CN115466407A - Method for extracting humic acid from lignite - Google Patents
Method for extracting humic acid from lignite Download PDFInfo
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Abstract
The invention belongs to the technical field of humic acid extraction. The invention provides a method for extracting humic acid from lignite, which comprises the following steps: ultrasonically mixing lignite and an ethanol solution to obtain a product I; reacting the product I with an activating agent to obtain a product II; centrifuging the product II to obtain a solid-phase precipitate and a liquid phase; and (3) forming a mixed solution by the cleaning solution of the solid-phase precipitate and the liquid phase, and adjusting the pH value of the mixed solution by using mixed acid to obtain humic acid. The ultrasonic mixing of the invention can not only improve the extraction rate of humic acid, but also reduce the usage amount of the subsequent activating agent, and the hydrogen peroxide generated by the distilled water in the ethanol solution during the ultrasonic mixing can be used as an oxidizing agent to increase the content of acid-based functional groups in the lignite; the heavy metal content in the humic acid can be reduced through the hydrothermal treatment; the method for extracting humic acid from lignite by ultrasonic-hydrothermal combined extraction is simple, short in production period, high in humic acid extraction rate and suitable for large-scale application.
Description
Technical Field
The invention relates to the technical field of humic acid extraction, in particular to a method for extracting humic acid from lignite.
Background
China has abundant coal resources, the reserve of lignite accounts for more than 55% of the total reserve of coal, but low-rank coal has high water content, low heat value, high ash content, poor stability and easy spontaneous combustion, so the low-rank coal is not fully utilized all the time. How to realize clean, efficient and high-added-value utilization of low-rank coal has great significance on coal consumption reformation.
The content of humic acid in the low-rank coal is 10-80%, and the humic acid extracted from the low-rank coal has high biochemical activity and belongs to a high value-added product. Humic acid is a high molecular weight biopolymer, largely present in lignite, weathered coal and peat in the form of free acid and metal salts, and is a complex organic matter formed by the decomposition and conversion of plant debris by microorganisms and by the action of a series of activities of the earth's crust. The humic acid compound contains a plurality of functional groups such as phenolic hydroxyl, carboxyl, alcoholic hydroxyl, hydroxyquinone, enol group, sulfo group, amino group, quinonyl and semi-quinonyl and the like, and is formed by randomly connecting one or more condensed ring aromatic nuclei through bridge bonds.
The wide application of humic acid promotes the continuous development of humic acid extraction technology, and novel extraction technology is continuously developed. The method for extracting humic acid mainly comprises an alkali dissolution and acid precipitation method, an acid extraction agent method and a microorganism dissolution method. Different extraction methods have different effects on humic acid. The alkaline solution acidification method is to remove insoluble humic acid particles from the product of the alkaline extraction process, then precipitate soluble humate in the acidic extraction process, and then purify the deposit to obtain humic acid, wherein the soluble compound in the acidic solution is fulvic acid; the acid extractant method is a method for obtaining humate by soaking and filtering with a hydrochloric acid solution, washing with distilled water to be neutral or nearly neutral, extracting with an alkali extract, and then heating and carrying out reduced pressure suction filtration on the alkali extract, and although the method can shorten the filtering time and improve the separation efficiency, a large amount of fulvic acid is lost in the acid washing process; the microbial dissolution method is used for producing humic acid through the degradation of microorganisms, the reaction process is mild, but the method has the defects of long production period and low yield. For the above reasons, there is a need for further improvement of the extraction method of humic acid.
The hydrothermal reinforced extraction of humic acid is based on the theory that subcritical water can dissolve organic matters, and in a special closed container, water is used as a reaction medium, and the reaction container is heated to create a high-temperature and high-pressure reaction environment, so that generally insoluble or insoluble substances are dissolved. Subcritical water refers to water which is still kept in a liquid state under a certain pressure and has a water temperature between a boiling point (100 ℃) and a critical point (374 ℃), and has the following characteristics: the dielectric constant is reduced, and the characteristics similar to those of an organic solvent are shown; enhancement of self-ionization, H + And OH - The concentration is increased, so that subcritical water has an acid-base catalysis function; the viscosity and the surface tension are reduced, and the contact of reactants and the hydrolysis of organic macromolecules are facilitated, so that the mass transfer resistance is reduced, and the reaction rate is improved. The application of ultrasonic waves in chemical engineering can be divided into two categories: firstly, the product quality (small and regular particle size distribution) is improved by an ultrasonic method; secondly, the ultrasonic energy is utilized to enhance the unit operation rate (such as solid and liquid extraction). The cavitation of the ultrasonic wave accelerates the effective components in the object to be tested to enter the solvent, and further increases the extraction rate of the effective components.
