CN111470915B - Long-acting water-soluble iron fertilizer and preparation method thereof - Google Patents
Long-acting water-soluble iron fertilizer and preparation method thereof Download PDFInfo
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- CN111470915B CN111470915B CN202010526767.3A CN202010526767A CN111470915B CN 111470915 B CN111470915 B CN 111470915B CN 202010526767 A CN202010526767 A CN 202010526767A CN 111470915 B CN111470915 B CN 111470915B
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
- C05D9/02—Other inorganic fertilisers containing trace elements
Abstract
A long-acting water-soluble iron fertilizer and a preparation method thereof relate to the field of fertilizers. The preparation method of the long-acting water-soluble iron fertilizer suitable for the acid soil comprises the following steps: mixing graphene oxide and soluble ferrous salt in a solution system, and carrying out coprecipitation under an alkaline condition to obtain a composite product; and oxidizing the composite product. The iron fertilizer prepared by the preparation method is water-soluble, can be fully dispersed in water to form a suspension water-soluble fertilizer, and after the iron fertilizer is applied to soil, compared with iron ions in the soil, the iron oxide loaded on the graphene oxide is not easy to wash away by rainwater, and under the corrosion of acid soil, the iron oxide is gradually corroded into the iron ions to be absorbed by plants, so that the aims of long-acting slow release and water solubility of the iron fertilizer are effectively fulfilled, and the application frequency of the iron fertilizer is reduced.
Description
Technical Field
The application relates to the field of fertilizers, in particular to a long-acting water-soluble iron fertilizer and a preparation method thereof.
Background
Pineapple belongs to the genus of pineapple of the family of bromeliaceae, is a perennial herb, is one of the most influential fruits in tropical and subtropical zones, and is mainly planted in tropical areas of south China. Soil in a pineapple main production area is mostly brick red soil, is acidic to strong acidic, and has high iron content, but the pineapple is a herbaceous plant sensitive to manganese, and the high acidity causes manganese toxicity, so that the absorption of iron ions by the pineapple is seriously influenced, and the phenomenon of iron deficiency of the pineapple is commonly caused.
The existing solutions are mostly researches on foliage spraying of soluble ferric salts, such as 'foliage spraying of Mg, Fe and Zn influences the growth and yield of pineapples, tropical agricultural science, volume 32, stage 6 and page numbers 4-6', and the researches show that after foliage spraying of ferrous sulfate, the yield, the single fruit weight and the commodity fruit rate of pineapples are improved. However, in tropical and subtropical regions, rainwater is abundant, iron ions are easy to be leached with water, the effect is extremely unstable after the iron fertilizer is applied, and the iron fertilizer needs to be continuously applied to meet the growth requirement, so that the method is time-consuming and labor-consuming.
Disclosure of Invention
The present application provides a long-acting water-soluble iron fertilizer and a preparation method thereof, which can effectively solve at least one technical problem described above.
In a first aspect, an embodiment of the present application provides a method for preparing a long-acting water-soluble iron fertilizer suitable for acidic soil, including:
mixing graphene oxide and soluble ferrous salt in a solution system, and carrying out coprecipitation under an alkaline condition to obtain a composite product.
And oxidizing the composite product.
In the implementation process, the graphene oxide and the soluble ferrous salt are subjected to liquid-phase chemical coprecipitation under an alkaline condition, so that iron oxide formed by ferrous ions is loaded on the graphene oxide to prepare a composite product, the original composite product with a positive potential is provided with a negative potential through further oxidation of the composite product (hereinafter, the step is referred to as secondary oxidation), and a long-acting water-soluble iron fertilizer which can be fully dispersed in water and form a suspension water-soluble fertilizer is obtained, after the long-acting water-soluble iron fertilizer is applied to soil along with water, compared with iron ions in the soil, the iron oxide loaded on the graphene oxide is not easily washed away by rainwater, and under the corrosion of acid soil, the iron oxide loaded on the surface of the graphene oxide is gradually corroded into the iron ions to be absorbed by plants, so that the purposes of long-acting slow release and water solubility of the iron fertilizer are effectively achieved, and effectively reduces the application times of the iron fertilizer.
In one possible embodiment, the weight ratio of graphene oxide to soluble ferrous salt is from 1:1 to 20: 1.
Optionally, the weight ratio of the graphene oxide to the soluble ferrous salt is 9:1-12: 1.
In the implementation process, the iron oxide is effectively ensured to be loaded on the graphene oxide by the reasonable proportion of the graphene oxide and the soluble ferrous salt.
