CN113332949A - Method for reducing composite molten salt in adsorbent by adjusting calcination temperature and atmosphere - Google Patents
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Abstract
The invention discloses a method for reducing composite molten salt in an adsorbent by adjusting calcination temperature and atmosphere, which comprises the step of adding quicklime and alkali metal salt in the absence of CO2Calcining in the gas environment, and then carrying out step cooling to obtain a calcium-based adsorbent; the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere effectively reduces the alkali metal-alkaline earth metal composite molten carbonate in the obtained calcium-based adsorbent, thereby greatly improving the CO content of the calcium-based adsorbent2Adsorption capacity; the method has the advantages of simple steps and easy operation.
Description
Technical Field
The invention belongs to the technical field of chemistry, and particularly relates to a method for reducing composite molten salt in an adsorbent by adjusting calcination temperature and atmosphere.
Background
The calcium circulation technology is a novel CO which is recommended and developed by the world in order to deal with global climate change2/SO2One of the trapping techniques. It has already received a great deal of scientific research investment in China, America, European Union, Australia, Canada, etc., and is widely concerned by mainstream scientific research institutions at home and abroad.
A commonly used method for preparing the calcium adsorbent in the existing calcium circulation technology is an impregnation method, and high-activity salt is generally impregnated on the surface of a calcium-based adsorbent, wherein the high-activity salt accounts for 0.1-2.0% of the mass of the adsorbent. Because alkali metal has better high-temperature activity, the alkali metal salt is generally used for impregnation, so that the ion diffusion capacity of the surface of the adsorbent is improved, and the CO of the adsorbent is enhanced2Trapping capacity.
Professor Anthony Canada suggested dipping limestone with trace amounts of NaCl or Na as early as 20032CO3CO after multiple cycles thereof2The adsorption capacity can be improved by about 40 percent and is increased from 0.10 (gCO)2/g adsorbent) to 0.14 (gCO)2Per gram of adsorbent). The southeast university and Shandong university also make more basic researches on the alkali metal salt impregnated modified calcium-based adsorbent, and respectively research KMnO4、KCl、K2CO3NaCl and Na2CO3Impregnating pure CaCO with various pure alkali metal salts3Experiments show that most of the alkali metal salts have obvious modification effect, and CO is recycled for many times2The adsorption capacity can be improved by about 100%. In addition, Mn (NO) has been studied3)2And the salt such as calcium lignosulfonate and the like is used for carrying out impregnation modification on the calcium-based adsorbent, so that a good improvement effect is also found. From the above studies, it was found that the CO content of the calcium-based adsorbent can be increased by impregnating the calcium-based adsorbent with an alkali metal salt2The capture capacity, the lifting amplitude is mostly between 40-100%.
Whether the lifting range is 40-100% or not is further obtained by using an immersion methodThe great improvement effect is a problem which is focused on. Through scientific experiments, the patent applicant proposes an improved dipping method in the early stage to enable calcium-based CO2The performance of the adsorbent is improved by 150-200%. The main difference between the improved method and the conventional method is that the limestone is added with a calcination-hydration process before being mixed and soaked with alkali metal salt, as shown in fig. 2:
from 2018 to the present time, the applicant is always searching for a root cause for improving the performance of the calcium-based adsorbent by an improved impregnation method, and further improving the calcium-based CO on the basis of seeking for 150-200% of improvement range2Method of adsorbent performance. Through a large number of experiments and analysis researches, the patent applicant finds that the mixture of alkali metal salt and calcium can generate alkali metal-alkaline earth metal composite molten carbonate K under certain conditions2Ca(CO3)2And Na2Ca(CO3)2The composite molten carbonate remains in the calcium-based adsorbent, occupies the surface space of the adsorbent, reduces the ion diffusion capacity of the surface of the adsorbent, and has obvious inhibiting effect on the performance of the adsorbent. Researches on the adsorbents prepared by a common impregnation method and an improved impregnation method show that the adsorbents obtained by the common impregnation method contain a large amount of composite molten carbonate, so that the modification effect is poor; even in the modified impregnation method, many of such complex molten carbonates exist, and thus there is still room for further improvement in the modified impregnation method.
