CN111345301A - Brassinolide soluble granule and preparation method thereof - Google Patents
Brassinolide soluble granule and preparation method thereof Download PDFInfo
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- CN111345301A CN111345301A CN202010284674.4A CN202010284674A CN111345301A CN 111345301 A CN111345301 A CN 111345301A CN 202010284674 A CN202010284674 A CN 202010284674A CN 111345301 A CN111345301 A CN 111345301A
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- brassinolide
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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
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/22—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom rings with more than six members
-
- 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
- A01N25/12—Powders or granules
- A01N25/14—Powders or granules wettable
-
- 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
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a brassinolide soluble granule and a preparation method thereof. The brassinolide soluble granule consists of brassinolide, cosolvent, humectant and soluble carrier, and is prepared through dissolving brassinolide, cosolvent and humectant in organic solvent, spraying the mixed solution onto the soluble carrier and final eliminating solvent.
Description
Technical Field
The invention relates to a processing technology of pesticide, in particular to a brassinolide soluble granule and a preparation method thereof.
Background
Brassinolide (BR) also called Brassinolide is firstly separated from rape pollen in 1970 by Drechell et al in America and is a plant endogenous steroid bioactive substance with sterol (Ergosterol) as a framework.
In 1979, the structure was extracted and identified by American scientists from 225kg rape pollen, and the results are published in Nature journal. In the mid nineties, japanese scientists developed research work on the synthesis and agricultural application of BRs with sustained effectiveness, see literature: shuru Takatasutto et al, Twenty-third Annual Meeting of the plant Growth Society of America, July14-18, 1996. In more than ten years, scientists in various countries in the world develop research and popularization work in aspects of synthesis, plant physiology, biochemistry, agricultural application and the like, and the research and popularization work is applied to tens of millions of acres of crops with more than 80 varieties, so that a good effect is achieved.
The brassinolide has several unique physiological activities of regulating plant growth, and can excite the latent energy of plant, regulate and promote plant growth and give full play to growth advantages, and its bioactivity is hundreds times higher than that of conventional plant growth regulator in very small concentration (1X 10)-6～1x10－5mg/L) shows obvious biological effect, and some physiological effects of the biological agent show certain characteristics of auxin, gibberellic acid and cytokinin.
Researches prove that the brassinolide can inhibit activities of oxidase and hydrolase in plants, increase plant respiration and adjust balance of endogenous hormones, keep higher osmotic potential of plant tissues and maintain the capabilities of keeping young and delaying senescence, thereby promoting plant growth and reproduction and achieving the purpose of increasing yield; compared with known plant growth regulators such as auxin, cytokinin, gibberellin (920), abscisic acid, ethylene and the like, the plant growth regulator has stronger biological activity, lower using amount, higher safety and better effect of increasing both production and income in agriculture. In 1982, the eighth international plant growth material conference is agreed to be a new generation of agricultural production data, namely the sixth world plant growth regulator.
The main functions are as follows:
1. promoting the division, elongation and growth of plant cells;
2. the pollen insemination is facilitated, and the fruit setting rate is improved;
3. the chlorophyll content is improved, and the photosynthesis is increased;
4. enhancing the stress resistance of the plants.
Because the solubility of brassinolide in a solvent is very low and the solubility in water is only 5mg/L, it is difficult to prepare an aqueous suspension. In the selectable agricultural organic solvent, the solubility of the brassinolide is also extremely low, for example, the solubility in aromatic solvent oil is only 50mg/L, and simultaneously, because the dosage of the brassinolide is extremely low, the current commercially available preparation formulation is mainly a non-environment-friendly emulsifiable solution product, the content is between 0.004 and 0.01 percent, and the content is wettable powder, and the content is between 0.01 and 0.1 percent.
The two formulations have obvious defects, the content of organic solvents such as xylene and petroleum solvent oil in the missible oil is up to 70-90%, the missible oil enters the environment when being used, and the pollution is serious. The wettable powder has the problem of dust drift in use. Meanwhile, the low-concentration preparation product has large volume, and brings great inconvenience to storage, transportation and use.