Therefore, the method for extracting the humic acid from the lignite by ultrasonic-hydrothermal combination is provided, the yield of the humic acid is further improved, and the method has a good application prospect.
Disclosure of Invention
The invention aims to provide a method for extracting humic acid from lignite aiming at overcoming the defects of the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for extracting humic acid from lignite, which comprises the following steps:
1) Carrying out ultrasonic mixing on lignite and an ethanol solution to obtain a product I;
2) Reacting the product I with an activating agent to obtain a product II;
3) Centrifuging the product II to obtain a solid-phase precipitate and a liquid phase; and (4) forming a mixed solution by the cleaning solution of the solid-phase precipitate and the liquid phase, and adjusting the pH value of the mixed solution by using mixed acid to obtain humic acid.
Preferably, the particle size of the lignite obtained in the step 1) is 60-80 meshes; the mass concentration of the ethanol solution is 25-40%.
Preferably, the mass volume ratio of the lignite and the ethanol solution in the step 1) is 0.5-3 g:10 to 60mL.
Preferably, the power of the ultrasonic mixing in the step 1) is 180-240W, and the time of the ultrasonic mixing is 50-70 min.
Preferably, the activating agent in step 2) is potassium hydroxide, calcium hydroxide or sodium hydroxide; the mass ratio of the activating agent to the lignite obtained in the step 1) is 0.5-4.5: 1 to 3.
Preferably, the reaction temperature of the step 2) is 150-190 ℃, and the reaction time is 4-7 h.
Preferably, the cleaning solution for the solid-phase precipitate in the step 3) is a cleaning solution obtained by washing the solid-phase precipitate with water to neutrality.
Preferably, the mixed acid of step 3) comprises nitric acid and phosphoric acid; the volume ratio of the nitric acid to the phosphoric acid is 1-2: 2 to 6; the concentration of the nitric acid is 4-6 mol/L, and the concentration of the phosphoric acid is 8-12 mol/L.
Preferably, the pH of the mixed solution in step 3) is adjusted to 1 to 1.5.
The beneficial effects of the invention include the following:
1) The ultrasonic mixing of the invention can not only destroy the physical structure of the lignite, increase the contact area of the lignite and the ethanol solution, improve the extraction rate of humic acid, but also reduce the use amount of the subsequent activating agent, and the hydrogen peroxide generated by the distilled water in the ethanol solution during the ultrasonic mixing can be used as an oxidizing agent to increase the content of acid-based functional groups in the lignite.
2) According to the invention, the ethanol solution is used as the extracting solution of the lignite, so that the dispersibility and the solubility of the lignite can be improved, and the yield of humic acid is further improved.
3) The hydrothermal treatment of the invention can remove a large amount of oxygen-containing functional groups in the lignite, thereby reducing the complexation of the oxygen-containing functional groups with heavy metals and reducing the content of the heavy metals in humic acid.
4) The method has the advantages of simple process, short production period and high extraction rate of humic acid, and is suitable for large-scale application.
Drawings
Fig. 1 is an SEM image of lignite and humic acid of example 1; wherein, a is an SEM picture of lignite, and b is an SEM picture of humic acid of example 1;
fig. 2 is an XRD pattern of lignite and humic acid of example 1;
FIG. 3 is a FT-IR chart of humic acid of example 1.
Detailed Description
The invention provides a method for extracting humic acid from lignite, which comprises the following steps:
1) Ultrasonically mixing lignite and an ethanol solution to obtain a product I;
2) Reacting the product I with an activating agent to obtain a product II;
3) Centrifuging the product II to obtain a solid-phase precipitate and a liquid phase; and (3) forming a mixed solution by the cleaning solution of the solid-phase precipitate and the liquid phase, and adjusting the pH value of the mixed solution by using mixed acid to obtain humic acid.