In one possible embodiment, mixing graphene oxide and a soluble ferrous salt in a solution system comprises:
and mixing the graphene oxide dispersion liquid with a soluble ferrite solution, or mixing the graphene oxide dispersion liquid with a soluble ferrite.
Optionally, the concentration of graphene oxide in the graphene oxide dispersion is 0.1-10 mg/mL.
In the implementation process, the graphene oxide dispersion liquid is introduced to ensure that the iron oxide can be uniformly loaded on the surface of the graphene oxide.
In one possible embodiment, the graphene oxide comprises graphene oxide sheets, the graphene oxide sheets having a size of no more than 1 μm.
In the implementation process, the size of the graphene oxide sheet is not more than 1 μm, so that the obtained composite product is small in size, not only can effectively adsorb iron oxide, but also is convenient to suspend in water in the later period.
In one possible embodiment, the co-precipitation under basic conditions comprises: adjusting pH to 9-11 with alkali, and heating at 60-100 deg.C for 2-8 h.
Alternatively, the base comprises ammonia, sodium hydroxide or potassium hydroxide.
In one possible embodiment, the step of oxidizing the composite product comprises:
mixing the composite product with oxidant water solution, heating to 30-80 deg.C, and oxidizing for 5-50 min.
Optionally, the oxidizing agent comprises hydrogen peroxide. Wherein the addition of hydrogen peroxide does not introduce impurities.
Optionally, the composite product is washed with water before being oxidized to remove excess alkali on the surface. It should be noted that, when the alkali used in the co-precipitation step is sodium hydroxide or potassium hydroxide, the obtained composite product (iron oxide/graphene oxide composite material) is washed twice more than the composite product obtained when the alkali is ammonia water, and then the subsequent secondary oxidation step is performed.
In one possible embodiment, the method for preparing graphene oxide includes: the graphene oxide is prepared by chemically stripping graphite to obtain graphene oxide, ultrasonically stripping the graphene oxide, oxidizing the graphene oxide, and ultrasonically crushing the graphene oxide.
Optionally, ultrasonic stripping is performed at 20-800W for 2-60 min.
In the implementation process, the flaky graphene oxide is obtained through ultrasonic stripping, the oxidation degree of the graphene oxide is improved through oxidation, and the particle size of the graphene oxide can be effectively reduced through ultrasonic crushing.
In a second aspect, an embodiment of the present application provides a long-acting water-soluble iron fertilizer, which is prepared by the preparation method of the long-acting water-soluble iron fertilizer provided in the first aspect of the present application, wherein the long-acting water-soluble iron fertilizer can be dispersed in water to form a suspension.
In the implementation process, the long-acting water-soluble iron fertilizer prepared by the preparation method provided by the first aspect can be dispersed in water to form a suspension water-soluble iron fertilizer, and after the long-acting water-soluble iron fertilizer is applied to soil, compared with iron ions in the soil, iron oxide loaded on graphene oxide is not easily washed away by rainwater, and under the corrosion of acid soil, the iron oxide is gradually corroded into the iron ions to be absorbed by plants, so that the purposes of long-acting slow release and water solubility of the iron fertilizer are effectively achieved, the application times of the iron fertilizer are reduced, and meanwhile, the solid long-acting water-soluble iron fertilizer is small in size and convenient to transport and can be mixed with water when in use.
In a possible embodiment, the dosage of the long-acting water-soluble iron fertilizer is not less than 1.1 kg/mu calculated by the iron element.
In one possible embodiment, the application means comprises drip irrigation.
In the implementation process, as most of the soil in the pineapple planting field is acidic and more rainwater is generated, the purposes of long-acting slow release and water solubility of the iron fertilizer are effectively achieved by applying the long-acting water-soluble iron fertilizer, the application times of the iron fertilizer are reduced, the labor cost is reduced, and the utilization rate of the fertilizer is effectively improved in a drip irrigation mode.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained from the drawings without inventive effort.
Fig. 1 is an SEM image of graphene oxide sheets prepared in example 1;
FIG. 2 is a photograph of a composite product obtained in example 1 mixed with water;
FIG. 3 is an XPS spectrum of carbon in the composite product of example 1 prior to secondary oxidation;
FIG. 4 is an XPS spectrum of carbon in the composite product after secondary oxidation in example 1;
FIG. 5 is a TEM image of the long-acting water-soluble iron fertilizer prepared in example 1;
FIG. 6 is a photograph of the suspended liquid iron fertilizer prepared in example 1.
