CN110876378A - Intelligent microcapsule suspending agent and preparation method thereof - Google Patents
Intelligent microcapsule suspending agent and preparation method thereof Download PDFInfo
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- CN110876378A CN110876378A CN201911263659.5A CN201911263659A CN110876378A CN 110876378 A CN110876378 A CN 110876378A CN 201911263659 A CN201911263659 A CN 201911263659A CN 110876378 A CN110876378 A CN 110876378A
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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
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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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
- A01N25/02—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 liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/18—In situ polymerisation with all reactants being present in the same phase
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Abstract
An intelligent microcapsule suspension comprising: according to weight percentage, 1-5% of polypropylene oxide, 2-5% of emulsifier, 2-10% of thiacloprid, 10-15% of caprylic/capric triglyceride, 5-15% of cyclohexanone, 1-5% of polyacrylic acid, 2-5% of surfactant, 0.1-0.3% of xanthan gum, 3-5% of glycerol, 0.1-0.3% of carbazone, 0.5-2% of magnesium aluminum silicate, 1-2% of hydrochloric acid and water are supplemented to 100%. The preparation method comprises the following steps: preparing an oil phase, preparing a water phase, emulsifying, adjusting pH, microencapsulating and preparing a suspending agent. The invention also provides a preparation method of the intelligent microcapsule suspending agent, which has self-assembly and self-repair pH sensitivity, and the prepared suspending agent belongs to a water-based sanitary pest control formulation which is green, efficient, environment-friendly, safe and convenient to use, is suitable for various mosquito repellent products, and has wide market prospect.
Description
Technical Field
The invention relates to an insecticide, in particular to an intelligent microcapsule suspending agent and a preparation method thereof.
Background
Thiacloprid is a nicotinic acetylcholine receptor (nAChRs) agonist that interferes with synaptic signaling in the central nervous system of insects. Thiacloprid has the functions of acute contact poisoning and stomach toxicity and has systemic activity. Thiacloprid is applied to leaf surfaces, so that sucking and chewing mouthpart pests on pomes, drupes, small berries, cotton, grains, vegetables, sugar beets, potatoes, rice and ornamental plants can be effectively prevented and treated. Pests to be controlled include: aphids, whiteflies, plant hoppers, whiteflies, psyllids, pear psyllids, beetles (e.g., potato beetles, apple weevils, and rice weevils), monochamus alternatus, wheat midges, and lepidopteran pests such as leaf miners and codling moths.
The thiacloprid has good control effect on rice planthoppers, the effect of the thiacloprid exceeds that of pymetrozine, nitenpyram, thiamethoxam and the like, and the lasting period is long; the control effect of thiacloprid on aphids exceeds imidacloprid with the same dosage; the thiacloprid and spirotetramat have good control effect on the watermelon bemisia tabaci and long lasting period; thiacloprid can effectively prevent and control trialeurodes vaporariorum; the special effect of thiacloprid on monochamus alternatus hope is applied to forest protection in China, and the propagation channel of the pine wilt disease is effectively cut off.
The microcapsule suspending agent is the most advanced formulation of pesticides in the world at present, and has the technical advantages of controllable release, long lasting period and the like. However, the variety of the current microcapsule suspending agents is lack, the main reason is that the selection of the microcapsule for the capsule core and the wall material is harsh, and improper selection can cause the microcapsule to be easy to break during storage and transportation, or to be difficult to break to release the capsule core in daily use. Meanwhile, higher reaction temperature is needed in the microcapsule encapsulation process, and the production cost is increased.
The commercial or common formula of the 2% thiacloprid microcapsule suspending agent mainly uses urea-formaldehyde resin as a wall material, cyclohexanone and methanol as organic solvents, ammonium chloride as an acid catalyst, and an emulsifier 0201B is added to obtain the thiacloprid microcapsule. But are very prone to rupture during storage and transportation.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide an intelligent microcapsule suspending agent and a preparation method thereof, which have self-assembly and self-repair pH sensitivity and well solve the problem of capsule rupture and the problem of cost.
