CN114600895A - Method for synthesizing slow release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate - Google Patents
Method for synthesizing slow release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate Download PDFInfo
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- CN114600895A CN114600895A CN202210178834.6A CN202210178834A CN114600895A CN 114600895 A CN114600895 A CN 114600895A CN 202210178834 A CN202210178834 A CN 202210178834A CN 114600895 A CN114600895 A CN 114600895A
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- bispyribac
- calcium
- release agent
- sodium
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
Abstract
The invention discloses a method for synthesizing a slow-release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate, which comprises the steps of adding calcium, aluminum and chlorine into water according to the molar ratio of Ca to Al to Cl of 2 to 1 to stir uniformly; adding bispyribac-sodium, controlling the pH value, and carrying out heat preservation stirring reaction; further carrying out solid-liquid separation, drying and crushing to obtain the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent. The invention breaks through the limitation that the traditional sustained release agent mostly uses macromolecular organic matters as carriers, uses hydrated calcium chloroaluminate as a main body, uses bispyribac-sodium as an object, and adopts one-step assembly to obtain the bispyribac-sodium-hydrated calcium chloroaluminate sustained release agent which has good and stable release performance.
Description
Technical Field
The invention relates to the technical field of intercalation assembly chemistry, in particular to a method for synthesizing a sustained release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate.
Background
In the application of the bispyribac-sodium, the pesticide effect is reduced due to drenching, leaching or improper use, other crops are harmed, and the ground surface, underground water and soil are polluted. Therefore, the development of safe and efficient green bispyribac-sodium, the creation of a novel formulation of bispyribac-sodium, the realization of the controllability of the release quantity, the release time and the release space of bispyribac-sodium, and the development of the novel formulation of bispyribac-sodium become important directions for the research of bispyribac-sodium formulations in recent years.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for synthesizing a sustained release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate, which can solve the technical problems.
(II) technical scheme
In order to solve the technical problems, the invention provides the following technical scheme: the method for synthesizing the slow release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate comprises the following steps: adding calcium, aluminum and chlorine into water according to the molar ratio of Ca to Al to Cl of 2 to 1, and uniformly stirring; adding bispyribac-sodium, controlling the pH value, and carrying out heat preservation stirring reaction; further carrying out solid-liquid separation, drying and crushing to obtain the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent.
Preferably, the calcium includes calcium oxide and its salts, calcium hydroxide and its calcium-containing natural minerals and calcium aluminates.
Preferably, the aluminum includes aluminum oxide and salts thereof, meta-aluminate and salts thereof, aluminum hydroxide and polymers thereof, aluminum-containing minerals and slag.
Preferably, chlorine includes hydrochloric acid, hypochlorous acid, chloric acid and salts thereof.
Preferably, the calcium, aluminum and chlorine are a single compound or two or three compositions.
Preferably, the control range of the pH value is 4-12.
Preferably, the control range of the pH value is 6-8.
Preferably, the heat preservation temperature of the heat preservation stirring reaction is 20-110 ℃.
Preferably, the heat preservation temperature of the heat preservation stirring reaction is 65-90 ℃.
Preferably, the heat preservation time of the heat preservation stirring reaction is 8-168 hours.
(III) advantageous effects
Compared with the prior art, the invention provides a method for synthesizing the slow release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate, which has the following beneficial effects: the invention breaks through the limitation that the traditional sustained-release agent mostly uses macromolecular organic matters as carriers, uses hydrated calcium chloroaluminate as a main body and bispyribac-sodium as an object, and adopts one-step assembly to obtain the bispyribac-sodium-hydrated calcium chloroaluminate sustained-release agent (bispyribac-sodium intercalated calcium chloroaluminate sustained-release agent), and the bispyribac-sodium-hydrated calcium chloroaluminate sustained-release agent has good and stable release performance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for synthesizing a slow release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate, which comprises the following steps: adding calcium, aluminum and chlorine into water according to the molar ratio of Ca to Al to Cl of 2 to 1, and uniformly stirring; adding bispyribac-sodium, controlling the pH value, and carrying out heat preservation stirring reaction; further carrying out solid-liquid separation to keep solid, drying and crushing to obtain the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent, wherein the drying time can be 8-168 hours.
Preferably, the calcium includes calcium oxide and its salts, calcium hydroxide and its calcium-containing natural minerals and calcium aluminates. Aluminum includes alumina and its salts, meta-aluminate and its salts, aluminum hydroxide and its polymers, aluminum-containing minerals and slags. Chlorine includes hydrochloric acid, hypochlorous acid, chloric acid and salts thereof.
