CN114835142B - Method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate - Google Patents
Method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate Download PDFInfo
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- CN114835142B CN114835142B CN202210532811.0A CN202210532811A CN114835142B CN 114835142 B CN114835142 B CN 114835142B CN 202210532811 A CN202210532811 A CN 202210532811A CN 114835142 B CN114835142 B CN 114835142B
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B32/50—Carbon dioxide
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Abstract
The present invention relates to a kind ofThe method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate includes such steps as removing particulates from industrial kiln tail gas, denitration and desulfurizing, pressurizing the treated tail gas to 0.1-0.7 MPa, dewatering, and using double-tower temp. -changing adsorption equipment to make NOx and SO 2 And (3) removing the purified tail gas, introducing the tail gas into a four-tower pressure swing adsorption device to separate carbon dioxide, and finally introducing the obtained carbon dioxide into a lithium hydroxide solution to prepare lithium carbonate. The invention removes trace sulfide and nitrogen oxide in the tail gas by using a temperature swing adsorption method, SO that SO in the tail gas 2 And total NOx concentration<The invention also adopts a pressure swing adsorption method to recycle carbon dioxide, the obtained carbon dioxide gas has high purity, high recovery rate and large treatment capacity, and the separated and refined high-purity carbon dioxide can be used as raw materials in carbonization process to produce battery-grade lithium carbonate, thereby realizing the recycling utilization of carbon dioxide in industrial kiln tail gas.
Description
Technical Field
The invention relates to a method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate, belonging to the technical field of environmental engineering.
Background
Over 10 years ago, world CO 2 The discharge amount rises year by year, resulting in CO in the air 2 The concentration is too high and the greenhouse effect is more obvious, thus forming a serious threat to the survival safety of human beings and the sustainable development of social economy; worldwide, 60 million tons of CO must be reduced each year 2 The emission can effectively prevent global climate change and how to control CO 2 The emissions of (2) have become a serious problem worldwide.
Most of industrial kiln (combustion) fuels are natural gas, and natural gas kiln flue gas CO 2 Low concentration (5-15%), low partial pressure (0.10-1 bar), complex composition and CO 2 The trapping and recovery efficiency is relatively low. At the same time, CO 2 A great deal of compression energy is required before transportation and storage, the energy consumption and the cost of carbon capture are high, and meanwhile, the CO 2 Is an important regeneration resource of kiln tail gas, and develops industrial kiln flue gas CO 2 Recovery and utilization pair reduction of CO 2 The emission is of great significance.
In the prior art, CO 2 The recovery and separation technology mainly comprises an absorption method, a low-temperature condensation method, a membrane separation method and an adsorption method. The cryocondensation method is only applicable to CO 2 The working condition of the concentration higher than 60 percent is that the method needs more equipment, has large investment, high energy consumption and poor separation effect, and is generally only suitable for the exploitation sites of oil fields; the membrane separation method has the advantages of simple process, convenient operation and low energy consumption, and has the defects of frequently needing pretreatment, dehydration and filtration, and being difficult to obtain high-purity CO 2 The method comprises the steps of carrying out a first treatment on the surface of the CO at present 2 The recovery and the trapping are mostly carried out by adopting a chemical absorption method, and the method can be used for CO in gas 2 Low content, CO after concentration 2 The concentration can reach 99.99%, but the process has the advantages of high investment cost, high chemical absorbent loss, serious equipment corrosion, high energy consumption and high separation and recovery cost.