Detailed Description
Embodiments of the present application will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present application and should not be construed as limiting the scope of the present application. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The water-soluble iron fertilizer means that the obtained iron fertilizer can be suspended in water to form a suspended liquid fertilizer.
The application provides a preparation method of a long-acting water-soluble iron fertilizer suitable for acid soil, which comprises the following steps:
s1, obtaining graphene oxide.
Wherein the graphene oxide comprises graphene oxide sheets, the graphene oxide sheets having a size of not more than 1 μm.
For example, the graphene oxide sheets can have a size of 50nm to 1 μm, alternatively, the graphene oxide sheets can have a size of 100nm to 1 μm.
Among them, the graphene oxide sheet may be purchased directly from the market, or may be prepared by a chemical exfoliation method (including a Brodie method, a staudenmier method, or a Hummers method) by itself, as long as the above size requirements are satisfied.
Optionally, the preparation method of graphene oxide comprises: the graphene oxide is prepared by chemically stripping graphite to obtain graphene oxide, ultrasonically stripping the graphene oxide, oxidizing the graphene oxide, and then ultrasonically crushing the graphene oxide.
Wherein the graphite comprises one or more of natural graphite, thermal cracking graphite and expanded graphite, and is selected from natural graphite, and the chemical stripping method comprises Brodie method, Staudenmaier method or Hummers method.
Optionally, the ultrasonic peeling is performed at 20-800W, for example, at 200W, 300W, 500W, 600W, 700W, 800W, or the like for 2-60min, which effectively peels the graphene oxide into sheets.
And oxidizing the graphene oxide after ultrasonic stripping, wherein the oxidation can be carried out for 5-60min by using a Hummers method, the oxidation degree of the last graphene oxide sheet is effectively ensured, and finally, the size of the graphene oxide sheet is reduced to be not more than 1 mu m through ultrasonic crushing.
S2, obtaining soluble ferrous salt.
The soluble ferrous salt includes but is not limited to ferrous chloride, and may also be ferrous sulfate, or a mixture of ferrous chloride and ferrous sulfate.
And S3, mixing the graphene oxide and the soluble ferrous salt in a solution system, and carrying out coprecipitation under an alkaline condition to obtain a composite product.
The weight ratio of the graphene oxide to the soluble ferrous salt is 1:1-20:1, for example, the weight ratio of the graphene oxide to the soluble ferrous salt is 1:1, 3:1, 6:1, 9:1, 10:1, 13:1, or 15:1, 17:1, and the like.
Optionally, the weight ratio of the graphene oxide to the soluble ferrous salt is 9: 1-12: 1.
the mixing of the graphene oxide and the soluble ferrous salt in the solution system includes, but is not limited to, adding the graphene oxide and the soluble ferrous salt into a solution, such as water, respectively, and mixing.
Optionally, mixing the graphene oxide and the soluble ferrous salt in a solution system comprises: and mixing the graphene oxide dispersion liquid with a soluble ferrite solution, or mixing the graphene oxide dispersion liquid with the soluble ferrite, so as to ensure the uniformity of the load, wherein the solvents of the graphene oxide dispersion liquid and the soluble ferrite solution are both water.
Alternatively, the concentration of graphene oxide in the graphene oxide dispersion is 0.1-10mg/mL, for example, 0.1mg/mL, 1mg/mL, 3mg/mL, 5mg/mL, 7mg/mL, or 9mg/mL, and the like.
Alternatively, co-precipitating under basic conditions comprises: adjusting pH value of the solution system to 9-11 with alkali, and heating at 60-100 deg.C for 2-8 h.
The alkali includes ammonia water, and the alkali may be sodium hydroxide, potassium hydroxide, or the like, in addition to ammonia water.
S4, oxidizing the composite product.
Optionally, the composite product is water washed at least once before oxidation of the composite product.
Optionally, the step of oxidizing the composite product comprises: mixing the composite product with oxidant water solution, heating to 30-80 deg.C, and oxidizing for 5-50 min.
Wherein the oxidizing agent is, for example, potassium permanganate, hydrogen peroxide, and the like, and optionally, the oxidizing agent comprises hydrogen peroxide. The oxidized composite product can be suspended in water by oxidizing the composite product, and the magnetism of the iron oxide is reduced, so that the long-acting water-soluble iron fertilizer is prevented from being agglomerated.