Therefore, through detailed scientific research, the patent proposes a method for adjusting the preparation temperature and the atmosphere condition, and reducing the generation of alkali metal-alkaline earth metal composite molten carbonate, thereby greatly improving the CO content of the calcium-based adsorbent2Adsorption capacity.
Therefore, the technical personnel in the field are dedicated to develop a method for reducing the composite molten salt in the adsorbent, and aim to further develop the methodStep up the calcium-based CO2/SO2The adsorption performance of the adsorbent.
Disclosure of Invention
In view of the above problems, the present invention has been made to provide a method for reducing a composite molten salt in an adsorbent by adjusting a calcination temperature and an atmosphere, which overcomes or at least partially solves the above problems.
In order to achieve the above object, the present invention provides a method for reducing composite molten salt in an adsorbent by adjusting calcination temperature and atmosphere, comprising mixing quicklime and alkali metal salt in the absence of CO2Calcining in the gas environment, and then carrying out step cooling to obtain a calcium-based adsorbent;
further, the alkali metal salts include alkali metal sodium salts, alkali metal potassium salts;
further, the alkali metal sodium salt is NaCl, NaBr, Na2CO3、NaHCO3One or more of (a) and (b); the alkali metal potassium salt is KCl, KBr, KHCO3、K2CO3One or more of (a);
further, the temperature of the calcination is not less than 850 ℃;
further, the calcining time is 0.5-2 hours;
further, the step cooling comprises two stages of cooling, the first stage cooling being in the absence of CO2Cooling to 100-400 ℃ in a gas environment; the second stage of cooling is cooling to room temperature in air;
further, said CO-free2The gas environment of the gas source is one or more of a water vapor gas environment, a nitrogen gas environment, an argon gas environment and an oxygen gas environment;
further, the calcining temperature is 850-1000 ℃;
further, the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and the atmosphere comprises the following specific steps:
step 1, calcining limestone in air for 0.5-2 hours at the temperature of 700-1100 ℃ to obtain quicklime;
step 2, adding the quick lime obtained in the step 1 into an alkali metal salt solution, mixing and stirring to form paste, and airing and drying to obtain a salt-doped lime solid;
step 3, the salt-doped lime solid obtained in the step 2 is free of CO2Calcining for 0.5-2 hours at 850-1000 ℃ in the gas environment;
step 4, continuously maintaining the solid after calcination in the step 3 to be free of CO2The first stage of cooling is carried out in the gas environment, and the cooling temperature is 100-400 ℃;
step 5, placing the solid cooled in the step 4 in air to continue cooling in the second stage, and cooling to room temperature to obtain a calcium-based adsorbent;
further, in the step 2, the percentage content of the alkali metal salt solution is 1-3%;
further, in the step 2, the weight ratio of the quicklime to the alkali metal salt compound in the alkali metal salt solution is 100: 1-30: 1;
in the preferred embodiment of the invention, the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere is characterized in that the alkali metal salt is potassium carbonate;
in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and the atmosphere, in the step 1, the limestone calcination temperature is 700 ℃;
in another preferred embodiment of the present invention, in the method for reducing the composite molten salt in the sorbent by adjusting the calcination temperature and the atmosphere, in step 1, the limestone calcination temperature is 950 ℃;
in another preferred embodiment of the invention, in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and the atmosphere, in step 1, the limestone calcination temperature is 1100 ℃;
in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and the atmosphere, in the step 1, the limestone calcination time is 0.5 hour;
in another preferred embodiment of the present invention, in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere, in step 1, the limestone calcination time is 1 hour;
in another preferred embodiment of the present invention, in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere, in step 1, the limestone calcination time is 2 hours;
in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and the atmosphere, in the step 2, the percentage of the alkali metal salt solution is 1%;
in another preferred embodiment of the invention, in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere, in the step 2, the percentage content of the alkali metal salt solution is 2%;
in another preferred embodiment of the invention, in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere, in the step 2, the percentage content of the alkali metal salt solution is 3%;
in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and the atmosphere, in the step 2, the weight ratio of the quicklime to the alkali metal salt compound in the alkali metal salt solution is 100: 1;
