CN112778048A - Liquid selenium fertilizer rich in marine active ingredients and preparation method thereof - Google Patents
Liquid selenium fertilizer rich in marine active ingredients and preparation method thereof Download PDFInfo
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- CN112778048A CN112778048A CN202110088344.2A CN202110088344A CN112778048A CN 112778048 A CN112778048 A CN 112778048A CN 202110088344 A CN202110088344 A CN 202110088344A CN 112778048 A CN112778048 A CN 112778048A
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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
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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
- 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
- C05G5/00—Fertilisers characterised by their form
- C05G5/20—Liquid fertilisers
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Abstract
The invention belongs to the technical field of selenium fertilizer processing, and particularly relates to a liquid selenium fertilizer rich in marine active ingredients and a preparation method thereof. The liquid selenium fertilizer rich in marine active ingredients comprises deionized water, ascorbic acid solution, sodium selenite solution, seaweed extract and green alga polysaccharide, wherein the volume of the deionized water is the following ratio of the raw materials: volume of ascorbic acid: volume of sodium selenite: weight of seaweed extract: the weight of the green alga polysaccharide is 10: 2: 2: 3.3: 2. the preparation method of the liquid selenium fertilizer rich in the marine active ingredients comprises the following steps: 1) adding the sodium selenite solution into deionized water according to the proportion, stirring, adding the ascorbic acid solution, and stirring to obtain a nano selenium solution; 2) adding the seaweed extract and the green alga polysaccharide into the nano selenium solution according to the proportion in sequence, and stirring uniformly to obtain the liquid selenium fertilizer. The liquid selenium fertilizer prepared by the method has the advantages of good fertilizer efficiency, stable performance, environmental protection and low cost.
Description
Technical Field
The invention belongs to the technical field of selenium fertilizer processing, and particularly relates to a liquid selenium fertilizer rich in marine active ingredients and a preparation method thereof.
Background
The selenium-rich fertilizers are various, and can be divided into inorganic selenium fertilizers and organic selenium fertilizers according to different forms of selenium in the fertilizers; according to different fertilizing modes, the fertilizer can be divided into a leaf selenium-rich fertilizer and a matrix selenium-rich fertilizer; according to different material states, the fertilizer can be divided into solid selenium-rich fertilizer and liquid selenium-rich fertilizer; in addition, there are some new selenium fertilizers, such as: biological selenium-rich fertilizer and nano selenium-rich fertilizer.
The seaweed essence is a black powdery or flaky seaweed fertilizer, and contains various plant essential elements besides alginic acid, which is a natural polysaccharide, such as: nitrogen, potassium, magnesium, calcium, etc.; also contains 18 amino acids which can be directly absorbed and utilized by plants, such as: alanine, arginine, glycine, lysine, glutamic acid, etc.; the seaweed extract can promote the germination of seeds and improve the germination rate; the development of the roots of the plants is promoted, so that the plants can better absorb water and nutrients; the activity of various enzymes in the plant body is improved, and the balanced growth and development of the plant are facilitated; can also enhance the stress resistance of plants, improve the yield of crops and the like. Compared with other fertilizers, the seaweed extract has the advantages of small using amount, good effect, complete nutrition, low cost, safety, environmental protection, no pollution to the environment and no toxic and side effects on human, livestock and poultry, and is an ideal multifunctional seaweed fertilizer.
The green algae polysaccharide is extracted from green algae, has high activity, and has the functions of stabilizing cell wall structure and protecting cell membrane in plant body. The green algae polysaccharide extracted from green algae has wide sources, various types, low toxic and side effects, high safety and various biological activities.
The selenium-rich fertilizer can not only improve the selenium content of crops and improve the nutritional quality, but also reduce the content of heavy metals such as arsenic, lead, cadmium and the like in the crops.
In the preparation process of the liquid selenium fertilizer, the nano selenium solution is required to be prepared firstly, then the fertilizer raw material is added to prepare the liquid selenium fertilizer, and meanwhile, the stabilizer is also required to be added to avoid the nano selenium from being separated out and precipitated easily, so that the preparation process is complex and the cost is high; in addition, sodium dodecyl sulfate, which is a surfactant, is commonly used as a stabilizer in the process of synthesizing the nano-selenium, but the sodium dodecyl sulfate has great pollution to the environment.