The application provides a long-acting water-soluble iron fertilizer which is prepared by the preparation method of the long-acting water-soluble iron fertilizer, wherein the long-acting water-soluble iron fertilizer can be dispersed in water to form a suspension.
It is noted that the long-acting water-soluble iron fertilizer provided by the application is suitable for acid soil.
Wherein the dosage of the long-acting water-soluble iron fertilizer is not less than 1.1 kg/mu calculated according to the iron element.
Optionally, the fertilizing means of the long-acting water-soluble iron fertilizer comprises drip irrigation.
Example 1
1. Graphene oxide is prepared from natural graphite by a Hummers method, and the graphene oxide is subjected to ultrasonic peeling at 300W for 30 min.
2. And (3) oxidizing the product obtained in the step 1 by using a Hummers method for 15 min.
3. And (3) carrying out ultrasonic crushing on the product obtained in the step (2) to obtain graphene oxide sheets with the size of less than 1 mu m, wherein an SEM image of the obtained graphene oxide sheets is shown in figure 1.
4. And (3) mixing the graphene oxide sheets obtained in the step (3) with water to obtain 0.5mg/mL graphene oxide sheet dispersion liquid, mixing the graphene oxide sheet dispersion liquid with ferrous chloride (the weight of the ferrous chloride and the graphene oxide sheets is 10:1), adjusting the pH value to 11 with ammonia water, heating at 80 ℃ for 5 hours to obtain a composite product, and filtering and washing the composite product for three times.
Wherein, the composite product is mixed with water and placed in a transparent bottle for observation, as shown in figure 2, the composite product is obviously layered with the water, wherein the dark part is the composite product.
5. An XPS spectrum of the carbon element in the water-washed composite product is obtained as a graph 3, the water-washed composite product is mixed with hydrogen peroxide with the mass concentration of 10%, the mixture is heated to 50 ℃ and oxidized for 20min to obtain the long-acting water-soluble iron fertilizer suitable for the acid soil, the XPS spectrum of the carbon element in the hydrogen peroxide-oxidized composite product (namely, the long-acting water-soluble iron fertilizer) is obtained as a graph 4, and a TEM image of the long-acting water-soluble iron fertilizer as shown in a graph 5 is obtained at the same time.
In addition, comparing fig. 3 and fig. 4, it can be seen that the oxygen-containing groups of the composite product after the oxidation treatment are effectively increased. The black particles in fig. 5 are ferrite, and it can be seen that the ferrite particles are distributed more uniformly on the graphene oxide sheet.
The element content of the long-acting water-soluble iron fertilizer obtained in example 1 was measured, and the element content data (mass fraction) of the long-acting water-soluble iron fertilizer is shown in table 1.
TABLE 1 elemental content data (mass fraction)
The long-acting water-soluble iron fertilizer prepared in example 1 was mixed with water and placed in a transparent bottle to obtain a suspension liquid iron fertilizer as shown in fig. 6, and it can be seen from fig. 6 that the long-acting water-soluble iron fertilizer was uniformly dispersed in water to form a suspension.
The Zeta potential analyzer is used for measuring the Zeta potential of the long-acting water-soluble iron fertilizer, and the Zeta potential of the long-acting water-soluble iron fertilizer is shown in table 2.
TABLE 2 Zeta potential of long-acting water-soluble iron fertilizer
| Zeta potential | |
| Long-acting water-soluble iron fertilizer | -58.20mV |
According to the table 2, it can be seen that the long-acting water-soluble iron fertilizer has good dispersibility and can form stable suspension.
Example 2
1. Preparing graphene oxide from the thermally cracked graphite by a Hummers method, and ultrasonically stripping the graphene oxide at 500W for 35 min.
2. And (2) oxidizing the product obtained in the step 1 by using a Hummers method for 20 min.
3. And (3) carrying out ultrasonic crushing on the product obtained in the step (2) to obtain the graphene oxide sheet with the size of less than 1 mu m.
4. And (3) mixing the graphene oxide sheets obtained in the step (3) with water to obtain 1mg/mL graphene oxide sheet dispersion liquid, mixing the graphene oxide sheet dispersion liquid with ferrous chloride (the weight of the ferrous chloride and the graphene oxide sheets is 10:1), adjusting the pH value to 11 with ammonia water, heating at 85 ℃ for 5 hours to obtain a composite product, filtering the composite product and washing with water for three times.
5. And mixing the washed composite product with hydrogen peroxide with the mass concentration of 10%, heating to 50 ℃, and oxidizing for 20min to obtain the long-acting water-soluble iron fertilizer suitable for the acid soil.
