CN111109251B - Wetting dispersant and pendimethalin suspending agent using same - Google Patents
Wetting dispersant and pendimethalin suspending agent using same Download PDFInfo
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- CN111109251B CN111109251B CN201911312465.XA CN201911312465A CN111109251B CN 111109251 B CN111109251 B CN 111109251B CN 201911312465 A CN201911312465 A CN 201911312465A CN 111109251 B CN111109251 B CN 111109251B
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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
-
- 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
- A01N25/30—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 characterised by the surfactants
-
- 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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
- A01N33/18—Nitro compounds
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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Zoology (AREA)
- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Dispersion Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a wetting dispersant and a pendimethalin suspending agent using the wetting dispersant, belonging to the technical field of pesticide preparation processing. The wetting dispersant consists of the following components in percentage by mass: 20% -40% of block polyether dispersant; 30% -50% of polycarboxylate dispersant; 10% -20% of alkyl sulfonate dispersant; 20-40% of modified polyether dispersant. The pendimethalin suspending agent processed by the wetting dispersant has the advantages of good storage stability, no crystallization, no creaming and the like.
Description
Technical Field
The invention relates to the technical field of pesticide preparation processing, and particularly provides a wetting dispersant and a pendimethalin suspending agent using the wetting dispersant.
Background
With the continuous enhancement of environmental awareness and safety knowledge of people, research and development of the pesticide formulation with water-based property, environmental protection, slow release, multiple functions, labor saving and refinement become a hot spot at home and abroad. The pesticide water suspending agent has good environmental compatibility and pesticide effect, low cost and safe processing and use, is unique in water-based preparations and has great development potential.
The problem difficult to solve in the processing process of the aqueous suspending agent is mainly that in the face of a preparation method and a process of low-melting-point raw pesticide, the raw pesticide with the melting point lower than 70 ℃ is easy to soften and dissolve when the aqueous suspending agent is prepared, so that materials are thickened, finally, sanding is difficult, and phenomena of creaming, crystallization and caking are easy to occur in the process of thermal storage or long-term storage.
Pendimethalin is an aniline herbicide, has a melting point of 54-58 ℃, and belongs to a low-melting-point raw pesticide. The original drug often has the problems of grinding or creaming during storage, crystallization and the like when the suspension is processed.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a wetting dispersant and a pendimethalin suspending agent using the wetting dispersant; the pendimethalin suspending agent processed by the wetting dispersant has the advantages of good storage stability, no crystallization, no creaming and the like.
In order to solve the technical problems, the invention provides the following technical scheme:
on one hand, the invention provides a wetting dispersant, which comprises the following components in percentage by mass:
preferably, the wetting dispersant consists of the following components in percentage by mass:
further, the block polyether dispersant is one or more of ethylene glycol block polyether, propylene glycol block polyether, hydroxyl polyethylene oxide block copolymer and fatty alcohol ethylene oxide propylene oxide block copolymer.
Further, the polycarboxylate dispersant is polyacrylic acid sodium salt and/or polyacrylic acid ammonium salt.
Further, the alkyl sulfonate dispersing agent is one or more of alkyl phenol sulfonate, alkyl benzene sulfonate, tristyryl phenol sulfonate and alkenyl sulfonate.
Further, the modified polyether dispersant is one or more of alkylphenol modified polyoxyethylene ether, fatty alcohol modified polyoxyethylene ether, fatty acid modified polyoxyethylene ether and castor oil modified polyoxyethylene ether.
On the other hand, the invention also provides a pendimethalin suspending agent which comprises the wetting dispersant, wherein the wetting dispersant accounts for 10-20% of the suspending agent by mass.
Further, the pendimethalin suspending agent also comprises a pendimethalin raw pesticide, an antifreezing agent, a defoaming agent, a thickening agent and water.
Further, in the pendimethalin suspending agent, the dosage of each substance is as follows:
preferably, in the pendimethalin suspension, the dosage (mass percent) of each substance is as follows:
preferably, the antifreezing agent is ethylene glycol, propylene glycol and the like; the thickener is white carbon black, bentonite, xanthan gum, etc.
In another aspect, the invention also provides a preparation method of the pendimethalin suspending agent, which comprises the following steps: weighing the raw materials according to a proportion, uniformly mixing, adding into a grinding machine, adding zirconia beads, and grinding for 1 hour on a sand mill at a rotating speed of 1600 rpm.