How to prepare the liquid selenium fertilizer with good fertilizer efficiency and environmental protection is a problem which needs to be solved urgently in the prior art.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, aims to prepare a stable liquid selenium fertilizer, and provides a liquid selenium fertilizer rich in marine active ingredients and a preparation method thereof.
The technical scheme of the invention is as follows:
the liquid selenium fertilizer rich in marine active ingredients is prepared by mixing the following raw materials, wherein the raw materials comprise deionized water, ascorbic acid solution, sodium selenite solution, seaweed essence and green alga polysaccharide, and the ratio of the raw materials to the raw materials is that the volume of the deionized water, the volume of the ascorbic acid, the volume of the sodium selenite, the weight of the seaweed essence and the weight of the green alga polysaccharide are 10: 2: 3.3: 2.
Preferably, the concentration of the sodium selenite is 0.2 mol/L.
Preferably, the concentration of the ascorbic acid solution is 1.2 mol/L.
The invention also discloses a preparation method of the liquid selenium fertilizer rich in marine active ingredients, which comprises the following steps:
1) adding the sodium selenite solution into deionized water according to the proportion, uniformly stirring, then adding the ascorbic acid solution, and rapidly and uniformly stirring to obtain a nano selenium solution for later use;
2) adding the seaweed extract and the green alga polysaccharide into the nano selenium solution prepared in the step 1) in sequence according to the proportion, and uniformly stirring to obtain the liquid selenium fertilizer.
The invention has the following beneficial effects:
1. according to the invention, the algae essence and the chlorella polysaccharide are applied to the preparation of the nano selenium, and further applied to the preparation of the liquid selenium fertilizer, so that the prepared liquid selenium fertilizer can effectively improve the fertilizer efficiency of the selenium fertilizer while reducing environmental pollution.
2. The liquid selenium fertilizer disclosed by the invention utilizes the seaweed extract and the green alga polysaccharide which do not pollute the environment as fertilizer raw materials, is added into the nano selenium solution to replace sodium dodecyl sulfate which pollutes the environment, also has the effect of a stabilizer, and can keep stable performance at normal temperature and low temperature without using the stabilizer, so that the cost is reduced, and the quality of the liquid selenium fertilizer is ensured.
3. The liquid selenium fertilizer prepared by the invention can increase the selenium content of plants, and has more lasting fertilizer efficiency compared with quick-acting selenium fertilizer.
Drawings
FIG. 1 is a standard curve diagram of fluorescence intensity of a selenium standard solution for measuring selenium content according to the present invention;
FIG. 2 is a diagram showing the change of selenium content in a sample after fertilization in a fertilizer efficiency test of the liquid selenium fertilizer.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The liquid selenium fertilizer rich in marine active ingredients is prepared by mixing the following raw materials, wherein the raw materials comprise deionized water, ascorbic acid solution, sodium selenite solution, seaweed essence and green alga polysaccharide, and the ratio of the raw materials to the raw materials is that the volume of the deionized water, the volume of the ascorbic acid, the volume of the sodium selenite, the weight of the seaweed essence and the weight of the green alga polysaccharide are 10: 2: 3.3: 2; the concentration of the sodium selenite is 0.2 mol/L; the concentration of the ascorbic acid solution is 1.2 mol/L.
The preparation method of the liquid selenium fertilizer rich in marine active ingredients comprises the following steps:
1) adding 0.2mol/L and 2mL of sodium selenite solution into 10mL of deionized water, uniformly stirring, then adding 1.2mol/L and 2mL of ascorbic acid solution, and rapidly and uniformly stirring to obtain nano-selenium solution for later use;
2) adding 3.3g of seaweed extract and 2.0g of green alga polysaccharide into the nano selenium solution prepared in the step 1) in sequence, and stirring uniformly to obtain the liquid selenium fertilizer.
