CN113248321A - Preparation method of light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals - Google Patents
Preparation method of light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals Download PDFInfo
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- CN113248321A CN113248321A CN202110547252.6A CN202110547252A CN113248321A CN 113248321 A CN113248321 A CN 113248321A CN 202110547252 A CN202110547252 A CN 202110547252A CN 113248321 A CN113248321 A CN 113248321A
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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
- 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
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
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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
- C05G3/80—Soil conditioners
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- Pest Control & Pesticides (AREA)
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Abstract
The invention discloses a preparation method of a light-operated slow-release fulvic acid fertilizer capable of repairing metal, which comprises the steps of adding weathered coal into tap water, stirring, adding calcium peroxide, heating for 2 hours, slowly adding ammonium bicarbonate, stirring, adding urea, stirring again, carrying out suction filtration, and drying to obtain activated weathered coal; uniformly mixing biochar, ferroferric oxide and activated weathered coal; adding into sodium alginate solution to obtain mixed solution; slowly dripping into ferric chloride solution by using an injector, washing the gel ball for 3-5 times by using deionized water after full reaction, and freeze-drying for 20-24 h to obtain the light-controlled slow-release fulvic acid fertilizer. The release of fulvic acid is controlled by utilizing the good photoresponse of the biochar, the good removal performance of functional groups such as carboxyl, hydroxyl and the like on heavy metal ions is utilized, and the magnetic recovery of the carrier is carried out by utilizing ferroferric oxide, so that the secondary pollution to the environment is reduced.
Description
Technical Field
The invention relates to the technical field of agricultural fertilizers, in particular to the technical field of light-operated slow-release fulvic acid fertilizers.
Background
Weathered coal refers to coal exposed to or located in the shallow layers of the earth's surface, commonly referred to as outcrop coal. After weathering and oxidation, weathered coal partially loses the value of being used as power fuel and coking coal, but contains a large amount of regenerated humic acid, and humic acid substances have the functions of improving the physical and chemical properties of soil, improving the utilization efficiency of fertilizer, stimulating the growth of crops, enhancing the stress resistance of crops and improving the quality of agricultural products. The essence of the humic acid is fulvic acid, has high quality, good concentration and complete solubility, is a substance with the best activity, drought resistance and stress resistance in the humic acid, can inhibit the dormancy of plants, enables the plants to continuously and circularly absorb various nutrients, enhances the physiological functions of the plants, and achieves the purposes of quick growth, yield increase and income increase. Meanwhile, the activated coal contains various oxygen-containing active functional groups, such as carboxyl, phenolic hydroxyl, quinonyl, alcoholic hydroxyl and the like, and the functional groups have five functions of improving soil, enhancing fertilizer efficiency, stimulating growth, promoting stress resistance and improving quality when being applied to agricultural production, and are generally accepted by the agricultural and foreign communities.
At present, the phenomenon that the heavy metal content of crops exceeds the standard in China often occurs, the heavy metal pollution condition of soil is not optimistic, and the development of a soil heavy metal remediation technology is urgently needed. At present, soil heavy metal remediation methods mainly comprise physical methods (an electric method, a deep ploughing method and a soil-bearing method), chemical methods (a passivation method and a leaching method) and biological methods (a plant enrichment method and a microorganism remediation method). Wherein, the chemical method has rapid effect, simple and convenient use and wider application. However, most chemical agents cause secondary pollution to the soil. Therefore, the development of a green, highly effective heavy metal treatment agent is urgently required.
Disclosure of Invention
The invention provides a preparation method of a light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals.
A preparation method of a light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals comprises the following steps:
step 1, adding weathered coal into tap water at the temperature of 30-40 ℃, stirring for 30-40 min, adding calcium peroxide, heating the mixed solution to 80-90 ℃, slowly adding ammonium bicarbonate after 2 h, stirring for 30-40 min, adding urea, stirring for 30-40 min, performing suction filtration, and drying at the temperature of 50-60 ℃ to obtain activated weathered coal rich in fulvic acid;
step 2, mixing the biochar, the ferroferric oxide and the activated weathered coal treated in the step 1 according to the ratio of (2-4): (1-3): (15-30) mixing uniformly according to the mass ratio to obtain mixed powder A;
step 3, adding 10-20 g of the mixed powder A obtained in the step 2 into 50-150 mL of sodium alginate solution to prepare a mixed liquid B;
and 4, slowly dripping the mixed liquid B obtained in the step 3 into an iron chloride solution by using an injector, washing the gel ball for 3-5 times by using deionized water after full reaction, and freeze-drying for 20-24 hours at the temperature of minus 50-minus 60 ℃ to obtain the light-controlled slow-release fulvic acid fertilizer C.