Compared with the prior art, the invention has the following beneficial effects:
the block polyether dispersant, the polycarboxylate dispersant, the alkyl sulfonate dispersant and the modified polyether dispersant are compounded, and the block polyether dispersant contains regularly arranged hydrophilic and hydrophobic groups, so that the block polyether dispersant has good wrapping property on raw medicines, and a prepared sample has good stability. The polycarboxylate dispersant has a unique comb-shaped structure, contains a plurality of anchoring groups, can be tightly combined with original drugs, and can remarkably improve the stability of formulations such as pesticide aqueous suspension and the like. The alkyl sulfonate dispersing agent has the advantages of easily available raw materials, low price, easy compounding with various auxiliary agents, mature synthesis process, good surface activity and strong hydrophilicity as an anionic surfactant, and can effectively reduce the tension of an oil-water interface to achieve the emulsification effect. The modified polyether dispersant has good wetting effect, and can enable the technical granules to be better contacted with the dispersant in a water system. Due to the comprehensive effect of the additives, the low-melting-point raw pesticide achieves good wrapping and dispersing effects, so that the stability is achieved. The wetting dispersant with better dispersion performance is obtained, and the pendimethalin suspending agent prepared by the method has the advantages of good storage stability, no crystallization, no creaming and the like.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
The reagents and materials used in the examples and comparative examples were commercially available unless otherwise specified.
The invention provides a wetting dispersant and a pendimethalin suspending agent using the wetting dispersant, and specific examples are as follows.
Example 1
A wetting dispersant is composed of the following components in percentage by mass: 35 percent of hydroxyl polyethylene oxide block copolymer, 30 percent of polyacrylic acid sodium salt, 15 percent of tristyrylphenol sulfonate and 20 percent of alkylphenol modified polyoxyethylene ether.
The mixed auxiliary agent is adopted to process 20 percent pendimethalin suspending agent, and the specific method comprises the following steps: weighing 10g of the mixed wetting dispersant, placing the weighed wetting dispersant into a sample cup of a sand mill, adding 62.8g of tap water, 5g of ethylene glycol, 0.2g of defoamer and 2g of xanthan gum, uniformly mixing to obtain an aqueous solution, and then adding 2g of white carbon black and 20g of pendimethalin raw medicine, and uniformly mixing to obtain slurry to be ground. To the slurry to be ground, 120g of zirconia beads were added, and the mixture was ground on a sand mill at 1600 rpm for 1 hour. And collecting ground slurry after 1 hour to obtain a 20 percent pendimethalin suspending agent sample.
Example 2
A wetting dispersant is composed of the following components in percentage by mass: 25% of fatty alcohol ethylene oxide propylene oxide block copolymer, 40% of polyacrylic acid ammonium salt, 10% of dodecyl benzene sulfonate and 25% of fatty acid modified polyoxyethylene ether.
The mixed auxiliary agent is adopted to process 10 percent pendimethalin suspending agent, and the specific method comprises the following steps: weighing 10g of the mixed wetting dispersant, placing the weighed wetting dispersant into a sample cup of a sand mill, adding 72.9g of tap water, 2g of ethylene glycol, 0.1g of defoamer and 2g of xanthan gum, uniformly mixing to obtain an aqueous solution, adding 5g of white carbon black and 10g of pendimethalin raw medicine, and uniformly mixing to obtain slurry to be ground. To the slurry to be ground, 120g of zirconia beads were added, and the mixture was ground on a sand mill at 1600 rpm for 1 hour. And collecting ground slurry after 1 hour to obtain a 10 percent pendimethalin suspending agent sample.
Example 3
A wetting dispersant is composed of the following components in percentage by mass: 30% of propylene glycol block polyether, 35% of polyacrylic acid sodium salt, 12% of alkenyl sulfonate and 23% of castor oil modified polyoxyethylene ether.