Separation and purification of CO by adsorption method 2 The method has the advantages of low energy consumption, long service period of the adsorbent, simple process flow, high automation degree, good environmental benefit, no pollution and the like, and the key of the adsorption method is that the performance of the adsorbent, but the carbon dioxide concentration of kiln tail gas is low, and the performance of the adsorbent is easy to be subjected to nitrogenThe influence of oxide, sulfide, moisture and the like ensures that the adsorption capacity of the adsorbent is low, the recycling treatment cost is high, and the selectivity of the adsorbent used in the prior industry to carbon dioxide is low. Recently, CO separation by purification of tail gas of industrial furnace is reported 2 The adsorbents of (a) are zeolite material-13X molecular sieve and carbon-based material-activated carbon, and other materials do not enter the adsorbent productization stage yet. The 13X molecular sieve has extremely strong hydrophilicity, and the smoke contains water, sulfide, nitride and other components on the surface of the smoke and CO 2 Has strong competitive adsorption and seriously affects the separation and purification of CO 2 The method comprises the steps of carrying out a first treatment on the surface of the Activated carbon has low sensitivity to moisture but at low pressure, activated carbon is resistant to CO 2 The adsorption capacity is lower than zeolite. On the other hand, in the prior art, the PSA is used for purifying, separating and recovering CO 2 The research of the method is limited to simulating smoke, the components are less, and the components of the tail gas of the actual industrial kiln are complex, and the impurities are more, so that CO in the tail gas of the industrial kiln 2 The recycling method has more challenges, and needs to be researched and improved on the basis of the prior art.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate.
In order to achieve the above object, the present invention provides the following technical solutions:
a method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate, comprising the following steps:
(1) Pretreatment:
removing particles from industrial kiln tail gas through a cyclone dust collector, and then performing denitration treatment and desulfurization treatment to obtain pretreated tail gas;
(2) Adsorption purification of trace sulfide and nitrogen oxide:
pressurizing the tail gas pretreated in the step (1) to 0.1-0.7 MPa by a compressor, then entering a water-gas separation tank for dehydration, and then adopting a double-tower temperature swing adsorption device for carrying out NOx and SO 2 Removing the waste gas to obtain purified tail gas;
the double-tower temperature swing adsorption device comprises two adsorption towers, wherein the two adsorption towers contain adsorbents;
(3) Separating and refining carbon dioxide:
introducing the purified tail gas into a four-tower pressure swing adsorption device for separating carbon dioxide, wherein the four-tower pressure swing adsorption device comprises 4 pressure swing adsorption towers which are sequentially connected, and the 4 pressure swing adsorption towers are filled with adsorbents for absorbing CO in the flue gas purification tail gas 2 The other components which are not easy to be adsorbed are directly emptied from the top of the tower; finally, desorbing the adsorbents in the four pressure swing adsorption towers to obtain carbon dioxide gas;
(4) Preparation of lithium carbonate:
and (3) introducing the carbon dioxide gas obtained in the step (3) into the lithium hydroxide solution, stirring and mixing uniformly, stopping introducing the carbon dioxide gas when a large amount of solids appear in the solution, heating to 90-110 ℃, preserving heat for 10-60 minutes, centrifuging while the solution is hot, obtaining a lithium carbonate crude product, and purifying to obtain the battery-grade lithium carbonate.
In the step (1), the denitration treatment adopts a high-temperature SCR process, and is performed in an SCR denitration catalytic reactor, ammonia water is used as a reducing agent, and V 2 O 5 -WO 3 -MoO 3 /TiO 2 The reaction temperature is 300-400 ℃ for the denitration catalyst.
In the step (2), the adsorbent is one or the combination of more than two of active carbon, modified silica gel, modified fly ash, active zeolite or mordenite with iodine value more than 1000.
In the step (2), after the two adsorption towers of the double-tower temperature swing adsorption device are saturated, the temperature is raised to 80-150 ℃, hot nitrogen is adopted for blowing and regenerating for 1-20min, the adsorbent can be recycled, and the blowing tail gas enters the step (1) for denitration treatment and desulfurization treatment.
Further, in the step (3), the adsorbent is any one or the combination of more than two of nitrogen doped activated carbon, carbon fiber, carbon nanotube, graphene, high hydrophobic 13X, high silicon ZSM-5, all-silicon ZSM molecular sieve or mesoporous silica in any proportion.
Further, in the step (4), the concentration of the lithium hydroxide solution is 50-90g/L.
Further, in the step (4), the purification method is as follows: adding water into the lithium carbonate crude product, controlling the solid-liquid ratio to be 1:1-1:5, stirring and heating to 90-95 ℃, centrifugally separating while the solution is hot, repeating for 1-3 times, and then drying in vacuum.