In order to achieve the above object, the present invention provides an intelligent microcapsule suspension comprising: according to weight percentage, 1-5% of polypropylene oxide, 2-5% of emulsifier, 2-10% of thiacloprid, 10-15% of caprylic/capric triglyceride, 5-15% of cyclohexanone, 1-5% of polyacrylic acid, 2-5% of surfactant, 0.1-0.3% of xanthan gum, 3-5% of glycerol, 0.1-0.3% of carbazone, 0.5-2% of magnesium aluminum silicate, 1-2% of hydrochloric acid and water are supplemented to 100%.
Further, the emulsifier is selected from one or more of styryl phenol polyoxyethylene ether, alkylphenol polyoxyethylene polyether and sulfate or phosphate thereof, alkylphenol polyoxyethylene formaldehyde condensate sulfate and calcium dodecyl benzene sulfonate.
Further, the surfactant is selected from one or more of sodium naphthalene sulfonate formaldehyde condensate, alkylphenol polyoxyethylene formaldehyde condensate sulfate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate, alkyl naphthalene formaldehyde condensate sulfonate, macromolecular hydrophobic branched copolymer and polymeric carboxylate; the water is ultrapure water.
In order to achieve the above object, the present invention provides a method for preparing an intelligent microcapsule suspension, comprising the steps of:
(1) preparing an oil phase: adding polypropylene oxide, caprylic/capric triglyceride, cyclohexanone, thiacloprid and an emulsifier into a reaction kettle, raising the temperature in the reaction kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, and uniformly stirring for 30 minutes;
(2) preparing a water phase: adding water and polyacrylic acid into a shearing kettle, raising the temperature in the shearing kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, and stirring at a constant speed for 30 minutes;
(3) emulsification: slowly adding the prepared oil phase into the water phase, shearing and stirring, and fully shearing and stirring for 20 minutes to obtain a milky white liquid;
(4) adjusting the pH value: adding hydrochloric acid into the milky white liquid, and adjusting the pH value to 4;
(5) microencapsulation: stirring at constant speed for half an hour to obtain microcapsule suspension;
(6) preparing a suspending agent: adding a mixed solution of xanthan gum, glycerol, karson, magnesium aluminum silicate, a surfactant and water into the microcapsule suspension, and uniformly stirring for 60 minutes to obtain the microcapsule suspension.
Further, the uniform stirring speed in the step (1) is 500-.
Further, the uniform stirring speed in the step (2) is 300-.
Further, the shear stirring rate in the step (3) is 7000-12000 r/min.
Further, the hydrochloric acid is dropwise added within 2min in the step (4).
Further, the uniform stirring speed in the step (5) is 100-.
Further, the uniform stirring speed in the step (6) is 300-.
The invention has the beneficial effects that: polyacrylic acid with self-assembly and self-repair pH sensitivity is used as a wall material, and polypropylene oxide is used as a crosslinking agent. Polyacrylic acid and polypropylene oxide can spontaneously carry out polymerization reaction under acidic conditions without a catalyst and harsh reaction temperature, thereby showing self-assembly capability. When the capsule wall is damaged, the polyacrylic acid and the polypropylene oxide can continue to perform polymerization reaction spontaneously due to the acidity of the environment of the suspending agent system, so that the self-repairing capability is shown. The polyacrylic acid has pH sensitivity, so the pH sensitivity of the microcapsule can be controlled by adjusting different proportions of the polyacrylic acid and the polypropylene oxide, thereby achieving more accurate release. In daily use, microcapsules of different pH sensitivities may be suitable for different pesticidal subjects. The self-assembly self-repair pH-sensitive intelligent microcapsule suspending agent has the characteristic of self-repair of the capsule wall, and can avoid the problems of poor product stability and the like caused by capsule breakage in transportation and storage. Meanwhile, the capsule wall also has a pH response function, and the proportional relation of different components in the capsule wall can be controlled, so that different pH response capabilities are achieved, the pesticide has long lasting period, and the pesticide is labor-saving and efficient. The self-assembly self-repair pH-sensitive intelligent microcapsule suspending agent belongs to a water-based sanitary pest control formulation which is green, efficient, environment-friendly, safe and convenient to use, is suitable for various mosquito repellent products, and has a wide market prospect.
