CN112106769A - Emamectin benzoate dry suspending agent and preparation method thereof - Google Patents

Emamectin benzoate dry suspending agent and preparation method thereof Download PDF

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CN112106769A
CN112106769A CN202010951994.0A CN202010951994A CN112106769A CN 112106769 A CN112106769 A CN 112106769A CN 202010951994 A CN202010951994 A CN 202010951994A CN 112106769 A CN112106769 A CN 112106769A
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emamectin benzoate
agent
dry suspending
suspending agent
benzoate dry
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谭葵
莫俊锐
王爱臣
廖联安
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Huizhou Yinnong Technology Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/12Powders or granules
    • A01N25/14Powders or granules wettable
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/32Ingredients for reducing the noxious effect of the active substances to organisms other than pests, e.g. toxicity reducing compositions, self-destructing compositions
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system

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Abstract

The application provides an emamectin benzoate dry suspending agent and a preparation method thereof. The emamectin benzoate dry suspending agent comprises the following components in parts by mass: 5-15 parts of emamectin benzoate; 20-40 parts of a dispersing agent; 2-8 parts of a wetting agent; 1-5 parts of a disintegration aid; 0.5 to 1 portion of anti-decomposition agent; 50-70 parts of filler; 0.5 to 1 portion of defoaming agent. The emamectin benzoate dry suspending agent has good dispersibility, suspension rate and drug effect.

Description

Emamectin benzoate dry suspending agent and preparation method thereof
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to an emamectin benzoate dry suspending agent and a preparation method thereof.
Background
Currently, emamectin benzoate (emamectin benzoate, abbreviated as emamectin benzoate) is developed by Merck & Co in the united states, and is a novel high-efficiency semi-synthetic antibiotic pesticide synthesized by taking a fermentation product, abamectin B1, as a raw material. It has stomach toxicity, contact poisoning and strong penetrating action, has the characteristics of super-high efficiency, low toxicity, low residue, no public nuisance and other biological pesticides, is a mainstream product of pesticides in the current market, and is widely applied to different crops. Emamectin benzoate has the effect of enhancing neuronal activity such as glutamate and gamma-aminobutyric acid (GABA), thereby allowing large amounts of chloride ions to enter nerve cells, causing loss of cell function, disrupting nerve conduction, and allowing larvae to stop feeding immediately after contact, with irreversible paralysis, and maximal lethality within 3-4 days. Because the compound pesticide is tightly combined with soil, does not leach and accumulate in the environment, can be transferred by Translaminar movement, is easily absorbed by crops and permeates into the epidermis, so that the pesticide-applied crops have long-term residual effect, a second insecticidal lethality peak appears more than 10 days, and meanwhile, the compound pesticide is rarely influenced by environmental factors such as wind, rain and the like.
The dry suspending agent (DF) is formed by dehydrating an aqueous suspension system, is a novel formulation with great development prospect, is essentially the same as water dispersible granules, and has the difference that the dry suspending agent is prepared by wet grinding granulation, namely, the dry suspending agent is processed into the aqueous suspending agent and then is prepared into a finished product by spray drying granulation, so the finished product is generally in a small round sphere shape in appearance, while the main stream of the water dispersible granules is a dry process technology, the existing dry suspending agent is extrusion granulation and fluidized bed granulation, and the finished product is in a column shape or a sphere shape.
The fineness of natural particles after the dry suspending agent is diluted can reach 1-5 mu m generally, is obviously better than 10-40 mu m of the product diluted in water of the traditional water dispersible granule dry granulation, the fineness is obviously improved, and the suspension rate, the dispersibility and the drug effect performance can be directly improved.
In addition, as wet grinding, spray drying and granulation are adopted, the dust harm is basically avoided, the working environment of a workshop is greatly improved, and the method is greatly beneficial to the environment and the health of workers.
However, the existing emamectin benzoate dry suspending agent still has the problems of poor suspension rate, poor dispersibility and poor drug effect.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the emamectin benzoate dry suspending agent with good suspension rate, dispersibility and drug effect and the preparation method thereof.
The emamectin benzoate dry suspending agent comprises the following components in parts by mass:
Figure BDA0002677306760000021
in one embodiment, the dispersant is at least one of a polycarboxylate-type dispersant, a lignosulfonate-type dispersant, an alkyl naphthalene sulfonate formaldehyde condensate, and sodium methylene dinaphthalene sulfonate.
In one embodiment, the wetting agent is at least one of a sulfonate wetting agent, a sulfate wetting agent, a benzenesulfonate wetting agent, an alkylnaphthalenesulfonate anion wetting agent, and sodium lauryl sulfate.
