CN109107595A - A kind of method of carbon dioxide-water-alcohol system recycling base metal catalysts - Google Patents

A kind of method of carbon dioxide-water-alcohol system recycling base metal catalysts Download PDF

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Publication number
CN109107595A
CN109107595A CN201811061937.4A CN201811061937A CN109107595A CN 109107595 A CN109107595 A CN 109107595A CN 201811061937 A CN201811061937 A CN 201811061937A CN 109107595 A CN109107595 A CN 109107595A
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water
carbon dioxide
alcohol
residue
base metal
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CN201811061937.4A
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Inventor
王志青
梅艳钢
黄戒介
房倚天
张永奇
刘哲语
李俊国
李莉
李翔宇
聂伟
余中亮
宋双双
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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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Priority to CN201811061937.4A priority Critical patent/CN109107595A/en
Publication of CN109107595A publication Critical patent/CN109107595A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/20—Carbon compounds
    • B01J27/232—Carbonates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
    • B01J23/04—Alkali metals
    • 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
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Catalysts (AREA)

Abstract

A kind of method of carbon dioxide-water-alcohol system recycling base metal catalysts, this method leach the water-soluble and water-insoluble alkali metal in catalytic gasification residue by carbon dioxide-water-alcohol system, realize the recycling of insoluble alkali metal.By the way that the solubility of alcohol extracting high carbon dioxide in water is added into hydro-thermal reaction system, to improve carbon dioxide in the acidity of hydro-thermal dissociation process, insoluble alkali metal leaches in residue after gasifying rate and degree are accelerated.The present invention has the advantages that the alkali metal rate of recovery is high, leaching condition is mild, environmental-friendly.