The preparation method of the intelligent microcapsule suspending agent comprises the steps of firstly, uniformly dispersing an oil phase containing thiacloprid and a cross-linking agent polypropylene oxide in a water phase containing wall material polyacrylic acid to form an O/W stable system, enabling the wall material to generate polymerization reaction to generate a capsule wall by adjusting the pH value of the O/W system and adopting an interface polymerization method, forming microcapsules with capsule cores wrapped in the capsule wall, and finally adding a thickening agent and a surfactant to compound to form the microcapsule suspending agent. The oil phase of the microcapsule is prepared by taking polypropylene oxide, caprylic/capric triglyceride, cyclohexanone, thiacloprid technical and emulsifier as raw materials, and the water phase of the microcapsule is prepared by using ultrapure water and polyacrylic acid. Then transferring the oil phase into a water phase for shearing emulsification, and preparing the thiacloprid microcapsule by using an interfacial polymerization method, wherein the effective capsule forming rate of the thiacloprid microcapsule reaches 90-97%. The invention also determines the factors influencing the encapsulation of the thiacloprid microcapsule, such as the shearing and stirring rate, the dosage of the cross-linking agent polypropylene oxide and the dosage of the wall material polyacrylic acid, thereby obtaining the optimal process parameters of the microencapsulation. The preparation method has the advantages of simple preparation process, low production cost, safe production and use, controllable release, environmental protection and the like, and has remarkable social and economic benefits.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example one
Preparation of 2% thiacloprid microcapsule suspending agent
Preparing an oil phase: adding 2% of thiacloprid, 1% of polypropylene oxide, 2% of styrylphenol polyoxyethylene ether, 10% of caprylic/capric triglyceride and 5% of cyclohexanone into a reaction kettle together according to the weight percentage, raising the temperature of the reaction kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, starting a stirrer, and stirring at a constant speed of 520r/min for 30 minutes. Preparing a water phase: adding 20% of ultrapure water and 1% of polyacrylic acid into a shearing kettle, raising the temperature of the shearing kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, starting a stirrer, and stirring at a constant speed of 330r/min for 30 minutes. Emulsification: transferring the oil phase into the water phase, preserving the heat at 50 +/-5 ℃, starting a stirrer to shear and stir for 20 minutes at the shear stirring speed of 7800r/min to obtain milky white liquid. Adjusting the pH value: adding hydrochloric acid with the total weight percentage of 1% into the milky white liquid, dripping within two minutes, and preserving the temperature at 50 +/-5 ℃. Microencapsulation: and starting a stirrer, and stirring at a constant speed of 110r/min for 30 minutes to prepare the thiacloprid microcapsule suspension. Preparing a suspending agent: adding a solution prepared from 2% of alkyl naphthalene formaldehyde condensate sulfonate, 3% of glycerol, 0.1% of xanthan gum, 0.1% of kason, 0.5% of magnesium aluminum silicate and the balance of ultrapure water which is complemented to 100% into the microcapsule suspension, preserving the temperature at 50 +/-5 ℃, and uniformly stirring for 60 minutes at the stirring speed of 320 r/min. Finally obtaining the 2 percent thiacloprid microcapsule suspending agent.
