CN115448792A - Polydopamine nanosphere-based slow-release pesticide fertilizer and preparation process thereof - Google Patents
Polydopamine nanosphere-based slow-release pesticide fertilizer and preparation process thereof Download PDFInfo
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- CN115448792A CN115448792A CN202210957588.4A CN202210957588A CN115448792A CN 115448792 A CN115448792 A CN 115448792A CN 202210957588 A CN202210957588 A CN 202210957588A CN 115448792 A CN115448792 A CN 115448792A
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- fertilizer
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- polydopamine
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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
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C9/00—Fertilisers containing urea or urea compounds
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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
- C05G5/30—Layered or coated, e.g. dust-preventing coatings
- C05G5/35—Capsules, e.g. core-shell
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
- Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a polydopamine nanosphere-based slow-release pesticide fertilizer and a preparation process thereof, and belongs to the technical field of slow release of pesticide fertilizers. The slow-release pesticide fertilizer takes the poly-dopamine nanospheres as a template, the pesticide fertilizer is wrapped inside the template, and the metal salt fertilizer is attached to the outside of the template. The slow release pesticide fertilizer comprises the following components: 50-70wt% of medical fertilizer, 5-25wt% of metal salt fertilizer and 10-30wt% of polydopamine nanospheres. The slow-release pesticide fertilizer has the characteristics of no toxicity and degradability, and has a good application prospect.
Description
Technical Field
The invention belongs to the technical field of slow release of medicinal fertilizers, and particularly relates to a polydopamine nanosphere-based slow release medicinal fertilizer and a preparation process thereof.
Background
The fertilizer is a chemical substance which can provide nutrients required by the growth and development of crops, improve the soil properties and improve the yield and quality of the crops; the pesticide is chemical for preventing and controlling diseases and pests and regulating plant growth. Therefore, chemical fertilizers and pesticides are two important production data in agricultural production.
The loss of a large amount of medical fertilizers brings huge economic losses, and causes serious water, soil and air pollution, thus threatening human health. The slow release of the pesticide fertilizer is an important way for solving the problem of pesticide fertilizer loss. At present, the slow-release fertilizer is mostly prepared from non-degradable, toxic and environmentally-friendly raw materials, and does not accord with the current policy, so that the slow-release fertilizer which is degradable, non-toxic and environmentally-friendly needs to be developed.
Dopamine (DA, or 3-hydroxytyrosine, 3, 4-dihydroxyphenylethylamine) is an endogenous nitrogen-containing organic compound that can be polymerized to form Polydopamine (PDA), and the synthesis is schematically shown below:
the polydopamine has strong adhesion and chemical functionality, and can react with various functional groups. Although many researches have been carried out to develop a slow-release pesticide fertilizer with good slow-release effect, most of the researches use various high polymer materials as hard templates, and polydopamine is attached to the surface after the pesticide fertilizer is adsorbed, which puts higher requirements on the safety of pesticide fertilizer raw materials.
Therefore, a new technology for slow-release pesticide fertilizer needs to be developed.
Disclosure of Invention
In order to avoid introducing a template agent and improve the utilization rate of polydopamine, the invention aims to provide a polydopamine nanosphere-based slow-release pesticide fertilizer, and the invention also aims to provide a preparation process of the slow-release pesticide fertilizer.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the slow release medical fertilizer takes polydopamine nanospheres as templates, the medical fertilizer is wrapped inside the templates, and the metal salt fertilizer is attached to the outside of the templates.
The slow release pesticide fertilizer comprises the following components: 50-70wt% of pesticide fertilizer, 5-25wt% of metal salt fertilizer and 10-30wt% of polydopamine nanospheres.
The pesticide fertilizer is a fertilizer or a pesticide, the fertilizer is one or more of urea, ammonium bicarbonate, ammonium chloride, calcium phosphate, calcium superphosphate and ammonium phosphate, and the pesticide is one or more of fosthiazate, omethoate, emamectin benzoate and tebufenozide.
The metal salt fertilizer is at least one of soluble salts of potassium, calcium and magnesium.
The preparation process of the polydopamine nanosphere-based slow-release pesticide fertilizer comprises the following steps:
s1, adding dopamine and a pesticide fertilizer into water and dispersing;
s2, adding an alkaline ion exchange resin into the solution obtained in the S1, adjusting the pH to 8-11 (neutralizing acid with the alkaline ion exchange resin, providing an alkaline environment, adsorbing residual chloride ions and the like in the dopamine preparation process at the same time), stirring for 6-24h at 20-80 ℃, filtering, collecting solids, and drying;
and S3, adding water into the metal salt fertilizer to prepare a metal salt solution, adding the solid obtained in the S2 into the metal salt solution, stirring for 8-24h at room temperature, filtering, collecting the solid, and drying to obtain the polydopamine nanosphere-based slow-release medicinal fertilizer.
And in the solution obtained in the S1, the molar concentration of the dopamine is 0.1 to 1mol/L.