The invention has the beneficial effects that:
the invention provides a method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate, which can recover carbon dioxide in the industrial kiln tail gas to the maximum extent and has no three wastes, and the invention removes trace sulfide and nitrogen oxides in the industrial kiln tail gas by using a temperature swing adsorption method, and purifies SO in the tail gas after treatment 2 And total NOx concentration<1ppm; the invention adopts the pressure swing adsorption method to recycle the carbon dioxide, and the purity of the obtained carbon dioxide gas is high (the volume concentration of the carbon dioxide)>99%) and high recovery rate and treatment capacity; the separated and refined high-purity carbon dioxide is used as a raw material in the carbonization process to produce battery-grade lithium carbonate, so that the recycling of carbon dioxide in the tail gas of an industrial kiln is realized, and the method has important significance in reducing carbon emission and carbon neutralization.
Description of the drawings:
FIG. 1 is a process flow diagram of the method of example 1 for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate;
FIG. 2 is a flow chart of the process of the adsorption purification of trace sulfide and nitrogen oxides and the separation and purification of carbon dioxide in example 1;
wherein, 1-compressor; 2-a water-gas separation tank; 3-a double-tower temperature swing adsorption device; 4-four tower pressure swing adsorption device.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which are derived by a person skilled in the art based on the embodiments of the invention, fall within the scope of protection of the invention.
Example 1
In the embodiment, the kiln tail gas adopted is natural gas oxygen-enriched combustion kiln tail gas, and the water vapor content is 4.70-6.78% by volume and O is analyzed 2 The concentration is 13.90-15.10 v%, CO 2 The concentration is 2.51-4.39 v%, the concentration of NOx is 0.037-0.060 v% (500-800 ppm), SO 2 The concentration is 0.014v% (-400 ppm), the concentration of CO is 0.02-0.6 v%, H 2 The concentration is 0.01 to 0.06 percent, and the balance is N 2 . The method for recycling carbon dioxide in the tail gas of the industrial kiln is characterized in that the recycled carbon dioxide gas is used for preparing high-purity battery-grade lithium carbonate by an ore lithium extraction enterprise, and comprises the following steps:
as shown in fig. 1-2, a method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate comprises the following steps:
(1) Pretreatment:
removing particles from industrial kiln tail gas through a cyclone dust collector, and then adopting a denitration and desulfurization system to perform denitration treatment and desulfurization treatment to obtain pretreated tail gas;
the denitration and desulfurization system comprises an SCR denitration catalytic reactor, a waste heat boiler and a spray absorption tower which are sequentially connected, wherein the denitration treatment adopts a high-temperature SCR process, and is performed in the SCR denitration catalytic reactor, ammonia water is used as a reducing agent, and V 2 O 5 -WO 3 -MoO 3 /TiO 2 In order to obtain the denitration catalyst, the reaction temperature is 300-400 ℃, nitrogen oxides NOx in the tail gas reacts with ammonia water to produce nitrogen and water, the concentration of the nitrogen oxides in the tail gas is controlled to be 1-10ppm, the nitrogen oxides enter a waste heat boiler to exchange heat and cool down, the temperature is reduced to be lower than 300 ℃, the nitrogen oxides enter a spray absorption tower to carry out desulfurization treatment, alkaline limestone slurry droplets sprayed from top to bottom in the spray absorption tower are in countercurrent contact with the alkaline limestone slurry droplets, and acid oxides SO in the tail gas are obtained 2 The tail gas is fully purified because other pollutants and the like are absorbed; absorption of SO 2 The slurry after the reaction is reacted to generate CaSO 3 Formation of CaSO by forced in situ oxidation and crystallization 4 ·2H 2 O。
The pretreated tail gas was subjected to component analysis, and the results are shown in table 1:
TABLE 1
It can be seen that the NOx in the tail gas is 1-10mg/m after the denitration treatment and the desulfurization treatment 3 ，SO 2 <50mg/m 3 The gauge pressure is only 0.02-0.1KPa.
