CN102476008A - Method for recovering and recycling alkali metal catalyst - Google Patents
Method for recovering and recycling alkali metal catalyst Download PDFInfo
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- CN102476008A CN102476008A CN2010105657702A CN201010565770A CN102476008A CN 102476008 A CN102476008 A CN 102476008A CN 2010105657702 A CN2010105657702 A CN 2010105657702A CN 201010565770 A CN201010565770 A CN 201010565770A CN 102476008 A CN102476008 A CN 102476008A
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Abstract
The invention provides a method for recovering an alkali metal catalyst from gas of a coal gasification furnace. The method comprises the following steps that: a, the gas of the coal gasification furnace passes through a filter adopting porous coke as a filtering medium, such that at least the partial alkali metal catalyst is trapped on the porous coke; b, the gas leaving the filter is introduced into a gas washing tower, such that the remaining alkali metal catalyst is dissolved in the water to form the water solution of the alkali metal catalyst. The present invention further relates to a coal gasification method for recovering and recycling the alkali metal catalyst.
Description
Invention field
The present invention relates to reclaim the method for catalyst, more specifically, the present invention relates to from method from recovery base metal catalysts the gas of coal gasifier.The invention still further relates to the coal gasification method that reclaims and recycle base metal catalysts.
Background technology
The catalysis gasification technique of coal is meant that coal is CO, H by the gasifying agent gasification under the catalytic action of catalyst
2, CH
4Technology Deng gas.Three sections stove catalysis gasification techniques of the catalytic coal gasifaction system methane research that typical catalytic coal gasifaction technology has an EXXON and Japanese catalytic coal gasifaction hydrogen producing technology and Chinese Xin Ao group company are seen patent US3932146, JP2004292720, CN101792680.General alkaline metal salt and/or the alkaline-earth metal salt of using is called base metal catalysts and alkaline-earth metal catalyst respectively usually as catalyst in the above-mentioned technology.Because coal gasification is carried out under higher temperature usually, wherein for example alkaline metal salt gasification at high temperature easily of some catalyst, and usually discharge gasification furnace with the gas that obtains after the coal gasification, cause the loss of catalyst.So hope from the gas that leaves coal gasifier, to reclaim these catalyst, and it utilized again.
Yet, from gas phase, reclaiming base metal catalysts and be not easy, the main method of the work (US3998607, US4057512, US4417972) of EXXON aspect catalyst recovery is to set up multistage washing retracting device.Its main technique flow process characteristics are to separate with grain slag through washing step by step base metal catalysts as much as possible is washed in the middle of the solution, and then obtain the solid of alkaline metal salt through methods such as dryings, are reused for the catalytic gasification process at last again.Its main weak point is that water consumption is big, energy consumption is higher relatively, technological process is more loaded down with trivial details, corresponding fixed investment is also higher.
Summary of the invention
For overcoming the above problems, in first aspect of the present invention, provide a kind of from method from recovery base metal catalysts the gas of coal gasifier, may further comprise the steps:
A. make this gas through being the filter of filter medium, at least a portion base metal catalysts is trapped on this porous coal tar with the porous coal tar;
The gas that b. will leave above-mentioned filter feeds in the aeration tower, and making the base metal catalysts of remainder be dissolved in the water becomes the aqueous solution of base metal catalysts.
In preferred embodiments, the present invention is further comprising the steps of after above-mentioned steps b:
C. the said aqueous solution from step b is carried out reverse-osmosis treated, to improve the concentration of base metal catalysts in this aqueous solution;
D. the aqueous solution from step c is carried out ion-exchange treatment, the anion so that the anion exchange in the base metal catalysts is become to want randomly carries out concentration to the alkali metal salt soln that obtains then.