The mixed auxiliary agent is adopted to process 15 percent pendimethalin suspending agent, and the specific method comprises the following steps: weighing 15g of the mixed wetting dispersant, placing the weighed wetting dispersant into a sample cup of a sand mill, adding 67.8g of tap water, 5g of ethylene glycol, 0.2g of defoamer, mixing 2g of xanthan gum uniformly to form an aqueous solution, adding 2g of white carbon black and 10g of pendimethalin raw medicine, and mixing uniformly to obtain slurry to be ground. To the slurry to be ground, 120g of zirconia beads were added, and the mixture was ground on a sand mill at 1600 rpm for 1 hour. And collecting ground slurry after 1 hour to obtain a 15 percent pendimethalin suspending agent sample.
Example 4
A wetting dispersant is composed of the following components in percentage by mass: 40% of glycol block polyether, 30% of polyacrylic ammonium salt, 15% of alkylphenol sulfonate and 15% of fatty alcohol modified polyoxyethylene ether.
The mixed auxiliary agent is adopted to process 10 percent pendimethalin suspending agent, and the specific method comprises the following steps: weighing 20g of the mixed wetting dispersant, placing the weighed wetting dispersant into a sample cup of a sand mill, adding 60g of tap water, 8g of ethylene glycol and 1g of defoamer, mixing 2g of xanthan gum to obtain a uniform aqueous solution, adding 1g of white carbon black and 10g of pendimethalin raw drug, and uniformly mixing to obtain slurry to be ground. To the slurry to be ground, 120g of zirconia beads were added, and the mixture was ground on a sand mill at 1600 rpm for 1 hour. And collecting ground slurry after 1 hour to obtain a 10 percent pendimethalin suspending agent sample.
Example 5
A wetting dispersant is composed of the following components in percentage by mass: 15% of propylene glycol block polyether, 20% of ethylene glycol block polyether, 30% of polyacrylic ammonium salt, 15% of alkylphenol sulfonate, 10% of alkylphenol modified polyoxyethylene ether and 10% of fatty alcohol modified polyoxyethylene ether.
The rest is the same as in example 1.
Example 6
A wetting dispersant is composed of the following components in percentage by mass: 10% of fatty alcohol ethylene oxide propylene oxide block copolymer, 20% of propylene glycol block polyether, 20% of polyacrylic ammonium salt, 15% of polyacrylic sodium salt, 10% of alkylbenzene sulfonate, 2% of alkenyl sulfonate and 23% of castor oil modified polyoxyethylene ether.
The rest is the same as in example 3.
To further illustrate the beneficial effects of the present invention, the following comparative examples were constructed, for reasons of space only, using example 1 as an example.
Comparative example 1
The hydroxy polyethylene oxide block copolymer of example 1 was replaced by sodium polyacrylate, and the remaining components and pendimethalin suspension were processed without change.
Comparative example 2
The sodium polyacrylate salt in example 1 was replaced by tristyrylphenol sulfonate, and the remaining components and pendimethalin suspension were processed without change.
Comparative example 3
The tristyrylphenol sulfonate in example 1 was replaced with alkylphenol modified polyoxyethylene ether, and the other components and pendimethalin suspension were processed without change.
Comparative example 4
The alkylphenol modified polyoxyethylene ether in the example 1 is replaced by hydroxyl polyethylene oxide block copolymer, and the other components and the processing method of pendimethalin suspending agent are not changed.
Comparative example 5
The sodium polyacrylate salt in the example 1 is replaced by sodium lignosulfonate with the same mass fraction, and the processing methods of the other components and the pendimethalin suspending agent are not changed.
Comparative example 6
Using the wetting and dispersing agent described in example 1, and the mixed adjuvant, 5.7% emamectin benzoate suspending agent (70% active ingredient) was processed by the following specific method: weighing 10g of the mixed wetting dispersant, placing the weighed wetting dispersant into a sample cup of a sand mill, adding 72.66g of tap water, 5g of ethylene glycol, 0.2g of defoamer, mixing 2g of xanthan gum to obtain a uniform aqueous solution, and then adding 2g of white carbon black and 8.14g of emamectin benzoate raw material, and uniformly mixing to obtain slurry to be ground. To the slurry to be ground, 120g of zirconia beads were added, and the mixture was ground on a sand mill at 1600 rpm for 1 hour. The ground slurry was collected after 1 hour to give a 5.7% emamectin benzoate suspension sample.
