CN115124732B - Preparation method of nano humic acid and method for improving fertilizer efficiency by using same - Google Patents
Preparation method of nano humic acid and method for improving fertilizer efficiency by using same Download PDFInfo
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- CN115124732B CN115124732B CN202210806562.XA CN202210806562A CN115124732B CN 115124732 B CN115124732 B CN 115124732B CN 202210806562 A CN202210806562 A CN 202210806562A CN 115124732 B CN115124732 B CN 115124732B
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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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- 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
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- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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Abstract
The invention belongs to the technical field of fertilizers, and relates to a preparation method of nano humic acid and a method for improving fertilizer efficiency by using the same, wherein the preparation method of the nano humic acid comprises the following steps: 1. preparing humic acid; 2. and preparing nano humic acid by using the humic acid. The prepared nano humic acid has a large number of functional groups and a large specific surface area, can be complexed with a fertilizer, delays the release and fixation of the fertilizer in soil, and promotes plants to absorb and utilize phosphorus and the like in the fertilizer.
Description
Technical Field
The invention belongs to the technical field of fertilizers, relates to a nanoscale material and a fertilizer synergistic method thereof, and particularly relates to a preparation method of nano humic acid and a method for improving fertilizer efficiency by using the nano humic acid.
Background
Nitrogen, phosphorus and potassium are indispensable nutrient elements in the plant growth process, and the content of the nutrient elements in soil is directly related to the growth state of crops. For this purpose, fertilizers are applied to increase the nitrogen, phosphorus and potassium content of the soil. A large amount of fertilizer is applied to soil, but the utilization rate is low in the season. The lower utilization rate leads to a series of problems of fertilizer waste, water eutrophication, environmental pollution and the like in the crop planting process in order to pursue high yield and high benefit, and the fertilizing amount is far beyond the crop demand. Therefore, how to reasonably and efficiently apply the fertilizer and improve the utilization efficiency of the fertilizer becomes an important problem which needs to be solved urgently at present.
At present, fertilizer synergistic research is mostly based on changing a fertilization mode, adding a synergist and the like. However, with the continuous development of the technology, the mechanized farming scale is continuously enlarged, the labor cost is continuously increased, the demand on the crop yield is continuously increased, the process for improving the utilization rate of the phosphate fertilizer by changing the fertilization mode is complex, the technical requirement is high, and the requirement of people on convenient fertilization is gradually difficult to meet. To this end, many scholars have begun to increase fertilizer utilization by adding different materials to the fertilizer formulation.
Humic acid is a special and complex high molecular organic compound, widely distributed on the earth surface, such as low-rank coal (lignite, weathered coal, peat), soil, rivers, lakes, oceans and the like, has obvious effects on improving the quality of the soil and improving the productivity of the soil, and is a common fertilizer synergistic carrier.
At present, industrial humic acid products are mainly prepared by low-end coal resources such as weathered coal, lignite and the like, and the production process is laggard. The nano organic fertilizer has small size and large specific surface area, can mineralize a plurality of nutrient elements which cannot be synthesized artificially, has the sustained and controlled release effect, can provide all-round and full-nutrient cultivation supply for plants, and has important significance for the development of modern agriculture.
Based on the characteristics, the research of make internal disorder or usurp for the preparation of nano humic acid and the reaction between the nano humic acid and the fertilizer is urgently needed to be combined with the properties of the humic acid and the nano material so as to improve the fertilizer efficiency of the fertilizer by utilizing the nano humic acid.
Disclosure of Invention
The invention aims to overcome the defects of the prior fertilizer synergistic material with common size, and provides a preparation method of nano humic acid and a method for improving the fertilizer efficiency of the fertilizer by using the nano humic acid as a synergistic carrier.