Example 3
1. Preparing graphene oxide from natural graphite by a Hummers method, and ultrasonically stripping the graphene oxide at 600W for 30 min.
2. And (3) oxidizing the product obtained in the step 1 by using a Hummers method for 25 min.
3. And (3) carrying out ultrasonic crushing on the product obtained in the step (2) to obtain a graphene oxide sheet with the size of less than 1 mu m.
4. And (3) mixing the graphene oxide sheets obtained in the step (3) with water to obtain 5mg/mL graphene oxide sheet dispersion liquid, mixing the graphene oxide sheet dispersion liquid with ferrous chloride (the weight of the ferrous chloride and the graphene oxide sheets is 3:1), adjusting the pH value to 10 by using ammonia water, heating for 7 hours at 70 ℃ to obtain a composite product, filtering the composite product and washing for three times.
5. And mixing the washed composite product with hydrogen peroxide with the mass concentration of 10%, heating to 55 ℃, and oxidizing for 20min to obtain the long-acting water-soluble iron fertilizer suitable for the acid soil.
Example 4
1. Graphene oxide is prepared from natural graphite by a Hummers method, and the graphene oxide is subjected to ultrasonic peeling at 800W for 20 min.
2. And (3) oxidizing the product obtained in the step 1 by using a Hummers method for 15 min.
3. And (3) carrying out ultrasonic crushing on the product obtained in the step (2) to obtain a graphene oxide sheet with the size of less than 1 mu m.
4. And (3) mixing the graphene oxide sheets obtained in the step (3) with water to obtain 0.1mg/mL graphene oxide sheet dispersion liquid, mixing the graphene oxide sheet dispersion liquid with ferrous chloride (the weight of the ferrous chloride and the graphene oxide sheets is 12:1), adjusting the pH value to 10 by using ammonia water, heating at 100 ℃ for 4 hours to obtain a composite product, filtering the composite product and washing for three times.
5. And mixing the washed composite product with hydrogen peroxide with the mass concentration of 10%, heating to 60 ℃, and oxidizing for 30min to obtain the long-acting water-soluble iron fertilizer suitable for the acid soil.
Example 5
A suspended liquid iron fertilizer, which comprises water and the long-acting water-soluble iron fertilizer provided by any one of embodiments 1 to 4, wherein the long-acting water-soluble iron fertilizer is dispersed in the water to form a suspension.
Test examples
In the acid brick red soil in the area of the Leizhou peninsula, the same pineapple varieties are adopted as a test group, a control group 1 and a control group 2, and during the period from the pineapple field planting (8 months in the current year) to the pineapple harvesting (3 months in the third year), the field management, the planting density and the like of the control group 1, the control group 2 and the test group are the same, and the differences are only that:
the test group applied the long-acting water-soluble iron fertilizer provided in example 1 once in the 3 rd month after the pineapple field planting in the following manner: the fertilizer is applied to the soil near the root of the pineapple by adopting a drip irrigation technology, wherein the dosage of the long-acting water-soluble iron fertilizer is 4.4 kg/mu.
Control group 2 was fertilized by the usual means: 4 times of iron fertilizer is sprayed on the leaf surfaces every year, 0.5 kg/mu of ferrous sulfate is applied after 0-3 months of field planting, 0.5 kg/mu of ferrous sulfate is applied after 4-8 months of field planting, 1 kg/mu of ferrous sulfate is applied after 9-10 months of field planting, and 1 kg/mu of ferrous sulfate is applied after 11-12 months of field planting.
The yields, commercial fruit yields and soluble solids, vitamin C and titratable acid contents of the pineapple fruits obtained from the control group 1, the control group 2 and the test group were determined according to the method provided by the experimental technical procedure part 8, pineapple, of the variety of tropical crops NY/T2668.8-2018, and the results are shown in table 3.
TABLE 3 test results
From table 3, it can be seen that, although the soluble solids content of the test group was slightly lower than that of the control group 2 under the condition of the equivalent application amount of the iron element, the yield of the test group was 2.6% higher than that of the control group 2, and the commercial fruit rate was increased by 2%, and it can be seen that the vitamin C content was slightly lower than that of the control group 1 without applying the iron fertilizer, and the vitamin C content in the test group was significantly increased by applying the fertilizer to the control group 2.