In one embodiment, the filler is at least one of calcined kaolin, light calcium carbonate, corn starch, diatomaceous earth, precipitated barium sulfate, white carbon, and inert clay.
In one embodiment, the disintegration aid is at least one of glucose, urea, and ammonium sulfate.
In one embodiment, the anti-decomposition agent is at least one of PG, TBHQ, BHA, and BHT.
A preparation method of emamectin benzoate dry suspending agent comprises the following steps:
adding a dispersing agent, a wetting agent, a disintegrating aid, an anti-decomposition agent and a defoaming agent into water for mixing operation to obtain a mixed solution;
adding emamectin benzoate and a filler into the mixed solution for dispersion operation to obtain a mixture;
crushing and grinding the mixture to obtain mixed slurry; and
and carrying out spray drying operation on the mixed slurry to obtain the emamectin benzoate dry suspending agent.
In one embodiment, the dispersion operation is performed by using a homogenizer, the working speed of the homogenizer is 1400 r/min-1500 r/min, and the time of the dispersion operation is 25 min-35 min.
In one embodiment, the pulverizing and grinding operation specifically includes the steps of:
crushing the mixture by a sand mill to obtain a crushed material;
and grinding the crushed material by using a sand mill to obtain a ground material, wherein the stop node of the grinding operation is that the material particle size D98 in the ground material is not more than 4 mu m.
In one embodiment, the spray drying operation specifically comprises:
spray drying and screening are carried out by adopting a pressure type spray dryer to obtain the emamectin benzoate dry suspending agent, wherein the temperature of the spray drying is 110-140 ℃.
Compared with the prior art, the invention has at least the following advantages:
in the emamectin benzoate dry suspending agent, the suspending rate and the dispersibility of the emamectin benzoate are improved by using the dispersing agent, the wetting agent, the disintegration assistant and the filler, the decomposition rate of the emamectin benzoate is reduced by the decomposition resisting agent, and the pharmacodynamic performance of the emamectin benzoate is improved. Namely, the emamectin benzoate dry suspending agent prepared by adding the dispersing agent, the wetting agent, the disintegration aid, the filler and the anti-decomposition agent has better suspension rate, dispersibility and pharmacodynamic property.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a flow chart of the steps of the preparation method of emamectin benzoate dry suspension according to an embodiment of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The application provides an emamectin benzoate dry suspending agent. The emamectin benzoate dry suspending agent comprises the following components in parts by mass: 5-15 parts of emamectin benzoate; 20-40 parts of a dispersing agent; 2-8 parts of a wetting agent; 1-5 parts of a disintegration aid; 0.5 to 1 portion of anti-decomposition agent; 50-70 parts of filler; 0.5 to 1 portion of defoaming agent.
In the emamectin benzoate dry suspending agent, the suspending rate and the dispersibility of the emamectin benzoate are improved by using the dispersing agent, the wetting agent, the disintegrating aid and the filler, the decomposition rate of the emamectin benzoate is reduced by the anti-decomposition agent, and the pharmacodynamical performance of the emamectin benzoate is improved. Namely, the emamectin benzoate dry suspending agent prepared by adding the dispersing agent, the wetting agent, the disintegration aid, the filler and the anti-decomposition agent has better suspension rate, dispersibility and pharmacodynamic property.
For better understanding of the emamectin benzoate dry suspension of the present application, the following further explains the emamectin benzoate dry suspension of the present application, an embodiment of which is emamectin benzoate dry suspension. The emamectin benzoate dry suspending agent comprises the following components in parts by mass: 5-15 parts of emamectin benzoate; 20-40 parts of a dispersing agent; 2-8 parts of a wetting agent; 1-5 parts of a disintegration aid; 0.5 to 1 portion of anti-decomposition agent; 50-70 parts of filler; 0.5 to 1 portion of defoaming agent.