In order to achieve the above purpose, the invention provides the following technical scheme:
the preparation method of the nano humic acid is characterized by comprising the following steps:
1. preparing humic acid, which specifically comprises:
1.1 Grinding and sieving weathered coal;
1.2 Mixing the sieved weathered coal with NaOH solution and stirring the mixture evenly at room temperature; wherein the concentration of the NaOH solution is 0.5M, and the solid-to-liquid ratio of the weathered coal to the NaOH solution is 1:10;
1.3 Transferring the uniformly stirred mixed solution into a centrifuge, and removing impurities through centrifugation to obtain a humic acid solution;
1.4 Adjusting the pH value of the humic acid solution to 1 by using an HCl solution, standing, stirring, transferring the stirred solution into a centrifugal machine, performing centrifugal separation, and removing a supernatant to obtain the roughly extracted humic acid;
1.5 Uniformly mixing the roughly extracted humic acid with a mixed solution of an HCl solution and an HF solution, wherein the volume ratio of the HCl solution to the HF solution is 1;
1.6 ) washing the crude humic acid with deionized water to remove Cl - ；
1.7 Washing, and freeze-drying to obtain humic acid;
2. preparing nano humic acid, which specifically comprises the following steps:
2.1 And grinding): putting the humic acid prepared in the step 1 into a grinding tank for grinding to form a uniform sample;
2.2 Pulsed ultrasound): putting the ground uniform sample into a beaker, adding deionized water, and carrying out pulse strong ultrasonic stripping to form a nano humic acid solution with multiple active sites;
2.3 And (4) centrifugal separation: transferring the nano humic acid solution after ultrasonic treatment to a centrifugal machine for centrifugal separation, and discarding supernatant liquid after the centrifugal separation is finished;
2.4 Freeze-drying: and taking the precipitate out of the centrifuge, standing in a refrigerator, taking out, drying in a freeze dryer, and drying to obtain the nano humic acid.
Preferably, in the step 2.1), the grinding tank is an agate grinding tank, and the agate grinding tank is symmetrically placed into a ball mill during grinding, and is ground at the rotating speed of 300rpm for 8-12 hours to form a uniform sample.
Preferably, in the step 2.2), the ratio of the uniform sample to the deionized water is 2g:2000mL, and the pulse strong ultrasonic stripping is to perform ultrasonic treatment for 2 to 6 hours at the frequency of 10 seconds of work and 10 seconds of pause under the condition of ultrasonic continuous pulse power of 800W.
Preferably, in the step 2.3), the centrifugal separation is specifically: centrifugation was carried out at 10000rpm for 5 minutes.
Preferably, the step 2.4) is specifically: and taking the precipitate out of the centrifuge, standing in a refrigerator at-80 ℃ for 12 hours, taking out, drying in a freeze dryer at-50 ℃ for 12 hours, and drying to obtain the nano humic acid.
Preferably, in the step 1.4), the concentration of the HCl solution is 6.0M, the standing time is 24 hours, the rotation speed during centrifugal separation is 8000rpm, and the centrifugal separation time is 10 minutes.
In addition, the invention also provides nano humic acid which is characterized by being prepared by adopting the preparation method.
The invention also provides a method for improving fertilizer efficiency, which is characterized in that the nano humic acid is added into soil to react with fertilizer in the soil so as to improve the fertilizer efficiency.
Preferably, the dosage of the nano humic acid is as follows: adding 0.1-0.3 g nano humic acid into every 1kg of soil.
Preferably, the fertilizer contains N0.15 g and P per 1kg of soil 2 O 5 0.2g、K 2 O 0.15 g。
Compared with the prior art, the preparation method of the nano humic acid and the method for improving the fertilizer efficiency by using the same have one or more of the following beneficial technical effects:
1. the prepared nano humic acid has rough surface, dense gaps, good dispersibility, reduced particle size, a large amount of functional groups and larger specific surface area.
2. The prepared nano humic acid is mixed with fertilizer and applied, can fully react with the fertilizer, delays the release and fixation of the fertilizer in soil and promotes the growth and development of plants.
Drawings
FIG. 1 is a flow chart of the preparation method of nano humic acid of the invention.
FIG. 2 is a flow chart of humic acid preparation according to the present invention.
FIG. 3 is a flow chart of the present invention for preparing nano humic acid by using humic acid.
FIG. 4 is SEM image of nano humic acid prepared by the invention.
FIG. 5 is FTIR chart of humic acid and nano humic acid prepared by the present invention.
FIG. 6 is a schematic diagram showing the content of available phosphorus in potting soil using humic acid and nano-humic acid of the present invention.
FIG. 7 shows humic acid and humic acid derivatives which utilize the present invention picture of growth of potted pepper with nano humic acid.
Detailed Description
The present invention is further illustrated by the following examples and examples, which are not intended to limit the scope of the present invention.
The invention relates to a preparation method of nano humic acid and a method for improving fertilizer efficiency by using the nano humic acid as a synergistic carrier to act with a fertilizer.
Fig. 1 shows a flow chart of the preparation method of nano humic acid of the invention. As shown in fig. 1, the preparation method of nano humic acid of the invention comprises the following steps:
1. preparing humic acid.
In the invention, firstly, humic acid is required to be prepared, and nano humic acid is prepared by taking the humic acid as a raw material. Specifically, as shown in fig. 2, the preparation of humic acid comprises:
1. grinding weathered coal, and sieving.