(2) Adsorption purification of trace sulfide and nitrogen oxide:
pressurizing the tail gas pretreated in the step (1) to 0.7MPa by a compressor, then, dehydrating the tail gas in a water-gas separation tank, and controlling the mass concentration of water in the tail gas<50mg/m 3 And the dehydrated tail gas enters a double-tower temperature swing adsorption device. The double-tower temperature swing adsorption device comprises an adsorption tower A and an adsorption tower B which are connected, wherein the adsorption tower A and the adsorption tower B both contain adsorbents (iodine value is>1400mg/g of organic amine impregnated activated carbon, supplied by national pharmaceutical group chemical reagent Co., ltd.) and both ends were packed with quartz sand. The dehydrated tail gas enters an adsorption tower A from the upper end at room temperature to carry out trace NOx and SO 2 Removing the tail gas from the lower end of the adsorption tower A to obtain purified tail gas which is used as the subsequent CO 2 Separating and refining raw materials; heating the adsorption tower A to 150 ℃ after the adsorption tower A is saturated, switching the tail gas to the adsorption tower B for adsorption, adopting hot nitrogen at 150 ℃ and normal pressure to purge and regenerate for 5min, and directly introducing the purged tail gas into the denitration and desulfurization system in the step (1); the adsorption tower A is cooled to room temperature after being completely regenerated and then enters the next circulation for adsorption; and (3) heating the adsorption tower B and blowing nitrogen when the adsorption tower A adsorbs, wherein the adsorption and regeneration processes of the two towers are alternately performed.
(3) Separating and refining carbon dioxide:
introducing the purified tail gas into a four-tower pressure swing adsorption device for separating carbon dioxide, wherein the four-tower pressure swing adsorption device comprises 4 pressure swing adsorption towers C, D, E, F which are sequentially connected, and the 4 pressure swing adsorption towers are filled with adsorbent 13X molecular sieves (synthesized by adopting the method of the embodiment 1 in CN 200910183869.3) for absorbing and purifying CO in the tail gas 2 Inert alumina is filled at two ends of the absorber for encapsulation; adsorption cleanerAfter the converted tail gas enters a C-F four-tower pressure swing adsorption device, the C-F four-tower adsorption process comprises the following steps: one column is in the adsorption stage and the other three are in the depressurization, purge and pressurization stages, respectively. Taking a C tower as an example, the tail gas (1) enters the C tower to be adsorbed to obtain high-purity CO 2 (volume concentration)>99.9 percent) and directly discharging the purified tail gas; (2) pressure drop: putting the C tower into the D tower in the forward direction; (3) the gas in the forward pressure-releasing-C tower is forward released to the E tower; (4) reversely releasing pressure: reducing the gas to a minimum pressure (normal pressure) to desorb the adsorbed species and to discharge a portion; (5) flushing: the tower C is reversely flushed by pure gas discharged from the tower F in the forward direction so as to achieve the final regeneration; (6) homogenizing pressure rise: pressurizing the C column (7) by using the equalizing gas of the D column: column C was charged with column E (in adsorption) product gas to the desired adsorption pressure.