Preferably, the weathered coal in step 1 of the present invention is 10 to 20 g.
Preferably, the amount of tap water added in step 1 of the present invention is 100-150 mL.
Preferably, the calcium peroxide added in step 1 of the present invention is 1 to 2 g.
Preferably, the amount of ammonium bicarbonate added in step 1 of the present invention is 2 to 4 g.
Preferably, 5-8 g of urea is added in step 1 of the present invention.
Preferably, the biochar added in step 2 of the present invention is 50-100 mesh.
Preferably, the ferroferric oxide added in the step 2 of the method is 50-100 meshes.
Preferably, the mass concentration of the sodium alginate solution added in the step 3 of the invention is 1-3%.
Preferably, the mass concentration of the ferric chloride solution added in the step 4 of the invention is 1-3%.
The fulvic acid and the biochar have good adsorption performance and stable chemical properties, can reduce the bioavailability of heavy metals in soil, can be used as a fertilizer to improve the crop yield, has low cost and wide sources, and has obvious advantages and application values in repairing the soil polluted by the heavy metals. The invention utilizes the good photoresponse of the biochar to control the release of the fulvic acid, utilizes the good removal performance of functional groups such as carboxyl, hydroxyl and the like on heavy metal ions, and utilizes ferroferric oxide to carry out magnetic recovery on the carrier, thereby reducing the secondary pollution to the environment.
Drawings
Fig. 1 shows the release amount of fulvic acid in water of the light-controlled slow-release fulvic acid fertilizer under irradiation of different light sources in example 2 of the present invention.
FIG. 2 shows the effect of the optically controlled slow release fulvic acid fertilizer on the concentration of different cationic heavy metals in example 2 of the present invention.
Detailed Description
A preparation method of a light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals comprises the following steps:
step 1, adding 10-20 g of weathered coal into 100-150 mL of tap water at 30-40 ℃, stirring for 30-40 min, adding 1-2 g of calcium peroxide, heating the mixed solution to 80-90 ℃, slowly adding 2-4g of ammonium bicarbonate after 2 h, stirring for 30-40 min, adding 5-8 g of urea, stirring for 30-40 min, performing suction filtration, and drying at 50-60 ℃ to obtain activated weathered coal rich in fulvic acid;
step 2, mixing 50-100 meshes of biochar, 50-100 meshes of ferroferric oxide and the activated weathered coal treated in the step 1 according to the ratio of (2-4): (1-3): (15-30) mixing uniformly according to the mass ratio to obtain mixed powder A;
step 3, adding 10-20 g of the mixed powder A obtained in the step 2 into 50-150 mL of sodium alginate solution with the mass concentration of 1-3% to prepare mixed liquid B;
and 4, slowly dropwise adding the mixed liquid B obtained in the step 3 into a ferric chloride solution with the mass concentration of 1-3% by using an injector, washing the gel spheres for 3-5 times by using deionized water after full reaction, and freeze-drying for 20-24 hours at the temperature of minus 50-minus 60 ℃ to obtain the light-controlled slow-release fulvic acid fertilizer C.
Adding 30-50 mL of Cd-containing light-operated slow-release fulvic acid fertilizer C2+(10-30 mg/L) and Pb2+(10-30 mg/L) in the mixed solution, oscillating (150-170 rpm) for 12-36 h at 20-40 ℃, and measuring the residual Cd in the solution by using an inductively coupled plasma emission spectrometer2+And Pb2+The results show that Cd is present after 60 minutes2+The removal rate reaches 50 to 70 percent, and Pb is removed2+The removal rate reaches 50-60%.
Adding 2-3 g of the light-controlled slow-release fulvic acid fertilizer into 30-50 mL of deionized water, and testing the release amount of fulvic acid under the irradiation of infrared light (an infrared light source of 150- & lt 250 & gt W). The result shows that the release rate of the fulvic acid in the solution is 65-80% after 60 minutes.
And uniformly spreading the obtained light-operated slow-release fulvic acid fertilizer C on the soil surface according to 50-100 kg/mu, and then carrying out rotary tillage, wherein after 30 days, the yield increase of corn, rice and wheat is 60-110 kg/mu, 50-110 kg/mu and 60-120 kg/mu respectively.