In order to solve the problems, the invention provides a method for preparing brassinolide into soluble granules (WSG) through research. The soluble granule is a preparation which can be quickly dissolved in water to form a homogeneous solution for spraying, the preparation is an environment-friendly water-based novel pesticide preparation, is extremely convenient to store, transport and use, and can ensure higher content of effective components, so that the same control effect as missible oil can be obtained; the soluble granule has the main advantages of no environmental pollution due to the absence of organic solvents, no dust or little powder generation during production and use, safety for use and producers, and combining the advantages of emulsion and wettable powder, thereby becoming a popular dosage form in the international market.
Disclosure of Invention
The invention aims to solve the problem that the solubility of brassinolide of an agricultural growth hormone regulator in a solvent is too low in the prior art, and provides a soluble brassinolide granule.
In order to solve the problems in the prior art, the technical scheme provided by the invention is as follows: a soluble granula of brassinolide is prepared from brassinolide, cosolvent, humectant and soluble carrier through dissolving brassinolide, cosolvent and humectant in organic solvent, spraying the mixture on a soluble carrier, and removing solvent.
The organic solvent in the invention is selected from one or a mixture of ethers, alcohols and ketones; preferably, the organic solvent is one or a mixture of two or more of ethyl ether, methanol, ethanol and acetone.
The cosolvent in the invention is selected from one or the mixture of more than two of di-sec-octyl maleate sodium sulfonate (rapid penetrating agent T), alkylphenol polyoxyethylene ether and PO-EO block polyether.
The wetting agent in the invention is selected from one or a mixture of more than two of alkyl sulfate (such as sodium dodecyl sulfate), alkyl naphthalene sulfonate (such as penetrant BX), sodium lignin sulfonate and PO-EO block polyether.
The soluble carrier in the invention is selected from one or a mixture of more than two of urea, sulfate, phosphate, lactose and benzoate.
The brassinolide soluble granule comprises the following components in percentage by weight:
0.01 to 2.5 percent of brassinolide,
0.05 to 15 percent of cosolvent,
0.05 to 15 percent of wetting agent,
the balance being soluble carrier.
The brassinolide soluble granule comprises the following components in percentage by weight:
0.01 to 2.5 percent of brassinolide,
0.5 to 15 percent of cosolvent,
0.5 to 15% of a wetting agent,
the balance being soluble carrier.
The brassinolide soluble granule comprises the following components in percentage by weight:
0.01 to 2.5 percent of brassinolide,
1 to 15 percent of cosolvent,
1 to 15% of a wetting agent,
the balance being soluble carrier.
The preparation method of the brassinolide soluble granules comprises the following steps:
(1) preparing a carrier: treating the soluble carrier with a screen to obtain uniform carrier particles, and screening the carrier particles with proper particle size by a screening machine;
(2) dissolving: adding brassinolide, cosolvent and humectant into an organic solvent, fully stirring and completely dissolving for later use;
(3) coating: and (3) adding the soluble carrier obtained in the step (1) into a roller mixer, spraying the mixed solution dissolved in the step (2) into the roller mixer by using an atomizer, continuously stirring uniformly, and discharging to obtain the product.
In the preferable technical scheme of the invention, in the step (3), hot air with the temperature of 65 +/-5 ℃ is blown into the roller mixer.
A preferable preparation method of the brassinolide soluble granules comprises the following steps:
(1) preparing a carrier: treating the soluble carrier by a swing crusher or a granulator, selecting a proper screen to ensure that the treated carrier particles are relatively uniform, and screening the carrier particles with proper particle size by a screening machine;
(2) dissolving: quantitatively adding a solvent, brassinolide, a cosolvent and a wetting agent into a reaction kettle with a stirrer, fully stirring and completely dissolving, and then coating;
(3) coating: adding the screened soluble carrier into a horizontal roller mixing machine, spraying the dissolved brassinolide into the mixing machine by using an atomizer, simultaneously blowing hot air with the temperature of 65 +/-5 ℃ into the mixing machine, continuously stirring for 10-30 minutes, and discharging to obtain the product.
When the brassinolide soluble granules are used, the brassinolide soluble granules can be quickly dissolved by being put into water and can be directly sprayed to farmlands.
