CN112759456A - Solid selenium fertilizer and preparation method thereof - Google Patents
Solid selenium fertilizer and preparation method thereof Download PDFInfo
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- CN112759456A CN112759456A CN202110088362.0A CN202110088362A CN112759456A CN 112759456 A CN112759456 A CN 112759456A CN 202110088362 A CN202110088362 A CN 202110088362A CN 112759456 A CN112759456 A CN 112759456A
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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
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D3/00—Calcareous fertilisers
- C05D3/02—Calcareous fertilisers from limestone, calcium carbonate, calcium hydrate, slaked lime, calcium oxide, waste calcium products
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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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Abstract
The invention discloses a solid selenium fertilizer, which comprises distilled water, a sodium selenite solution, an ascorbic acid solution, shell powder and oyster shell powder, wherein the volume of the distilled water is as follows: volume of sodium selenite solution: volume of ascorbic acid solution: weight of shell powder: the weight of fresh oyster shell powder is 9: 2: 2: 5: 5. the invention also discloses a preparation method of the solid selenium fertilizer, which comprises the following steps: 1) adding the sodium selenite solution into distilled water, stirring, then adding the ascorbic acid solution, and uniformly stirring to obtain a mixed solution; 2) uniformly mixing shell powder and fresh oyster shell powder, pouring the shell powder into the mixed solution obtained in the step 1), stirring, and standing; 3) standing, precipitating the shell powder until supernatant is clear and colorless, performing suction filtration, and placing the solid shell powder in a tray for uniform dispersion; 4) and (4) putting the tray into a baking oven for drying to obtain the light pink solid selenium fertilizer. The solid selenium fertilizer provided by the invention is simple in preparation process, lasting in fertilizer efficiency and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of selenium fertilizer processing, and particularly relates to a solid selenium fertilizer and a preparation method thereof.
Background
Selenium has various biological effects, and has remarkable effects in scavenging free radicals, resisting tumor and cancer, and diseases such as keshan disease and cardiovascular disease caused by selenium deficiency. Soil surveys show that about 72% of the regions in china are selenium-deficient and low-selenium regions. Insufficient selenium intake can seriously impact the human's life health. Selenium supplement is a great event affecting the health of hundreds of millions of people, and regular use of agricultural products rich in selenium is the best method for supplementing selenium for human beings.
The selenium supplement can be started from dietary supplies of people, the selenium content in crops is increased through the use of the selenium-rich fertilizer, and people can absorb the absorbable selenium through heavy enrichment of a food chain, so that the selenium content of the people is increased.
The selenium-rich fertilizer comprises liquid selenium fertilizer and solid selenium fertilizer, and the existing solid selenium fertilizer has the defects of high raw material cost and poor fertilizer efficiency.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a solid selenium fertilizer and a preparation method thereof.
The technical scheme of the invention is as follows:
the solid selenium fertilizer is prepared by mixing the following raw materials, including distilled water, a sodium selenite solution, an ascorbic acid solution, shell powder and oyster shell powder, wherein the volume of the distilled water is the ratio of the raw materials: volume of sodium selenite solution: volume of ascorbic acid solution: weight of shell powder: the weight of fresh oyster shell powder is 9: 2: 2: 5: 5.
preferably, the concentration of the sodium selenite solution is 0.2M/L.
Preferably, the concentration of the ascorbic acid solution is 1.2M/L.
The invention also discloses a preparation method of the solid selenium fertilizer, which comprises the following steps:
1) adding the sodium selenite solution into distilled water according to the proportion, uniformly stirring, then adding the ascorbic acid solution, and rapidly and uniformly stirring to obtain a mixed solution, wherein the solution is rapidly changed into brick red;
2) uniformly mixing shell powder and oyster shell powder according to a ratio, slowly pouring the uniformly mixed shell powder into the mixed solution obtained in the step 1), stirring while pouring until the mixture is uniformly stirred, wherein the mixed solution is orange red, and then standing;
3) standing, gradually precipitating the shell powder until supernatant is clear and colorless, then performing suction filtration, separating the filtrate from the solid shell powder, and uniformly dispersing the solid shell powder in a clean tray;
4) and (3) putting the tray filled with the solid shell powder into a baking oven for drying to obtain the light pink solid selenium fertilizer.
Preferably, the drying temperature in the step 4) is 38-45 ℃.