Preferably, the calcium, aluminum and chlorine can be single compounds, such as calcium chloroaluminate; the calcium, aluminum and chlorine can also be two or three compositions, for example: calcium metaaluminate, calcium hypochlorite and calcium chloroaluminate.
Specifically, the pH value is controlled within a range of 4 to 12, preferably 6 to 8.
Specifically, the heat preservation temperature of the heat preservation stirring reaction is 20-110 ℃, and the best temperature is 65-90 ℃.
Specifically, the heat preservation time of the heat preservation stirring reaction is 8-168 hours, and the best time is 24-72 hours.
Compared with the prior art, the invention provides a method for synthesizing the slow release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate, which has the following beneficial effects: the invention breaks through the limitation that the traditional sustained-release agent mostly uses macromolecular organic matters as carriers, uses hydrated calcium chloroaluminate as a main body and bispyribac-sodium as an object, and adopts one-step assembly to obtain the bispyribac-sodium-hydrated calcium chloroaluminate sustained-release agent (bispyribac-sodium intercalated calcium chloroaluminate sustained-release agent), and the bispyribac-sodium-hydrated calcium chloroaluminate sustained-release agent has good and stable release performance: in water and Na2CO3The release performance of the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent is examined to be good in the solution; the stable release performance of the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent is verified in a phosphoric acid buffer solution and a mixed inorganic anion solution by different pH values respectively.
The hydrated calcium chloroaluminate has the composition of 3CaO2O3.CaCl2.10H2Layered bis-hydroxychlorides of O. It was first discovered by Fred when studying the reactivity of lime with aluminum chloride in 1897. Later, cement chemistry studies showed that this tetracalcium dichloroaluminate compound is also present in the monosulfoaluminate (AFm) phase of the cement gel, in the form of hexagonal plate-like crystals. Experiments show that the hydrated calcium chloroaluminate is stable within the pH range of 4-12, belongs to an environment-friendly ion exchange type layered structure, and is a low-cost adsorbent.
The first embodiment is as follows: slowly adding 30g of calcium chloride, calcium hydroxide and high-alumina cement in 100ml of water according to the molar ratio of Ca to Al to Cl of 2 to 1, and uniformly stirring; heating to 65 ℃, slowly adding 2g of bispyribac-sodium, controlling the pH value to be 6, and stirring for 48 hours at 85 ℃; carrying out solid-liquid separation (centrifugal separation), drying and crushing to obtain the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent.
Example two: slowly adding 30g of calcium chloride, calcium hydroxide and aluminum ore powder in 100ml of water according to the molar ratio of Ca to Al to Cl of 2 to 1, and uniformly stirring; heating to 65 ℃, slowly adding 2g of bispyribac-sodium, controlling the pH value to be 6, and stirring for 72 hours at 85 ℃; carrying out solid-liquid separation (centrifugal separation), drying and crushing to obtain the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent.
Example three: slowly adding 30g of calcium chloride, calcium hydroxide and aluminum oxide into 100ml of water according to the molar ratio of Ca to Al to Cl of 2 to 1, and uniformly stirring; slowly adding 2g of bispyribac-sodium, controlling the pH value to be 7, and stirring for 24 hours at the temperature of 85 ℃; carrying out solid-liquid separation (centrifugal separation), drying and crushing to obtain the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent.
Example four: slowly adding 30g of calcium oxide and aluminum trichloride into 100ml of water according to the molar ratio of Ca to Al to Cl of 2 to 1, and uniformly stirring; slowly adding 2g of bispyribac-sodium, controlling the pH value to be 7, and stirring for 24 hours at the temperature of 85 ℃; carrying out solid-liquid separation (centrifugal separation), drying and crushing to obtain the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent.
Example five: slowly adding 30g of calcium chloride and calcium metaaluminate in the total mass into 100ml of water according to the molar ratio of Ca to Al to Cl of 2 to 1, and uniformly stirring; slowly adding 2g of bispyribac-sodium, controlling the pH value to be 8, and stirring for 24 hours at the temperature of 85 ℃; carrying out solid-liquid separation (centrifugal separation), drying and crushing to obtain the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent.
Example six: slowly adding calcium oxide and polyaluminium chloride with the total mass of 30g into 100ml of water according to the molar ratio of Ca to Al to Cl of 2 to 1, and uniformly stirring; slowly adding 60ml ethanol water solution containing 2g bispyribac-sodium, controlling pH value to be 8, keeping temperature and stirring for 24 hours at 85 ℃; carrying out solid-liquid separation (centrifugal separation), drying and crushing to obtain the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent.