In the invention, the particle size of the lignite obtained in the step 1) is 60-80 meshes, preferably 65-75 meshes, more preferably 68-72 meshes, and more preferably 70 meshes; the mass concentration of the ethanol solution is 25 to 40%, preferably 30 to 40%, more preferably 35 to 40%, and still more preferably 35%.
In the invention, the mass volume ratio of the lignite in the step 1) to the ethanol solution is 0.5-3 g:10 to 60mL, preferably 1 to 2.5g:15 to 55mL, more preferably 1.5 to 2g:25 to 45mL, more preferably 1.5g:30mL.
In the present invention, the lignite is preferably dried lignite.
In the invention, the power of the ultrasonic mixing in the step 1) is 180-240W, preferably 190-230W, more preferably 200-220W, and more preferably 210W; the ultrasonic mixing time is 50 to 70min, preferably 55 to 65min, more preferably 58 to 62min, and still more preferably 60min.
In the invention, the activating agent in the step 2) is potassium hydroxide, calcium hydroxide or sodium hydroxide; the mass ratio of the activating agent to the lignite obtained in the step 1) is 0.5-4.5: 1 to 3, preferably 1 to 4:1.5 to 2.5, more preferably 2 to 3:1.8 to 2.2, more preferably 2.5:2.
in the invention, the activating agent is added in the step 2) and stirred for 5-8 min before the reaction, preferably 5.5-7.5 min, more preferably 6-7 min, and more preferably 6.5min.
In the invention, the reaction temperature in the step 2) is 150-190 ℃, preferably 160-180 ℃, more preferably 165-175 ℃, and more preferably 170 ℃; the reaction time is 4 to 7 hours, preferably 4.5 to 6.5 hours, more preferably 5 to 6 hours, and still more preferably 5.5 hours.
In the present invention, the product II is cooled to room temperature and then centrifuged.
In the invention, the cleaning solution of the solid-phase precipitate in the step 3) is obtained by washing the solid-phase precipitate with water to neutrality.
In the invention, the mixed solution formed by the cleaning solution of the solid-phase precipitate in the step 3) and the liquid phase is a precursor solution of humic acid.
In the invention, the mixed acid in the step 3) comprises nitric acid and phosphoric acid; the volume ratio of the nitric acid to the phosphoric acid is 1-2: 2 to 6, preferably 1.2 to 1.8:2.5 to 5.5, more preferably 1.4 to 1.6:3 to 5, more preferably 1.5:4; the concentration of the nitric acid is 4 to 6mol/L, preferably 4.5 to 5.5mol/L, and more preferably 5mol/L; the concentration of phosphoric acid is 8 to 12mol/L, preferably 9 to 11mol/L, more preferably 9.5 to 10.5mol/L, and still more preferably 10mol/L.
In the present invention, the pH of the mixed solution in step 3) is adjusted to 1 to 1.5, preferably 1.2 to 1.5, more preferably 1.4 to 1.5, and still more preferably 1.5.
In the invention, after the mixed acid in the step 3) is used for adjusting the pH value of the mixed solution to generate a precipitate, the precipitate is sequentially filtered and dried.
In the invention, the drying temperature is 50-70 ℃, preferably 55-65 ℃, more preferably 58-62 ℃, and more preferably 60 ℃; the drying time is 10 to 14 hours, preferably 11 to 13 hours, and more preferably 12 hours.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Mixing 0.5g of dried lignite with the grain diameter of 60 meshes and 10mL of 25% ethanol water solution in a power-180W ultrasonic generator for 60min to obtain a product I; and adding 0.5g of potassium hydroxide into the product I, stirring for 5min, and transferring to a reaction kettle at the temperature of 190 ℃ for reaction for 4h to obtain a product II.
Cooling the product II to room temperature, and then carrying out centrifugal treatment to obtain a solid-phase precipitate and a liquid phase; washing the solid-phase precipitate with water to neutrality to obtain a cleaning solution of the solid-phase precipitate, wherein the cleaning solution of the solid-phase precipitate and the liquid phase form a mixed solution, and adjusting the pH value of the mixed solution to 1 by using a mixed acid (containing nitric acid and phosphoric acid in a volume ratio of 1; and filtering the precipitate, and drying in an oven at 50 ℃ for 12h to obtain humic acid.