Example two
Preparation of 3% thiacloprid microcapsule suspending agent
Preparing an oil phase: adding 3% of thiacloprid, 1.5% of polypropylene oxide, 2.5% of styrylphenol polyoxyethylene ether, 11% of caprylic/capric triglyceride and 5.5% of cyclohexanone into a reaction kettle together according to the weight percentage, raising the temperature of the reaction kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, starting a stirrer, and stirring at a constant speed of 537r/min for 30 minutes. Preparing a water phase: adding 22% of ultrapure water and 1.5% of polyacrylic acid into a shearing kettle, raising the temperature of the shearing kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, starting a stirrer, and stirring at a constant speed of 333r/min for 30 minutes. Emulsification: transferring the oil phase into the water phase, keeping the temperature at 50 +/-5 ℃, starting a stirrer to shear and stir for 20 minutes at the shear stirring speed of 7960r/min to obtain a milky white liquid. Adjusting the pH value: adding hydrochloric acid with the total weight percentage of 1.2% into the milky white liquid, dripping within two minutes, and preserving the temperature at 50 +/-5 ℃. Microencapsulation: and starting a stirrer, and stirring at a constant speed of 113r/min for 30 minutes to prepare the thiacloprid microcapsule suspension. Preparing a suspending agent: adding a solution prepared from 2.5% sodium naphthalenesulfonate formaldehyde condensate, 3% glycerin, 0.12% xanthan gum, 0.1% cason, 0.7% magnesium aluminum silicate and the balance of ultrapure water which is complemented to 100% into the microcapsule suspension, preserving the temperature at 50 +/-5 ℃, and uniformly stirring for 60 minutes at the stirring speed of 356 r/min. Finally obtaining the 3 percent thiacloprid microcapsule suspending agent.
EXAMPLE III
Preparation of 4% thiacloprid microcapsule suspending agent
Preparing an oil phase: adding 4% of thiacloprid, 1.7% of polypropylene oxide, 2.8% of alkylphenol polyoxyethylene formaldehyde condensate sulfate, 11.5% of caprylic/capric triglyceride and 6% of cyclohexanone into a reaction kettle together according to the weight percentage, raising the temperature of the reaction kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, starting a stirrer, and stirring at a constant speed of 548r/min for 30 minutes. Preparing a water phase: adding 23% of ultrapure water and 1.6% of polyacrylic acid into a shearing kettle, raising the temperature of the shearing kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, starting a stirrer, and stirring at a constant speed of 343r/min for 30 minutes. Emulsification: transferring the oil phase into the water phase, keeping the temperature at 50 +/-5 ℃, starting a stirrer to shear and stir for 20 minutes at the shear stirring speed of 8345r/min to obtain milky liquid. Adjusting the pH value: adding hydrochloric acid with the total weight percentage of 1.3% into the milky white liquid, dripping within two minutes, and preserving the temperature at 50 +/-5 ℃. Microencapsulation: and starting a stirrer, and stirring at a constant speed of 115r/min for 30 minutes to prepare the thiacloprid microcapsule suspension. Preparing a suspending agent: adding a solution prepared from 2.7% of polycarboxylate, 3% of glycerol, 0.14% of xanthan gum, 0.1% of kason, 0.9% of magnesium aluminum silicate and the balance of ultrapure water which is complemented to 100% into the microcapsule suspension, keeping the temperature at 50 +/-5 ℃, and uniformly stirring for 60 minutes at a stirring speed of 366 r/min. Finally obtaining the 4 percent thiacloprid microcapsule suspending agent.