Second aspect, the present invention also provides a kind of coal gasification method that reclaims and recycle base metal catalysts, may further comprise the steps:
I. in coal gasifier, under the effect of base metal catalysts, coal is gasified, wherein contained the gas of base metal catalysts with gasifying agent;
Ii. make above-mentioned gas through being the filter of filter medium with the porous coal tar, so that at least a portion base metal catalysts is trapped on this porous coal tar, and the porous coal tar that will be loaded with base metal catalysts turns back in the gasification furnace;
The gas that iii. will leave above-mentioned filter feeds in the aeration tower, and making the base metal catalysts of remainder be dissolved in the water becomes the aqueous solution of base metal catalysts;
Iv. the said aqueous solution is carried out reverse-osmosis treated, to improve the concentration of base metal catalysts in this aqueous solution;
V. the aqueous solution from step I v is carried out ion-exchange treatment, the anion so that the anion exchange in the base metal catalysts is become to want randomly carries out concentration to the alkali metal salt soln that obtains then;
Vi. the alkali metal salt soln after will concentrating with turn back in the coal gasifier after coal mixes.
The accompanying drawing summary
Fig. 1 is the sketch map of the reverse osmosis step in the method for the present invention.
Fig. 2 is the indicative flowchart of method of the present invention.
It should be noted that accompanying drawing only is exemplary, does not plan to limit by any way the present invention.
Detailed Description Of The Invention
The existing method of introducing first aspect of the present invention in detail.
In the step a of first aspect of the present invention, make gas from coal gasifier through being the filter of filter medium, so that at least a portion base metal catalysts is trapped on this porous coal tar with the porous coal tar.
Wherein the coal gasifier among the present invention can be the coal gasifier of any kind, and for example lurgi gasifier, U-gas stove, E-gas stove, fluidized-bed gasification furnace, three sections stoves etc. can be referring to related patent U.S. Patent No. about the detailed structure of these gasification furnaces.In coal gasifier, coal is gasified with the gasifying agent reaction under the effect of base metal catalysts and/or alkaline-earth metal catalyst, obtains comprising H
2O, CO, CH
4, H
2And CO
2In one or more gas because coal gasification reaction at high temperature carries out, employed base metal catalysts for example alkaline metal salt material tends to gasified, and along with gas leaves coal gasifier from the gas vent that is usually located at the gas burner top; And alkaline-earth metal catalyst mainly is present in unreacted completely in the coal ash owing to be difficult to gasification under the temperature in coal gasifier, and leaves coal gasifier from the ash discharging hole that is usually located at the coal gasifier bottom.In addition, leave in the gas of coal gasifier and also contain small coal ash particle (being called flying dust again).In leaving the gas of coal gasifier; Base metal catalysts is frozen into small solid particle owing to temperature decreases after leaving gasification furnace; These small solid particles are mixed in the gas; Exist with aerocolloidal form, the small solid particle of some of them also possibly be deposited on the flying dust.In some cases, in addition some base metal catalysts be present in the said gas with the steam form.
Employed base metal catalysts is meant alkali metal salt in the coal gasifier, for example alkali carbonate, alkali halide, alkali metal sulfates, alkali silicate or alkali metal aluminosilicate or any several kinds mixture in them.Therefore, among the present invention, can be above one or more alkali metal salts from the base metal catalysts in the gas of coal gasifier.Owing to contain plurality of inorganic salt class composition as impurity in the coal; Therefore; Even if under the situation of only using alkali carbonate to come as catalyst coal is gasified; Since alkali carbonate at high temperature with coal in those inorganic salts complicated reaction takes place, also can generate for example other alkali metal salts such as alkali halide, alkali metal sulfates, alkali silicate or alkali metal aluminosilicate.These salts are also gasification easily at high temperature.So among the present invention, in the gas from coal gasifier, said base metal catalysts still can be one or more the mixture in alkali carbonate, alkali halide, alkali metal sulfates, alkali silicate or the alkali metal aluminosilicate.