It is to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The method for synthesizing the slow-release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate is characterized by comprising the following steps:
adding calcium, aluminum and chlorine into water according to the molar ratio of Ca to Al to Cl of 2 to 1, and uniformly stirring;
adding bispyribac-sodium, controlling the pH value, and carrying out heat preservation stirring reaction;
further carrying out solid-liquid separation, drying and crushing to obtain the bispyribac-sodium-calcium chloroaluminate hydrate sustained release agent.
2. The method for synthesizing the slow-release agent by the one-step intercalation assembly of the bispyribac-calcium chloroaluminate as claimed in claim 1, wherein: the calcium includes calcium oxide and its salt, calcium hydroxide and its calcium-containing natural mineral and calcium aluminate.
3. The method for synthesizing the slow-release agent by the one-step intercalation assembly of the bispyribac-calcium chloroaluminate as claimed in claim 1, wherein: the aluminum includes aluminum oxide and salts thereof, meta-aluminate and salts thereof, aluminum hydroxide and polymers thereof, aluminum-containing minerals and slag.
4. The method for synthesizing the slow-release agent by the one-step intercalation assembly of the bispyribac-calcium chloroaluminate as claimed in claim 1, wherein: the chlorine includes hydrochloric acid, hypochlorous acid, chloric acid and salts thereof.
5. The method for synthesizing the slow-release agent by the one-step intercalation assembly of the bispyribac-calcium chloroaluminate as claimed in claim 1, wherein: the calcium, the aluminum and the chlorine are single compounds or two or three compositions.
6. The method for synthesizing the slow-release agent by the one-step intercalation assembly of the bispyribac-calcium chloroaluminate as claimed in claim 1, wherein: the control range of the pH value is 4-12.
7. The method for synthesizing the slow release agent by the one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate as claimed in claim 6, wherein: the control range of the pH value is 6-8.
8. The method for synthesizing the slow-release agent by the one-step intercalation assembly of the bispyribac-calcium chloroaluminate as claimed in claim 1, wherein: the heat preservation temperature of the heat preservation stirring reaction is 20-110 ℃.
9. The method for synthesizing the slow-release agent by the one-step intercalation assembly of the bispyribac-calcium chloroaluminate as claimed in claim 8, wherein: the heat preservation temperature of the heat preservation stirring reaction is 65-90 ℃.
10. The method for synthesizing the slow-release agent by the one-step intercalation assembly of the bispyribac-calcium chloroaluminate as claimed in claim 1, wherein: the heat preservation time of the heat preservation stirring reaction is 8-168 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210178834.6A CN114600895A (en) | 2022-02-25 | 2022-02-25 | Method for synthesizing slow release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate |
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| CN202210178834.6A CN114600895A (en) | 2022-02-25 | 2022-02-25 | Method for synthesizing slow release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104026125A (en) * | 2014-06-18 | 2014-09-10 | 厦门大学 | Method for synthesizing sustained-release agent by intercalating pesticide into calcium chloroaluminate hydrate |
| CN104322487A (en) * | 2014-11-17 | 2015-02-04 | 江苏隆昌化工有限公司 | Method for synthesizing pesticide controlled-release formulation by modifying calcium chloroaluminate hydrate activated pillar |
| CN104396949A (en) * | 2014-11-17 | 2015-03-11 | 江苏隆昌化工有限公司 | Method for structural reconstruction of hydrated aluminum chloroaluminate to synthesize pesticide controlled release agent |
| CN104509531A (en) * | 2014-11-17 | 2015-04-15 | 江苏隆昌化工有限公司 | One-step assembly synthesis method of pesticide calcium chloroaluminate sustained release agent |
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2022
- 2022-02-25 CN CN202210178834.6A patent/CN114600895A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104026125A (en) * | 2014-06-18 | 2014-09-10 | 厦门大学 | Method for synthesizing sustained-release agent by intercalating pesticide into calcium chloroaluminate hydrate |
| CN104322487A (en) * | 2014-11-17 | 2015-02-04 | 江苏隆昌化工有限公司 | Method for synthesizing pesticide controlled-release formulation by modifying calcium chloroaluminate hydrate activated pillar |
| CN104396949A (en) * | 2014-11-17 | 2015-03-11 | 江苏隆昌化工有限公司 | Method for structural reconstruction of hydrated aluminum chloroaluminate to synthesize pesticide controlled release agent |
| CN104509531A (en) * | 2014-11-17 | 2015-04-15 | 江苏隆昌化工有限公司 | One-step assembly synthesis method of pesticide calcium chloroaluminate sustained release agent |
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