The invention has the advantages that:
the invention dissolves brassinolide, cosolvent and wetting agent in solvent, uniformly coats the brassinolide on a soluble carrier with certain shape and particle size by spraying, removes the solvent by drying or natural evaporation to prepare high-content granules, compared with the existing missible oil and wettable powder, the invention ensures the high content of the brassinolide as an effective component, so the control effect of the invention is completely consistent with the missible oil type of the brassinolide, and is higher than that of the wettable powder, and the invention has the following advantages:
1. the content of the active ingredient brassinolide is high and can reach 2.5 percent or even more.
2. The brassinolide preparation is a solid preparation without solvent, and is safe and convenient to package, store and transport;
3. the soluble granules have good solubility and can be quickly dissolved in water to form a homogeneous solution for spraying;
can be directly sprayed on farmlands, and is convenient to use;
4. greatly reduces the environmental pollution and is safe for production and users.
Detailed Description
The above-described scheme is further illustrated below with reference to specific examples. It should be understood that these examples are for illustrative purposes and are not intended to limit the scope of the present invention. The conditions used in the examples may be further adjusted according to the conditions of the particular manufacturer, and the conditions not specified are generally the conditions in routine experiments.
Introduction and summary
The present invention is illustrated by way of example and not by way of limitation. It should be noted that references to "an" or "one" embodiment in this disclosure are not necessarily to the same embodiment, but to at least one.
Various aspects of the invention are described below. It will be apparent, however, to one skilled in the art that the present invention may be practiced according to only some or all aspects of the present invention. For purposes of explanation, specific numbers, materials and configurations are set forth in order to provide a thorough understanding of the present invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced without specific details. In other instances, well-known features are omitted or simplified in order not to obscure the present invention.
The first embodiment is as follows:
0.316kg of ether, 0.032kg of brassinolide original drug sieved by a sieve with the fineness of 80 meshes and the fineness of 95 percent, 0.15kg of alkylphenol polyoxyethylene and 9kg of lauryl sodium sulfate are put into a 2000ml reaction bottle, stirred and dissolved for about 15 minutes after being dissolved and discharged for coating.
298.2kg of 20-60-mesh monopotassium phosphate particles are crushed and screened, added into a horizontal mixer with the volume of 2000L, started for mixing, the brassinolide solution is slowly sprayed in, the spraying is finished in about 2 minutes, the mixer continues to work for 10 minutes after the spraying is finished, and the brassinolide soluble granules with the concentration of 0.01 percent are obtained.
The 0.01% brassinolide soluble granules (namely 0.01% WSG) obtained by the preparation process are spheroidal irregular granules, and the specific technical indexes of the embodiment are shown in the following table 1 through detection:
TABLE 1
As can be seen from the above table of test data, the product of this example has a solution content of 0.0102% (m/m) after dissolution meeting the standard value, and the solution is stable after 18 hours, and has a dissolution time of 25s less than 120s of the standard value, so the solubility is good.
Example two:
3.158kg of ethanol, 0.316kg of brassinolide original drug sieved by a 95% sieve with the fineness of 80 meshes, 1kg of PO-EO block polyether (OP20), 0.5kg of rapid penetrating agent T and 1.5kg of sodium dodecyl sulfate are put into a 10l glass reactor, stirred and dissolved to be clear, and discharged for coating after about 15 minutes.
295.2kg of urea particles which are crushed and screened and have 20-60 meshes are added into a horizontal mixer with the volume of 2000L, the mixing is started, the brassinolide solution is slowly sprayed, hot air with the temperature of 65 +/-5 ℃ is blown into the mixer at the same time, the spraying is finished in about 10 minutes, the mixer continues to work for 10 minutes after the spraying is finished, and the 0.1 percent brassinolide soluble granules are obtained.
The 0.1% brassinolide soluble granules (namely 0.1% WSG) obtained by the preparation process are spheroidal irregular granules, and the specific technical indexes of the embodiment are shown in the following table 2 through detection:
TABLE 2
From the above table of data, it can be seen that the product of this example has a solution content of 0.0985% (m/m) after dissolution meeting the standard value, and the solution is stable after 18 hours, and the dissolution time 12s is less than 120s of the standard value, so the solubility is good.
