CN108651455A - A kind of Synergistic type tricyclazole suspending agent and preparation method thereof - Google Patents
A kind of Synergistic type tricyclazole suspending agent and preparation method thereof Download PDFInfo
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- CN108651455A CN108651455A CN201810367260.0A CN201810367260A CN108651455A CN 108651455 A CN108651455 A CN 108651455A CN 201810367260 A CN201810367260 A CN 201810367260A CN 108651455 A CN108651455 A CN 108651455A
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- tricyclazole
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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
- A01N25/30—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
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
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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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
- A01N43/42—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings condensed with carbocyclic rings
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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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/46—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom rings with more than six members
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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
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
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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
- A01N43/90—Biocides, 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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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
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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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/12—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing acyclic or cycloaliphatic radicals
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Abstract
The invention discloses a kind of Synergistic type tricyclazole suspending agents, are made of following materials by weight percentage：Tricyclazole 5 60%, surfactant 5 9%, synergist, 0.5 5%, ethylene glycol 3 7%, aluminium-magnesium silicate 0.01 2%, stabilizer 0.1 10%, xanthans 0.05 0.5%, hydroxymethylglycinate 0.2 0.5%, surplus is water.Reduction grain diameter is crushed by colloid mill, ultramicro grinding, high-pressure homogeneous three steps, grain size D (90) is made to reach 2 μm hereinafter, up to Synergistic type tricyclazole suspending agent of the invention.The tricyclazole agricultural chemicals suspension agent of the present invention, appearance stablity is non-discolouring, and suspensibility is high, and properties of product are stablized.
Description
Technical field
The invention belongs to Pesticide formulation technical fields, and in particular to a kind of Synergistic type tricyclazole suspending agent and its preparation
Method.
Background technology
Tricyclazole is also known as Tricyclazole, gram pest spirit, than gorgeous, rice blast azoles, is a kind of selectivity developed by Lilly Co., Eli.
Interior suction protects fungicide, patent No. BP1419121.
Tricyclazole sterling is white crystals, and vapour pressure is 266.6448 × 10-7 pas when 187~188 DEG C, 25 DEG C of fusing point.25
DEG C when solubility be：1.6 grams per liter of water, dichloromethane 33%, ethyl alcohol 25%, methanol 25%, acetone 10.4%, acetonitrile 10.4%,
Cyclohexanone 10.0%, benzene 4.2%, dimethylbenzene 2.1%, chloroform>500 grams per liters.Property is stablized, and is not easy by water and photodegradation, to heat
Stablize.
Tricyclazole is one kind, and there is the stronger protectiveness triazole bactericidal agent of interior suction performance, prevention rice blast to have spy
Effect, can be absorbed by the root, stem, leaf of rice after dispenser, and can the transporting in plant, sprayed 1~2 time during entire paddy growth
Medicine can effectively prevent the generation of rice blast.Tricyclazole anti-impact brushing force is strong, and spray meets rain and is not required to the medicine that fills spray after 1 hour.Mainly
It is that spore germination and attachment spore is inhibited to be formed, to effectively prevent germ from invading and reduce the generation of magnaporthe grisea spore.Three
Ring azoles has very strong interior suction and behavior in service, and slow, 7~10 weeks longevities of residure are decomposed in plant body and in soil.It can mix
Kind, dip the seedling root in or foliage spray, preventive effect are good.
Tricyclazole pesticidal preparations are in the majority with wettable powder, with the development of suspending agent technology, gradually have in recent years outstanding
Floating agent product emerges.Conventional tricyclazole suspending agent, using conventional surfactants as wetting dispersing agent, product drug effect is poor,
In order to solve the problems, such as that conventional products drug effect is poor, the present invention provides a kind of Novel synergistic type tricyclazole suspending agent and its preparation sides
Method.