Example 2
Mixing 1.5g of dried lignite with the particle size of 80 meshes and 30mL of 30% ethanol aqueous solution in a 210W ultrasonic generator for 50min to obtain a product I; and adding 0.75g of calcium hydroxide into the product I, stirring for 6min, and transferring to a reaction kettle at the temperature of 150 ℃ for reaction for 5h to obtain a product II.
Cooling the product II to room temperature, and then carrying out centrifugal treatment to obtain a solid-phase precipitate and a liquid phase; washing the solid-phase precipitate to neutrality by using water to obtain a cleaning solution of the solid-phase precipitate, forming a mixed solution by using the cleaning solution of the solid-phase precipitate and a liquid phase, and adjusting the pH value of the mixed solution to 1.5 by using mixed acid (comprising nitric acid and phosphoric acid with the volume ratio of 1; and filtering the precipitate, and drying in an oven at the temperature of 60 ℃ for 12h to obtain the humic acid.
Example 3
Mixing 1g of dry lignite with the particle size of 70 meshes and 20mL of 40% ethanol aqueous solution in an ultrasonic generator with the power of 240W for 70min to obtain a product I; adding 1.5g of sodium hydroxide into the product I, stirring for 7min, and then transferring the product I into a reaction kettle at the temperature of 170 ℃ for reaction for 7h to obtain a product II.
Cooling the product II to room temperature, and then carrying out centrifugal treatment to obtain a solid-phase precipitate and a liquid phase; washing the solid-phase precipitate with water to neutrality to obtain a cleaning solution of the solid-phase precipitate, wherein the cleaning solution of the solid-phase precipitate and the liquid phase form a mixed solution, and adjusting the pH value of the mixed solution to 1 by using a mixed acid (containing nitric acid and phosphoric acid in a volume ratio of 1; and filtering the precipitate, and drying in an oven at the temperature of 55 ℃ for 14h to obtain the humic acid.
Example 4
Mixing 3g of dried lignite with the particle size of 80 meshes and 60mL of 35% ethanol water solution in a 195W ultrasonic generator for 60min to obtain a product I; adding 4.5g of potassium hydroxide into the product I, stirring for 8min, and transferring to a reaction kettle at the temperature of 150 ℃ for reaction for 4h to obtain a product II.
Cooling the product II to room temperature, and then carrying out centrifugal treatment to obtain a solid-phase precipitate and a liquid phase; washing the solid-phase precipitate to neutrality by using water to obtain a cleaning solution of the solid-phase precipitate, forming a mixed solution by using the cleaning solution of the solid-phase precipitate and a liquid phase, and adjusting the pH value of the mixed solution to 1.2 by using mixed acid (comprising nitric acid and phosphoric acid with the volume ratio of 1; filtering the precipitate, and drying in an oven at 70 deg.C for 12 hr to obtain humic acid.
Example 5
Mixing 3g of dry lignite with the grain size of 70 meshes and 60mL of 30% ethanol water solution in an ultrasonic generator with the power of 210W for 60min to obtain a product I; adding 3g of calcium hydroxide into the product I, stirring for 6min, and transferring to a reaction kettle at the temperature of 150 ℃ for reaction for 4h to obtain a product II.
Cooling the product II to room temperature, and then carrying out centrifugal treatment to obtain a solid-phase precipitate and a liquid phase; washing the solid-phase precipitate to neutrality by using water to obtain a cleaning solution of the solid-phase precipitate, forming a mixed solution by using the cleaning solution of the solid-phase precipitate and a liquid phase, and adjusting the pH value of the mixed solution to 1.4 by using mixed acid (comprising nitric acid and phosphoric acid with the volume ratio of 1; filtering the precipitate, and drying in an oven at 60 deg.C for 10 hr to obtain humic acid.
Example 6
The pH of the mixed solution was adjusted to 1 by using a mixed acid (containing nitric acid and phosphoric acid in a volume ratio of 1:2, the concentration of nitric acid was 5mol/L, and the concentration of phosphoric acid was 10 mol/L), and the other operations were the same as in example 5.
Example 7
The same procedure as in example 5 was repeated except that the amount of calcium hydroxide was changed to 1.5 g.
Example 8
The mass of calcium hydroxide was changed to 4.5g, and the procedure was otherwise the same as in example 5.