Comparative example 1
Comparative example 1 differs from example 1 in that:
only 3.3g of seaweed extract is added in the step 2) and mixed with the nano selenium solution in the step 1) to prepare nano selenium liquid selenium fertilizer; other technical contents are exactly the same as those of embodiment 1.
Comparative example 2
Comparative example 2 differs from example 1 in that:
only 2.0g of chlorella polysaccharide is added in the step 2) and mixed with the nano selenium solution in the step 1) to prepare nano selenium liquid selenium fertilizer; other technical contents are exactly the same as those of embodiment 1.
Assay analysis
Content determination and analysis of selenium in liquid selenium fertilizer prepared by the method of example 1, comparative example 1 and comparative example 2
1. Pretreatment of
Firstly, digesting liquid fertilizer: and (3) accurately transferring 0.25mL of the liquid selenium fertilizer of the embodiment 1, the comparative example 1 and the comparative example 2 by using a liquid transfer gun respectively, placing the liquid selenium fertilizer into 3 digestion tubes, adding 10mL of nitric acid, covering a preservative film, and performing cold digestion overnight.
Heating the second day graphite electric heating plate to 100 ℃ for reaction for more than 2h, then adjusting the temperature to 120 ℃ for digestion reaction for 1h, cooling for 10-15 min, adding 2mL perchloric acid, continuing digestion reaction for 1h, then adjusting the temperature to 150 ℃ for digestion reaction for 2h, finally adjusting the temperature to 180 ℃ for acid removal until 1mL of the solution remains. 2.5mL of concentrated HCl was added and covered with a preservative film for cold digestion overnight.
Thirdly, on the third day, the sample is moved into a 25mL color comparison tube, is subjected to constant volume to a scale mark by using 10% hydrochloric acid, is diluted by 1000 times, and is tested by using an atomic fluorescence photometer.
Preparing a blank solution: accurately transferring 10mL of nitric acid by using a liquid transfer gun, placing the nitric acid into a digestion tube, covering a preservative film for cold digestion overnight, and then processing according to the second to third steps.
Preparing standard solution: the solution was diluted to 10ng/L per 100-fold with 1000mg/mL of selenium standard solution.
2. Preparation of standard liquid, reducing agent and carrier liquid
Standard solution: the national standard tetravalent selenium standard solution is 1000mg/mL to prepare the mother solution of 10 ng/L.
Reducing agent: weighing 10g KHB4And 2.5g of NaOH in a reducing agent bottle, and the volume is increased to 500 mL.
Carrier fluid: 100ml of concentrated hydrochloric acid is added with deionized water to a volume of 1000ml in a volumetric flask.
3. Determination of selenium content by hydride atomic fluorescence spectrometry
The parameters of the atomic fluorescence photometer used for the measurement are shown in table 1 below.
TABLE 1 Instrument parameters and measurement parameters
| Parameters of the instrument | Parameter value | Measuring parameters | Measured value |
| Negative high pressure | 280V | Time of reading | 12.0s |
| Lamp current | 80mA | Delay time | 3.0s |
| Atomizer temperature | 25℃ | Measurement method | Standard curve method |
| Atomizer altitude | 8mm | Reading mode | Peak area |
| Flow of carrier gas | 300mL/min | Sample introduction volume | 1mL |
| Flow of shield | 800min/min | Sample introduction mode | Automatic |
Respectively putting 0.00mL, 0.10mL, 0.20mL, 0.40mL, 0.60mL, 0.80mL and 10.0mL of selenium standard solution into a 100mL volumetric flask, fixing the volume to the scale with carrier fluid, and uniformly mixing to be measured. The mass concentrations of the selenium standard series solution are respectively 0 mug/L, 1.000 mug/L, 2.000 mug/L, 4.000 mug/L, 6.000 mug/L, 8.000 mug/L and 10.000 mug/L. The fluorescence intensity was measured with an atomic fluorescence spectrometer, and a standard curve was prepared with the mass concentration as the abscissa and the fluorescence intensity as the ordinate. The obtained standard curve equation is IF 146.4086C-10.1467 as shown in the standard graph 1.
The fluorescence intensities measured by an atomic fluorescence spectrometer were respectively IF.