Example four
Preparation of 10% thiacloprid microcapsule suspending agent
Preparing an oil phase: adding 10% of thiacloprid, 5% of polypropylene oxide, 3% of alkylphenol polyoxyethylene formaldehyde condensate sulfate, 2% of calcium dodecyl benzene sulfonate, 15% of caprylic/capric triglyceride and 13% of cyclohexanone into a reaction kettle together according to the weight percentage, raising the temperature of the reaction kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, starting a stirrer, and stirring at a constant speed of 665r/min for 30 minutes. Preparing a water phase: adding 30% of ultrapure water and 5% of polyacrylic acid into a shearing kettle, raising the temperature of the shearing kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, starting a stirrer, and stirring at a constant speed of 387r/min for 30 minutes. Emulsification: transferring the oil phase into the water phase, keeping the temperature at 50 +/-5 ℃, starting a stirrer to shear and stir for 20 minutes at a shear stirring speed of 11350r/min to obtain a milky liquid. Adjusting the pH value: adding hydrochloric acid with the total weight percentage of 1.8% into the milky white liquid, dripping within two minutes, and preserving the temperature at 50 +/-5 ℃. Microencapsulation: and starting a stirrer, and stirring at a constant speed of 186r/min for 30 minutes to prepare the thiacloprid microcapsule suspension. Preparing a suspending agent: adding a solution prepared from 3% of polycarboxylate, 2% of alkyl naphthalene formaldehyde condensate sulfonate, 5% of glycerol, 0.25% of xanthan gum, 0.2% of cason, 1.5% of magnesium aluminum silicate and the balance of ultrapure water which is supplemented to 100% into the microcapsule suspension, keeping the temperature at 50 +/-5 ℃, and uniformly stirring for 60 minutes at the constant speed of 451 r/min. Finally obtaining the 10 percent thiacloprid microcapsule suspending agent.
And (3) comparing the stability:
1.1, comparing the heat storage stability with the commercial 2% thiacloprid microcapsule suspending agent:
15 g of the obtained 2% thiacloprid microcapsule suspension and 15 g of the commercially available 2% thiacloprid microcapsule suspension are respectively placed in 3 ampoule bottles for sealing and are stored under heat at 54 ℃ for 2 weeks. After the end of the heat-storage, samples were taken for content measurement and observed for the degree of capsulorhexis using an electron microscope, the results of which are given in the following table:
| capsular formation rate before heat storage | Percentage of broken capsule after heat storage | |
| Products of the invention | 96.7％ | Is free of |
| A certain commercial product | 83.2％ | 30.3％ |
The results show that: the heat storage stability of the 2% thiacloprid microcapsule suspending agent is superior to that of the commercial 2% thiacloprid microcapsule suspending agent.
1.2, stability over time compared to a commercial 2% thiacloprid microcapsule suspension:
taking 15 g of each of the 2% thiacloprid microcapsule suspending agent obtained in the first step and the commercially available 2% thiacloprid microcapsule suspending agent, respectively placing the obtained two 15 g of the suspending agents in 3 ampoule bottles for sealing, placing the obtained product at normal temperature for 24 months, sampling for content measurement, and observing the capsule breaking degree by using an electron microscope, wherein the results are shown in the following table:
the results show that: the 2% thiacloprid microcapsule suspending agent provided by the invention hardly breaks the capsule after being placed for 24 months, and the stability with time is superior to that of the commercial 2% thiacloprid microcapsule suspending agent.
2.1, comparing the heat storage stability with the commercial 3% thiacloprid microcapsule suspending agent:
and (3) taking 15 g of the 3% thiacloprid microcapsule suspending agent obtained in the second step and 15 g of the commercially available 3% thiacloprid microcapsule suspending agent, respectively placing the suspending agent and the commercially available 3% thiacloprid microcapsule suspending agent into 3 ampoule bottles for sealing, and storing the suspending agent and the commercially available 3% thiacloprid microcapsule suspending agent in a hot state at 54 ℃ for 2 weeks. After the end of the heat-storage, samples were taken for content measurement and observed for the degree of capsulorhexis using an electron microscope, the results of which are given in the following table:
| content of thiacloprid before heat storage | Content of thiacloprid after heat storage | Draining water | |
| Products of the invention | 3.02％ | 3.01％ | 2.03％ |
| A certain commercial product | 3.05％ | 2.99％ | 4.94％ |
| Capsular formation rate before heat storage | Percentage of broken capsule after heat storage | |
| Products of the invention | 97.7％ | 0.6％ |
| A certain commercial product | 80.2％ | 32.3％ |
The results show that: the heat storage stability of the 3% thiacloprid microcapsule suspending agent is superior to that of the commercial 3% thiacloprid microcapsule suspending agent.