In the emamectin benzoate dry suspending agent, the emamectin benzoate is prepared into the emamectin benzoate dry suspending agent, so that the photolysis rate of the emamectin benzoate is reduced, the pharmacodynamic performance of the emamectin benzoate is improved, and the dispersibility of the emamectin benzoate is improved. The wetting agent increases the surface wettability of the emamectin benzoate, and further improves the dispersibility of the emamectin benzoate dry suspending agent. The dispersing agent and the emamectin benzoate have good binding capacity, the dispersion stability of the emamectin benzoate is improved, and the speed of forming a stable dispersion system by the emamectin benzoate is improved. The disintegration aid has the effect of quickly dispersing emamectin benzoate particles in water, so that the emamectin benzoate can quickly form a stable system in the water. The wetting agent, the disintegration assistant and the dispersing agent act together, so that the suspension rate and the dispersibility anti-decomposition agent of the emamectin benzoate dry suspending agent are improved, the decomposition rate of the emamectin benzoate is reduced, the stability of the emamectin benzoate dry suspending agent is improved, and the pesticide effect of the emamectin benzoate dry suspending agent is further improved. The filler accelerates the dissolving and dispersing speed of the emamectin benzoate, and further improves the stability and the dispersion uniformity of the emamectin benzoate dry suspending agent. The defoaming agent is used for eliminating foam generated in the preparation process of the emamectin benzoate, so that the dispersibility and stability of the emamectin benzoate are improved. The dispersant, the wetting agent, the disintegrating aid and the filler are used in a matched mode, and the anti-decomposition agent is added in parts by mass, so that the dispersion stability and the drug effect stability of the emamectin benzoate are effectively improved, and the suspension rate, the dispersibility and the drug effect performance of the emamectin benzoate dry suspension agent are further improved.
In one embodiment, the dispersant is at least one of a polycarboxylate-type dispersant, a lignosulfonate-type dispersant, an alkyl naphthalene sulfonate formaldehyde condensate, and sodium methylene dinaphthalene sulfonate. The polycarboxylate dispersant, the lignosulfonate dispersant, the alkyl naphthalene sulfonate formaldehyde condensate and the sodium methylene dinaphthalene sulfonate have good dispersing effect on the emamectin benzoate, and the dispersibility and the stability of the emamectin benzoate dry suspending agent are improved.
In one embodiment, the polycarboxylate type dispersant is at least one of D518, Tersperse2700, YUS-WG7, D800, and 550S. It is understood that the main component of D518 is a sodium polycarboxylate salt. Tersperse2700 has a sodium polycarboxylate salt as a main component. The main component of YUS-WG7 is a sodium salt of a polycarboxylic acid. The main component of D800 is a sodium polycarboxylate. The active ingredient of 550S is a sodium polycarboxylate. D518, Tersperse2700, YUS-WG7, D800 and 550S have good dispersing effect on emamectin benzoate, and the dispersibility of the emamectin benzoate dry suspending agent is improved.
In one embodiment, the lignosulfonate dispersant is at least one of Reax910, ReaxAG, ultrazinen a, Ufoxane3A, 603W, and JRNS 1. The main component of Reax910 is sodium lignosulfonate. The main component of ReaxAG is sodium lignosulfonate. The main component of UltrazineNA is sodium lignosulfonate. The main component of Ufoxane3A is sodium lignosulfonate. 603W contains sodium lignosulfonate as main component. The main component of JRNS1 is sodium lignosulfonate. It can be understood that the Reax910, the ReaxAG, the UltrazineNA, the Ufoxane3A, the UltrazineW and the JRNS1 have better affinity with the emamectin benzoate, and the problem of poor dispersibility of the emamectin benzoate dry suspending agent caused by coagulation of the emamectin benzoate in the process of preparing the emamectin benzoate dry suspending agent is avoided, namely the dispersibility of the emamectin benzoate dry suspending agent is improved.
In one embodiment, the alkyl naphthalene sulfonate formaldehyde condensate is at least one of Morwet D-425, PSR 19, and BB 4. The main component of the Morwet D-425 is alkyl naphthalene sulfonic acid formaldehyde condensation polymer sodium salt. The main component of PSR 19 is an ammonium arylsulfonate polymer. The main component of BB4 is polynaphthalene formaldehyde sulfonic acid sodium salt. It can be understood that the Morwet D-425, PSR 19 and BB4 have good dispersing effect on the emamectin benzoate, and the stability of the emamectin benzoate dry suspending agent is promoted.
It can be understood that emamectin benzoate is easily decomposed by light, in order to meet the requirement that the obtained emamectin benzoate dry suspending agent has better sample indexes, the appearance is generally set to be white or light color, therefore, the emamectin benzoate dry suspending agent needs to be stored away from light, but in the actual transportation and storage processes, the light-resistant storage is difficult to achieve, so that the problem of reduced drug efficacy performance of the emamectin benzoate dry suspending agent is caused, and in order to avoid the problems of reduced drug efficacy and reduced utilization rate of the emamectin benzoate dry suspending agent in the actual transportation and storage processes, in one embodiment, the dispersing agent at least comprises lignosulfonate. It can also be understood that the lignosulfonate is a brown dispersant, so that the emamectin benzoate dry suspending agent is brown, the emamectin benzoate is protected, the decomposition rate of the emamectin benzoate is reduced, and the stability of the emamectin benzoate dry suspending agent in the transportation and storage processes is improved.