Example 1
Step 1, adding 10 g of weathered coal into 100 mL of tap water heated to 30-40 ℃, stirring for 30-40 min, adding 1 g of calcium peroxide, heating the mixed solution to 80-90 ℃, slowly adding 2g of ammonium bicarbonate after 2 h, stirring for 30-40 min, adding 5 g of urea, stirring for 30-40 min, performing suction filtration, and drying at 50-60 ℃ to obtain activated weathered coal rich in fulvic acid;
step 2, mixing 50-100 meshes of biochar, 50-100 meshes of ferroferric oxide and the activated weathered coal treated in the step 1 according to the ratio of (2-4): (1-3): (15-30) mixing uniformly according to the mass ratio to obtain mixed powder A;
step 3, adding 10 g of the mixed powder A obtained in the step 2 into 50mL of sodium alginate solution with the mass concentration of 1% to prepare mixed liquid B;
and 4, slowly dropwise adding the mixed liquid B obtained in the step 3 into a ferric chloride solution with the mass concentration of 1% by using an injector, washing the gel spheres for 3-5 times by using deionized water after full reaction, and freeze-drying for 20-24 hours at the temperature of minus 50-minus 0 ℃ to obtain the light-controlled slow-release fulvic acid fertilizer C.
30 mL of Cd-containing light-operated slow-release fulvic acid fertilizer C obtained in example 1 is added2+(10 mg/L) and Pb2+Oscillating (150-2+And Pb2+The results show that after 60 minutes，Cd2+The removal rate reaches 52 percent, and Pb is removed2+The removal rate reaches 50 percent;
adding 2g of the light-controlled slow-release fulvic acid fertilizer C obtained in the embodiment 1 into 30 mL of deionized water, and testing the release amount of fulvic acid under infrared light irradiation (an infrared light source of 150-; the result shows that after 60 minutes, the release rate of fulvic acid in the solution is 65%;
the light-controlled slow-release fulvic acid fertilizer C obtained in the embodiment 1 is uniformly spread on the soil surface according to 50-100 kg/mu, and then rotary tillage is carried out, wherein after 30 days, the yield increase of corn, rice and wheat is respectively 60 kg/mu, 50 kg/mu and 60 kg/mu.
Example 2
Step 1, adding 15 g of weathered coal into 120 mL of tap water heated to 30-40 ℃, stirring for 30-40 min, adding 1.5 g of calcium peroxide, heating the mixed solution to 80-90 ℃, slowly adding 3g of ammonium bicarbonate after 2 h, stirring for 30-40 min, adding 6 g of urea, stirring for 30-40 min, performing suction filtration, and drying at 50-60 ℃ to obtain activated weathered coal rich in fulvic acid;
step 1, mixing 50-100 mesh biochar, 50-100 mesh ferroferric oxide and the activated weathered coal treated in the step 1 according to the ratio of (2-4): (1-3): (15-30) mixing uniformly according to the mass ratio to obtain mixed powder A;
step 1, adding 15 g of the mixed powder A obtained in the step 2 into 100 mL of sodium alginate solution with the mass concentration of 2% to prepare mixed liquid B;
and step 1, slowly dropwise adding the mixed liquid B obtained in the step 3 into a ferric chloride solution with the mass concentration of 2% by using an injector, washing the gel spheres for 3-5 times by using deionized water after full reaction, and freeze-drying for 20-24 hours at the temperature of minus 50-minus 60 ℃ to obtain the light-controlled slow-release fulvic acid fertilizer C.
As shown in figure 2, 40 mL of Cd-containing light-operated slow-release fulvic acid fertilizer C obtained in example 2 is added2+(10-30 mg/L) and Pb2+Oscillating (150-170 rpm) for 12-36 h at 20-40 ℃ in the (20 mg/L) mixed solution, and measuring the residual Cd in the solution by using an inductively coupled plasma emission spectrometer2+And Pb2+The results show that Cd is present after 60 minutes2+RemovingThe ratio reaches 60 percent, Pb2+The removal rate reaches 55 percent;
as shown in fig. 1, 2.5 g of the light-controlled slow-release fulvic acid fertilizer C obtained in example 2 is added into 30-50 mL of deionized water, and the release amount of fulvic acid is tested under infrared light irradiation (infrared light source 150-; the result shows that after 60 minutes, the release rate of the fulvic acid in the solution is 72 percent;
uniformly spreading the granular fertilizer C obtained in the example 2 on the soil surface according to 50-100 kg/mu, and then carrying out rotary tillage, wherein the yield increase of corn, rice and wheat is 75 kg/mu, 65 kg/mu and 80 kg/mu respectively after 30 days.
Table 1 is the effect of applying the fertilizer prepared in example 2 on the yield of corn, rice and wheat.
