grain slag is 2:1, and the total potassium recovery rate is 98.8 percent
Example 4
In N2Weighing 1g of catalyst residue under the atmosphere, grinding to 60-100 meshes, and adding KHCO3Adding the solution into the treated catalyst residue, adjusting the pH to 8, introducing CO into a reaction kettle2The temperature is 150 ℃, the pressure is 1.2MPa, the stirring speed is 300r/min, and the time is 30 min. Then adding calcium oleate solution into a reaction kettle, wherein the mass ratio of the alkaline residue is 2:1, and the atmosphere is N2Temperature of 160 ℃, pressure of 2MPa and stirring speed of 400r/min, time 2 h. The product was then washed with water 3 times and centrifuged, and the separated liquid was extracted. The mass ratio of the grain slag is 4:1, and the total potassium recovery rate is 97.4 percent
Example 5
In N2Weighing 1g of catalyst residue under the atmosphere, grinding to 60-100 meshes, and adding KHCO3Adding the solution into the treated catalyst residue, adjusting the pH to 8, introducing CO into a reaction kettle2The temperature is 150 ℃, the pressure is 1.2MPa, the stirring speed is 400 r/min, and the time is 20 min. Then adding the calcium acetate solution into a reaction kettle, wherein the ratio of caustic sludge to caustic sludge is 2:1, the atmosphere is air, the temperature is 160 ℃, the pressure is 2.5MPa, the stirring speed is 800 r/min, and the time is 2 hours. The product was then washed with water 3 times and centrifuged, and the separated liquid was extracted. The mass ratio of the grain slag is 5:1, and the total potassium recovery rate is 96.8 percent
Example 6
In N2Weighing 1g of catalyst residue under the atmosphere, grinding to 60-100 meshes, and adding KHCO3Adding the solution into the treated catalyst residue, adjusting the pH to 9, introducing CO into the reaction kettle2The temperature is 150 ℃, the pressure is 1.2MPa, the stirring speed is 300r/min, and the time is 30 min. Then adding the calcium gluconate solution into the reaction kettle, wherein the ratio of alkali to residue is 8:1, the atmosphere is air, the temperature is 160 ℃, the pressure is 2.5MPa, the stirring speed is 400 r/min, and the time is 2 hours. The product was then washed with water 3 times and centrifuged, and the separated liquid was extracted. The mass ratio of the grain slag is 1:1, and the total potassium recovery rate is 96.3 percent
The results of the above examples show that under the process conditions of the present invention, the recovery rate of total potassium reaches more than 96%, wherein under the process conditions of example 3, the mass ratio of water to slag is 2:1, and the recovery rate of total potassium is 98.8%.
Claims (1)
1. A catalyst recovery method for coal catalytic gasification reaction comprises pretreatment of catalytic gasification residues, alkali dissolution and alkali washing absorption, and is characterized by comprising the following steps:
step 1): after quenching the catalytic gasification residues, collecting and grinding the catalytic gasification residues under the condition of air isolation to obtain residues;
step 2): adding the residue obtained in the step 1) into an alkali solution for alkali dissolution;
step 3): adding an alkali solution into the material prepared in the step 2) for alkali washing absorption to generate a digestion reaction;
step 4): washing and centrifugally separating the product obtained in the step 3), and extracting a separation solution;
said collecting and grinding in step 1) is at N2The grinding is carried out under an atmosphere, and the particle size of the residue after grinding is 0.250-0.425 mm.
The alkali solution in the step 2) is KHCO3The pH of the aqueous solution is controlled to be 7-9, and the alkaline solution is CO2The reaction is carried out under the atmosphere, the temperature is 80-150 ℃, the pressure is 1.2-2.5 MPa, the stirring speed is 200-800 r/min, and the time is 20-60 min.
The alkali solution in the step 3) is one or more of calcium hydroxide, calcium oxide, calcium gluconate, calcium acetate and calcium oleate; the alkaline wash absorption is in N2Or the reaction is carried out in an air atmosphere at the temperature of 150-220 ℃, the pressure of 1.5-2.5 MPa, the stirring speed of 200-800 r/min and the time of 1-4 h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101484554A (en) * | 2006-06-01 | 2009-07-15 | 格雷特波因特能源公司 | Catalytic steam gasification process with recovery and recycle of alkali metal compounds |
| CN101910370A (en) * | 2007-12-28 | 2010-12-08 | 格雷特波因特能源公司 | Catalytic gasification method for recovery of alkali metals from coke |
| CN104815673A (en) * | 2015-03-11 | 2015-08-05 | 新奥科技发展有限公司 | Recovery method for potassium catalyst in coal catalytic gasification ash |
-
2017
- 2017-04-21 CN CN201710266391.5A patent/CN108728174B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101484554A (en) * | 2006-06-01 | 2009-07-15 | 格雷特波因特能源公司 | Catalytic steam gasification process with recovery and recycle of alkali metal compounds |
| CN101910370A (en) * | 2007-12-28 | 2010-12-08 | 格雷特波因特能源公司 | Catalytic gasification method for recovery of alkali metals from coke |
| CN104815673A (en) * | 2015-03-11 | 2015-08-05 | 新奥科技发展有限公司 | Recovery method for potassium catalyst in coal catalytic gasification ash |
Non-Patent Citations (1)
| Title |
|---|
| 中温煤-水蒸气气化过程催化剂的回收利用研究;陈杰;《中国优秀硕士学位论文库》;20120105;正文第29-42页 * |
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