In one embodiment, the wetting agent is at least one of a sulfonate wetting agent, a sulfate wetting agent, a benzenesulfonate wetting agent, an alkylnaphthalenesulfonate anion wetting agent, and sodium lauryl sulfate. It can be understood that the sulfonate wetting agent, the sulfate wetting agent, the benzenesulfonate wetting agent, the alkylnaphthalenesulfonate anion wetting agent and the sodium dodecyl sulfate improve the surface wetting effect of the emamectin benzoate, improve the dispersibility of the emamectin benzoate, and further improve the dispersibility and the suspension rate of the emamectin benzoate dry suspending agent.
In one embodiment, the sulfonate wetting agent is at least one of L/WET-P, L/WET-MAX, YUS-SXC, and DR 40. The main component of the L/WET-P is alkyl sulfonate. The main component of L/WET-MAX is alkyl sulfonate. The main component of YUS-SXC is sodium dodecyl benzene sulfonate. The major component of DR40 is alkylnaphthalene sulfonate. It can be understood that the L/WET-P, L/WET-MAX, YUS-SXC and DR40 effectively reduce the surface tension of the emamectin benzoate, further improve the surface wetting effect of the emamectin benzoate, and further improve the dispersibility and the suspension rate of the emamectin benzoate dry suspending agent.
In one embodiment, the sulfate-based wetting agent is YUS-LXC. The main component of YUS-LXC is sodium tridecyl sulfate. It can be understood that the affinity between YUS-LXC and emamectin benzoate is better, the wetting effect of the surface of the emamectin benzoate is better improved, and the dispersibility and the suspension rate of the emamectin benzoate dry suspending agent are further improved.
In one embodiment, the benzenesulfonate wetting agent is YUS-TXC. The main component of YUS-TXC is phenolsulfonic acid phenol formaldehyde urea polycondensate sodium salt. It can be understood that the affinity between YUS-TXC and emamectin benzoate is better, the wetting effect of the surface of the emamectin benzoate is better improved, and the dispersibility and the suspension rate of the emamectin benzoate dry suspending agent are further improved.
In one embodiment, the alkylnaphthalene sulfonate anionic wetting agent is MorwetEFW. The main component of MorwetEFW is alkyl naphthyl sodium sulfate. It can be understood that the MorwetEFW has good water solubility, improves the wetting speed of the emamectin benzoate, has good surface wetting effect on the emamectin benzoate, and improves the dispersibility and the suspension rate of the emamectin benzoate dry suspending agent.
In one embodiment, the filler is at least one of calcined kaolin, light calcium carbonate, corn starch, diatomaceous earth, precipitated barium sulfate, white carbon, and inert clay. It can be understood that the calcined kaolin, the light calcium carbonate, the corn starch, the diatomite, the precipitated barium sulfate, the white carbon black and the inert clay have relatively proper viscosity strength after being wetted, and are beneficial to improving the granulation effect of the emamectin benzoate, so that the emamectin benzoate dry suspending agent has relatively good suspension rate.
It will be appreciated that, since the emamectin benzoate dry suspension is used as a crop pesticide, the acid or base substances in the dry suspension have a greater effect on the soil in which the crop is growing, which further aggravates the acidification and salinization of the soil and thus affects the growth of the crop, and therefore, in order to reduce the effect of the emamectin benzoate dry suspension on the growth of the crop, in one embodiment, the filler comprises at least precipitated barium sulfate. It can also be understood that the commonly used filler is a meta-acid or meta-alkali substance, which aggravates the acid-alkalization of the soil, destroys the soil environment for the growth of crops, and in order to avoid the acid-alkalization of the soil, further reduces the influence of the emamectin benzoate dry suspending agent on the growth of crops.
In one embodiment, the disintegration aid is at least one of glucose, urea, and ammonium sulfate. It can be understood that, because the emamectin benzoate is slightly soluble in water, the emamectin benzoate cannot be rapidly and stably dissolved in water, that is, the dispersibility and the suspension rate of the emamectin benzoate dry suspension agent are reduced, therefore, at least one of glucose, urea and ammonium sulfate is added into the emamectin benzoate, and the glucose, the urea and the ammonium sulfate can rapidly disperse the emamectin benzoate particles, so that the emamectin benzoate can rapidly form a stable system. The effect of mixing two or more of glucose, urea and ammonium sulfate is more excellent.