Description

A kind of method of carbon dioxide-water-alcohol system recycling base metal catalysts
Technical field
The invention belongs to catalytic coal gasifaction technical fields, are related to a kind of recovery method of catalytic gasification base metal catalysts.
Background technique
Coal gasification is the important technology realizing Coal Clean and efficiently utilizing, and is the leading technology of coal chemical industry, and catalytic gasification Have many advantages, such as that gasification reaction temperature is low, gasification reaction rate is fast, adjustable gas composition, the thermal efficiency and calorific value of gas are higher, Thus, extensive concern of the catalytic gasification by researcher.The catalyst of catalytic gasification is mainly alkali metal, alkaline-earth metal and mistake Cross metal, wherein catalytic action is preferably mainly base metal catalysts.But the addition of alkali metal improve catalytic gasification at This, meanwhile, the discharge of the residue after gasifying containing alkali can be potentially hazardous to environment generation, therefore, the alkali metal in catalytic gasification residue Catalyst must recycling and reusing.
Base metal catalysts are related to its recovery method and effect in the metamorphosis of catalytic gasification process, and alkali metal is urged Agent mainly exists in the form of two kinds in catalytic gasification process: water-soluble alkali and water-insoluble alkali metal.Water-soluble alkali gold The partially recycled of base metal catalysts can be realized by water extraction by belonging to.During catalytic gasification, alkali metal can be with silicon in coal Aluminium ore substance reaction generates alumino-silicate not soluble in water and nepheline class compound, meanwhile, partial alkaline-metal can also in coal tar Carbon reaction, generate and be similarly difficult to the alkali metal of carbon-based combination, this partial alkaline-metal through the water-soluble recycling for realizing alkali metal. For this purpose, researcher does a lot of work to alkali metal recycling in residue after gasifying.Ju Dian energy company (GPE) develops a kind of water Method (the CN of heat plus carbon dioxide leaching (hereinafter referred to as hydro-thermal carbon dioxide leaches) recycling base metal catalysts 1019100373 A), the method achieve the partially recycled of water-insoluble alkali metal；Zhu Yanfang discloses a kind of catalytic coal gasifaction Catalyst recovery technology (107115896 A of CN), this method realize base metal catalysts using micro-wave digestion-centrifugation washing Recycling；New Austria's energy development resolution method containing Ca is to recycle the alkali metal in residue after gasifying (108067216 A of CN).But dioxy It is relatively small to change carbon solubility in water, hydro-thermal carbon dioxide leaching method is limited by Solubilities of Carbon Dioxide, leaching rate compared with Slowly.And resolution method energy consumption is higher, while generating a large amount of waste residues containing Ca.Therefore on the whole for, existing alkali metal recycling side Method haves the shortcomings that energy consumption is high, waste residue yield is big and catalyst recovery yield is lower, thus, develop it is a kind of it is environmental-friendly, low energy consumption, The high alkali metal recovery method of catalyst recovery yield is very necessary for the industrial application of catalytic gasification.
Summary of the invention
The object of the present invention is to provide a kind of carbon dioxide-water-alcohols environmental-friendly, low energy consumption, catalyst recovery yield is high The method of system recycling base metal catalysts.
The present invention is catalytic gasification residue obtained by catalytic gasification using carbon dioxide-water-alcohol system, improves dioxy by alcohol Change the solvability of carbon in water, the dissolution using carbon dioxide fortified water to alkali metal, to improve base metal catalysts Leaching and the rate of recovery realize base metal catalysts recycling.
Carbon dioxide of the present invention-water-alcohol system recycling base metal catalysts method, includes the following steps:
(1) mixed solution containing alkali metal catalytic gasification residue Yu water and alcohol is 0.1-5MPa, 40- in pressure carbon dioxide Under the conditions of 220 DEG C, 5-120min is leached；
(2) it after the filtering of the mixture of catalytic gasification residue and water and alcohol, obtains the solution containing alkali metal and alkali metal leaching is residual Slag realizes the recycling of base metal catalysts.
Base metal catalysts are salt or alkali containing Na, K in the step (1).
Residue is the carbon containing complete lime-ash of residue or carbon conversion in the step (1).
Alcohol is the low-carbon alcohols such as methanol, ethyl alcohol, ethylene glycol or propyl alcohol in the step (1).
The mass content of alcohol is 1-50wt% in the mixed solution of water and alcohol in the step (1).
Water-alcohol solution and catalytic gasification mass of residue ratio are 5-100:1 in the step (1).
Advantages of the present invention is as follows with technical effect:
1, the rate of recovery of base metal catalysts is higher, and leaching condition is more mild, and low energy consumption；
2, alkali metal is recycled with carbonate form, guarantees that the catalyst of recycling has good catalytic action；
3, using the solubility of alcohol extracting high carbon dioxide, carbon dioxide-aqueous systems are improved in the acidity of alkali metal leaching process.
Technical solution provided by the invention is to recycle base metal catalysts from catalytic gasification residue, in carbon dioxide-water- The recycling for realizing water-insoluble alkali metal in catalytic gasification residue is leached in alcohol system by hydro-thermal.This method utilizes hydro-thermal reaction Decomposition, by the acidity of carbon dioxide, the high feature of the solubility in alcoholic solution is sufficiently combined with carbon dioxide.Thus, it should Alkali metal recovery method has the characteristics that the alkali metal rate of recovery is high, leaching condition is mild, environmental-friendly, has good industrialization Application prospect.
Specific embodiment
The present invention is described in further details below by embodiment, but invention protection scope do not limit to it is described interior Hold.
Embodiment 1: the present embodiment is using the bold and unconstrained coal of grandson family as raw material, with Na2CO3For catalyst, the catalytic gasification 120 at 800 DEG C Min, obtaining efficiency of carbon con version is 98.3% catalysis gas residue, and Na existence form is mainly water solubility Na in catalytic gasification residue2CO3With Water-insoluble sodium silicoaluminate.Catalytic gasification residue leads to 10wt% ethyl alcohol, and in the case where pressure carbon dioxide is 1 MPa, temperature is 100 DEG C 120 min of lower leaching obtain the solution containing Na, are obtained by filtration containing Na2CO3Ethanol water is after the recovery residual with catalyst Slag.
Specific step is as follows:
(a) 10 wt% Na will be loaded2CO3Coal gasify at 800 DEG C, obtain the catalytic gasification residue containing Na；
(b) it is 20 that catalytic gasification residue and 10wt% ethanol water, which consolidate mass ratio by liquid, pressure carbon dioxide 1MPa, 100 120min is leached at DEG C；
(c) it after the filtering of catalytic gasification residue and ethanol water, obtains the solution containing Na catalyst and Na leaches residue, it is real The recycling of existing base metal catalysts.
Recycling filtrate is measured, the rate of recovery for measuring Alkali-Metal Na is 96.7%.