Example three:
15.8kg of methanol, 1.579kg of brassinolide original drug sieved by a sieve with the fineness of 80 meshes and the fineness of 95 percent, 7.5kg of rapid penetrant and 7.5kg of sodium lignosulfonate are put into a 50l reactor, stirred and dissolved for about 15 minutes to be discharged for coating.
281.9kg of lactose particles which are crushed and screened and have 20-60 meshes are added into a horizontal mixer with the volume of 2000L, the mixing is started, the brassinolide solution is slowly sprayed in, the spraying is finished in about 30 minutes, the mixer is continuously operated for 15 minutes after the spraying is finished, and the brassinolide soluble granules with the content of 0.5 percent are obtained.
The 0.5% brassinolide soluble granules (namely 0.5% WSG) obtained by the preparation process are spheroidal irregular granules, and the specific technical indexes of the embodiment are shown in Table 3 through detection
Shown in the figure:
TABLE 3
As can be seen from the above table of test data, the product of this example has a solution content of 0.510% (m/m) after dissolution meeting the standard value, and the solution is stable after 18 hours, and the dissolution time 43s is less than 120s of the standard value, so the solubility is good.
Example four:
78.95kg of acetone, 7.895kg of brassinolide original drug with fineness of 80 meshes and sieving by a 95% sieve, 37.5kg of rapid penetrant and 37.5kg of penetrant BX are put into a 200l reactor, stirred and dissolved for about 15 minutes after being dissolved and cleared, and discharged for coating.
215.6kg of 20-60 mesh sodium benzoate particles are crushed and screened, added into a horizontal mixer with the volume of 2000L, the mixture is started, the brassinolide solution is slowly sprayed, the spraying is finished within about 120 minutes, the mixer continues to work for 30 minutes after the spraying is finished, and the brassinolide soluble granules with the concentration of 2.5 percent are obtained.
The 2.5% brassinolide soluble granules (i.e. 2.5% WSG) obtained by the preparation process are spheroidal irregular granules, and the specific technical indexes of the embodiment are shown in table 4 through detection:
TABLE 4
As can be seen from the detection data in the table above, the product of this example has a solution content of 2.52% (m/m) after dissolution meeting the standard value, and the solution is stable after 18 hours, and the dissolution time 36s is less than 120s of the standard value, so the solubility is good.
Commercially available 0.01% brassinolide wettable powder (0.01% WP) and 0.004% brassinolide emulsifiable concentrate (0.004% EC) were collected for detection, and the results are shown in tables 5 and 6:
commercially available 0.01% brassinolide wettable powder (0.01% WP) Table 5
Commercial 0.004% brassinolide emulsifiable concentrate (0.004% EC) Table 6
The detection result shows that the commercially available 0.01% brassinolide wettable powder (0.01% WP) and 0.004% brassinolide emulsifiable concentrate (0.004% EC) are dispersed in the system in a heterogeneous state after entering water. The brassinolide soluble granules are dissolved in water after entering the water, are dispersed in a molecular state, and have better biological effect than the missible oil and wettable powder system in the prior art.
The embodiment of the invention carries out a specific application effect experiment:
the invention selects the finished products (0.01% WSG, 0.1% WSG, 0.5% WSG and 2.5% WSG in sequence) of the four embodiments, 0.01% brassinolide wettable powder (0.01% WP), 0.004% brassinolide emulsifiable concentrate (0.004% EC) blank (CK) contrast test, the test crops are cabbage and rice seedlings, the test crops are evenly sprayed after being diluted by 30kg of water per mu, the fresh weight difference of each square meter is measured after 30 days, the effect is evaluated according to the difference of the fresh weight, and the test data are shown in the following table 7:
TABLE 7
As can be seen from the table above, the yield increasing effect of the brassinolide soluble granules prepared by the invention is obviously higher than that of wettable powder and brassinolide emulsion formulations, and the invention has the following advantages: 1. the storage and transportation are safe; 2. the use is convenient; 3. dissolving rapidly; 4. the environmental pollution is reduced; 5. is safe for production and users.
The above-described specific embodiments are merely preferred embodiments of the present invention, and it should be noted that, for those skilled in the art, various modifications or substitutions can be made without departing from the principle of the present invention, and these modifications or substitutions should also be regarded as the protection scope of the present invention.
