CN114681937A - Method for preparing dry suspending agent by combining spray drying and boiling granulation - Google Patents

Method for preparing dry suspending agent by combining spray drying and boiling granulation Download PDF

Info

Publication number
CN114681937A
CN114681937A CN202011633893.5A CN202011633893A CN114681937A CN 114681937 A CN114681937 A CN 114681937A CN 202011633893 A CN202011633893 A CN 202011633893A CN 114681937 A CN114681937 A CN 114681937A
Authority
CN
China
Prior art keywords
suspending agent
dry suspending
water
spray drying
granulation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011633893.5A
Other languages
Chinese (zh)
Inventor
张路路
洪湖
周同磊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cac Nantong Chemical Co ltd
Original Assignee
Cac Nantong Chemical Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Cac Nantong Chemical Co ltd filed Critical Cac Nantong Chemical Co ltd
Priority to CN202011633893.5A priority Critical patent/CN114681937A/en
Publication of CN114681937A publication Critical patent/CN114681937A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/16—Evaporating by spraying
    • B01D1/18—Evaporating by spraying to obtain dry solids
    • 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
    • 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
    • A01N37/34—Nitriles
    • 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
    • A01N37/50—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 the nitrogen atom being doubly bound to the carbon skeleton
    • 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
    • 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
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
    • 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
    • A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/647—Triazoles; Hydrogenated triazoles
    • A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
    • 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
    • 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
    • A01N43/84—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 six-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,4
    • 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
    • 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
    • A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/24—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof
    • 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<
    • A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/16—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by suspending the powder material in a gas, e.g. in fluidised beds or as a falling curtain

Landscapes

  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Agronomy & Crop Science (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention provides a method for preparing a dry suspending agent by combining spray drying and boiling granulation. The method comprises the following steps: (1) preparing a preparation raw material of a dry suspending agent, mixing the preparation raw material with water, and crushing to obtain slurry; (2) then, spray drying the slurry obtained in the step (1) to obtain mother powder; (3) and (3) mixing the mother powder obtained in the step (2) with water, and carrying out boiling granulation, drying and screening to obtain the dry suspending agent. The preparation method solves the problem that the finished product of the dry suspending agent subjected to spray granulation has unqualified indexes such as wettability, wear resistance and dust, the wetting time of the dry suspending agent prepared by the method is less than or equal to 60s, the wear resistance index is more than or equal to 99%, the dust is less than or equal to 30mg, and the indexes of the water dispersible granule meet the national standard.