in another preferred embodiment of the invention, in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere, in the step 2, the weight ratio of the quicklime to the alkali metal salt compound in the alkali metal salt solution is 50: 1;
in another preferred embodiment of the invention, in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere, in the step 2, the weight ratio of the quicklime to the alkali metal salt compound in the alkali metal salt solution is 30: 1;
in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and the atmosphere, in the step 3, the calcination temperature of the salt-doped lime solid is 850 ℃;
in another preferred embodiment of the present invention, in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere, in step 3, the calcination temperature of the salt-doped lime solid is 900 ℃;
in another preferred embodiment of the present invention, in the method for reducing composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere, in step 3, the calcination temperature of the salt-doped lime solid is 950 ℃;
in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and the atmosphere, in the step 3, the calcination time of the salt-doped lime solid is 0.5 hour;
in another preferred embodiment of the present invention, in the method for reducing composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere, in step 3, the calcination time of the salt-doped lime solid is 1 hour;
in another preferred embodiment of the present invention, in the method for reducing composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere, in step 3, the calcination time of the salt-doped lime solid is 2 hours;
in the preferred embodiment of the invention, the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere does not contain CO in steps 3 and 42The gas environment of (2) is a water vapor gas environment;
in another preferred embodiment of the present invention, in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and atmosphere, steps 3 and 4, the method does not contain CO2The gas environment of (a) is a nitrogen gas environment;
in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and the atmosphere, in the step 4, the cooling temperature of the first stage cooling is 100 ℃;
in another preferred embodiment of the invention, in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and the atmosphere, in the step 4, the cooling temperature of the first stage cooling is up to 300 ℃;
in another preferred embodiment of the invention, in the method for reducing the composite molten salt in the adsorbent by adjusting the calcination temperature and the atmosphere, in the step 4, the cooling temperature of the first stage cooling is 400 ℃;
in a preferred embodiment of the invention, the starting material of the alkali metal sodium salt or alkali metal potassium salt is one or more of a sea salt and a lake salt;
in a preferred embodiment of the present invention, the calcium-based adsorbent is further subjected to a grinding treatment, the calcium-based adsorbent is obtained by further grinding the solid cooled to room temperature in step 5, and the particle size of the ground calcium-based adsorbent is not more than 0.3 mm;
the invention also provides the calcium-based adsorbent prepared by any one of the methods, wherein the calcium-based adsorbent internally comprises a macroporous structure with the diameter of 100-200 nm;
one or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
the method for reducing the composite molten salt in the adsorbent adopts the CO-free method2The gas environment of the method calcines and cools the quicklime and the alkali metal salt, optimizes and adjusts the calcination temperature, effectively reduces the alkali metal-alkaline earth metal composite molten carbonate in the obtained calcium-based adsorbent, and greatly improves the CO of the calcium-based adsorbent2Adsorption capacity;
the method for reducing the composite molten salt in the adsorbent adopts a water vapor atmosphere or a nitrogen atmosphere and the like which does not contain CO2The high-temperature calcination is carried out in the gas environment to avoid CO in the calcination atmosphere2The existence of gas can effectively avoid alkali metal ions sublimed and then CO2Combining to produce a composite molten carbonate;
the method for reducing the composite molten salt in the adsorbent has the advantages of less complicated steps and easy operation.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are drawings in some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a schematic flow chart of the method of example 1 of the present invention;
FIG. 2 is a schematic diagram of the conventional impregnation method and the conventional modified impregnation method for preparing the adsorbent.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
The method for reducing the composite molten salt in the adsorbent according to the present application will be described in detail with reference to examples.