In S3, the total concentration of metal ions in the metal salt solution is 1mol/L.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a slow-release pesticide fertilizer with a core-shell structure, which takes poly-dopamine nanospheres as a template, coats a pesticide fertilizer inside and is attached with a metal fertilizer outside. The main material of the slow-release pesticide fertilizer is dopamine and the like, does not contain other high polymer materials, does not contain heavy metal ions in the raw materials, has the characteristics of no toxicity and degradability, and has good application prospect.
Drawings
Fig. 1 is a schematic structural diagram of the polydopamine nanosphere-based slow-release fertilizer disclosed by the invention.
Detailed Description
The invention is further described with reference to specific examples.
The raw materials used in the examples:
dopamine: adding 30% HCl aqueous solution into 3, 4-dimethoxy phenethylamine, heating to 80 deg.C, stirring for 48 hr, and filtering to obtain dopamine.
Urea: from alatin (shanghai), U141075.
Basic ion exchange resin: is Amberlite IRA402 ion exchange resin available from Mecanne (Shanghai), A916581.
The rest raw materials are conventional commercial products.
Example 1
Taking 100mL of water, adding 15.3g of dopamine and 30.6g of urea, and stirring for 0.5h; adding alkaline ion exchange resin into the solution to adjust the pH value to 9, heating to 60 ℃, stirring for 12 hours to obtain polydopamine nanospheres with medicine fertilizers wrapped inside, and filtering and drying to obtain 41.4g of white powdery solid; and dispersing the dried solid into 400mL of 1mol/L potassium chloride solution, stirring for 24h, filtering and drying to finally obtain 55.2g of polydopamine nanosphere-based slow-release fertilizer with a core-shell structure (see figure 1).
Example 2
Taking 100mL of water, adding 15.3g of dopamine, 15.3g of urea and 15.3g of calcium superphosphate, and stirring for 1h; adding alkaline ion exchange resin into the solution to adjust the pH value to 10, heating to 60 ℃, stirring for 12 hours, filtering and drying to obtain 39.1g of white powdery solid; and dispersing the dried solid into 410mL of metal fertilizer solution containing 0.9mol/L potassium chloride and 0.1mol/L magnesium chloride, stirring for 12h, filtering and drying to finally obtain 52.1g of polydopamine nanosphere-based slow-release medicinal fertilizer.
Example 3
Taking 100mL of water, adding 15.3g of dopamine, 30.6g of urea and 15.3g of calcium superphosphate, and stirring for 0.5h; adding alkaline ion exchange resin into the solution to adjust the pH value to 10, heating to 60 ℃, stirring for 12 hours, filtering and drying to obtain 58.2 g of white powdery solid; and dispersing the dried solid into 450mL of metal fertilizer solution containing 0.9mol/L potassium chloride and 0.1mol/L magnesium chloride, stirring for 24h, filtering and drying to finally obtain 72.3 g of polydopamine nanosphere-based slow-release medicinal fertilizer.
Example 4
Taking 100mL of water, adding 15.3g of dopamine, 14.3 g of urea, 14.3 g of calcium superphosphate and 2.0g of fosthiazate, and stirring for 1h; adding alkaline ion exchange resin into the solution to adjust the pH value to 8, heating to 80 ℃, stirring for 12 hours, and filtering and drying 41.8 g of gray powder solid; and dispersing the dried solid into 430mL of metal fertilizer solution containing 0.8mol/L potassium chloride and 0.2mol/L magnesium chloride, stirring for 18h, filtering and drying to finally obtain 54.9g of polydopamine nanosphere-based slow-release medicinal fertilizer.
Example 5
Taking 100mL of water, adding 30.6g of dopamine, 30.6g of urea and 30.6g of ammonium phosphate, and stirring for 1h; adding alkaline ion exchange resin into the solution to adjust the pH value to 8, heating to 80 ℃, stirring for 12 hours, filtering and drying to obtain 90.1g of powdery solid; and dispersing the dried solid into 290mL of metal fertilizer solution containing 0.8mol/L potassium chloride and 0.2mol/L magnesium chloride, stirring for 12h, filtering and drying to finally obtain 99.1g of polydopamine nanosphere-based slow-release medicinal fertilizer.
The slow release fertilizer obtained in examples 1 to 5 was subjected to the following tests:
and (3) testing the slow release effect: according to the national standard of the slow release fertilizer (GB/T23348-2009), the determination is carried out by adopting a water dissolution rate method: weighing about 10g of fertilizer sample, putting the fertilizer sample into a small bag made of a 100-mesh nylon gauze, putting the small bag into a 250mL glass bottle, adding 200mL water, capping and sealing, putting the small bag into a biochemical constant-temperature incubator at 25 ℃, sampling every day, testing the nitrogen release amount of the small bag by using an automatic analyzer (refer to GB/T22923-2008), and calculating the cumulative nitrogen release rate by using the following calculation formula: v = W n W, wherein W n Is the mass fraction of nitrogen released measured on day n, and W is the mass fraction of total nitrogen, and the test results are shown in Table 1.