TABLE 1
Example 3
Step 1, adding 20 g of weathered coal into 150 mL of tap water heated to 30-40 ℃, stirring for 30-40 min, adding 2g of calcium peroxide, heating the mixed solution to 80-90 ℃, slowly adding 4g of ammonium bicarbonate after 2 h, stirring for 30-40 min, adding 8 g of urea, stirring for 30-40 min, performing suction filtration, and drying at 50-60 ℃ to obtain activated weathered coal rich in fulvic acid;
step 2, mixing 50-100 meshes of biochar, 50-100 meshes of ferroferric oxide and the activated weathered coal treated in the step 1 according to the ratio of (2-4): (1-3): (15-30) mixing uniformly according to the mass ratio to obtain mixed powder A;
step 3, adding 20 g of the mixed powder A obtained in the step 2 into 50-150 mL of sodium alginate solution with the mass concentration of 3% to prepare mixed liquid B;
step 4, slowly dripping the mixed liquid B obtained in the step 3 into a ferric chloride solution with the mass concentration of 3% by using an injector, washing the gel ball for 3-5 times by using deionized water after full reaction, and freeze-drying for 20-24 hours at the temperature of minus 50-minus 60 ℃ to obtain a light-controlled slow-release fulvic acid fertilizer C;
the light-controlled slow-release fulvic acid obtained in the example 3 is usedAdding 30-50 mL of Cd-containing fertilizer C2+(30 mg/L) and Pb2+(30 mg/L) in the mixed solution, oscillating (150-170 rpm) for 12-36 h at 20-40 ℃, and measuring the residual Cd in the solution by using an inductively coupled plasma emission spectrometer2+And Pb2+The results show that Cd is present after 60 minutes2+The removal rate reaches 70 percent, and Pb is removed2+The removal rate reaches 60 percent;
adding 3g of the light-controlled slow-release fulvic acid fertilizer C obtained in the embodiment 3 into 30-50 mL of deionized water, and testing the release amount of fulvic acid under the irradiation of infrared light (an infrared light source of 150-; the result shows that after 60 minutes, the release rate of the fulvic acid in the solution is 80 percent;
the light-controlled slow-release fulvic acid fertilizer C obtained in the embodiment 3 is uniformly spread on the soil surface according to 50-100 kg/mu, and then rotary tillage is carried out, wherein after 30 days, the yield increase of corn, rice and wheat is respectively 105 kg/mu, 110 kg/mu and 120 kg/mu.
Claims (10)
1. A preparation method of a light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals is characterized by comprising the following steps:
step 1, adding weathered coal into tap water at the temperature of 30-40 ℃, stirring for 30-40 min, adding calcium peroxide, heating the mixed solution to 80-90 ℃, slowly adding ammonium bicarbonate after 2 h, stirring for 30-40 min, adding urea, stirring for 30-40 min, performing suction filtration, and drying at the temperature of 50-60 ℃ to obtain activated weathered coal rich in fulvic acid;
step 2, mixing the biochar, the ferroferric oxide and the activated weathered coal treated in the step 1 according to the ratio of (2-4): (1-3): (15-30) mixing uniformly according to the mass ratio to obtain mixed powder A;
step 3, adding 10-20 g of the mixed powder A obtained in the step 2 into 50-150 mL of sodium alginate solution to prepare a mixed liquid B;
and 4, slowly dripping the mixed liquid B obtained in the step 3 into an iron chloride solution by using an injector, washing the gel ball for 3-5 times by using deionized water after full reaction, and freeze-drying for 20-24 hours at the temperature of minus 50-minus 60 ℃ to obtain the light-controlled slow-release fulvic acid fertilizer C.
2. The preparation method of the light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals according to claim 1, wherein the weathered coal in the step 1 is 10-20 g.
3. The method for preparing the light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals according to claim 1, wherein the amount of tap water added in the step 1 is 100-150 mL.
4. The preparation method of the light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals according to claim 1, wherein 1-2 g of calcium peroxide is added in the step 1.
5. The method for preparing the light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals according to claim 1, wherein 2-4g of ammonium bicarbonate is added in the step 1.
6. The method for preparing the light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals according to claim 1, wherein 5-8 g of urea is added in the step 1.
7. The preparation method of the light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals according to claim 1, wherein the biochar added in the step 2 is 50-100 meshes.
8. The preparation method of the light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals according to claim 1, wherein the ferroferric oxide added in the step 2 is 50-100 meshes.
9. The preparation method of the light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals according to claim 1, wherein the mass concentration of the sodium alginate solution added in the step 3 is 1-3%.
10. The preparation method of the light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals according to claim 1, wherein the mass concentration of the ferric chloride solution added in the step 4 is 1-3%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114702360A (en) * | 2022-04-26 | 2022-07-05 | 东华大学 | Soil heavy metal restoration agent, and preparation method and application thereof |
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| CN103408345A (en) * | 2013-06-19 | 2013-11-27 | 中农舜天生态肥业有限公司 | Humic acid synergistic composite fertilizer and preparation method thereof |
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Application publication date: 20210813 |