The preparation method of the shell powder and the fresh oyster shell powder comprises the following steps:
5) cleaning shells and fresh oyster shells, draining, respectively breaking, and placing into a drying oven for air blowing and drying;
6) crushing the crushed and dried shells and fresh oyster shells into powder by using a crusher respectively, and then sieving the powder by using a 60-mesh sieve;
7) and putting the sieved shell powder and oyster shell powder into a ball mill for ball milling for 100-fold 120 minutes to obtain the shell powder and the oyster shell powder with smaller particle size.
Preferably, the drying temperature of the drying box in the step 5) is 40-45 ℃.
Preferably, the crushing fineness of the crusher in the step 6) is 50-300 meshes.
The invention has the following beneficial effects:
1. in the process of preparing the solid selenium fertilizer, firstly, ascorbic acid and sodium selenite solution react to produce selenium, the selenium is reduced into red nano-selenium with the particle size of 20-60 nm by utilizing the strong reducibility of the ascorbic acid, and then the nano-selenium is adsorbed by utilizing shell powder and oyster shell powder through the physical adsorption effect, so that the solid selenium fertilizer is formed. Because the toxicity of the nano-selenium is far lower than that of the sodium selenite, the invention reduces the sodium selenite into the nano-selenium firstly, thereby reducing the risk of the subsequent production.
2. After the solid selenium fertilizer prepared by adsorbing nano selenium by using the shell powder and the oyster shell powder is used for fertilizing crops, the shell powder and the oyster shell powder have the effects of adjusting the pH value of soil and adsorbing heavy metals in the soil, so that the antagonism of the heavy metals in the soil on the selenium absorption of the crops can be relieved, and the utilization rate of the crops on the solid selenium fertilizer can be improved.
3. The preparation method of the solid selenium fertilizer has the advantages of simple process, low cost and good fertilizer efficiency.
4. Compared with quick-acting selenium fertilizer, the solid selenium fertilizer prepared by the method has more lasting fertilizer efficiency and higher absorption and utilization rate of crops to selenium.
5. The shell powder and the fresh oyster shell powder are adopted to prepare the solid selenium fertilizer, so that the solid waste is changed into valuable, the environment is protected, the pollution is avoided, and the resource utilization maximization can be realized.
Drawings
FIG. 1 is a graph showing the change of selenium content in plant samples after fertilizer efficiency tests.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The solid selenium fertilizer is prepared by mixing the following raw materials, including distilled water, a sodium selenite solution, an ascorbic acid solution, shell powder and oyster shell powder, wherein the volume of the distilled water is the ratio of the raw materials: volume of sodium selenite solution: volume of ascorbic acid solution: weight of shell powder: the weight of fresh oyster shell powder is 9: 2: 2: 5: 5.
preferably, the concentration of the sodium selenite solution is 0.2M/L.
Preferably, the concentration of the ascorbic acid solution is 1.2M/L.
The invention also discloses a preparation method of the solid selenium fertilizer, which comprises the following steps:
1) adding 0.2M/L and 100mL of sodium selenite solution into 450mL of distilled water, uniformly stirring, then adding 1.2M/L and 100mL of ascorbic acid solution, and rapidly and uniformly stirring to obtain a mixed solution, wherein the solution is rapidly changed into brick red;
2) uniformly mixing 250g of shell powder and 250g of oyster shell powder, slowly pouring the uniformly mixed shell powder into the mixed solution obtained in the step 1), stirring while pouring until the mixture is uniformly stirred, wherein the mixed solution is orange red, and then standing;
3) standing, gradually precipitating the shell powder until supernatant is clear and colorless, then performing suction filtration, separating the filtrate from the solid shell powder, and uniformly dispersing the solid shell powder in a clean tray;
4) and (3) putting the tray filled with the solid shell powder into a baking oven for drying, and drying at the temperature of 38-45 ℃ to obtain the light pink solid selenium fertilizer.
The preparation method of the shell powder and the fresh oyster shell powder comprises the following steps:
5) cleaning shells and fresh oyster shells, draining, respectively breaking, placing into a drying oven, and drying by blowing at 40-45 deg.C;
6) pulverizing the crushed and dried shell and fresh oyster shell into powder by a pulverizer respectively, and sieving with a 60-mesh sieve, wherein the pulverizing fineness of the pulverizer is 50-300 meshes;
7) and putting the shell powder and the fresh oyster shell powder obtained after sieving into a ball mill for ball milling for 100-fold 120 minutes to obtain the shell powder and the fresh oyster shell powder with smaller particle size.