Invention content
To solve the deficiencies in the prior art, a kind of Synergistic type tricyclazole suspending agent of present invention offer and its preparation side
Method.It is realized especially by following technical proposals：
A kind of Synergistic type tricyclazole suspending agent, is made of following materials by weight percentage：Tricyclazole 5-60%, surface-active
Agent 3-15%, synergist 0.5-10%, bleeding agent 1-10%, ethylene glycol 3-7%, aluminium-magnesium silicate 0.01-2%, stabilizer 0.1-
10%, xanthans 0.05-0.5%, hydroxymethylglycinate 0.01-0.03%, surplus are water.
Preferably, a kind of Synergistic type tricyclazole suspending agent, is made of following materials by weight percentage：Tricyclazole 20-50%,
Surfactant 3-10%, synergist 0.5-10%, bleeding agent 1-5%, ethylene glycol 3-5%, aluminium-magnesium silicate 0.01-2%, stabilization
Agent 0.1-5%, xanthans 0.05-0.3%, hydroxymethylglycinate 0.01-0.03%, surplus are water.
The surfactant is dodecyl polyoxyethylene (3) ether sulfuric acid triethanolamine, different tridecanol ether (6) phosphate
Any one or two kinds of combinations of sylvite.
The bleeding agent is sodium secondary alkyl sulfonate.
The synergist is any one of glycine betaine, azone, thiophene ketone, organosilicon, lecithin, vitamin E or several.
The stabilizer is：Citric acid, acetic acid, any one of phosphoric acid, potassium dihydrogen phosphate or several.
It is a kind of to prepare above-mentioned Synergistic type tricyclazole suspending agent method, mainly include the following steps：
(1) according to formula tricyclazole, surfactant, aluminium-magnesium silicate, stabilizer, synergist, hydroxymethylglycinate, water
It is stirred pulp object, coarse crushing is carried out by colloid mill；
(2) material after coarse crushing in step (1) is placed in grinding machine and carries out superfine grinding, crushing, control material grain size D
(90) 2 μm of ＜；
(3) spent glycol dissolves xanthans, is then added into step (2) and obtains in the material of ultramicro grinding, with cutting
It is uniform to cut machine shearing；
(4) material obtained after being stirred evenly in step (3) is placed in homogeneous in homogenizer, makes material particle homogenization.
The abrasive media of grinding machine is zirconium oxide in the step (2), and abrasive media grain size is 0.5-2.0mm, the mill
Sand machine operating temperature is 20-30 DEG C.
The rotating speed that cutter works in the step (3) is 1500-3000r/min.
Homogenizer is high pressure homogenizer in the step (4), and the operating pressure of the high pressure homogenizer is 50MPa.
Compared with prior art, the present invention haing the following advantages：
Glycine betaine, azone, thiophene ketone, organosilicon, lecithin, vitamin E is added as increasing in the present invention in suspending agent formula
Agent is imitated, while introducing dodecyl polyoxyethylene (3) ether sulfuric acid triethanolamine, different tridecanol ether (6) phosphate kalium salt conduct
Surfactant, sodium secondary alkyl sulfonate are bleeding agent, can be effectively increased the permeability of preparation, improve drug effect.
Specific implementation mode
Embodiment 1
(1) according to formula tricyclazole, surfactant, aluminium-magnesium silicate, stabilizer, synergist, sodium secondary alkyl sulfonate, Huang
Virgin rubber, hydroxymethylglycinate, water are stirred pulp object, and coarse crushing is carried out by colloid mill.
(2) it is placed in grinding machine and carries out ultramicro grinding, control 2 μm of grain size D (90) ＜.
(3) spent glycol is dissolved into xanthans, is added in material and stirs evenly.
(4) it is placed in homogeneous in homogenizer, makes particle homogenization.
Suspending agent obtained, the sticky homogeneous liquid of appearance measure, grain size through Malvern laser fineness gage
(D90) it is 1.6 μm.