2.2, stability over time compared to a commercial 3% thiacloprid microcapsule suspension:
the prepared 3% thiacloprid microcapsule suspending agent (product obtained by the second implementation) and the commercially available 3% thiacloprid microcapsule suspending agent are respectively 15 g, the obtained suspending agents are respectively placed in 3 ampoule bottles for sealing, after 24 months of normal temperature placement, sampling is carried out for content measurement, and an electron microscope is used for observing the capsule breaking degree, and the results are shown in the following table:
the results show that: the 3% thiacloprid microcapsule suspending agent provided by the invention hardly breaks the capsule after being placed for 24 months, and the stability with time is superior to that of the commercial 3% thiacloprid microcapsule suspending agent.
3.1, comparing the heat storage stability with that of a common formula of 4% thiacloprid microcapsule suspending agent:
and (3) respectively placing 15 g of the 4% thiacloprid microcapsule suspending agent obtained in the step three and the 4% thiacloprid microcapsule suspending agent in the common formula in 3 ampoule bottles for sealing, and performing heat storage for 2 weeks at the temperature of 54 ℃. After the end of the heat-storage, samples were taken for content measurement and observed for the degree of capsulorhexis using an electron microscope, the results of which are given in the following table:
| content of thiacloprid before heat storage | Content of thiacloprid after heat storage | Draining water | |
| Products of the invention | 4.03％ | 4.01％ | 2.07％ |
| Common formula product | 4.07％ | 3.89％ | 7.94％ |
| Capsular formation rate before heat storage | Percentage of broken capsule after heat storage | |
| Products of the invention | 96.9％ | 1.1％ |
| Common formula product | 70.3％ | 46.3％ |
The results show that: the heat storage stability of the 4% thiacloprid microcapsule suspending agent is superior to that of the 4% thiacloprid microcapsule suspending agent in the common formula.
3.2, comparing the stability with the ordinary formula of 4% thiacloprid microcapsule suspending agent over time:
taking 15 g of the 4% thiacloprid microcapsule suspending agent obtained in the third implementation and 15 g of the 4% microcapsule suspending agent in the common formula, respectively placing the suspending agent and the 4% microcapsule suspending agent in 3 ampoule bottles for sealing, placing the ampoules at normal temperature for 24 months, sampling for content measurement, and observing the capsule breaking degree by using an electron microscope, wherein the results are shown in the following table:
the results show that: the 4% thiacloprid microcapsule suspending agent of the invention hardly breaks the capsule after being placed for 24 months, and the stability with time is superior to that of the 4% thiacloprid microcapsule suspending agent of the common formula.
4.1, comparing the heat storage stability with that of a common formula of 10% thiacloprid microcapsule suspending agent:
and respectively placing 15 g of the 10% thiacloprid microcapsule suspending agent obtained in the fourth step and 15 g of the 10% thiacloprid microcapsule suspending agent in the common formula into 3 ampoule bottles for sealing, and performing heat storage for 2 weeks at the temperature of 54 ℃. After the end of the heat-storage, samples were taken for content measurement and observed for the degree of capsulorhexis using an electron microscope, the results of which are given in the following table:
| content of thiacloprid before heat storage | Content of thiacloprid after heat storage | Draining water | |
| Products of the invention | 10.03％ | 9.95％ | 2.37％ |
| Common formula product | 10.07％ | 9.33％ | 20.32％ |
| Capsular formation rate before heat storage | Percentage of broken capsule after heat storage | |
| Products of the invention | 96.9％ | 3.9％ |
| Common formula product | 40.3％ | 86.3％ |
The results show that: the heat storage stability of the 10% thiacloprid microcapsule suspending agent is superior to that of the common formula, namely the 10% thiacloprid microcapsule suspending agent.