Porous coal tar among the present invention be meant a kind of after Overheating Treatment coal dust; It has the characteristic of porous; And for example prepare through following method: the coal that with granularity is 1-2mm is removing fugitive constituent 10-30min under the temperature below 800 ℃ under the inert atmosphere; Under the temperature between 700-900 ℃, carried out activation 0.5-1 hour then, refilter and remove the fine grained of granularity less than 1mm with steam and oxygen.The character of the porous coal tar that for example, uses in embodiments of the invention is following: specific area is greater than 100m
2/ g, porosity is greater than 10%, and Morse hardness is greater than 4, and the Ha Shi abrasion resistance index is greater than 75.When being loaded into such porous coal tar in the filter, it can play the effect of filter medium.When from the gas of coal gasifier when being the filter of filter medium with this porous coal tar; Below the generation active one or more and at least a portion base metal catalysts in the gas is trapped on this porous coal tar: 1. filtration: the solid particle in the gas; Comprise independent base metal catalysts particulate and be deposited on the base metal catalysts particulate on the flying dust, be trapped within on the porous coal tar through filtration; 2. cooling-adhewsive action: because of the porous coal tar makes gaseous bases metallic catalyst condensation and further solidify and then attached on this porous coal tar to the cooling of said gas.In embodiments of the invention, contained base metal catalysts gross weight is compared in the weight of the base metal catalysts that is trapped and the gas, usually＞50wt%, be preferably greater than 60wt%, more preferably greater than 70wt%.In a preferred embodiment of the invention, can this porous coal tar that is loaded with base metal catalysts be turned back in the said coal gasifier, to realize the recycle of base metal catalysts.The catalyst that the is not trapped catalyst of remainder (or be called) then along with gas leaves this filter, enters into the step b of first aspect of the present invention.
In the step b of first aspect of the present invention, the gas that leaves above-mentioned filter is fed in the aeration tower, making the base metal catalysts of remainder be dissolved in the water becomes the aqueous solution of base metal catalysts.This aeration tower and relevant gas washing technology are well known to those skilled in the art, for example gas are fed and carry out gas washing in the liquid, or gas is contacted with liquid countercurrent and carry out gas washing, and employed liquid is generally water.Because base metal catalysts is very easily water-soluble usually, so in gas washing technology, can make that the base metal catalysts that leaves remainder contained in the gas of above-mentioned filter is almost all soluble in water, obtains the aqueous solution of base metal catalysts.So far, will all reclaim from the base metal catalysts in the gas in the coal gasifier.Yet often concentration is very low for the aqueous solution of the base metal catalysts of this step b gained, can't directly turn back in the gasification furnace to recycle.Another can't directly use the reason of the aqueous solution of this base metal catalysts to be to contain in this aqueous solution various anion; The catalytic efficiency of considering the alkali metal salt that alkali metal cation and some anion constitute will be higher than other alkali metal salt; Old friends hope the alkali metal salt that is reclaimed is changed into these catalytic efficiency higher alkali metal salt as far as possible usually; For example it is found that; The catalytic efficiency of alkali carbonate will be higher than other alkali metal salt, and old friends hope the alkali metal salt of non-alkali carbonate is converted into alkali carbonate usually.Certainly, also can change into any anionic alkali metal salt of wanting that has by needs as the case may be.So in a preferred embodiment of the invention, also process following steps c and d concentrate and ion-exchange treatment the aqueous solution of this base metal catalysts, so that recycle the base metal catalysts that is recovered in the aqueous solution.
In the step c of first aspect of the present invention, the said aqueous solution from step b is carried out reverse-osmosis treated, to improve the concentration of base metal catalysts in this aqueous solution.Counter-infiltration is for process of osmosis, and its principle is referring to Fig. 1.In the process of osmosis of routine, with one can hold back solute for example the pellicle of salt weak solution or pure water and concentrated solution are separated, the water in the weak solution can spontaneously under the effect of osmotic pressure move to concentrated solution one side.If applied pressure is with then the water in the concentrated solution can be to the migration of weak solution one side greater than above-mentioned osmotic pressure poor (being called operating pressure difference) of applied pressure at the weak solution place at the concentrated solution place, this phenomenon is called counter-infiltration.The result of counter-infiltration is that concentrated solution is denseer, and weak solution is rarer, so counter-infiltration can be used for improving solution concentration.In embodiments of the invention, said counter-infiltration is carried out under following condition: the pore size of reverse osmosis membrane is the 8-10 dust, and operating pressure difference is 1-10MPa, and molecular weight cut off is less than 500.Through this reverse-osmosis treated, can make the concentration of base metal catalysts in the aqueous solution bring up to original 2-10 doubly, and the energy consumption of counter-infiltration be merely tradition evaporation concentrating method energy consumption 1/2～1/3.