The solid selenium fertilizer prepared by the invention is soaked in distilled water, and the distilled water is slowly changed into red from colorless, which indicates that the selenium in the solid selenium fertilizer is slowly released into water.
Analysis of experiments
Firstly, determining the content of selenium in the solid selenium fertilizer prepared by the method
1. Preparation of selenium Standard solution
On the first day, 6 digestion colorimetric tubes are taken, 0.5g of solid selenium fertilizer is respectively weighed by an electronic balance, 3 of the solid selenium fertilizer are added into the digestion colorimetric tubes, the other 3 solid selenium fertilizer are used as blank control groups, 8mL of concentrated nitric acid is respectively injected into 6 test tubes by a pipette, 1mL of hydrogen peroxide is added, and the mixture is subjected to cold nitrolysis at night.
The next day, placing the digestion colorimetric tube on a temperature-controlled electric heating plate, heating at 100 ℃ for more than 2 hours, adjusting the reaction temperature to 120 ℃ for continuous reaction, adding 2mL of perchloric acid after 1 hour, continuing the reaction for 1 hour until white smoke appears, adjusting the temperature to 150 ℃, reacting for 2 hours, adjusting the temperature to 160 ℃ until the white smoke is exhausted, and removing the acid to the scale mark. And after all the digestion colorimetric tubes are flushed with acid to about 1mL, cooling for 10-15 min, and then injecting 2.5mL of concentrated hydrochloric acid into all the digestion colorimetric tubes by using a liquid transfer gun.
On the third day, all digestion cuvettes were transferred to 25mL cuvettes and each was made up to 25mL with concentrated hydrochloric acid and then the selenium content was measured by atomic fluorescence spectrometry.
Transferring the cooled selenium standard solution into a 10mL colorimetric tube, measuring the total selenium content by using a hydride generation-atomic fluorescence spectrometer, using a 10% HCl solution as a carrying current, using a 2% potassium borohydride solution and a 0.5% sodium hydroxide solution as reducing agents, and simultaneously performing a blank test.
The parameters of the hydride generation-atomic fluorescence spectrometer 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 | 9.0s |
| Lamp current | 80mA | Delay time | 3.0s |
| Atomizer temperature | 25℃ | Measurement method | Standard curve method |
| Atomizer altitude | 10mm | Reading mode | Peak area |
| Flow of carrier gas | 300mL*min-1 | Sample introduction volume | 1.0mL |
| Flow of shield | 800mL*min-1 | Sample introduction mode | Automatic |
Through determination, the selenium content of the prepared solid selenium fertilizer is 6.395 g/Kg.
Secondly, the solid selenium fertilizer prepared by the invention has an effect test I
In order to verify the fertilizer efficiency of the solid selenium fertilizer prepared by the invention, an outdoor test is carried out, the fertilizer is applied to the plant, the change of the selenium content in the plant before and after the fertilizer is applied is observed, and whether the increase of the selenium content in the plant is promoted or not is judged.
1. 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, each treatment mode was simultaneous application of sodium selenite, solid selenium fertilizer and no selenium fertilizer, and the test treatment data of each test group is shown in table 2 below.
Table 2 test treatments
| Serial number | Treatment of | Selenium application amount | Application method |
| Process 1 | Sodium selenite | 2.4 g/mu | Watering root |
| Treatment 2 | Solid selenium fertilizer | 12.0 g/mu | Mix soil and withdraw at the root |
| Treatment 3 | Control | 0 g/mu |
2. 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 l.
The abscissa of the graph in FIG. l is the number of days after fertilization in days and the ordinate is the selenium content of the sample in mg/Kg.