In one embodiment, the anti-disintegration agent is at least one of PG, TBHQ, BHA, and BHT. The main component of PG is propyl gallate. The main component of TBHQ is tert-butylhydroquinone. The major component of BHA is butylated hydroxyanisole. The main component of BHT is dibutylhydroxytoluene. It can be understood that, because the emamectin benzoate is easily affected by factors such as acid and alkali, and light, the emamectin benzoate is decomposed to reduce the utilization rate of the emamectin benzoate, that is, the drug effect of the emamectin benzoate is reduced, therefore, at least one of PG, TBHQ, BHA and BHT is added to the emamectin benzoate, and the PG, TBHQ, BHA and BHT all improve the stability of the emamectin benzoate and the utilization rate of the emamectin benzoate, and the effect of mixing two or more of the anti-decomposition agents PG, TBHQ, BHA and BHT is better.
It is further emphasized that the combination of dispersant Ufoxane3A and filler precipitated barium sulfate was found to be consistent with the integrity of the combination over a number of experiments.
In one embodiment, the defoamer is at least one of an organosiloxane, an organosilicone, AF1501, SAG1572, DDF, and CJK. The main component of AF1501 is a modified organopolysiloxane mixture. The main component of SAG1572 was silicone. The main component of DDF is a fatty acid salt. The main component of CJK is polyether fatty acid ester. It can be understood that the organic siloxane, the organic silicone, the AF1501, the SAG1572, the DDF and the CJK have strong bubble eliminating effect, and eliminate foams generated in the preparation process of the emamectin benzoate, so that the dispersibility and the stability of the emamectin benzoate are improved. In order to better understand the emamectin benzoate dry suspending agent, the application also provides a preparation method of the emamectin benzoate dry suspending agent. The preparation method of the emamectin benzoate dry suspending agent comprises the following steps: adding a dispersing agent, a wetting agent, a disintegrating aid, an anti-decomposition agent and a defoaming agent into water for mixing operation to obtain a mixed solution; adding emamectin benzoate and a filler into the mixed solution for dispersion operation to obtain a mixture; crushing and grinding the mixture to obtain mixed slurry; and carrying out spray drying operation on the mixed slurry to obtain the emamectin benzoate dry suspending agent.
The preparation method of the emamectin benzoate dry suspending agent is simple in steps, and the obtained emamectin benzoate dry suspending agent has good sample indexes and has high suspension rate, dispersibility and pharmacodynamic properties by controlling the adding sequence of the dispersing agent, the wetting agent, the disintegration aid, the decomposition resisting agent, the defoaming agent, the emamectin benzoate and the filler.
In order to better understand the preparation method of the emamectin benzoate dry suspending agent, the following further explains the preparation method of the emamectin benzoate dry suspending agent, and the preparation method of the emamectin benzoate dry suspending agent of one embodiment comprises the following steps:
s100, adding a dispersing agent, a wetting agent, a disintegrating aid, an anti-decomposition agent and a defoaming agent into water for mixing operation to obtain a mixed solution. When the emamectin benzoate dry suspending agent is prepared, the dispersing agent, the wetting agent, the disintegration assistant, the anti-decomposition agent and the defoaming agent act together to improve the stability and the dispersibility of the emamectin benzoate, so that the suspension rate, the dispersibility and the pharmacodynamic performance of the emamectin benzoate dry suspending agent are effectively improved, and the stability of the emamectin benzoate dry suspending agent is improved.
S200, adding the emamectin benzoate and the filler into the mixed solution for dispersion operation to obtain a mixture. The water solubility of the emamectin benzoate is poor, and the emamectin benzoate is directly dissolved in water to be difficult to form a stable dispersion system, so that the dissolution and dispersion of the emamectin benzoate can be accelerated by adding the filler, and the stability and the dispersion uniformity of the emamectin benzoate are improved.
And S300, crushing and grinding the mixture to obtain mixed slurry. After grinding, the particle size of the mixture is reduced, so that the particle size of the mixture is more uniform, and the components in the obtained mixed slurry are uniformly mixed.
S400, carrying out spray drying operation on the mixed slurry to obtain the emamectin benzoate dry suspending agent.
The preparation method of the emamectin benzoate dry suspending agent is simple in steps, and the obtained emamectin benzoate dry suspending agent has good sample indexes and has high suspension rate, dispersibility and pharmacodynamic properties by controlling the adding sequence of the dispersing agent, the wetting agent, the disintegration aid, the decomposition resisting agent, the defoaming agent, the emamectin benzoate and the filler.