In the steps d of first aspect of the present invention; The aqueous solution to from steps d carries out ion-exchange treatment; With the anion that the anion exchange in the base metal catalysts is wanted; For example be exchanged into carbanion, the solution of the salt that randomly alkali metal cation that obtains and this anion of wanting is constituted then carries out concentration.Wherein, said ion-exchange treatment is carried out in ion-exchanger, and the ion-exchange reagent of use is to contain the anionic aqueous solution that this is wanted, the for example aqueous solution of carbonated radical ion.The said method comprise any raising solute concentration that concentrates is such as but not limited to evaporating solvent etc.
Dense alkali metal catalyst solution through above step a-d processing back gained can be used for mixing with coal once more, gets in the gasification furnace then to recycle.
The existing method of introducing second aspect of the present invention with reference to Fig. 2 in detail.
In the step I of second aspect of the present invention, in coal gasifier, under the effect of base metal catalysts, coal is gasified with gasifying agent, wherein contained the gas of base metal catalysts.
Wherein the coal gasifier among the present invention can be the coal gasifier of any kind, and for example lurgi gasifier, U-gas stove, E-gas stove, fluidized-bed gasification furnace, three sections stoves etc. can be referring to related patent U.S. Patent No. about the detailed structure of these gasification furnaces.In coal gasifier, coal is gasified with the gasifying agent reaction under the effect of base metal catalysts and/or alkaline-earth metal catalyst, obtains comprising H
2O, CO, CH
4, H
2And CO
2In one or more gas; Because coal gasification reaction at high temperature carries out; Employed base metal catalysts for example alkaline metal salt material tends to gasified; The gas that is wherein contained base metal catalysts, this gas leaves coal gasifier from the gas vent that is usually located at the gas burner top; And alkaline-earth metal catalyst mainly is present in unreacted completely in the coal ash owing to be difficult to gasification under the temperature in coal gasifier, and leaves coal gasifier from the ash discharging hole that is usually located at the coal gasifier bottom.In addition, leave in the gas of coal gasifier and also contain small coal ash particle (being called flying dust again).In leaving the gas of coal gasifier; Base metal catalysts is frozen into small solid particle owing to temperature decreases after leaving gasification furnace; These small solid particles are mixed in the gas, exist with aerocolloidal form, and the small solid particle of some of them also is deposited on the flying dust.In some cases, in addition some base metal catalysts be present in the said gas with the steam form.
Employed base metal catalysts is meant alkali metal salt in the coal gasifier, for example alkali carbonate, alkali halide, alkali metal sulfates, alkali silicate or alkali metal aluminosilicate or any several kinds mixture in them.Therefore, among the present invention, can be above one or more alkali metal salts from the base metal catalysts in the gas of coal gasifier.Owing to contain plurality of inorganic salt class composition as impurity in the coal; Therefore; Even if under the situation of only using alkali carbonate to come as catalyst coal is gasified; Since alkali carbonate at high temperature with coal in those inorganic salts complicated reaction takes place, also can generate for example other alkali metal salts such as alkali halide, alkali metal sulfates, alkali silicate or alkali metal aluminosilicate.These salts are also gasification easily at high temperature.So among the present invention, in the gas from coal gasifier, said base metal catalysts still can be one or more the mixture in alkali carbonate, alkali halide, alkali metal sulfates, alkali silicate or the alkali metal aluminosilicate.
Employed gasifying agent includes but not limited to oxygen, air, oxygen-enriched air, steam among the present invention, or the like.
