CN111138684A - Method for extracting humic acid from lignite - Google Patents
Method for extracting humic acid from lignite Download PDFInfo
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- CN111138684A CN111138684A CN201911418808.0A CN201911418808A CN111138684A CN 111138684 A CN111138684 A CN 111138684A CN 201911418808 A CN201911418808 A CN 201911418808A CN 111138684 A CN111138684 A CN 111138684A
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- lignite
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F11/00—Other organic fertilisers
- C05F11/02—Other organic fertilisers from peat, brown coal, and similar vegetable deposits
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
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Abstract
The invention discloses a method for extracting humic acid from lignite, which comprises the steps of (1) crushing lignite to 50-100 meshes, putting the crushed lignite into a gas-solid reactor, introducing high-temperature oxygen and steam mixed gas, and reacting the mixed gas under the action of a catalyst; (2) dissolving the reaction product obtained in the step (1) into a mixed aqueous solution of citric acid and acetic acid for reaction, and separating a liquid phase and a solid phase after the reaction, wherein the liquid phase is a fulvic acid solution; (3) dissolving the solid phase in the step (2) into KOH and K2CO3Reacting in the mixed solution to generate a liquid phase and a solid phase, separating the liquid phase, adding citric acid and acetic acid to adjust the pH value to be less than or equal to 2, and generating a precipitate; (4) filtering and drying the precipitateAnd generating the solid of the humic acid. The invention extracts humic acid from lignite, can fully decompose lignite, generates humic acid containing more hydroxyl, carboxyl, quinone and the like, does not introduce ions which are not beneficial to saline-alkali soil improvement, and is very suitable for the saline-alkali soil improvement.
Description
Technical Field
The invention relates to the field of fertilizers for improving saline-alkali soil, in particular to a method for extracting humic acid from lignite.
Background
Saline-alkali soil is a generic term for saline soil and alkaline earth. The saline soil mainly refers to saline soil with high chloride or sulfate content, and the soil is alkaline but not necessarily high in pH value. The alkaline earth is soil containing carbonate or heavy phosphate, the pH value is higher, the soil is alkaline, the content of organic matters in saline-alkali soil is low, the soil fertility is low, the physicochemical property is poor, more anions and cations are harmful to crops, and the seedlings of the crops are not easy to promote. The fertilizing principle of the saline-alkali soil is mainly applying organic fertilizer and high-efficiency compound fertilizer, and controlling the use of low-concentration fertilizer. The organic fertilizer contains a large amount of organic matters, plays a role in buffering harmful anions and cations in soil, and is beneficial to rooting and seedling promotion.
Humic acid is produced by microbial degradation of dead biological substances, such as lignin, can react with metal ions in water, is beneficial to the transmission of nutrient elements to crops, can improve the soil structure and is beneficial to the growth of the crops. Has the functions of exchange, adsorption, complexation, chelation and the like with metal ions; in the dispersion system, the polymer serves as polyelectrolyte and has the functions of agglomeration, peptization, dispersion and the like. The humic acid molecules also have a certain number of free radicals and have physiological activity. The humic acid is acidic, and can be used for well improving the saline-alkali soil.
The humic acid can be extracted from the lignite by a nitric acid oxidation method, a hydrogen peroxide oxidation method and the like, but the defects that the raw materials are dangerous, the energy consumption is high, the active groups contained in the humic acid products are few, the follow-up utilization of saline-alkali soil is not facilitated and the like exist.
Disclosure of Invention
In order to solve the technical problems, the invention discloses a method for extracting humic acid from lignite, which has the advantages of simple raw materials, low energy consumption, high extraction rate and more generated active groups.
The technical scheme of the invention is as follows: a method for extracting humic acid from lignite comprises the following steps:
(1) pulverizing lignite to 50-100 meshes, putting the pulverized lignite into a gas-solid reactor, introducing high-temperature oxygen and steam mixed gas, and reacting the high-temperature oxygen and the steam mixed gas under the action of a catalystThe preparation method comprises the following steps of; (2) dissolving the reaction product obtained in the step (1) into a mixed aqueous solution of citric acid and acetic acid for reaction, and separating a liquid phase and a solid phase after the reaction, wherein the liquid phase is a fulvic acid solution; (3) dissolving the solid phase in the step (2) into KOH and K2CO3Reacting in the mixed solution to generate a liquid phase and a solid phase, separating the liquid phase, adding citric acid and acetic acid to adjust the pH value to be less than or equal to 2, and generating a precipitate; (4) filtering and drying the precipitate to generate the solid of the humic acid and the humic acid.