In the invention, weathered coal is used as a raw material to prepare humic acid. Wherein, through the grinding, can grind weathered coal into weathered coal granule to subsequent reaction.
In the present invention, it is preferable that the number of meshes of the sieve used for sieving is 20.
2. And mixing the sieved weathered coal with a NaOH solution, and uniformly stirring the mixed solution at room temperature.
Wherein the concentration of the NaOH solution is 0.5M, and the solid-liquid ratio of the weathered coal and the NaOH solution is 1. While stirring, the stirring time was 24 hours. In this way, sufficient contact and reaction between the various components (i.e., weathered coal particles and NaOH solution) is facilitated.
3. Transferring the stirred solution into a centrifugal machine, and removing impurities through centrifugal separation to obtain the humic acid solution.
Specifically, the rotation speed at the time of centrifugal separation was 8000rpm, and the centrifugal separation time was 10 minutes. Therefore, separation of humic acid and impurities can be better realized.
4. And (3) adjusting the pH value of the humic acid solution to 1 by using an HCl solution, standing, stirring, transferring the stirred solution to a centrifugal machine, performing centrifugal separation, and removing a supernatant to obtain the roughly extracted humic acid.
Wherein the concentration of the HCl solution is 6.0M. The time for standing was 24 hours, the rotational speed for centrifugal separation was 8000rpm, and the centrifugal separation time was 10 minutes. Therefore, better separation can be realized, so as to obtain the roughly extracted humic acid conveniently.
5. Mixing the roughly extracted humic acid with a mixed solution of HCl solution and HF solution, shaking after mixing, and filtering out the mixed solution after shaking for 24 hours. Thereby, the coarsely extracted humic acid is washed by the mixed solution to remove inorganic substances, and the coarsely extracted humic acid is purified.
The concentration of the HCl solution is 0.1M, the concentration of the HF solution is 0.3M, and the HCl solution and the HF solution are uniformly mixed according to the proportion of 1:1 to obtain the mixed solution. And the solid-liquid ratio of the roughly extracted humic acid to the mixed solution is always kept to be 1.
Preferably, the roughly extracted humic acid is washed 3 times with the mixed solution using exactly the same conditions. That is, after filtration, the roughly extracted humic acid is mixed with a mixed solution of HCl solution and HF solution, and after mixing, shaking is performed, and after shaking for 24 hours, the mixed solution is filtered off. This was repeated three times. Therefore, the purification of humic acid can be better realized.
6. Washing the purified crude humic acid with deionized water to remove Cl - 。
Wherein the solid-liquid ratio of the crude humic acid to the deionized water is 1. Cl remaining in the washing in step 5 can be removed by washing with deionized water - And the like.
7. And (4) freeze-drying the washed humic acid to obtain humic acid, and drying and storing the humic acid for later use.
Wherein the freeze drying time is 12 hours, and the freeze drying temperature is-50 ℃. Thus, the prepared humic acid is convenient to be fully dried.
2. Preparing the nano humic acid.
And (4) preparing the nano humic acid material by using the humic acid prepared in the step one as a raw material. As shown in fig. 3, the preparation of nano humic acid specifically comprises:
1. and (6) grinding.
Namely, the humic acid prepared in the first step is put into an agate grinding tank, and is symmetrically put into a ball mill for grinding in the agate grinding tank to form a sample.
Specifically, 5g of humic acid prepared in the first step is put into an agate grinding tank, and is symmetrically put into a ball mill in the agate grinding tank, and is ground for 8 to 12 hours at the rotating speed of 300rpm to form a sample. Humic acid powder can be prepared by grinding, so as to facilitate subsequent treatment and reaction.
2. Pulsed ultrasound.
That is, the ground sample was put into a beaker, deionized water was added, and sonication was performed in ultrasonic waves.
Specifically, 2g of the ground sample is placed in a beaker, 2000mL of deionized water is added, and ultrasound is performed for 2-6 hours at a frequency of 10 seconds of operation and 10 seconds of pause under the condition of 800W of continuous pulse ultrasonic power.
3. And (4) centrifugal separation.
That is, the solution after ultrasonic treatment is transferred to a centrifuge for centrifugal separation, and the supernatant liquid is discarded after the centrifugal separation is finished.
Specifically, the solution after ultrasonic treatment is transferred to a centrifuge, centrifugation is carried out for 5 minutes at 10000rpm, and supernatant liquid is discarded after the centrifugation.
4. Freeze drying
Namely, taking out the precipitate from a centrifuge tube of a centrifuge, standing in a refrigerator, drying in a freeze dryer, and drying to obtain the nano humic acid.