In the step I i of second aspect of the present invention; Make from the gas of step I through being the filter of filter medium with the porous coal tar; So that at least a portion base metal catalysts is trapped on this porous coal tar, and the porous coal tar that will be loaded with base metal catalysts turns back in the gasification furnace.The wherein character of porous coal tar and preparation method, and concrete filter method are identical with the step a of first aspect of the present invention.And returning the method for going in the gasification furnace, the porous coal tar that will be loaded with base metal catalysts can use any known way.For example in a kind of continuation mode, when filtering gas, the porous coal tar is progressively moved in filter, and the porous coal tar that constantly will be loaded with base metal catalysts shift out filter from coal gasifier with the porous coal tar, turn back in the coal gasifier then.Perhaps, in a kind of intermittent mode, clean out the coal tar that is loaded with base metal catalysts at regular intervals and they are turned back in the coal gasifier.
The step I ii of second aspect of the present invention is identical with the step b of first aspect present invention.
The step I v of second aspect of the present invention is identical with the step c of first aspect present invention.
The step v of second aspect of the present invention is identical with the steps d of first aspect present invention.
In the step vi of second aspect of the present invention, with the alkali metal salt soln after concentrating with turn back in the coal gasifier after coal mixes.This can use the hybrid technology of any routine to carry out.
Abovely specific embodiments of the present invention is described, but those skilled in the art obviously it will also be appreciated that other embodiment in claim scope of the present invention with reference to accompanying drawing.
Embodiment
In conjunction with flow process shown in Figure 2; Specify embodiment of the present invention through following examples; These embodiment are only from illustrational purpose and providing, for example, for narrate clear and complete for the purpose of; Mentioned a lot of concrete processing steps and equipment among the embodiment, these processing steps and equipment are not all to be that the method for embodiment of the present invention is necessary.Embodiment does not plan to limit by any way scope of the present invention yet, and true scope of the present invention is only confirmed by claim.
With potash is that catalyst gasifies to coal in the syllogic gasification furnace, will be that 500-700 ℃ gas sends into the porous coal tar from the temperature that contains the base metal catalysts colloidal solid of this syllogic gasification furnace is the filter of filter medium; Through after filtration, find that about 60% catalyst is held back by this porous coal tar, the porous coal tar that is loaded with catalyst progressively to be shifted out filter and turns back in the said gasification furnace, the time of staying of porous coal tar in filter is 30-120 minute; Said gas is gone into water scrubber through filter is laggard, and remaining base metal catalysts is all soluble in water; The aqueous solution (concentration 5-20%) that is dissolved with catalyst gets into the reverse osmosis separation device, through reverse-osmosis treated concentration is increased to 20-50%; Through ion-exchanger wherein each kind of sylvite changed into potash more than 95% again; Get in the said syllogic gasification furnace after the dense solution of potassium carbonate that generates mixes with raw coal by the catalyst proportion requirement and recycle.
Advantage of the present invention is following:
The combination that the present invention adopts the porous coal tar to filter, wash can be reclaimed the base metal catalysts in the coal gasifier exit gas in 100% ground.Use the porous coal tar to be filter medium; Can easily this porous coal tar of holding back some base metal catalysts directly be turned back to the utilization again that realizes base metal catalysts in the gasification furnace together; This is easy to realize on engineering, and has greatly alleviated follow-up washing and concentrated live load.And the base metal catalysts aqueous solution of washing back gained is again through the combination of counter-infiltration and ion-exchange; Can improve the concentration of the base metal catalysts aqueous solution and change it into the form (for example carbonate) of the alkali metal salt that is suitable as the coal gasification catalyst most, the said catalyst of recycle effectively.Wherein the use of reverse osmosis technology has greatly reduced the energy consumption of enrichment process.
Claims (10)
1. one kind from from the method that reclaims base metal catalysts the gas of coal gasifier, may further comprise the steps:
A. make this gas through being the filter of filter medium, at least a portion base metal catalysts is trapped on this porous coal tar with the porous coal tar;
The gas that b. will leave above-mentioned filter feeds in the aeration tower, and making the base metal catalysts of remainder be dissolved in the water becomes the aqueous solution of base metal catalysts.