4.2, comparing the stability with the ordinary formula of 10% thiacloprid microcapsule suspending agent over time:
the prepared 10% thiacloprid microcapsule suspending agent (product obtained by the fourth step of the invention) and the common formula 10% microcapsule suspending agent are respectively 15 g, the obtained mixture is respectively placed in 3 ampoule bottles for sealing, the obtained product is placed at normal temperature for 24 months, a sample is taken for content measurement, and an electron microscope is used for observing the capsule breaking degree, and the results are shown in the following table:
the results show that: the 10% thiacloprid microcapsule suspending agent provided by the invention hardly breaks the capsule after being placed for 24 months, and the stability with time is superior to that of the ordinary formula, namely the 10% thiacloprid microcapsule suspending agent.
Those of ordinary skill in the art will understand that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An intelligent microcapsule suspension, comprising: according to weight percentage, 1-5% of polypropylene oxide, 2-5% of emulsifier, 2-10% of thiacloprid, 10-15% of caprylic/capric triglyceride, 5-15% of cyclohexanone, 1-5% of polyacrylic acid, 2-5% of surfactant, 0.1-0.3% of xanthan gum, 3-5% of glycerol, 0.1-0.3% of carbazone, 0.5-2% of magnesium aluminum silicate, 1-2% of hydrochloric acid and water are supplemented to 100%.
2. The intelligent microcapsule suspension of claim 1, wherein the emulsifier is selected from one or more of styrylphenol polyoxyethylene ether, alkylphenol polyoxyethylene polyether and sulfate or phosphate thereof, alkylphenol polyoxyethylene formaldehyde condensate sulfate, and calcium dodecylbenzene sulfonate.
3. The smart microcapsule suspension concentrate of claim 1, wherein the surfactant is selected from one or more of sodium naphthalene sulfonate formaldehyde condensate, alkyl phenol polyoxyethylene formaldehyde condensate sulfate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate, alkyl naphthalene formaldehyde condensate sulfonate, polymeric hydrophobic branched copolymer, and polymeric carboxylate.
4. A preparation method of an intelligent microcapsule suspending agent is characterized by comprising the following steps:
(1) preparing an oil phase: adding polypropylene oxide, caprylic/capric triglyceride, cyclohexanone, thiacloprid and an emulsifier into a reaction kettle, raising the temperature in the reaction kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, and uniformly stirring for 30 minutes;
(2) preparing a water phase: adding water and polyacrylic acid into a shearing kettle, raising the temperature in the shearing kettle to 50 ℃, keeping the temperature at 50 +/-5 ℃, and stirring at a constant speed for 30 minutes;
(3) emulsification: slowly adding the oil phase into the water phase, shearing and stirring, and fully shearing and stirring for 20 minutes to obtain a milky white liquid;
(4) adjusting the pH value: adding hydrochloric acid into the milky white liquid, and adjusting the pH value to 4;
(5) microencapsulation: stirring at constant speed for 30 minutes to obtain microcapsule suspension;
(6) preparing a suspending agent: adding a mixed solution of xanthan gum, glycerol, karson, magnesium aluminum silicate, a surfactant and water into the microcapsule suspension, and uniformly stirring for 60 minutes to obtain the microcapsule suspension.
5. The method for preparing the intelligent microcapsule suspension agent according to claim 4, wherein the uniform stirring speed in the step (1) is 500-700 r/min.
6. The method for preparing an intelligent microcapsule suspension agent according to claim 4, wherein the uniform stirring speed in the step (2) is 400 r/min.
7. The method for preparing a smart microcapsule suspension according to claim 4, wherein the shear stirring rate in step (3) is 7000-12000 r/min.
8. The method for preparing a smart microcapsule suspension according to claim 4, wherein the hydrochloric acid is added dropwise within 2min in the step (4).
9. The method for preparing an intelligent microcapsule suspension agent according to claim 4, wherein the uniform stirring speed in the step (5) is 100-200 r/min.
10. The method for preparing an intelligent microcapsule suspension agent according to claim 4, wherein the uniform stirring speed in step (6) is 300-500 r/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111418583A (en) * | 2020-05-01 | 2020-07-17 | 利民化学有限责任公司 | Prothioconazole intelligent microcapsule suspending agent and preparation method thereof |
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