Comparative example 7
The wetting dispersant described in example 1 is adopted, and a mixed auxiliary agent is adopted to process a 25% pymetrozine suspending agent (95.5% of effective components), and the specific method comprises the following steps: weighing 10g of the mixed wetting dispersant, placing the weighed wetting dispersant into a sample cup of a sand mill, adding 54.62g of tap water, 5g of ethylene glycol, 0.2g of defoamer, mixing 2g of xanthan gum to obtain a uniform aqueous solution, adding 2g of white carbon black and 26.18g of pymetrozine raw drug, and uniformly mixing to obtain slurry to be ground. To the slurry to be ground, 120g of zirconia beads were added, and the mixture was ground on a sand mill at 1600 rpm for 1 hour. And collecting ground slurry after 1 hour to obtain a 25% pymetrozine suspending agent sample.
The suspending agent samples prepared in examples 1 to 6 and comparative examples 1 to 7 of the present invention were measured for their indexes of grinding granule, suspension percentage, amount of water evolved upon heat storage, particle size after heat storage, stability at room temperature upon heat storage, etc., and the results are shown in table 1.
TABLE 1 results of performance index test on samples processed in different examples and comparative examples
As can be seen from the results in Table 1, the pendimethalin suspending agent processed by the wetting dispersant prepared by the invention has the advantages of small grinding particle size, high suspension rate and stable performance in heat storage and heat storage to normal temperature. The pendimethalin suspending agent sample processed by adopting the auxiliary agent in the comparative example has the main problems that the heat storage particle size is obviously increased, the heat storage is converted into normal temperature, and the sample is unqualified. The wetting dispersant is applied to the preparation of pymetrozine suspending agent, and the suspension rate is poor, so that the wetting dispersant is proved to be specially used for preparing pendimethalin suspending agent and has poor preparation effect on other pesticide suspending agents. Meanwhile, after detection, the performance of the pendimethalin suspending agent processed by the commercial wetting dispersant on the market is inferior to that of the sample processed by the wetting dispersant of the invention, and the detailed description is not repeated for reasons of space limitation.
Exploring the control effect of the pendimethalin suspending agent prepared by the invention on green bristlegrass in a cotton field, taking examples 1-6 and comparative examples 1-5 as well as a commercially available 30% pendimethalin suspending agent as an example, the using amount of active ingredients is 54 g/mu, treating three subareas by each medicament, and recording the average value; the random blocks are arranged, the area of the cell is 2 multiplied by 20 to 40 square meters, and 0.5 meter of isolation area is reserved among the blocks.
Spraying with conventional stem and leaf. Converting the dosage, the synergistic dosage and the water mixing amount of the community according to the specified dosage, uniformly mixing and spraying. The medicine is applied by cell and is even. The control effect is investigated for 1 time respectively 10 days, 20 days and 30 days after the application, 3 points of a single diagonal line are sampled in each treatment area, 0.5 square meter is fixedly investigated for each point, the number of the weeds is recorded respectively, and the fresh weight of the overground part of the weeds is measured in the last investigation. Counting the number of residual weeds, weighing the fresh weight of the weeds and calculating the control effect of the plants.
Plant control effect (%) × (1- (number of weeds after treatment field application × number of weeds before control field application)/(number of weeds before treatment field application × number of weeds after control field application)) × 100
TABLE 2 Experimental results for weed control of pendimethalin suspension
As can be seen from Table 2, the samples prepared by using the adjuvant of the invention have no obvious difference from the samples sold in the market in the aspect of weeding and controlling effects; the control effect of individual examples is far better than that of the samples sold in the market.