Table 1 sustained release test results
| 1d dissolution Rate (%) | 15d dissolution Rate (%) | Dissolution rate (%) of 30d | 45d dissolution rate (%) | Dissolution rate (%) at 60d | |
| Example 1 | 0.66 | 5.53 | 20.11 | 58.60 | 85.21 |
| Example 2 | 0.62 | 5.86 | 21.52 | 57.88 | 84.67 |
| Example 3 | 0.61 | 5.49 | 20.37 | 58.15 | 84.78 |
| Example 4 | 0.64 | 5.61 | 20.68 | 57.46 | 84.57 |
| Example 5 | 0.65 | 5.82 | 21.33 | 58.73 | 85.19 |
Therefore, the slow-release pesticide fertilizers obtained in the examples 1 to 5 have good slow-release effect.
Claims (7)
1. The slow release medical fertilizer is characterized in that the slow release medical fertilizer takes polydopamine nanospheres as templates, the medical fertilizer is wrapped inside the templates, and metal salt fertilizer is attached to the outside of the templates.
2. The polydopamine nanosphere-based slow release fertilizer according to claim 1, wherein the slow release fertilizer comprises the following components: 50-70wt% of medical fertilizer, 5-25wt% of metal salt fertilizer and 10-30wt% of polydopamine nanospheres.
3. The polydopamine nanosphere-based slow-release pesticide fertilizer according to claim 1, characterized in that the pesticide fertilizer is a fertilizer or a pesticide, the fertilizer is one or more of urea, ammonium bicarbonate, ammonium chloride, calcium phosphate, calcium superphosphate and ammonium phosphate, and the pesticide is one or more of fosthiazate, omethoate, emamectin benzoate and tebufenozide.
4. The polydopamine nanosphere-based slow-release medicinal fertilizer as claimed in claim 1, wherein the metal salt fertilizer is at least one of soluble salts of potassium, calcium and magnesium.
5. The preparation process of the polydopamine nanosphere-based slow release fertilizer according to any one of claims 1 to 4, characterized by comprising the following steps:
s1, adding dopamine and a pesticide fertilizer into water and dispersing;
s2, adding an alkaline ion exchange resin into the solution obtained in the S1 to adjust the pH to 8 to 11, stirring for 6 to 24h at the temperature of 20 to 80 ℃, filtering, collecting a solid and drying;
and S3, adding water into the metal salt fertilizer to prepare a metal salt solution, adding the solid obtained in the S2 into the metal salt solution, stirring at room temperature for 8 to 24h, filtering, collecting the solid, and drying to obtain the polydopamine nanosphere-based slow-release medicinal fertilizer.
6. The preparation method of the polydopamine nanosphere-based slow-release medicinal fertilizer according to claim 5, wherein the molar concentration of dopamine in the solution obtained in S1 is 0.1 to 1mol/L.
7. The preparation method of the polydopamine nanosphere-based slow-release fertilizer according to claim 5, wherein in S3, the total concentration of metal ions in the metal salt solution is 1mol/L.
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| CN202210957588.4A CN115448792A (en) | 2022-08-11 | 2022-08-11 | Polydopamine nanosphere-based slow-release pesticide fertilizer and preparation process thereof |
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| CN202210957588.4A CN115448792A (en) | 2022-08-11 | 2022-08-11 | Polydopamine nanosphere-based slow-release pesticide fertilizer and preparation process thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976855A (en) * | 2012-12-18 | 2013-03-20 | 石河子大学 | Polydopamine coated controlled-release fertilizer |
| AU2020101495A4 (en) * | 2020-06-10 | 2020-08-27 | Guangdong Bioengineering Institute Guangzhou Sugarcane Industry Research Institute | Pesticide nano preparation and preparation method thereof |
| CN112142521A (en) * | 2020-10-06 | 2020-12-29 | 青岛一亩地农业科技有限责任公司 | Environment-friendly multielement slow-release fertilizer and preparation method thereof |
| AU2020104156A4 (en) * | 2020-12-17 | 2021-03-04 | Zhejiang University | A nano-capsule type polydopamine drug material and method for preparing the same |
| KR20210114151A (en) * | 2020-03-10 | 2021-09-23 | (주)화이바이오메드 | Method for Manufacturing and Use of Urease-powered Polydopamine Nanomotors |
-
2022
- 2022-08-11 CN CN202210957588.4A patent/CN115448792A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976855A (en) * | 2012-12-18 | 2013-03-20 | 石河子大学 | Polydopamine coated controlled-release fertilizer |
| KR20210114151A (en) * | 2020-03-10 | 2021-09-23 | (주)화이바이오메드 | Method for Manufacturing and Use of Urease-powered Polydopamine Nanomotors |
| AU2020101495A4 (en) * | 2020-06-10 | 2020-08-27 | Guangdong Bioengineering Institute Guangzhou Sugarcane Industry Research Institute | Pesticide nano preparation and preparation method thereof |
| CN112142521A (en) * | 2020-10-06 | 2020-12-29 | 青岛一亩地农业科技有限责任公司 | Environment-friendly multielement slow-release fertilizer and preparation method thereof |
| AU2020104156A4 (en) * | 2020-12-17 | 2021-03-04 | Zhejiang University | A nano-capsule type polydopamine drug material and method for preparing the same |
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