Example 1 preparation of calcium-based sorbent
Calcining limestone in air at 950 ℃ for 0.5 hour to obtain quicklime;
50 g of quicklime is put into 50 g (percentage content is 2%) of potassium chloride solution to be fully mixed and stirred to obtain a pasty mixture, and the pasty mixture is aired and dried to obtain salt-doped lime solid;
calcining the solid of the lime doped with the salt for 1 hour at 900 ℃ in a steam gas environment;
continuously carrying out first-stage cooling under the environment of vapor gas, wherein the cooling temperature is 400 ℃;
cooling in the air to room temperature in the second stage;
and finally, grinding the cooled solid into powder with the particle size not exceeding 0.3mm to obtain the calcium-based adsorbent product.
Example 2 preparation of calcium-based sorbent
Calcining limestone in air at 850 ℃ for 2 hours to obtain quick lime;
50 g of quicklime is put into 50 g (percentage content is 2%) of potassium carbonate solution to be fully mixed and stirred to obtain a pasty mixture, and the pasty mixture is aired and dried to obtain salt-doped lime solid;
calcining the solid of the lime doped with the salt for 2 hours at 850 ℃ in a nitrogen gas environment;
continuously carrying out first-stage cooling under the nitrogen gas environment, wherein the cooling temperature is 300 ℃;
cooling in the air to room temperature in the second stage;
and finally, grinding the cooled solid into powder with the particle size not exceeding 0.3mm to obtain the calcium-based adsorbent product.
Example 3 preparation of calcium-based sorbent
Calcining limestone in air at 950 ℃ for 1 hour to obtain quick lime;
50 g of quicklime is put into 100 g (the percentage content is 1%) of potassium chloride solution to be fully mixed and stirred to obtain a pasty mixture, and the pasty mixture is aired and dried to obtain a solid doped with salt lime;
calcining the solid of the lime doped with the salt for 0.5 hour at 950 ℃ in a nitrogen gas environment;
continuously carrying out first-stage cooling under the nitrogen gas environment, wherein the cooling temperature is 100 ℃;
cooling in the air to room temperature in the second stage;
and finally, grinding the cooled solid into powder with the particle size not exceeding 0.3mm to obtain the calcium-based adsorbent product.
Comparative examples 4,
Calcining limestone in air at 950 ℃ for 0.5 hour to obtain quicklime;
50 g of quicklime is put into 50 g (percentage content is 2%) of potassium chloride solution to be fully mixed and stirred to obtain a pasty mixture, and the pasty mixture is aired and dried to obtain salt-doped lime solid;
directly calcining the solid of the lime doped with the salt in the air at 900 ℃ for 1 hour;
cooling to room temperature;
and finally, grinding the cooled solid into powder with the particle size not exceeding 0.3mm to obtain the calcium-based adsorbent product.
Comparative examples 5,
Calcining limestone in air at 850 ℃ for 2 hours to obtain quick lime;
50 g of quicklime is put into 50 g (percentage content is 2%) of potassium carbonate solution to be fully mixed and stirred to obtain a pasty mixture, and the pasty mixture is aired and dried to obtain salt-doped lime solid;
directly calcining the solid of the lime doped with the salt in the air at 850 ℃ for 2 hours;
cooling to room temperature;
and finally, grinding the cooled solid into powder with the particle size not exceeding 0.3mm to obtain the calcium-based adsorbent product.
Comparative examples 6,
Calcining limestone in air at 950 ℃ for 1 hour to obtain quick lime;
50 g of quicklime is put into 100 g (the percentage content is 1%) of potassium chloride solution to be fully mixed and stirred to obtain a pasty mixture, and the pasty mixture is aired and dried to obtain a solid doped with salt lime;
directly calcining the solid of the lime doped with the salt in the air at 950 ℃ for 0.5 hour;
cooling to room temperature;
and finally, grinding the cooled solid into powder with the particle size not exceeding 0.3mm to obtain the calcium-based adsorbent product.