In a word, the wetting dispersant can be used for processing pendimethalin suspending agent samples with qualified performance, particularly solving the creaming problem of the pendimethalin suspending agent samples in the process of thermal storage to normal-temperature placement, and reducing the risk of the product deteriorating in the shelf life.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (4)
1. The pendimethalin suspending agent is characterized by comprising the following components in percentage by mass:
10-20% of wetting dispersant;
2-8% of an antifreezing agent;
0.1 to 1 percent of defoaming agent;
1-5% of a thickening agent;
10-20% of pendimethalin raw drug;
water is complemented to 100 percent;
the wetting dispersant consists of the following components in percentage by mass:
20-40% of block polyether dispersant;
30-50% of polycarboxylate dispersant;
10-20% of alkyl sulfonate dispersant;
20-40% of modified polyether dispersant;
the block polyether dispersant is one or more of ethylene glycol block polyether, propylene glycol block polyether, hydroxyl polyethylene oxide block copolymer and fatty alcohol ethylene oxide propylene oxide block copolymer;
the polycarboxylate dispersant is polyacrylic acid sodium salt and/or polyacrylic acid ammonium salt;
the alkyl sulfonate dispersing agent is one or more of alkyl phenol sulfonate, alkylbenzene sulfonate, tristyryl phenol sulfonate and alkenyl sulfonate;
the modified polyether dispersant is one or more of alkylphenol modified polyoxyethylene ether, fatty alcohol modified polyoxyethylene ether, fatty acid modified polyoxyethylene ether and castor oil modified polyoxyethylene ether.
2. The pendimethalin suspension concentrate of claim 1, which is characterized by comprising the following components in percentage by mass:
25-35% of block polyether dispersant;
30-40% of polycarboxylate dispersant;
10-15% of alkyl sulfonate dispersant;
20-25% of modified polyether dispersant.
3. The pendimethalin suspension concentrate of claim 1, consisting of the following components by mass: 10g of wetting dispersant, 5g of ethylene glycol, 0.2g of defoaming agent, 2g of xanthan gum, 2g of white carbon black, 20g of pendimethalin raw drug and 62.8g of tap water;
the wetting dispersant consists of the following components in percentage by mass: 35% of hydroxy polyethylene oxide block copolymer, 30% of sodium polyacrylate, 15% of tristyrylphenol sulfonate and 20% of alkylphenol modified polyoxyethylene ether.
4. A process for preparing a pendimethalin suspension concentrate as claimed in any one of claims 1 to 3, wherein the raw materials are weighed in proportion, mixed well and then added to a grinder, and then zirconia beads are added and ground on a sand mill at 1600 rpm for 1 hour.
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| CN111903672A (en) * | 2020-07-27 | 2020-11-10 | 南京太化化工有限公司 | Auxiliary agent for suspending agent and validamycin and carbendazim compound suspending agent |
| CN112841189B (en) * | 2021-01-26 | 2023-03-17 | 河南远见农业科技有限公司 | Herbicide for paddy field and preparation method and application thereof |
| CN115067328A (en) * | 2022-07-26 | 2022-09-20 | 浙江中山化工集团股份有限公司 | Low-melting-point original drug suspending agent and preparation method thereof |
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| US5679619A (en) * | 1986-05-23 | 1997-10-21 | American Cyanamid Company | Aqueous suspension concentrate compositions of pendimethalin |
| CN102187862B (en) * | 2010-11-22 | 2013-08-21 | 南通联农农药制剂研究开发有限公司 | Pesticide composition containing pendimethalin and preparation method thereof |
| CN102396450B (en) * | 2011-12-28 | 2015-04-01 | 新疆锦华农药有限公司 | Pendimethalin suspension and preparation method thereof |
| CN102428923A (en) * | 2012-01-16 | 2012-05-02 | 河北博嘉农业有限公司 | Pendimethalin and pyrithiobac-sodium compounded herbicide |
| CN104542669A (en) * | 2015-01-09 | 2015-04-29 | 浙江新农化工股份有限公司 | Weeding composition containing pendimethalin and ethoxysulfuron as well as preparation and application thereof |
| CN105432604B (en) * | 2015-11-16 | 2017-12-05 | 浙江天丰生物科学有限公司 | A kind of low-melting compound suspending agent and preparation method thereof |
| CN105875607B (en) * | 2016-05-16 | 2018-07-03 | 中国农业大学 | A kind of Pendimethalin microcapsule suspending agent and preparation method thereof |
| CN108782549A (en) * | 2018-07-17 | 2018-11-13 | 郭秦 | A kind of compounding low melting point suspending agent technique |
| CN109221114B (en) * | 2018-10-15 | 2021-06-04 | 浙江理工大学 | Preparation method of comb-type dispersing agent for pendimethalin suspending agent |
| CN109452267A (en) * | 2018-11-22 | 2019-03-12 | 深圳诺普信农化股份有限公司 | The preparation method and aqueous pesticide formulations of aqueous pesticide formulations |
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