In one embodiment, a homogenizer is adopted for dispersion operation, the working rotating speed of the homogenizer is 1400 r/min-1500 r/min, and the time of the dispersion operation is 25 min-35 min. The mixture obtained after mixing at the rotating speed of 1400-1500 r/min and the dispersion time of 25-35 min has high dispersion uniformity, so that the prepared emamectin benzoate dry suspending agent has high suspension rate and dispersibility.
In one embodiment, the pulverizing and grinding operation specifically comprises the steps of:
and (4) crushing the mixture by using a sand mill to obtain a crushed material. The purpose of the crushing operation is to reduce the particle size of particles in the mixture, further reduce the particle size of the emamectin benzoate dry suspending agent, and further improve the dispersibility and the suspension rate of the emamectin benzoate dry suspending agent.
And grinding the crushed material by a sand mill to obtain a ground material, wherein the stop node of the grinding operation is that the material particle size D98 in the ground material is not more than 4 mu m. After grinding, the particle size of the mixture is further reduced, the mixture has better particle size distribution uniformity, and the dispersibility and the suspension rate of the emamectin benzoate dry suspending agent are further improved.
In one embodiment, the mixture is pulverized by a colloid mill to obtain a pulverized material. It can be understood that the colloid mill and the sand mill have good pulverization effect on the mixture, and the uniformity of the particle size of the pulverized material is improved.
It should be noted that the particle size D98 of the material is 4 μm or less, which means that the number of particles having a particle size of 4 μm or less in the ground material is 98% of the total number of particles.
In one embodiment, the water comprises the following components in parts by mass: 90 to 120 portions. It can be understood that too much water can cause too high water content of the sample during spray drying, and the energy consumption of the spray drying is increased; too little water addition can degrade the mobile phase of the mixed slurry, thereby reducing the efficiency of spray drying.
In one embodiment, the spray drying operation specifically comprises: spray drying and screening are carried out by adopting a pressure type spray dryer to obtain the emamectin benzoate dry suspending agent, wherein the temperature of spray drying is 110-140 ℃. It can be understood that if the drying temperature of the spray drying is too low, the moisture of the emamectin benzoate dry suspending agent is too high, and the stability of the emamectin benzoate dry suspending agent is reduced; if the temperature is too high, the activity of the emamectin benzoate dry suspending agent is damaged, the pharmacodynamic performance of the emamectin benzoate dry suspending agent is reduced, and the sample index of the emamectin benzoate dry suspending agent cannot meet the requirement.
Further, in one embodiment, the spray-drying operation is performed on the mixed slurry using a spray dryer in the present operation, wherein the spray dryer is operated at an environment of 130 ℃. The emamectin benzoate dry suspending agent obtained by performing spray drying operation on the mixed slurry at 130 ℃ has better stability, pharmacodynamic performance and sample indexes.
In one embodiment, the water content of the emamectin benzoate dry suspending agent is less than or equal to 3 percent of the total mass of the emamectin benzoate dry suspending agent. It can be understood that the sample index of the emamectin benzoate dry suspending agent cannot meet the requirement due to the excessively high or low water content, and the stability of the emamectin benzoate dry suspending agent is reduced due to the excessively high water content.
Some specific examples are listed below, and if mentioned%, all are expressed in weight percent. It should be noted that the following examples are not intended to be exhaustive of all possible cases, and that the materials used in the following examples are commercially available without specific recitation.
The compositions and contents of examples 1 to 7 are shown in Table 1:
Figure BDA0002677306760000121
Figure BDA0002677306760000131
table 1: the compositions and contents of examples 1 to 7
The emamectin benzoate dry suspending agents of examples 1 to 7 were prepared by the following preparation methods of emamectin benzoate dry suspending agents, respectively:
example 8
Adding a dispersing agent, a wetting agent, a disintegrating aid, an anti-decomposition agent and a defoaming agent into water, stirring and dissolving;
continuously adding emamectin benzoate, uniformly stirring, then supplementing to 100kg by using calcined kaolin filler, and performing mean value dispersion for 25min by using a homogenizer at the rotating speed of 1400 r/min;
crushing the substances by a sand mill to ensure that the particle size D98 of each substance is less than or equal to 2 mu m;
and (3) placing the crushed substances into a pressure type spray dryer, carrying out spray drying at 125 ℃, and screening to obtain the emamectin benzoate dry suspending agent.
Example 9
Adding a dispersing agent, a wetting agent, a disintegrating aid, an anti-decomposition agent and a defoaming agent into water, stirring and dissolving;
continuously adding emamectin benzoate, uniformly stirring, then supplementing to 100kg with a filler, and performing mean value dispersion for 30min by using a homogenizer at the rotating speed of 1470 r/min;
crushing the substances by a sand mill to ensure that the particle size D98 of each substance is less than or equal to 3 mu m;
and (3) placing the crushed substances into a pressure type spray dryer, carrying out spray drying and screening at 130 ℃ to obtain the emamectin benzoate dry suspending agent.