Claims (10)
1. A soluble granula of brassinolide is prepared from brassinolide, cosolvent, humectant and soluble carrier through dissolving brassinolide, cosolvent and humectant in organic solvent, spraying the mixture on a soluble carrier, and removing solvent.
2. The brassinolide soluble granule according to claim 1, wherein the organic solvent is selected from one or more of ethers, alcohols and ketones.
3. The brassinolide soluble granule according to claim 1, wherein the organic solvent is one or a mixture of two or more selected from the group consisting of ether, methanol, ethanol and acetone.
4. The brassinolide soluble granule according to claim 1, wherein the cosolvent is one or a mixture of two or more selected from the group consisting of sodium di-sec-octyl maleate sulfonate, alkylphenol ethoxylates, and PO-EO block polyether.
5. The brassinolide soluble granule according to claim 1, wherein the wetting agent is one or a mixture of two or more selected from alkyl sulfate, alkyl naphthalene sulfonate, sodium lignosulfonate and PO-EO block polyether.
6. Brassinolide soluble granules according to claim 1, wherein the alkyl sulphate is selected from sodium lauryl sulphate and the alkyl naphthalene sulphonate is selected from the penetrant BX.
7. The brassinolide soluble granule according to claim 1, wherein the soluble carrier is selected from one or a mixture of two or more of urea, sulfate, phosphate, lactose and benzoate.
8. The brassinolide soluble granule as claimed in claim 1, wherein the brassinolide soluble granule comprises the following components by weight percent:
0.01 to 2.5 percent of brassinolide,
0.05 to 15 percent of cosolvent,
0.05 to 15 percent of wetting agent,
the balance being soluble carrier.
9. A process for preparing the brassinolide soluble granules according to any one of claims 1 to 8, which comprises the steps of:
(1) preparing a carrier: treating the soluble carrier with a screen to obtain uniform carrier particles, and screening the carrier particles with proper particle size by a screening machine;
(2) dissolving: adding brassinolide, cosolvent and humectant into an organic solvent, fully stirring and completely dissolving for later use;
(3) coating: and (3) adding the soluble carrier obtained in the step (1) into a roller mixer, spraying the mixed solution dissolved in the step (2) into the roller mixer by using an atomizer, continuously stirring uniformly, and discharging to obtain the product.
10. The method of claim 9, wherein in step (3), hot air at 65 ± 5 ℃ is blown into the roller mixer.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111972425A (en) * | 2020-09-07 | 2020-11-24 | 安徽省四达农药化工有限公司 | Thidiazuron single agent, thidiazuron and brassinolide compound composition and preparation process thereof |
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|---|---|---|---|---|
| CN102388886A (en) * | 2011-10-12 | 2012-03-28 | 发事达(南通)化工有限公司 | Brassinolide water soluble granules and preparation process thereof |
| CN104273121A (en) * | 2013-07-03 | 2015-01-14 | 浙江新安化工集团股份有限公司 | 2,4-dichlorophenoxy quaternary ammonium salt soluble granules and preparation method thereof |
| CN108070017A (en) * | 2016-11-15 | 2018-05-25 | 江苏龙灯化学有限公司 | New crystal forms, the preparation method and the usage of propionylbrassinolide |
-
2020
- 2020-04-13 CN CN202010284674.4A patent/CN111345301A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102388886A (en) * | 2011-10-12 | 2012-03-28 | 发事达(南通)化工有限公司 | Brassinolide water soluble granules and preparation process thereof |
| CN104273121A (en) * | 2013-07-03 | 2015-01-14 | 浙江新安化工集团股份有限公司 | 2,4-dichlorophenoxy quaternary ammonium salt soluble granules and preparation method thereof |
| CN108070017A (en) * | 2016-11-15 | 2018-05-25 | 江苏龙灯化学有限公司 | New crystal forms, the preparation method and the usage of propionylbrassinolide |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111972425A (en) * | 2020-09-07 | 2020-11-24 | 安徽省四达农药化工有限公司 | Thidiazuron single agent, thidiazuron and brassinolide compound composition and preparation process thereof |
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