Specifically, the precipitate is taken out of a centrifuge tube of a centrifuge, is placed in a refrigerator at minus 80 ℃ for 12 hours, is taken out and is then placed in a freeze dryer for drying at minus 50 ℃ for 12 hours, and the nano humic acid is prepared.
The microscopic morphology of the nano humic acid prepared by the preparation method of the invention is observed by using a Scanning Electron Microscope (SEM), and the result is shown in figure 4. As can be seen from FIG. 4, the prepared nano humic acid has rough surface, dense gaps, good dispersibility and reduced particle size, which indicates that the prepared nano humic acid material is a nano humic acid material.
The Humic Acid (HA) and the Nano Humic Acid (NHA) prepared by the preparation method of the invention are scanned by Fourier infrared spectroscopy (FTIR), and the number of main functional groups of the humic acid and the nano humic acid is observed. As can be seen from FIG. 5, 3437cm -1 Stretching and vibrating for hydrogen bond association-OH, dissociation-OH and the like in humic acid; at 1700cm -1 On the left and right, there is a carboxylic acid carbonyl absorption peak; 1242cm -1 C-O vibration of aromatic ethers, and possibly C-O and O-H vibration of carboxylic acids and phenols. The FTIR spectrum results show that: the characteristics of the humic acid are not changed by the nano humic acid. And as the specific surface area of the nano humic acid is increased, the more characteristic functional groups are exposed on the surface, and the intensity of each characteristic absorption peak is enhanced.
The nano humic acid prepared by the preparation method of the invention is used as a synergistic carrier to carry out pot experiment to research the reaction between the nano humic acid and fertilizer and the influence of the nano humic acid on the fertilizer efficiency of the fertilizer.
Placing soil sample (vegetable planting soil from Maanshan city and county, anhui province)Air-drying in a shady and ventilated place, grinding and sieving with a 2mm sieve. Weighing 1kg of sieved soil sample, filling the soil sample into a plastic basin, and applying 0.15g of N and 0.15g of P to each kg of soil 2 O 5 0.2g、K 2 0.15g of O. The fertilizer is mixed with 0.1-0.3 g humic acid and 0.1-0.3 g nano humic acid respectively, and the mixture is filled into a dialysis bag and buried in the bottom of a plastic basin. Destructive sampling was performed on days 5, 12, 22, 50 after colonization.
The experimental results are as follows:
1. the content of available phosphorus in soil.
As can be seen from FIG. 6, the soil available phosphorus content decreased with the number of days of colonization within 50 days of culture, and the maximum value of each treatment appeared on day 5 of culture.
Compared with the treatment (CK) without adding any humic acid, the treatment (T1, T2) with adding humic acid and nano humic acid improves the effective phosphorus content of the soil to different degrees. The average content of available phosphorus in the soil treated by the common fertilization and the humic acid (T1) is increased by 26.3 mg/kg compared with that of CK, the average content of available phosphorus in the soil treated by the common fertilization and the nano humic acid (T2) is increased by 45.7mg/kg, and the average content of the available phosphorus in the soil treated by the common fertilization and the nano humic acid (T2) and the average content of the available phosphorus in the soil treated by the common fertilization and the nano humic acid (CK) are obviously different from that of CK in the middle and later stages (12-50 days). Under the condition of adding the synergistic carrier, the soil quick-acting phosphorus content of T2 is higher than that of T1 treatment in the whole growth period, and the average content is increased by 19.4mg/kg compared with the latter. On day 5, the difference with humic acid treatment forms a 5% significant level, which reaches 124.32mg/kg, and is higher than 7.2% of humic acid treatment. After 50 days of culture, the effective phosphorus content of the soil treated by the T2 is improved by 3.8 percent compared with that of the soil treated by the T1.
2. And (5) growing and developing the plants.
As shown in FIG. 7, the plant height and stem thickness of the nano humic acid treated plants show the optimal states, which are 32.90cm and 5.93mm respectively, and are obviously improved by 28.77 percent and 14.70 percent compared with CK treatment. The weight average of the dry and fresh plants added with humic acid is higher than that of the plants treated by CK. Wherein, the dry and fresh weight of the plants under the T2 treatment is the highest, namely 5.39g and 49.03g, wherein the overground part is respectively improved by 26.82% and 7.09% compared with the CK treatment, and the underground part is improved by 30.77% and 16.70%.