Example 10
Adding a dispersing agent, a wetting agent, a disintegrating aid, an anti-decomposition agent and a defoaming agent into water, stirring and dissolving;
continuously adding emamectin benzoate, uniformly stirring, then supplementing to 100kg by using calcined kaolin filler, and performing mean value dispersion for 35min by using a homogenizer at the rotating speed of 1500 r/min;
crushing the substances by a sand mill to ensure that the particle size D98 of the substances is less than or equal to 4 mu m;
and (3) placing the crushed substances into a pressure type spray dryer, carrying out spray drying at 140 ℃, and screening to obtain the emamectin benzoate dry suspending agent.
The following performance tests were performed on the emamectin benzoate dry suspending agents of examples 1 to 7 respectively obtained by the preparation method of the emamectin benzoate dry suspending agent of example 9.
Test 1
Test objects:
test groups: the emamectin benzoate dry suspending agents of the embodiments 1 to 7 are respectively obtained according to the preparation method of the emamectin benzoate dry suspending agent of the embodiment 9;
comparison group: (the components and contents of comparative groups 1 to 5 are shown in Table 2)
Figure BDA0002677306760000151
Table 2: the components and contents of comparative groups 1 to 5
The preparation method of the emamectin benzoate dry suspending agent in the comparative examples 1-5 comprises the following steps:
adding dispersant, wetting agent, disintegrating aid, anti-decomposition agent (if not added) and defoaming agent (if not added) into water, stirring and dissolving;
continuously adding emamectin benzoate, stirring uniformly, then supplementing to 100kg with light calcium carbonate filler or calcined kaolin, and performing mean value dispersion for 30min by using a homogenizer at the rotation speed of 1470 r/min;
crushing the substances by a sand mill to ensure that the particle size D98 of each substance is less than or equal to 4 mu m;
and (3) placing the crushed substances into a pressure type spray dryer, carrying out spray drying and screening at 130 ℃ to obtain the emamectin benzoate dry suspending agent.
The purpose is as follows:
the emamectin benzoate dry suspensions of examples 1 to 7 obtained by the methods 1 to 3 were subjected to slurry viscosity (mPa · s), disintegration time(s), suspension percentage (%), permanent foaming amount (mL), heat storage decomposition rate (%), suspension percentage after heat storage (%) and disintegration time after heat storage(s) tests.
As a result:
the performance test data of the emamectin benzoate dry suspending agents of examples 1 to 7 respectively obtained by the preparation method of the emamectin benzoate dry suspending agent of example 9 and the emamectin benzoate dry suspending agents of comparative examples 1 to 5 respectively obtained by the preparation method of the emamectin benzoate dry suspending agents of comparative examples 1 to 5 are shown in table 3:
Figure BDA0002677306760000161
table 3: results of performance tests on methylamino abamectin benzoate dry suspending agent in examples 1-7 and comparative examples 1-5
And (3) testing results:
as can be seen from table 2, the disintegration time and the suspension rate of the emamectin benzoate dry suspending agent in examples 1 to 7 are higher than those of the emamectin benzoate dry suspending agent in comparative examples 1 to 5, which indicates that the emamectin benzoate dry suspending agent in examples 1 to 7 has better dispersibility and suspension rate. The heat storage decomposition rate of the emamectin benzoate dry suspending agents in the examples 1 to 7 is lower than that of the emamectin benzoate dry suspending agents in the comparative examples 1 to 5, the suspension rate of the emamectin benzoate dry suspending agents in the examples 1 to 7 and the disintegration time of the emamectin benzoate dry suspending agents in the comparative examples 1 to 5 after heat storage are changed slightly, and the suspension rate of the emamectin benzoate dry suspending agents in the examples 1 to 7 after heat storage is changed slightly compared with that of the emamectin benzoate dry suspending agents in the comparative examples 1 to 5, so that the emamectin benzoate dry suspending agents in the examples 1 to 7 are higher in heat stability.
Test 2
The test method comprises the following steps:
adding a dispersing agent, a wetting agent, a disintegrating aid, an anti-decomposition agent and a defoaming agent into water, stirring and dissolving;
continuously adding emamectin benzoate, uniformly stirring, then supplementing to 100kg by using calcined kaolin filler, and performing mean value dispersion for 35min by using a homogenizer at the rotating speed of 1500 r/min;
crushing the substances by a sand mill to ensure that the particle size D98 of the substances is less than or equal to 4 mu m;
and (3) placing the crushed substances into a pressure type spray dryer, carrying out spray drying and screening at the temperature of X ℃ to obtain the emamectin benzoate dry suspending agent.