Table 1：20% tricyclazole suspending agent formula table
Embodiment 2
Raw material is weighed by 2 corresponding embodiment of table, 2 data, is prepared as described in Example 1.Suspending agent obtained, grain
Diameter (D90) is 1.6 μm.
Table 2：40% tricyclazole suspending agent formula table
| Component | Dosage (kilogram) |
| Tricyclazole | 40 |
| Dodecyl polyoxyethylene (3) ether sulfuric acid triethanolamine | 1.5 |
| Different tridecanol ether (6) phosphate potassium | 3 |
| Sodium secondary alkyl sulfonate | 5 |
| Vitamin E | 3 |
| Azone | 2 |
| Ethylene glycol | 5 |
| Aluminium-magnesium silicate | 0.5 |
| Xanthans | 0.15 |
| Citric acid | 0.50 |
| Potassium dihydrogen phosphate | 1 |
| Titanium dioxide | 3 |
| Hydroxymethylglycinate | 0.2 |
| Water | Complementary is to 100 |
Embodiment 3
Raw material is weighed by 3 corresponding embodiment of table, 3 data, is prepared as described in Example 1.Suspending agent obtained, grain
Diameter (D90) is 1.6 μm.
Table 3：55% tricyclazole suspending agent formula table
Comparative example 1
(1) tricyclazole, various auxiliary agents are added according to formula in table 4 by cutting kettle, shearing is uniform.
(2) material after coarse crushing in step (1) is placed in grinding machine and carries out ultramicro grinding, control material grain size D (90)
5 μm of ＜, grinding terminates, and stirs evenly the suspending agent of obtained tricyclazole, and appearance is orange thick liquid.
Table 4：40% tricyclazole suspending agent formula table
| Component | Dosage (kilogram) |
| Tricyclazole | 40 |
| SP-SC3266 | 5 |
| Ethylene glycol | 3 |
| Aluminium-magnesium silicate | 0.5 |
| Sodium benzoate | 0.2 |
| Antifoaming agent | 0.2 |
| Xanthans | 0.15 |
| Water | Complementary is to 100 |
1 penetrating power of test case detects
Penetrating power detection method：Diameter 35mm canvas disks are immersed in the pesticidal preparations dilute solution of known concentration
In.Due to having contained air in cotton fiber gap, cotton disk is made to float on liquid level.After solution penetrates into cotton, air quilt
Substitution, cotton disk are begun to decline.It measures cotton disk and settles the required time to since contact liquid level, to judge solution
Penetrating power it is strong and weak.
Sample in selection example 1-3, the sample in comparative example 1, on the market certain 75% tricyclazole wettable powder of company
Agent Xi Shi not be 2000 times, 5000 times, compared with tap water, 3 canvas piece sedimentation times of parallel determination, are averaged.
Pesticide solution penetrating power detects after table 5 adds builder
From the point of view of measuring result, Tebuconazole Bravo suspending agent of the invention has more lustful penetrating power, helps
In raising product drug effect.
The Synergistic type tricyclazole suspending agent of gained will be prepared in embodiment 1,2,3 and comparative example 1 in room temperature storage respectively
High temperature storage 14 days under the conditions of 14 days, 54 DEG C ± 2 DEG C uses《GB/T14825-2006 agricultural-chemical suspension rate assay methods》It surveys and suspends
Rate, specific data see the table below 4.Work as suspensibility>When 85%, then it is assumed that the product is certified products.
Table 4：Tricyclazole suspending agent suspensibility determination data table
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | |
| After room temperature 14 days | 99.7% | 99.5% | 99.2% | 95.0% |
| After heat storage 14 days | 99.6% | 99.2% | 99.3% | 92.5% |
Suspension refers to that the active compound particle of dispersion keeps the ability of suspension time length in suspension, usually uses suspensibility
To indicate.One good suspending agent should have good storage stability, i.e., higher suspensibility.