From the data in fig. l, it can be seen that 24 days after the fertilization, the selenium content of the processed bamboo liquid sample was 0.037 mg/Kg, the selenium content of the processed bamboo liquid sample was 0.059 mg/Kg, and the selenium content of the processed bamboo liquid sample was 0.029 mg/Kg, and it can be seen that the selenium content of the processed bamboo liquid sample was increased by applying sodium selenite, and the selenium content of the processed bamboo liquid sample was increased most by applying the solid selenium fertilizer, compared with the blank control. 32 days after the fertilization, the selenium content of the processed Dan bamboo liquid sample is 0.023 mg/Kg, the selenium content of the processed 2 Dan bamboo liquid sample is 0.032 mg/Kg, and the selenium content of the processed 3 Dan bamboo liquid sample is 0.019 mg/Kg. After 42 days of fertilization, the selenium content of the processed bamboo liquid sample is 0.025 mg/Kg, the selenium content of the processed bamboo liquid sample is 0.036 mg/Kg, and the selenium content of the processed bamboo liquid sample is 0.02l mg/Kg, so that compared with a blank control, the selenium content of the processed bamboo liquid sample can be effectively increased by applying sodium selenite, and the selenium content of the processed bamboo liquid sample is increased most after applying the solid selenium fertilizer.
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 bamboo liquid sample is in a descending trend, sodium selenite is a quick-acting selenium fertilizer, and the selenium content of the bamboo liquid sample reaches the highest value within 12 days after the fertilizer is applied. The selenium content in the treatment 2 is in a trend of increasing firstly and then decreasing, the peak value of the release of the solid selenium fertilizer is reached in about 24 days after the fertilizer is applied, and the release is gradually slowed down later.
According to the analysis of experimental results, the sodium selenite and the solid selenium fertilizer can promote the increase of the selenium content of the Dan bamboo liquid 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 solid selenium fertilizer gradually loses efficacy within a relatively long time after being fertilized, and the fertilizer efficiency time is relatively long during the effect taking.
Selenium element is an element which can promote the growth of plants when being added in a small amount and can poison the plants when being added in an excessive amount, so that the selenium element has the characteristic of being used as a fertilizer, namely, the selenium application amount in each time must be within a safety threshold value, and the selenium element can poison crops when exceeding the threshold value. Therefore, the treatment 1 in the table 2 is represented as a non-slow release fertilizer, and the selenium application amount is referred to the general selenium fertilizer application amount. The solid selenium fertilizer prepared by the invention is a slow release fertilizer, and the selenium application amount of the treatment 2 in the table 2 is 5 times of that of the treatment 1. However, from the results, the selenium content in the plants treated from beginning to end in the experimental period 2 is only 0.7-1.5 times of the selenium content in the plants treated in the experimental period 1, and is far lower than 5 times, which indicates that the solid selenium fertilizer prepared by the invention is high in safety to crops as a slow release fertilizer. Treatment 2 had a relatively slower onset of action, but a longer lasting and safer fertilizer effect than treatment 1.
Thirdly, the fertilizer efficiency test of the solid selenium prepared by the invention II
1. Purpose of the experiment
The test is carried out in order to verify whether the solid selenium fertilizer prepared by the invention has fertilizer efficiency.
2. Test method
Selecting water culture corn seedlings with long trefoil stage and uniform vigor, and setting two treatments of fertilization and non-fertilization, wherein the four treatments are repeated, and each repeated ten plants form a group. No fertilizer is applied as a control treatment, 1/1000 solid selenium fertilizer is used as a test treatment, 1g of the solid selenium fertilizer is weighed and put into a 300-mesh nylon net, and the nylon net is put into 1L of deionized water to be soaked to prepare the nutrient solution. And respectively placing the corn seedlings in nutrient solution and clear water for culturing, timely replenishing water to 1L every day, and respectively measuring the selenium content of the whole corn of the control group and the whole corn of the treatment group after one week.
3. Measurement items
Selenium content of the whole corn.
4. Test materials
The method comprises the steps of water planting corn seedlings in the trefoil stage, solid selenium fertilizer, an electronic balance, weighing paper, a 1L beaker and a 300-mesh nylon net.
5. Test determination
After water culture for 7 days, cleaning the whole corn seedling with deionized water, drying in an oven at 105 ℃ for 30 minutes to inactivate enzyme, drying at 60 ℃, and crushing into powder by a crusher for later use. And (3) measuring the selenium content of the whole corn plant by using an atomic fluorescence photometer method.
6. Test results
The average selenium content of the control group of corn plants was 0.25mg/Kg and the average selenium content of the test group of corn plants was 18.72 mg/Kg. The average value of the selenium content of the corn plants in the test group is 74.88 times of the average value of the selenium content of the corn plants in the control group, which shows that the solid selenium fertilizer can effectively improve the selenium content in the plants and has obvious fertilizer efficiency.