That is to say, the long-acting water-soluble iron fertilizer provided by the application can promote the increase of the pineapple yield, the quality is not reduced, the purposes of long-acting slow release and water solubility of the iron fertilizer are realized, the application times of the iron fertilizer are reduced, and the labor cost is saved.
In summary, the preparation method of the long-acting water-soluble iron fertilizer provided by the application has controllable operation, and by liquid-phase chemical coprecipitation, ferrous ions form iron oxide and are loaded on graphene oxide to form a composite product, and by secondary oxidation of the composite product, the prepared long-acting water-soluble iron fertilizer can be fully dispersed in water to form a suspended liquid iron fertilizer, and after the suspended liquid iron fertilizer is applied to soil along with water, compared with iron ions in soil, the iron oxide loaded on the graphene oxide is not easily washed away by rainwater, and under the corrosion of acid soil, the iron oxide is gradually corroded into iron ions to be absorbed by plants, so that the purposes of long-acting slow release and water solubility of the iron fertilizer are effectively realized, and the application times of the iron fertilizer are reduced.
The foregoing is merely exemplary of the present application and is not intended to limit the present application, which may be modified or varied by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (13)
1. A preparation method of a long-acting water-soluble iron fertilizer suitable for acid soil is characterized by comprising the following steps:
mixing graphene oxide and soluble ferrous salt in a solution system, and carrying out coprecipitation under an alkaline condition to obtain a composite product;
oxidizing the composite product to enable the composite product to be suspended in water;
wherein the co-precipitation under basic conditions comprises: adjusting pH to 9-11 with alkali, and heating at 60-100 deg.C for 2-8 hr;
the step of oxidizing the composite product comprises: mixing the composite product with an aqueous solution of an oxidant, heating to 30-80 ℃, and oxidizing for 5-50min, wherein the oxidant comprises hydrogen peroxide.
2. The preparation method of the long-acting water-soluble iron fertilizer as claimed in claim 1, wherein the weight ratio of the graphene oxide to the soluble ferrous salt is 1:1-20: 1.
3. The preparation method of the long-acting water-soluble iron fertilizer as claimed in claim 1, wherein the weight ratio of the graphene oxide to the soluble ferrous salt is (9: 1-12): 1.
4. The method for preparing the long-acting water-soluble iron fertilizer according to claim 1, wherein mixing the graphene oxide and the soluble ferrous salt in a solution system comprises:
and mixing the graphene oxide dispersion liquid with a soluble ferrite solution, or mixing the graphene oxide dispersion liquid with the soluble ferrite.
5. The preparation method of the long-acting water-soluble iron fertilizer as claimed in claim 4, wherein the concentration of the graphene oxide in the graphene oxide dispersion liquid is 0.1-10 mg/mL.
6. The method for preparing the long-acting water-soluble iron fertilizer according to any one of claims 1 to 5, wherein the graphene oxide comprises graphene oxide sheets, and the size of the graphene oxide sheets is not more than 1 μm.
7. The method for preparing the long-acting water-soluble iron fertilizer as claimed in claim 1, wherein the alkali comprises ammonia water, sodium hydroxide or potassium hydroxide.
8. The method for preparing the long-acting water-soluble iron fertilizer as claimed in claim 1, wherein the composite product is washed with water before being oxidized.
9. The preparation method of the long-acting water-soluble iron fertilizer as claimed in claim 1, wherein the preparation method of the graphene oxide comprises the following steps: the graphene oxide is prepared by chemically stripping graphite to obtain graphene oxide, ultrasonically stripping the graphene oxide, oxidizing the graphene oxide, and ultrasonically crushing the graphene oxide.
10. The method for preparing the long-acting water-soluble iron fertilizer as claimed in claim 9, wherein the ultrasonic peeling is performed for 2-60min under the condition of 20-800W.
11. A long-acting water-soluble iron fertilizer prepared by the method for preparing the long-acting water-soluble iron fertilizer according to any one of claims 1 to 10, wherein the long-acting water-soluble iron fertilizer can be dispersed in water to form a suspension.
12. The long-acting water-soluble iron fertilizer according to claim 11, wherein the amount of the long-acting water-soluble iron fertilizer is not less than 1.1 kg/mu calculated as the iron element.
13. The long-acting water-soluble iron fertilizer according to claim 11 or 12, wherein the long-acting water-soluble iron fertilizer is applied by drip irrigation.
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| CN105503441A (en) * | 2016-01-15 | 2016-04-20 | 武汉理工大学 | Method for preparing slow-release iron fertilizer through ferrous sulfate |
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