Further, in the step (1), the ratio of oxygen to water vapor is 1: 2 to 5.
Further, the temperature in the step (1) is 100-200 ℃, and the pressure is 0.2-0.5 MPa.
Further, the ratio of citric acid to acetic acid in the step (2) is 4-6: 1.
further, the catalyst in the step (1) is one of vanadium oxide, niobium oxide and tantalum oxide adhered on the molecular sieve.
Further, the adhesive on the molecular sieve is aluminum phosphate.
Further, the preparation steps of the catalyst are as follows: and spraying an aluminum phosphate solution on the molecular sieve, stirring, adding one of vanadium oxide, niobium oxide and tantalum oxide powder, stirring, and quickly drying.
Further, the mass ratio of the molecular sieve to one of vanadium oxide, niobium oxide and tantalum oxide powder is 50-60: 1.
further, the application of the humic acid prepared by the method for extracting the humic acid from the lignite in the saline-alkali soil improvement fertilizer is included.
The invention improves the method for extracting humic acid from lignite, firstly, lignite is degraded with oxygen and water vapor under the action of a certain temperature and pressure catalyst, so that benzene rings and fat chains of some organic matters in lignite are broken in advance, then, the degraded products are extracted by using citric acid and acetic acid, firstly, fulvic acid in the humic acid is extracted, and finally, KOH and K are used2CO3Extracting the solid phase after extracting the citric acid and the acetic acid by the mixed solution, and extracting the fulvic acid and the fulvic acid. Other redundant ions which are not beneficial to use in saline-alkali soil are not introduced into the extracted humic acid productAnd the saline-alkali soil improver contains more active groups such as hydroxyl, carboxyl, quinonyl and the like, and can promote saline-alkali soil improvement and plant growth. The invention has potential market value.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1
A method for extracting humic acid from lignite comprises the following steps:
(1) crushing lignite to 50-100 meshes, putting the crushed lignite into a gas-solid reactor, introducing high-temperature oxygen and steam mixed gas, and reacting under the action of a catalyst; (2) dissolving the reaction product obtained in the step (1) into a mixed aqueous solution of citric acid and acetic acid for reaction, and separating a liquid phase and a solid phase after the reaction, wherein the liquid phase is a fulvic acid solution; (3) dissolving the solid phase in the step (2) into KOH and K2CO3Reacting in the mixed solution to generate a liquid phase and a solid phase, separating the liquid phase, adding citric acid and acetic acid to adjust the pH value to be less than or equal to 2, and generating a precipitate; (4) filtering and drying the precipitate to generate the solid of the humic acid and the humic acid.
Further, in the step (1), the ratio of oxygen to water vapor is 1: 2. the temperature in the step (1) is 100-200 ℃, and the pressure is 0.2-0.5 MPa. In the step (2), the ratio of citric acid to acetic acid is 4: 1. the catalyst in the step (1) is one of vanadium oxides adhered to the molecular sieve. The adhesive on the molecular sieve is aluminum phosphate. The preparation steps of the catalyst are as follows: and spraying an aluminum phosphate solution on the molecular sieve, stirring, adding vanadium oxide, stirring, and quickly drying. The mass ratio of the molecular sieve to the vanadium oxide is 50-60: 1.
example 2
Example 2 is essentially the same as example 1, except that in step (1) the ratio of oxygen to water vapor is 1: 3.5.
example 3
Example 3 is essentially the same as example 1, except that in step (1) the ratio of oxygen to water vapor is 1: 5
Example 4
A method for extracting humic acid from lignite comprises the following steps:
(1) crushing lignite to 50-100 meshes, putting the crushed lignite into a gas-solid reactor, introducing high-temperature oxygen and steam mixed gas, and reacting under the action of a catalyst; (2) dissolving the reaction product obtained in the step (1) into a mixed aqueous solution of citric acid and acetic acid for reaction, and separating a liquid phase and a solid phase after the reaction, wherein the liquid phase is a fulvic acid solution; (3) dissolving the solid phase in the step (2) into KOH and K2CO3Reacting in the mixed solution to generate a liquid phase and a solid phase, separating the liquid phase, adding citric acid and acetic acid to adjust the pH value to be less than or equal to 2, and generating a precipitate; (4) filtering and drying the precipitate to generate the solid of the humic acid and the humic acid.