The calculation formula of the selenium content is as follows:
x ═ (fluorescence intensity IF +10.1467)/146.4086 (3.1)
C＝(X*VStator)/(VSample (I)×1000) (3.2)
In the formula:
c is the content (g/L) of selenium in the sample;
x is the mass concentration (mu g/L) of selenium in the sample;
VstatorVolume (mL) for sample volumetric capacity;
Vsample (I)The sample was weighed (mL).
The fluorescence intensity IF was substituted into the formulae (3.1) and (3.2), respectively, to obtain the selenium content in the sample.
The fluorescence intensity measured by atomic fluorescence photometer and the selenium content of the sample calculated therefrom are shown in table 2 below.
TABLE 2 fluorescence intensity and selenium content of the samples
| Example 1 | Comparative example 1 | Comparative example 2 | |
| Fluorescence intensity IF | 1460.571 | 1458.729 | 1364.675 |
| Selenium content (g/L) | 1.005 | 1.003 | 0.939 |
The phenomenon of the sample observed by standing at different temperatures:
at normal temperature, brick red selenium precipitate exists at the bottom of the comparative example 1, and a sample system is unstable; comparative example 2 has a small amount of precipitate, and the use is not affected after shaking up; in example 1, no precipitate was precipitated, and the sample was stable.
At 4 ℃, the bottom of the comparative example 1 precipitates, and the sample system is unstable; comparative example 2 has brick red selenium precipitation at the bottom, selenium gathers, the system can be used after shaking up, but the bottom selenium still sticks to the bottom of the bottle; example 1 had no precipitate and the sample stability was good. In conclusion, the liquid selenium fertilizer prepared by the method is stable under the conditions of normal temperature and low temperature in the embodiment 1, and the liquid selenium fertilizer prepared by the method is good in stability.
Second, fertilizer efficiency test of liquid selenium fertilizer prepared in example 1
In order to verify the fertilizer efficiency of the liquid selenium fertilizer prepared by the invention, an outdoor test is carried out, the liquid selenium fertilizer is applied to plants, the change of the selenium content in the plants before and after the fertilizer application is observed, and whether the increase of the selenium content in the plants is promoted or not is judged.
(1) Test site
Wild Danzhuilin in Pubei county.
(2) Test treatment
Selecting wild Danzhu with uniform growth vigor as a research object, randomly selecting Danzhu and dividing into 9 test cells, wherein the length multiplied by the width of each test cell is 2m multiplied by 2m, and the area is 4m2And the distance of more than 5m is reserved between the cells to prevent the cells from influencing each other. The 9 test cells were divided into three test groups, and the treatment mode of each test group was simultaneous administration of sodium selenite (treatment 1) and realnessThe liquid selenium fertilizer of example 1 (treatment 2) was applied and no selenium fertilizer (treatment 3) was applied, and the test treatment data for each test group is shown in table 3 below.
TABLE 3 test treatment
| Serial number | Treatment of | Selenium application amount | Application method |
| Process 1 | Sodium selenite | 2.4 g/mu |
|
| Treatment | |||
| 2 | Liquid selenium fertilizer | 2.4 g/mu | Watering root |
| Treatment 3 | Control | 0 g/mu | - |
(3) Test method
The Dan bamboo liquid sample is Dan bamboo liquid, the Dan bamboo liquid samples of each test group are respectively taken 12 days, 24 days, 32 days and 42 days after fertilization, the collected Dan bamboo liquid samples are sealed and stored, the Dan bamboo liquid samples are taken back to a laboratory to measure the total selenium content, and the measurement result is shown in figure 2.
In FIG. 2, the abscissa is the number of days after fertilization in days and the ordinate is the selenium content of the sample in mg/Kg.
From fig. 2, the selenium content of the danzhu liquor samples corresponding to different test points and each treatment group is summarized as shown in table 4 below.
TABLE 4 selenium content in samples at various time points after fertilization of different treatment groups
As can be seen from the data in fig. 2 and table 4, at 12 days after fertilization, the selenium content of the sample was effectively increased by the application of sodium selenite and increased by the application of liquid selenium fertilizer, compared to the blank control. At 24 days, 32 days and 42 days after fertilization, the selenium content of the samples was increased by the application of sodium selenite, which was the most increased by the application of liquid selenium fertilizer, compared to the blank control.