Test examples 7,
Calcium base obtained in examples 1 to 3 and comparative examples 4 to 6Respectively introducing CO-rich adsorbent products2For 15min, the calcium-based adsorbent can fully adsorb CO2Taking out the calcium-based adsorbent to detect the adsorption amount, detecting each sample for three times, and taking an average value; the results of the test data are shown in table 1:
TABLE 1 CO after multiple cycle stabilization2Adsorption amount (g-CO)2/g-adsorbent)
Example 1 | Example 2 | Example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
1 | 0.32 | 0.29 | 0.33 | 0.27 | 0.23 | 0.26 |
2 | 0.32 | 0.31 | 0.32 | 0.26 | 0.23 | 0.27 |
3 | 0.33 | 0.29 | 0.32 | 0.26 | 0.24 | 0.27 |
Mean value of | 0.32 | 0.29 | 0.32 | 0.26 | 0.23 | 0.27 |
As is clear from the data in Table 1, the CO content of the calcium-based adsorbents obtained in examples 1 to 3 of the present application was measured2The adsorption amount is 0.29 to 0.32 g-CO2A/g-adsorbent; CO of calcium-based adsorbents obtained in comparative examples 4 to 62The adsorption amount is 0.23 to 0.27g-CO2A/g-adsorbent;
shows that compared with the calcium-based adsorbents obtained in comparative examples 4 to 6, the calcium-based adsorbents obtained in examples 1 to 3 of the invention have CO2The adsorption capacity of the CO is obviously higher than that of the CO in the calcium-based adsorbents obtained in comparative examples 4-62The amount of adsorption; CO of calcium-based adsorbent obtained in examples 1 to 3 of the present invention2Compared with a comparative example, the adsorption performance is improved by 20 percent;
other technical schemes of the invention have similar beneficial effects as above.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A method for reducing composite molten salt in adsorbent by adjusting calcining temperature and atmosphere is characterized by comprising the steps of mixing quicklime and alkali metal salt in a CO-free state2Calcining in a gas environment, and then carrying out step cooling to obtain the calcium-based adsorbent.
2. The method of claim 1,
the step cooling comprises two stages of cooling, the first stage of cooling being in the absence of CO2Cooling to 100-400 ℃ in a gas environment; the second stage cooling is cooling to room temperature in air.
3. The method according to claim 1 or 2,
said CO-free2The gas environment of (2) is one or more of a water vapor gas environment, a nitrogen gas environment, an argon gas environment and an oxygen gas environment.
4. The method of claim 1,
the alkali metal salts comprise alkali metal sodium salts and alkali metal potassium salts;
the temperature of the calcination is not less than 850 ℃;
the calcining time is 0.5-2 hours.
5. The method of claim 4,
the alkali metal sodium salt is NaCl, NaBr, Na2CO3、NaHCO3One or more of (a) and (b); the alkali metal potassium salt is KCI, KBr, KHCO3、K2CO3One or more of (a);
the calcining temperature is 850-1000 ℃.
6. The method of claim 1,
the method comprises the following steps:
step 1, calcining limestone in air for 0.5-2 hours at the temperature of 700-1100 ℃ to obtain quicklime;
step 2, adding the quick lime obtained in the step 1 into an alkali metal salt solution, mixing and stirring to form paste, and airing and drying to obtain a salt-doped lime solid;
step 3, the salt-doped lime solid obtained in the step 2 is free of CO2Calcining for 0.5-2 hours at 850-1000 ℃ in the gas environment;
step 4, continuously maintaining the solid after calcination in the step 3 to be free of CO2The first stage of cooling is carried out in the gas environment, and the cooling temperature is 100-400 ℃;
and 5, placing the solid cooled in the step 4 in air to continue cooling in the second stage, and cooling to room temperature to obtain the calcium-based adsorbent.
7. The method of claim 6, wherein the step 2,
in the step 2, the percentage content of the alkali metal salt solution is 1-3%.
8. The method of claim 6, wherein the step 3,
in the step 2, the weight ratio of the quicklime to the alkali metal salt compound in the alkali metal salt solution is 100: 1-30: 1.
9. The method of claim 6,
and 5, grinding the obtained calcium-based adsorbent, wherein the particle size of the ground calcium-based adsorbent is not more than 0.3 mm.
10. The calcium-based adsorbent prepared by the method of any one of claims 1 to 9, wherein the calcium-based adsorbent comprises a macroporous structure with a diameter of 100-200 nm.
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