2. the method for claim 1, further comprising the steps of:
C. the said aqueous solution from step b is carried out reverse-osmosis treated, to improve the concentration of base metal catalysts in this aqueous solution;
D. the aqueous solution from step c is carried out ion-exchange treatment, the anion so that the anion exchange in the base metal catalysts is become to want randomly carries out concentration to the alkali metal salt soln that obtains then.
3. coal gasification method that reclaims and recycle base metal catalysts may further comprise the steps:
I. in coal gasifier, under the effect of base metal catalysts, coal is gasified, wherein contained the gas of base metal catalysts with gasifying agent;
Ii. make above-mentioned gas through being the filter of filter medium with the porous coal tar, so that at least a portion base metal catalysts is trapped on this porous coal tar, and the porous coal tar that will be loaded with base metal catalysts turns back in the gasification furnace;
The gas that iii. will leave above-mentioned filter feeds in the aeration tower, and making the base metal catalysts of remainder be dissolved in the water becomes the aqueous solution of base metal catalysts;
Iv. the said aqueous solution is carried out reverse-osmosis treated, to improve the concentration of base metal catalysts in this aqueous solution;
V. the aqueous solution from step I v is carried out ion-exchange treatment, the anion so that the anion exchange in the base metal catalysts is become to want randomly carries out concentration to the alkali metal salt soln that obtains then;
Vi. the alkali metal salt soln after will concentrating with turn back in the coal gasifier after coal mixes.
4. claim 1 or 3 method, the specific area of wherein said porous coal tar is greater than 100m
2/ g, porosity is greater than 10%, and Morse hardness is greater than 4, and the Ha Shi abrasion resistance index is greater than 75.
5. claim 1 or 3 method, wherein said base metal catalysts is one or more in the following material: alkali carbonate, alkali metal chloride, alkali metal sulfates, alkali silicate or alkali metal aluminosilicate.
6. claim 1 or 3 method; Wherein said porous coal tar prepares through following method: the coal that with granularity is 1-2mm removes fugitive constituent 10-30min under the temperature below 800 ℃ under inert atmosphere; Under the temperature between 700-900 ℃, carried out activation 0.5-1 hour then, refilter and remove the fine grained of granularity less than 1mm with steam and oxygen.
7. the method for claim 3, the said porous coal tar that wherein in step I i, will be loaded with base metal catalysts with continuation mode turns back in the gasification furnace.
8. claim 1 or 3 method, wherein said base metal catalysts is present in the said gas that leaves coal gasifier with the form of particulate or steam.
9. claim 2 or 3 method, wherein said counter-infiltration is carried out under following condition: the pore size of reverse osmosis membrane is the 8-10 dust, and operating pressure difference is 1-10MPa, and molecular weight cut off is less than 500.
10. the method for claim 3, the wherein said anion of wanting is a carbanion.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106590747A (en) * | 2016-12-22 | 2017-04-26 | 中国科学院山西煤炭化学研究所 | Catalytic pyrolysis gasification method of urban garbage |
| 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 |
| 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 |
| CN107586562A (en) * | 2017-10-16 | 2018-01-16 | 新奥科技发展有限公司 | A kind of method that stove is returned in catalytic coal gasifaction synthesis gas circulation |
| CN110240912A (en) * | 2019-05-30 | 2019-09-17 | 太原理工大学 | A kind of method that alkalinity compound additive is used to improve gasification reactivity of coke |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106590747A (en) * | 2016-12-22 | 2017-04-26 | 中国科学院山西煤炭化学研究所 | Catalytic pyrolysis gasification method of urban garbage |
| 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 |
| 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 |
| CN107586562A (en) * | 2017-10-16 | 2018-01-16 | 新奥科技发展有限公司 | A kind of method that stove is returned in catalytic coal gasifaction synthesis gas circulation |
| CN110240912A (en) * | 2019-05-30 | 2019-09-17 | 太原理工大学 | A kind of method that alkalinity compound additive is used to improve gasification reactivity of coke |
| CN110240912B (en) * | 2019-05-30 | 2021-06-08 | 太原理工大学 | Method for improving gasification coke reactivity by using alkaline composite additive |
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|---|---|
| CN102476008B (en) | 2015-05-20 |
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