With the increase of the fertilizing days, the selenium content of the treatment 3 has small fluctuation and is basically stabilized within a certain range. The selenium content of the treated sample 1 showed a downward trend, sodium selenite was a quick-acting selenium fertilizer, and the selenium content of the sample reached the highest value within 12 days after the fertilizer application. The selenium content in the treatment 2 is in a trend of increasing firstly and then decreasing, and the possible reason is that the peak value of the release of the liquid selenium fertilizer is reached in about 24 days after the fertilization, and then the release is gradually slowed down. After 24 days, the selenium content of treatment 1 was higher than that of treatment 3 and lower than that of treatment 2 as the number of fertilizing days increased.
According to the analysis of experimental results, the sodium selenite and the liquid selenium fertilizer can promote the increase of the selenium content of the sample, and show certain fertilizer efficiency. Sodium selenite, as a quick-acting fertilizer, loses the fertilizer effect in a short time and needs to be applied continuously to maintain the fertilizer effect. Compared with sodium selenite, the liquid selenium fertilizer has relatively longer onset time and fertilizer efficiency time after fertilization.
According to the invention, the algae essence and the chlorella polysaccharide are applied to the preparation of the nano selenium, and further applied to the preparation of the liquid selenium fertilizer, so that the prepared liquid selenium fertilizer can effectively improve the fertilizer efficiency of the selenium fertilizer while reducing environmental pollution.
The liquid selenium fertilizer disclosed by the invention utilizes the seaweed extract and the green alga polysaccharide which do not pollute the environment as fertilizer raw materials, is added into the nano selenium solution to replace sodium dodecyl sulfate which pollutes the environment, also has the effect of a stabilizer, and can keep stable performance at normal temperature and low temperature without using the stabilizer, so that the cost is reduced, and the quality of the liquid selenium fertilizer is ensured.
The liquid selenium fertilizer prepared by the invention can increase the selenium content of plants, and has more lasting fertilizer efficiency compared with quick-acting selenium fertilizer.
Claims (4)
1. The liquid selenium fertilizer rich in marine active ingredients is characterized in that: the seaweed polysaccharide is prepared by mixing the following raw materials, wherein the raw materials comprise deionized water, ascorbic acid solution, sodium selenite solution, seaweed extract and chlorella polysaccharide, and the volume of the deionized water is the ratio of the raw materials to the raw materials: volume of ascorbic acid: volume of sodium selenite: weight of seaweed extract: the weight of the green alga polysaccharide is 10: 2: 2: 3.3: 2.
2. the liquid selenium fertilizer rich in marine active ingredients as claimed in claim 1, wherein: the concentration of the sodium selenite is 0.2 mol/L.
3. The liquid selenium fertilizer rich in marine active ingredients as claimed in claim 1, wherein: the concentration of the ascorbic acid solution is 1.2 mol/L.
4. The method for preparing liquid selenium fertilizer rich in marine active ingredients as claimed in any one of claims 1 to 3, comprising the steps of:
1) adding the sodium selenite solution into deionized water according to the proportion, uniformly stirring, then adding the ascorbic acid solution, and rapidly and uniformly stirring to obtain a nano selenium solution for later use;
2) adding the seaweed extract and the green alga polysaccharide into the nano selenium solution prepared in the step 1) in sequence according to the proportion, and uniformly stirring to obtain the liquid selenium fertilizer.
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Cited By (2)
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| CN115259938A (en) * | 2022-07-14 | 2022-11-01 | 华南农业大学 | Seaweed selenium fertilizer and preparation method, use method and application thereof |
| CN115259957A (en) * | 2022-06-29 | 2022-11-01 | 河北工业大学 | Preparation method and application of blue algae-based carbon quantum dot nano selenium fertilizer |
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| CN115259957A (en) * | 2022-06-29 | 2022-11-01 | 河北工业大学 | Preparation method and application of blue algae-based carbon quantum dot nano selenium fertilizer |
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Application publication date: 20210511 |