Embodiment 2: the present embodiment is using the bold and unconstrained coal of grandson family as raw material, with K2CO3For catalyst, the catalytic gasification 50 at 900 DEG C Min, obtaining efficiency of carbon con version is 67.4% catalytic gasification residue, and catalytic gasification residue is by 50 wt% ethyl alcohol, in pressure carbon dioxide For under 5MPa, temperature is to leach 120 min at 220 DEG C to obtain the solution containing K, it is obtained by filtration containing K2CO3Ethanol water with Catalyst residue after the recovery.
Specific step is as follows:
(a) 10 wt% K will be loaded2CO3Coal gasify at 900 DEG C, obtain the catalytic gasification residue containing K；
(b) it is 100 that catalytic gasification residue and 50wt% ethanol water, which consolidate mass ratio by liquid, pressure carbon dioxide 5MPa, 220 120min is leached at DEG C；
(c) it after the filtering of the mixture of catalytic gasification residue and ethanol water, obtains the solution containing K catalyst and K leaching is residual Slag realizes the recycling of base metal catalysts.
Recycling filtrate is measured, the rate of recovery of measurement alkali metal K is 98.7%.
Embodiment 3: the present embodiment is using the bold and unconstrained coal of grandson family as raw material, with K2CO3For catalyst, the catalytic gasification at 900 DEG C 120min, obtaining efficiency of carbon con version is 96.5% catalytic gasification residue, and catalytic gasification residue is soaked by 1 wt% glycol water Out, in the case where pressure carbon dioxide is 0.1 MPa, temperature is that leaching 60min obtains the solution containing K at 40 DEG C, is obtained by filtration and contains There is K2CO3Ethylene glycol solution and catalyst residue after the recovery.
Specific step is as follows:
(a) 6wt% K will be loaded2CO3Coal gasify at 900 DEG C, obtain the catalytic gasification residue containing K；
(b) it is 50 that catalytic gasification residue and 1wt% glycol water, which consolidate mass ratio by liquid, pressure carbon dioxide 0.1MPa, 40 60min is leached at DEG C；
(c) it after the mixture filtering of the mixture of catalytic gasification residue and water, obtains the solution containing K catalyst and K is leached Residue realizes the recycling of base metal catalysts.
Recycling filtrate is measured, the rate of recovery of measurement alkali metal K is 78.6%.
Embodiment 4: the present embodiment is using the bold and unconstrained de-ash coal of grandson family as raw material, using KOH as catalyst, the catalytic gasification at 850 DEG C 50 min, obtaining efficiency of carbon con version is 68.3% catalytic gasification residue, and catalytic gasification residue is by 10 wt% methanol solutions, in dioxy Changing carbon pressure power is under 3 MPa, and temperature is to leach 30 min at 150 DEG C to obtain the solution containing K, is obtained by filtration containing K2CO3Methanol Aqueous solution and catalyst residue after the recovery.
Specific step is as follows:
(a) coal for loading 10 wt% KOH is gasified at 850 DEG C, obtains the catalytic gasification residue containing K；
(b) it is 5 that catalytic gasification residue and 10wt% methanol aqueous solution, which consolidate mass ratio by liquid, pressure carbon dioxide 3MPa, 150 DEG C Lower leaching 30min；
(c) it after the filtering of the mixture of catalytic gasification residue and methanol aqueous solution, obtains the solution containing K catalyst and K is leached Residue realizes the recycling of base metal catalysts.
Recycling filtrate is measured, the rate of recovery of measurement alkali metal K is 91.7%.
Embodiment 5: the present embodiment is using the bold and unconstrained coal of grandson family as raw material, using NaOH as catalyst, the catalytic gasification 100 at 850 DEG C Min, obtaining efficiency of carbon con version is 98.3% catalytic gasification residue, and catalytic gasification residue is by 30 wt% ethylene glycol solutions, in titanium dioxide Carbon pressure power is under 3 MPa, and temperature is to leach 5 min at 150 DEG C to obtain the solution containing Na, is obtained by filtration containing Na2CO3Second two Alcohol solution and catalyst residue after the recovery.
Specific step is as follows:
(a) coal for loading 5 wt% NaOH is gasified at 850 DEG C, obtains the catalytic gasification residue containing Na；
(b) catalytic gasification residue and 30 wt% glycol waters consolidate mass ratio by liquid as 30, pressure carbon dioxide 3MPa, 5min is leached at 150 DEG C；
(c) after the filtering of the mixture of catalytic gasification residue and glycol water, the solution and Na containing Na catalyst are obtained Residue is leached, realizes the recycling of base metal catalysts.
Recycling filtrate is measured, the rate of recovery for measuring Alkali-Metal Na is 81.4%.
Embodiment 6: the present embodiment is using the bold and unconstrained coal of grandson family as raw material, with Na2CO3For catalyst, the catalytic gasification at 800 DEG C 120min, obtaining efficiency of carbon con version is 93.3% catalytic gasification residue, and catalytic gasification residue is by 20 wt% aqueous propanol solutions, two Carbon oxide pressure is under 3MPa, and temperature is to leach 50 min at 200 DEG C to obtain the solution containing Na, is obtained by filtration containing Na2CO3 Aqueous propanol solution and catalyst residue after the recovery.
Specific step is as follows:
(a) 5wt% Na will be loaded2CO3Coal gasify at 800 DEG C, obtain the catalytic gasification residue containing Na；
(b) it is 60 that catalytic gasification residue and 20 wt% aqueous propanol solutions, which consolidate mass ratio by liquid, pressure carbon dioxide 3MPa, 200 50min is leached at DEG C；
(c) it after catalytic gasification residue and the mixture of aqueous propanol solution filter, obtains the solution containing Na catalyst and Na soaks Residue out realizes the recycling of base metal catalysts.
Recycling filtrate is measured, the rate of recovery for measuring Alkali-Metal Na is 93.7%.
Comparative example 1: the present embodiment is using the bold and unconstrained de-ash coal of grandson family as raw material, with Na2CO3For catalyst, gas is catalyzed at 800 DEG C Change 50 min, obtaining efficiency of carbon con version is 67.3% catalytic gasification residue, and catalytic gasification residue is 200 DEG C in temperature by water extraction 50 min of lower leaching obtain the solution containing Na, are obtained by filtration containing Na aqueous solution and catalyst residue after the recovery.
Specific step is as follows:
(a) 10 wt% Na will be loaded2CO3Coal gasify at 800 DEG C, obtain the catalytic gasification residue containing Na；
(b) it is 60 that catalytic gasification residue and water, which consolidate mass ratio by liquid, and 50 min are leached at 200 DEG C；
(c) it after the filtering of the mixture of catalytic gasification residue and water, obtains the solution containing Na catalyst and Na leaches residue, realize The recycling of base metal catalysts.
Recycling filtrate is measured, the rate of recovery for measuring Alkali-Metal Na is 55.8%.
Comparative example 2: the present embodiment is using the bold and unconstrained coal of grandson family as raw material, with Na2CO3For catalyst, the catalytic gasification 120 at 800 DEG C Min, obtaining efficiency of carbon con version is 91.2% catalytic gasification residue, and catalytic gasification lime-ash is leached by 20 wt% ethanol solutions, in temperature It is to leach 50 min at 200 DEG C to obtain the solution containing Na, is obtained by filtration after the recovery containing Na ethanol water and catalyst Residue.
Specific step is as follows:
(a) 10 wt% Na will be loaded2CO3Coal gasify at 800 DEG C, obtain the catalytic gasification residue containing Na；
(b) it is 60 that catalytic gasification residue and 20wt% ethanol water, which consolidate mass ratio by liquid, and 50 min are leached at 200 DEG C；
(c) it after the filtering of the mixture of catalytic gasification residue and ethanol water, obtains the solution containing Na catalyst and Na is leached Residue realizes the recycling of base metal catalysts.
Recycling filtrate is measured, the rate of recovery for measuring Alkali-Metal Na is 63.5%.
The rate of recovery of base metal catalysts under one, different condition of table