CO in tail gas 2 After the absorption is finished, desorbing the adsorbents in the four pressure swing adsorption towers to obtain carbon dioxide gas;
(4) Preparation of lithium carbonate:
dissolving 600kg of battery grade lithium hydroxide monohydrate in distilled water to prepare a lithium hydroxide solution with the concentration of 80g/L, placing the lithium hydroxide solution in a reaction kettle, stirring for 100min, and filtering out insoluble impurities through filter pressing to obtain a lithium hydroxide filtrate; introducing carbon dioxide gas obtained in the step (3) into the lithium hydroxide filtrate, preferably CO 2 The flow rate is 3L/s, the stirring speed is 70 rpm, and when a large amount of solids in the solution appear, CO is stopped 2 Heating to 100 ℃, preserving heat for 30 minutes, and then centrifugally separating to obtain a lithium carbonate crude product; adding water into the lithium carbonate crude product according to the solid-to-liquid ratio of 1:3, stirring and heating to 95 ℃, centrifuging while the mixture is hot to obtain a lithium carbonate wet product, repeating the above conditions for 1 time, and placing the lithium carbonate wet product into a vacuum box and drying to obtain the lithium carbonate. The purity of lithium carbonate was 99.99% as measured by the method in YS/T546-2021, high purity lithium carbonate.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate, comprising the steps of:
(1) Pretreatment:
removing particles from industrial kiln tail gas through a cyclone dust collector, and then performing denitration treatment and desulfurization treatment to obtain pretreated tail gas;
(2) Adsorption purification of trace sulfide and nitrogen oxide:
pressurizing the tail gas pretreated in the step (1) to 0.1-0.7 MPa by a compressor, then, entering a water-gas separation tank for dehydration, and then, adopting a double-tower temperature swing adsorption device for NOxAnd SO 2 Removing the waste gas to obtain purified tail gas;
the double-tower temperature swing adsorption device comprises two adsorption towers, wherein the two adsorption towers contain adsorbents;
(3) Separating and refining carbon dioxide:
introducing the purified tail gas into a four-tower pressure swing adsorption device for separating carbon dioxide, wherein the four-tower pressure swing adsorption device comprises 4 pressure swing adsorption towers which are sequentially connected, and the 4 pressure swing adsorption towers are filled with adsorbents for absorbing CO in the flue gas purification tail gas 2 The other components which are not easy to be adsorbed are directly emptied from the top of the tower; finally, desorbing the adsorbents in the four pressure swing adsorption towers to obtain carbon dioxide gas;
(4) Preparation of lithium carbonate:
introducing the carbon dioxide gas obtained in the step (3) into the lithium hydroxide solution, stirring and mixing uniformly, stopping introducing the carbon dioxide gas when a large amount of solids appear in the solution, heating to 90-110 ℃, preserving heat for 10-60 minutes, centrifuging while the solution is hot to obtain a lithium carbonate crude product, and purifying to obtain lithium carbonate;
in the step (2), the adsorbent is one or the combination of more than two of active carbon, modified silica gel, modified fly ash, active zeolite or mordenite with iodine value more than 1000 in any proportion;
in the step (3), the adsorbent is any one or the combination of more than two of nitrogen doped active carbon, carbon fiber, carbon nano tube, graphene, 13X molecular sieve, high-silicon ZSM-5, all-silicon ZSM molecular sieve or mesoporous silica in any proportion.
2. The method for recovering carbon dioxide and producing lithium carbonate from industrial kiln tail gas as claimed in claim 1, wherein in the step (1), the denitration treatment adopts a high-temperature SCR process, and is carried out in an SCR denitration catalytic reactor, and ammonia water is used as a reducing agent, V 2 O 5 -WO 3 - MoO 3 /TiO 2 The reaction temperature is 300-400 ℃ for the denitration catalyst.
3. The method for recovering carbon dioxide and producing lithium carbonate from industrial kiln tail gas according to claim 1, wherein in the step (2), after the two adsorption towers of the double-tower temperature swing adsorption device are saturated, the temperature is raised to 80-150 ℃, the two adsorption towers are regenerated for 1-20min by adopting hot nitrogen sweeping, the adsorbent is used after being recycled, and the sweeping tail gas enters the step (1) for denitration treatment and desulfurization treatment.
4. The method for recovering carbon dioxide and producing lithium carbonate from an off-gas of an industrial kiln according to claim 1, wherein in the step (4), the concentration of the lithium hydroxide solution is 50 to 90g/L.
5. The method for recovering carbon dioxide from industrial kiln tail gas and producing lithium carbonate according to any one of claims 1 to 4, wherein in step (4), the purification method is as follows: adding water into the lithium carbonate crude product, controlling the solid-liquid ratio to be 1:1-1:5, stirring and heating to 90-95 ℃, centrifugally separating while the solution is hot, repeating for 1-3 times, and then drying in vacuum.
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