The addition of humic acid, especially nano humic acid, can effectively promote the growth and development of pepper root systems. The T1 and T2 treatments significantly promoted an increase in total root length, total surface area, total root volume, mean diameter, and number of branches of pepper seedlings compared to CK treatment. The effect of the nano humic acid is better than that of humic acid, compared with T1 treatment, each index of T2 treatment is respectively improved by 41.89 percent, 38.11 percent, 7.72 percent, 12.66 percent and 52.53 percent, and the root system of the pepper plant grows and develops best.
Therefore, the nano humic acid can fully react with the fertilizer, delay the release and fixation of the fertilizer in the soil and promote the growth and development of plants.
The above examples of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes and modifications which are obvious to the technical scheme of the invention are covered by the protection scope of the invention.
Claims (10)
1. The preparation method of the nano humic acid is characterized by comprising the following steps:
1. preparing humic acid, which specifically comprises:
1.1 Grinding and sieving weathered coal;
1.2 Mixing the sieved weathered coal with NaOH solution and stirring the mixture evenly at room temperature; wherein the concentration of the NaOH solution is 0.5M, and the solid-to-liquid ratio of the weathered coal to the NaOH solution is 1:10;
1.3 Transferring the uniformly stirred mixed solution into a centrifugal machine, and removing impurities through centrifugal separation to obtain a humic acid solution;
1.4 Adjusting the pH value of the humic acid solution to 1 by using an HCl solution, standing, stirring, transferring the stirred solution into a centrifugal machine, performing centrifugal separation, and removing a supernatant to obtain the roughly extracted humic acid;
1.5 Uniformly mixing the roughly extracted humic acid with a mixed solution of an HCl solution and an HF solution, wherein the volume ratio of the HCl solution to the HF solution is 1;
1.6 ) washing the crude humic acid with deionized water to remove Cl - ；
1.7 Washing, and freeze-drying to obtain humic acid;
2. preparing nano humic acid, which specifically comprises the following steps:
2.1 Grinding: putting the humic acid prepared in the step 1 into a grinding tank for grinding to form a uniform sample;
2.2 Pulsed ultrasound): putting the ground uniform sample into a beaker, adding deionized water, and carrying out pulse strong ultrasonic stripping to form a nano humic acid solution with multiple active sites;
2.3 And (4) centrifugal separation: transferring the nano humic acid solution after ultrasonic treatment to a centrifuge, performing centrifugal separation, and discarding supernatant liquid after the centrifugal separation is finished;
2.4 Freeze-drying: and taking the precipitate out of the centrifuge, standing in a refrigerator, taking out, drying in a freeze dryer, and drying to obtain the nano humic acid.
2. The method for preparing nano humic acid according to claim 1, wherein in the step 2.1), the grinding tank is an agate grinding tank, and the agate grinding tank is symmetrically placed into a ball mill during grinding, and the grinding is carried out for 8-12 hours at the rotating speed of 300rpm, so as to form a uniform sample.
3. The method for preparing nano humic acid according to claim 1, wherein in the step 2.2), the proportion of the uniform sample to the deionized water is 2g:2000mL, and the pulse strong ultrasonic stripping is to perform ultrasonic treatment for 2 to 6 hours at the frequency of 10 seconds of work and 10 seconds of pause under the condition of ultrasonic continuous pulse power of 800W.
4. The method for preparing nano humic acid according to claim 1, wherein in the step 2.3), the centrifugal separation is specifically as follows: centrifugation was carried out at 10000rpm for 5 minutes.
5. The method for preparing nano humic acid according to claim 1, wherein the step 2.4) is specifically as follows: and taking the precipitate out of the centrifuge, standing in a refrigerator at-80 ℃ for 12 hours, taking out, drying in a freeze dryer at-50 ℃ for 12 hours, and drying to obtain the nano humic acid.
6. The method for preparing nano humic acid according to claim 1, wherein in the step 1.4), the concentration of HCl solution is 6.0M, the standing time is 24 hours, the rotating speed during centrifugal separation is 8000rpm, and the centrifugal separation time is 10 minutes.
7. Nano humic acid, characterized in that it is prepared by the preparation method of any one of claims 1 to 6.
8. A method for improving fertilizer efficiency, which is characterized in that the nano humic acid of claim 7 is added into soil to react with fertilizer in the soil so as to improve the fertilizer efficiency.
9. The method for improving fertilizer efficiency of fertilizer according to claim 8, wherein the dosage of nano humic acid is as follows: 0.1-0.3 g of the nano humic acid is added into every 1kg of soil.
10. The method of improving fertilizer efficiency of a fertilizer according to claim 9, wherein the fertilizer contains N0.15 g and P0 kg per 1kg of soil 2 O 5 0.2g、K 2 O 0.15g。
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