In the process of preparing the solid selenium fertilizer, firstly, ascorbic acid and sodium selenite solution react to produce selenium, the selenium is reduced into red nano-selenium with the particle size of 20-60 nm by utilizing the strong reducibility of the ascorbic acid, and then the nano-selenium is adsorbed by utilizing shell powder and oyster shell powder through the physical adsorption effect, so that the solid selenium fertilizer is formed. Because the toxicity of the nano-selenium is far lower than that of the sodium selenite, the invention reduces the sodium selenite into the nano-selenium firstly, thereby reducing the risk of the subsequent production.
In conclusion, after the solid selenium fertilizer prepared by adsorbing nano selenium by using the shell powder and the oyster shell powder is applied to crops, the shell powder and the oyster shell powder have the effects of adjusting the pH value of soil and adsorbing heavy metals in the soil, so that the antagonism of the heavy metals in the soil on the absorption of selenium elements by the crops can be relieved, and the utilization rate of the solid selenium fertilizer by the crops can be improved.
Claims (8)
1. The solid selenium fertilizer is characterized in that: the oyster shell powder is prepared by mixing the following raw materials, including distilled water, a sodium selenite solution, an ascorbic acid solution, shell powder and oyster shell powder, wherein the mixture ratio of the raw materials is the volume of the distilled water: volume of sodium selenite solution: volume of ascorbic acid solution: weight of shell powder: the weight of fresh oyster shell powder is 9: 2: 2: 5: 5.
2. the solid selenium fertilizer of claim 1, wherein: the concentration of the sodium selenite solution is 0.2M/L.
3. The solid selenium fertilizer of claim 1, wherein: the concentration of the ascorbic acid solution is 1.2M/L.
4. The method for preparing the solid selenium fertilizer as claimed in any one of claims 1 to 3, comprising the steps of:
1) adding the sodium selenite solution into distilled water according to the proportion, uniformly stirring, then adding the ascorbic acid solution, and rapidly and uniformly stirring to obtain a mixed solution, wherein the solution is rapidly changed into brick red;
2) uniformly mixing shell powder and oyster shell powder according to a ratio, slowly pouring the uniformly mixed shell powder into the mixed solution obtained in the step 1), stirring while pouring until the mixture is uniformly stirred, wherein the mixed solution is orange red, and then standing;
3) standing, gradually precipitating the shell powder until supernatant is clear and colorless, then performing suction filtration, separating the filtrate from the solid shell powder, and uniformly dispersing the solid shell powder in a clean tray;
4) and (3) putting the tray filled with the solid shell powder into a baking oven for drying to obtain the light pink solid selenium fertilizer.
5. The method for preparing the solid selenium fertilizer as claimed in claim 4, wherein: the drying temperature in the step 4) is 38-45 ℃.
6. The method for preparing the solid selenium fertilizer as claimed in claim 4, wherein the method for preparing the shell powder and the fresh oyster shell powder comprises the following steps:
5) cleaning shells and fresh oyster shells, draining, respectively breaking, and placing into a drying oven for air blowing and drying;
6) crushing the crushed and dried shells and fresh oyster shells into powder by using a crusher respectively, and then sieving the powder by using a 60-mesh sieve;
7) and putting the sieved shell powder and oyster shell powder into a ball mill for ball milling for 100-fold 120 minutes to obtain the shell powder and the oyster shell powder with smaller particle size.
7. The method for preparing the solid selenium fertilizer as claimed in claim 6, wherein: and 5) the drying temperature of the drying box is 40-45 ℃.
8. The method for preparing the solid selenium fertilizer as claimed in claim 6, wherein: and 6) the crushing fineness of the crusher is 50-300 meshes.
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| CN109665890A (en) * | 2018-12-29 | 2019-04-23 | 鼎元(天津)生物医药科技有限公司 | A kind of nano selenium fertilizer feed additives and preparation method thereof |
| CN110759320A (en) * | 2019-09-09 | 2020-02-07 | 浙江万方生物科技有限公司 | Preparation method of water-soluble nano elemental selenium for livestock and poultry |
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2021
- 2021-01-22 CN CN202110088362.0A patent/CN112759456A/en active Pending
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| CN1686789A (en) * | 2005-04-19 | 2005-10-26 | 浙江大学 | Load type nano selenium and preparation method |
| CN106083286A (en) * | 2016-05-27 | 2016-11-09 | 河南中医学院 | A kind of sugar alcohol chelating agen preventing and treating plant physiology disease |
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Application publication date: 20210507 |