Further, in the step (1), the ratio of oxygen to water vapor is 1: 3.5. the temperature in the step (1) is 100-200 ℃, and the pressure is 0.2-0.5 MPa. In the step (2), the ratio of citric acid to acetic acid is 4: 1. the catalyst in the step (1) is niobium oxide adhered on a molecular sieve. The adhesive on the molecular sieve is aluminum phosphate. The preparation steps of the catalyst are as follows: and spraying an aluminum phosphate solution on the molecular sieve, stirring, adding niobium oxide, stirring, and quickly drying. The mass ratio of the molecular sieve to the niobium oxide is 50-60: 1.
example 5
Example 5 is essentially the same as example 4 except that the step (1) catalyst is tantalum oxide adhered to a molecular sieve. The adhesive on the molecular sieve is aluminum phosphate. The preparation steps of the catalyst are as follows: and spraying an aluminum phosphate solution on the molecular sieve, stirring, adding tantalum oxide, stirring, and quickly drying. The mass ratio of the molecular sieve to the tantalum oxide is 50-60: 1.
example 6
A method for extracting humic acid from lignite comprises the following steps:
(1) crushing lignite to 50-100 meshes, putting the crushed lignite into a gas-solid reactor, introducing high-temperature oxygen and steam mixed gas, and reacting under the action of a catalyst; (2) dissolving the reaction product obtained in the step (1) into a mixed aqueous solution of citric acid and acetic acid for reaction, and separating a liquid phase and a solid phase after the reaction, wherein the liquid phase is a fulvic acid solution; (3) dissolving the solid phase in the step (2) into KOH and K2CO3Reacting in the mixture to form a liquid phase and a solid phase, and separating the liquid phaseThen adding citric acid and acetic acid to adjust the pH value to be less than or equal to 2, and generating precipitate; (4) filtering and drying the precipitate to generate the solid of the humic acid and the humic acid.
Further, in the step (1), the ratio of oxygen to water vapor is 1: 3.5. the temperature in the step (1) is 100-200 ℃, and the pressure is 0.2-0.5 MPa. In the step (2), the ratio of citric acid to acetic acid is 5: 1. the catalyst in the step (1) is vanadium oxide adhered on a molecular sieve. The adhesive on the molecular sieve is aluminum phosphate. The preparation steps of the catalyst are as follows: and spraying an aluminum phosphate solution on the molecular sieve, stirring, adding vanadium oxide, stirring, and quickly drying. The mass ratio of the molecular sieve to the vanadium oxide is 50-60: 1.
example 7
Example 7 is essentially the same as example 6, except that in step (2) the ratio of citric acid to acetic acid is 6: 1.
comparative example 1
Comparative example 1 is essentially the same as example 2 except that the adhesive is aluminum silicate.
Comparative example 2
Humic acid extracted from lignite by a nitric acid extraction method is commonly used in the market.
Comparative experiment
(1) Humic acid extraction rate experiment
The humic acid extraction test was carried out by the methods of examples 1 to 7 and comparative examples 1 to 2 using brown coal produced in Hulenbel mining areas of inner Mongolia as a raw material, and the produced humic acids including fulvic acid, fulvic acid and fulvic acid were dried and weighed, and the obtained yields are shown in Table 1.
Table 1 is a comparison table of humic acid yield
As can be seen from Table 1, the humic acid extraction rates of examples 1 to 7 were all 50% or more, which is comparable to the extraction rate of the nitric acid extraction method in general in comparative example 2, whereas the humic acid extraction rates of examples 1, 2, 6 and 7 using vanadium oxide as a catalyst were superior to those of comparative example 2. Comparative example 1 because the used binder was aluminum silicate, the catalytic activity of the catalyst was inferior to that of aluminum phosphate, the predecomposition ability of lignite was weak, and the yield of humic acid produced was low, only 48%.