The Synergistic type tricyclazole agricultural chemicals suspension agent of the present invention, suspensibility is high, and plate-out ability and good penetrability, properties of product are steady
It is fixed.The present invention is added in suspending agent formula using glycine betaine, azone, thiophene ketone, organosilicon, lecithin, vitamin E as in synergy
Agent, while dodecyl polyoxyethylene (3) ether sulfuric acid triethanolamine, different tridecanol ether (6) phosphate kalium salt are introduced as profit
Hygroscopic water powder, sodium secondary alkyl sulfonate can be effectively increased the permeability of preparation as bleeding agent, improve drug effect.
Claims (10)
1. a kind of Synergistic type tricyclazole suspending agent, which is characterized in that be made of following materials by weight percentage：Tricyclazole 5-
60%, surfactant 3-15%, synergist 0.5-10%, bleeding agent 1-10%, ethylene glycol 3-7%, aluminium-magnesium silicate 0.01-
2%, stabilizer 0.1-10%, xanthans 0.05-0.5%, hydroxymethylglycinate 0.01-0.03%, surplus are water.
2. a kind of Synergistic type tricyclazole suspending agent according to claim 1, which is characterized in that former by following weight percentage
Material composition：Tricyclazole 20-50%, surfactant 3-10%, synergist 0.5-10%, bleeding agent 1-5%, ethylene glycol 3-5%,
Aluminium-magnesium silicate 0.01-2%, stabilizer 0.1-5%, xanthans 0.05-0.3%, hydroxymethylglycinate 0.01-0.03%, surplus
For water.
3. a kind of Synergistic type tricyclazole suspending agent according to claim 1 or 2, which is characterized in that the surfactant
For dodecyl polyoxyethylene (3) ether sulfuric acid triethanolamine, any one or two kinds of groups of different tridecanol ether (6) phosphate kalium salt
It closes.
4. a kind of Synergistic type tricyclazole suspending agent according to claim 1 or 2, which is characterized in that the bleeding agent is
Sodium secondary alkyl sulfonate.
5. a kind of Synergistic type tricyclazole suspending agent according to claim 1 or 2, which is characterized in that the synergist is sweet tea
Any one of dish alkali, azone, thiophene ketone, organosilicon, lecithin, vitamin E are several.
6. a kind of Synergistic type tricyclazole suspending agent according to claim 1 or 2, which is characterized in that the stabilizer is：Lemon
Lemon acid, acetic acid, any one of phosphoric acid, potassium dihydrogen phosphate or several.
7. a kind of preparing Synergistic type tricyclazole suspending agent method described in claims 1 or 2, which is characterized in that include mainly as follows
Step：
(1) tricyclazole, surfactant, aluminium-magnesium silicate, stabilizer, synergist, hydroxymethylglycinate, water are stirred according to formula
It is mixed into slurry, coarse crushing is carried out by colloid mill；
(2) material after coarse crushing in step (1) is placed in grinding machine and carries out superfine grinding, crushing, control material grain size D (90)
2 μm of ＜；
(3) spent glycol dissolves xanthans, is then added into step (2) and obtains in the material of ultramicro grinding, uses cutter
Shearing is uniform；
(4) material obtained after being stirred evenly in step (3) is placed in homogeneous in homogenizer, makes material particle homogenization.
8. a kind of Synergistic type tricyclazole suspending agent preparation method according to claim 7, which is characterized in that the step
(2) abrasive media of grinding machine is zirconium oxide in, and abrasive media grain size is 0.5-2.0mm, and the grinding machine operating temperature is 20-
30℃。
9. a kind of Synergistic type tricyclazole suspending agent preparation method according to claim 7, which is characterized in that the step
(3) rotating speed that cutter works in is 1500-3000r/min.
10. a kind of Synergistic type tricyclazole suspending agent preparation method according to claim 7, which is characterized in that the step
(4) homogenizer is high pressure homogenizer in, and the operating pressure of the high pressure homogenizer is 50MPa.
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