The above X ℃ is 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃ and 150 ℃, respectively.
Test objects:
test groups: the emamectin benzoate dry suspensions of examples 4-1, 4-2, 4-3, 4-4, 4-5 and 4-6, which have the same composition and content as those of example 4, were obtained by the above-mentioned test methods.
The test purpose is as follows:
the emamectin benzoate dry suspending agent obtained in the example 4-1 to 4-6 by the test method is subjected to moisture (%), disintegration time(s), suspension rate after heat storage (%) and heat storage decomposition rate (%).
And (3) testing results:
the performance test data of the emamectin benzoate dry suspending agent of the embodiments 4-1 to 4-6 respectively obtained by the test method are shown in the table 4:
Figure BDA0002677306760000181
table 4: performance test data of emamectin benzoate dry suspending agent of example 4-1 to 4-6
And (3) testing results:
as can be seen from table 4, in the preparation process of the emamectin benzoate dry suspending agent, when the spray drying temperature is 110 ℃ to 140 ℃, the moisture content of the emamectin benzoate dry suspending agent is relatively good, and the emamectin benzoate dry suspending agent has relatively short disintegration time, relatively high suspension rate and relatively good thermal stability.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. The emamectin benzoate dry suspending agent is characterized by comprising the following components in parts by mass:
Figure FDA0002677306750000011
2. an emamectin benzoate dry suspension according to claim 1, wherein the dispersant is at least one of a polycarboxylate dispersant, a lignosulfonate dispersant, an alkyl naphthalene sulfonate formaldehyde condensate and sodium methylene dinaphthalenesulfonate.
3. An emamectin benzoate dry suspension of claim 1, wherein the wetting agent is at least one of a sulfonate wetting agent, a sulfate wetting agent, a benzenesulfonate wetting agent, an alkylnaphthalenesulfonate anionic wetting agent, and sodium lauryl sulfate.
4. Emamectin benzoate dry suspension according to claim 1, wherein the filler is at least one of calcined kaolin, light calcium carbonate, corn starch, diatomaceous earth, precipitated barium sulfate, white carbon and inert clay.
5. Emamectin benzoate dry suspension according to claim 1, wherein the disintegration aid is at least one of glucose, urea and ammonium sulphate.
6. The emamectin benzoate dry suspension of claim 1, wherein said anti-decomposition agent is at least one of PG, TBHQ, BHA and BHT.
7. A preparation method of emamectin benzoate dry suspending agent is characterized by comprising the following steps:
adding a dispersing agent, a wetting agent, a disintegrating aid, an anti-decomposition agent and a defoaming agent into water for mixing operation to obtain a mixed solution;
adding emamectin benzoate and a filler into the mixed solution for dispersion operation to obtain a mixture;
crushing and grinding the mixture to obtain mixed slurry; and
and carrying out spray drying operation on the mixed slurry to obtain the emamectin benzoate dry suspending agent.
8. The preparation method of emamectin benzoate dry suspending agent according to claim 7, wherein a homogenizer is used for the dispersion operation, the working speed of the homogenizer is 1400 r/min-1500 r/min, and the dispersion operation time is 25 min-35 min.
9. The preparation method of emamectin benzoate dry suspending agent according to claim 7, wherein the crushing and grinding operation comprises the following steps:
coarsely crushing the mixture by using a colloid mill to obtain a crushed material;
and grinding the crushed material by using a sand mill to obtain a ground material, wherein the stop node of the grinding operation is that the material particle size D98 in the ground material is not more than 4 mu m.
10. The preparation method of emamectin benzoate dry suspension according to claim 7, wherein the spray drying operation specifically comprises:
spray drying and screening are carried out by adopting a pressure type spray dryer to obtain the emamectin benzoate dry suspending agent, wherein the temperature of the spray drying is 110-140 ℃.
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CN112155011A (en) * 2020-09-17 2021-01-01 惠州市银农科技股份有限公司 Emamectin benzoate microcapsule suspending agent and preparation method thereof
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CN113498782A (en) * 2021-08-03 2021-10-15 惠州市银农科技股份有限公司 Emamectin benzoate nano preparation based on zein and preparation method thereof
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CN115956561A (en) * 2023-02-13 2023-04-14 惠州市银农科技股份有限公司 Emamectin benzoate nano dry suspending agent and preparation method thereof

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