Claims (6)

1. a kind of carbon dioxide-water-alcohol system recycling base metal catalysts method, it is characterised in that include the following steps:
(1) mixed solution containing alkali metal catalytic gasification residue Yu water and alcohol is 0.1-5MPa, 40- in pressure carbon dioxide Under the conditions of 220 DEG C, 5-120min is leached；
(2) it after the filtering of the mixture of catalytic gasification residue and water and alcohol, obtains the solution containing alkali metal and alkali metal leaching is residual Slag realizes the recycling of base metal catalysts.
2. a kind of carbon dioxide as described in claim 1-water-alcohol system recycling base metal catalysts method, feature exist Base metal catalysts are salt or alkali containing Na, K in the step (1).
3. a kind of carbon dioxide as described in claim 1-water-alcohol system recycling base metal catalysts method, feature exist Residue is the carbon containing complete lime-ash of residue or carbon conversion in the step (1).
4. a kind of carbon dioxide as described in claim 1-water-alcohol system recycling base metal catalysts method, feature exist Alcohol is methanol, ethyl alcohol, ethylene glycol or propyl alcohol in the step (1).
5. a kind of carbon dioxide as described in claim 1-water-alcohol system recycling base metal catalysts method, feature exist The mass content of alcohol is 1-50wt% in the mixed solution of water and alcohol in the step (1).
6. a kind of carbon dioxide as described in claim 1-water-alcohol system recycling base metal catalysts method, feature exist Water-alcohol solution and catalytic gasification mass of residue ratio are 5-100:1 in the step (1).
CN201811061937.4A 2018-09-12 2018-09-12 A kind of method of carbon dioxide-water-alcohol system recycling base metal catalysts Pending CN109107595A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
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
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
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
CN106635176A (en) * 2016-12-22 2017-05-10 中国科学院山西煤炭化学研究所 Coal catalytic gasification method

Patent Citations (4)

* Cited by examiner, † Cited by third party
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
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
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
CN106635176A (en) * 2016-12-22 2017-05-10 中国科学院山西煤炭化学研究所 Coal catalytic gasification method

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Title
XIANGZHOU YUAN, SHUMIN FAN, SEUNG WAN CHOI, HYUNG-TAEKIM: "Potassium catalyst recovery process and performance evaluation of the recovered catalyst in the K2CO3-catalyzed steam gasification system", 《APPLIED ENERGY》 *
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