Example 9
Calcium hydroxide is added into the product I, stirred and then transferred into a reaction kettle with the temperature of 190 ℃ for reaction for 6 hours, and the other operations are the same as the example 5.
The humic acid yields of the lignite of examples 1 to 9 were measured by the national standard GB/T11957-2001, and the results are shown in Table 1.
TABLE 1 humic acid yield
As can be seen from table 1, the extraction rates of humic acid in examples 1 to 9 are all above 65%, wherein the extraction rates in examples 3 and 4 can be above 80%, and the method for extracting humic acid from lignite by combining ultrasonic and hydrothermal methods has a good extraction effect.
SEM images, XRD images and FT-IR images of lignite and humic acid of example 1 were analyzed, and the results are shown in FIGS. 1 to 3.
As can be seen from FIG. 1, the surface of the lignite is smooth and flat, and the surface of humic acid extracted from lignite is uniformly distributed with a plurality of active substances, which is beneficial for the subsequent utilization of humic acid (such as an activating agent of carbon material).
The coal in fig. 2 is referred to as lignite, and it can be seen from fig. 2 that there are many diffraction peaks but most of them have no obvious peak pattern, which may be related to the complex mineral structure of lignite itself; siO in lignite compared to humic acid 2 And the diffraction peak of the crystal face of the kaolinite is stronger, the content is higher, hydroxide precipitate generated by the reaction of acid added in the acidification process and an alkaline catalyst is ionized, and the content of inorganic elements in the humic acid is reduced, so that inorganic compounds hardly exist in the humic acid.
As can be seen from FIG. 3, the humic acid concentration is 3600-3300 cm -1 A strong and broad absorption peak appears in the range, which should be a tensile vibration peak of the-OH functional group related to hydrogen bonding in phenolic acid and carboxylic acid structures since lignite hardly contains alcohol; 2925cm -1 And 2852cm -1 Is the tensile vibration peak of C-H in a saturated hydrocarbon group; 1706-1247 cm -1 Vibration absorption peaks of skeletons C = C and C = O of the aromatic ring; 815cm -1 The absorption band that appears nearby may be a deformation vibration peak of the aromatic ring outside the CH plane.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method for extracting humic acid from lignite is characterized by comprising the following steps:
1) Carrying out ultrasonic mixing on lignite and an ethanol solution to obtain a product I;
2) Reacting the product I with an activating agent to obtain a product II;
3) Centrifuging the product II to obtain a solid-phase precipitate and a liquid phase; and (4) forming a mixed solution by the cleaning solution of the solid-phase precipitate and the liquid phase, and adjusting the pH value of the mixed solution by using mixed acid to obtain humic acid.
2. The method according to claim 1, wherein the lignite of step 1) has a particle size of 60 to 80 mesh; the mass concentration of the ethanol solution is 25-40%.
3. The method according to claim 1 or 2, wherein the mass-to-volume ratio of the lignite and the ethanol solution in the step 1) is 0.5-3 g:10 to 60mL.
4. The method of claim 3, wherein the power of the ultrasonic mixing in step 1) is 180-240W, and the time of the ultrasonic mixing is 50-70 min.
5. The method of claim 4, wherein the activator of step 2) is potassium hydroxide, calcium hydroxide, or sodium hydroxide; the mass ratio of the activating agent to the lignite obtained in the step 1) is 0.5-4.5: 1 to 3.
6. The method as claimed in claim 5, wherein the reaction temperature in step 2) is 150-190 ℃ and the reaction time is 4-7 h.
7. The method as claimed in claim 6, wherein the washing solution of the solid phase precipitate in the step 3) is a washing solution obtained by washing the solid phase precipitate with water to neutrality.
8. The method of claim 6 or 7, wherein the mixed acid of step 3) comprises nitric acid and phosphoric acid; the volume ratio of the nitric acid to the phosphoric acid is 1-2: 2 to 6; the concentration of the nitric acid is 4-6 mol/L, and the concentration of the phosphoric acid is 8-12 mol/L.
9. The method according to claim 8, wherein the pH of the mixed solution in the step 3) is adjusted to 1 to 1.5.
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| CN116675873A (en) * | 2023-05-24 | 2023-09-01 | 云南云天化股份有限公司 | Method for efficiently extracting humic acid from lignite |
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