(2) Cotton yield test
The saline-alkali soil in the north coastal area of the state is taken as an experimental object, and the salt-alkali soil with basically the same properties is prepared by mixing the following components in percentage by weight according to the following steps of: the ratio of 8 is applied to saline-alkali soil before cotton sowing in spring, the per mu yield of cotton is counted after cotton harvesting in autumn, and the statistical result is shown in table 2.
Table 2 shows the yield per mu of cotton
As can be seen from Table 2, the per mu yields of cotton in examples 1 to 7 and comparative example 1 are higher than that in comparative example 2, which shows that the fertilizer for humic acid in saline-alkali soil prepared by the method of the invention contains more active factors, is beneficial to the growth of plants and has higher fertilizer efficiency than the fertilizer for humic acid prepared by the common nitric acid method.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein. In addition, the technical solutions between the various embodiments can be combined with each other, but must be based on the realization of those skilled in the art; where combinations of features are mutually inconsistent or impractical, such combinations should not be considered as being absent and not within the scope of the claimed invention.
Claims (9)
1. A method for extracting humic acid from lignite is characterized by comprising the following steps:
(1) crushing lignite to 50-100 meshes, putting the crushed lignite into a gas-solid reactor, introducing high-temperature oxygen and steam mixed gas, and reacting under the action of a catalyst;
(2) dissolving the reaction product obtained in the step (1) into a mixed aqueous solution of citric acid and acetic acid for reaction, and separating a liquid phase and a solid phase after the reaction, wherein the liquid phase is a fulvic acid solution;
(3) dissolving the solid phase in the step (2) into KOH and K2CO3Reacting in the mixed solution to generate a liquid phase and a solid phase, separating the liquid phase, adding citric acid and acetic acid to adjust the pH value to be less than or equal to 2, and generating a precipitate;
(4) filtering and drying the precipitate to generate the solid of the humic acid and the humic acid.
2. The method for extracting humic acid from lignite according to claim 1, wherein: in the step (1), the ratio of oxygen to water vapor is 1: 2 to 5.
3. The method for extracting humic acid from lignite according to claim 1, wherein: the temperature in the step (1) is 100-200 ℃, and the pressure is 0.2-0.5 MPa.
4. The method for extracting humic acid from lignite according to claim 1, wherein: in the step (2), the ratio of citric acid to acetic acid is 4-6: 1.
5. the method for extracting humic acid from lignite according to claim 1, wherein: the catalyst in the step (1) is one of vanadium oxide, niobium oxide and tantalum oxide adhered on the molecular sieve.
6. The method for extracting humic acid from lignite according to claim 5, wherein: the adhesive on the molecular sieve is aluminum phosphate.
7. The method for extracting humic acid from lignite according to claim 6, wherein the catalyst is prepared by the steps of: and spraying an aluminum phosphate solution on the molecular sieve, stirring, adding one of vanadium oxide, niobium oxide and tantalum oxide powder, stirring, and quickly drying.
8. The method for extracting humic acid from lignite according to claim 7, wherein: the mass ratio of the molecular sieve to one of vanadium oxide, niobium oxide and tantalum oxide powder is 50-60: 1.
9. the application of the humic acid prepared by the method for extracting the humic acid from the lignite according to claim 1 in saline-alkali soil improvement fertilizers.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548235A (en) * | 2020-05-12 | 2020-08-18 | 锡林郭勒职业学院 | Method for extracting humic acid from lignite companion |
| CN112409609A (en) * | 2020-11-24 | 2021-02-26 | 张坤 | Neutral and subacid sulfonated potassium fulvate and preparation method thereof |
| CN114933713A (en) * | 2022-06-22 | 2022-08-23 | 新疆圣大一方生物科技有限公司 | Preparation method of fulvic acid |
| 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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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111548235A (en) * | 2020-05-12 | 2020-08-18 | 锡林郭勒职业学院 | Method for extracting humic acid from lignite companion |
| CN112409609A (en) * | 2020-11-24 | 2021-02-26 | 张坤 | Neutral and subacid sulfonated potassium fulvate and preparation method thereof |
| CN114933713A (en) * | 2022-06-22 | 2022-08-23 | 新疆圣大一方生物科技有限公司 | Preparation method of fulvic acid |
| 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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Application publication date: 20200512 |