Description

Method for preparing dry suspending agent by combining spray drying and boiling granulation
Technical Field
The invention belongs to the field of pesticide preparations, particularly relates to a formula and a granulation mode of a pesticide dry suspending agent, and particularly relates to a method for preparing the dry suspending agent by combining spray drying and boiling granulation.
Background
The Dry Flowable (DF) dosage form is a solid preparation formed by spray drying on the basis of aqueous suspending agent, and compared with the conventional dosage form, the Dry Flowable (DF) dosage form has the advantages of no dust, good fluidity, fine active substance particle size, high suspension rate, rapid dispersion, convenient storage and transportation and the like, is widely applied to domestic and foreign markets, and is a new dosage form with wide prospect.
In the national standard GB/T19378-2017 pesticide formulation name and code, the dry suspending agent belongs to a water dispersible granule formulation (WG) in a dispersible solid preparation, and the indexes of the water dispersible granule comprise: content, moisture, pH value range, wet sieve test, suspension rate, dispersibility, durable foamability, dust, wear resistance, heat storage stability and the like.
At present, the granulation mode of the traditional water dispersible granule mainly comprises rotary extrusion, screw extrusion and the like, all indexes basically meet the requirements, but the dry suspending agent after the suspension agent is spray-dried is usually smaller than 60 meshes, the particle surface area is large and hollow, the wetting time is long, and the indexes such as dust, wear resistance and the like are unqualified for most pesticide dry suspending agents. In order to further improve the performance of the resulting dry suspension of pesticides, researchers have made improvements on the formulations of the dry suspensions generally.
For example, CN109730060A discloses a method for preparing a pesticide dry suspension, which comprises selecting a high-performance dispersant to prepare a pesticide suspension with a medium-high content, adding a water-soluble high-temperature resistant dispersant and a water-soluble disintegrating agent into a suspension system, shearing, mixing, and spray-drying to obtain a dry suspension product. The method is mainly suitable for preparing the original drug system with high content of suspending agent and great difficulty, such as the original drug with low melting point and melting point lower than 80 ℃, the original drug with high water solubility and water solubility higher than 0.5g/L, and the original drug which is easy to form hydrogen bonds and water clusters with water. The preparation method for preparing the dry suspending agent can improve the solid content ratio in the prepared suspending slurry, reduce the energy consumption of spray drying and improve the granulation rate and the particle size of the dry suspending agent. Although the method improves the granulation rate and the particle size of the dry suspending agent through the high-performance dispersing agent and the water-soluble high-temperature resistant dispersing agent, the dust content and the wear resistance of the dry suspending agent are not obviously improved; the pesticide dry suspending agent improved by the preparation method has a complex formula and low practicability.
Therefore, the preparation method of the dry suspending agent with short wetting time and qualified indexes such as dust, wear resistance and the like is of great significance to the field.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to solve the problem that the finished product prepared by spray granulation of the dry suspending agent is unqualified in wettability, wear resistance, dust and the like, and the particle size of the obtained particles is between 10 and 30 meshes through a further boiling granulation mode, so that the indexes of the dry suspending agent, such as wetting time, wear resistance, dust and the like, are qualified, and meet the indexes of water dispersible granules specified by the national standard.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a process for preparing a dry suspension by combining spray drying and boiling granulation, the process comprising the steps of:
(1) preparing a preparation raw material of a dry suspending agent, mixing the preparation raw material with water, and crushing to obtain slurry;
(2) then, spray drying the slurry obtained in the step (1) to obtain mother powder;
(3) and (3) mixing the mother powder obtained in the step (2) with water, and carrying out boiling granulation, drying and screening to obtain the dry suspending agent.
According to the invention, spray drying and boiling granulation are combined, spray drying is firstly carried out, then boiling granulation is carried out, and the two treatment steps are carried out in this order, the step of boiling granulation can further agglomerate fine particles obtained by spray drying, and then dry suspending agent with particle size of 10-30 meshes is obtained by screening, so that the surface area of the particles is obviously increased, the specific gravity of the particles is increased, the wetting time is accelerated, dust is reduced, the wear resistance is increased, and the like; through detection, all indexes of the dry suspending agent prepared by the method meet the standards of water dispersible granules.
In a preferred embodiment of the present invention, the mass ratio of the preparation raw material to water in step (1) is 1 (0.5 to 1.5), and may be, for example, 1:0.5, 1:0.6, 1:0.8, 1:1, 1:1.2, 1:1.3, 1:1.4, or 1: 1.5.
Preferably, the pulverization of step (1) comprises wet grinding.
Preferably, the particle size D90 of the slurry in the step (1) is 1-5 μm, for example, 1 μm, 1.5 μm, 2 μm, 2.5 μm, 3 μm, 3.5 μm, 4 μm or 4.5 μm.
Preferably, the solid content of the slurry in the step (1) is 40-60%, for example, 40%, 42%, 45%, 48%, 50%, 52%, 54%, 55%, 56%, 58%, 60%, etc.
As a preferable technical scheme of the invention, the preparation raw materials in the step (1) comprise, by mass, 5-90% of raw pesticide, 1-10% of wetting agent, 10-30% of dispersing agent, 0.1-2% of adhesive and the balance filler.
In the present invention, the raw material for preparation includes, by mass%, 5 to 90% (for example, 5%, 8%, 10%, 15%, 20%, 30%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 80%, 90%, or the like), a raw drug, 1 to 10% (for example, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, or 10%, or the like), a wetting agent, 10 to 30% (for example, 10%, 12%, 14%, 15%, 16%, 18%, 20%, 22%, 25%, 26%, 28%, or 30%, or the like), a dispersing agent, 0.1 to 2% (for example, 0.1%, 0.2%, 0.5%, 0.8%, 1%, 1.2%, 1.5%, 1.6%, 1.8%, or 2%, or the like), a binder, and the balance of a filler.
Preferably, the technical material comprises any one or a combination of at least two of dimethomorph, trifloxystrobin tebuconazole, chlorothalonil, azoxystrobin, kresoxim-methyl, tribenuron-methyl, isoxaflutole, emamectin benzoate, difenoconazole or pyraclostrobin boscalid.
The dry suspension preparation varieties prepared by the invention include, but are not limited to, 75% trifloxystrobin tebuconazole, 80% dimethomorph, 90% chlorothalonil, 82.5% chlorothalonil, 25% azoxystrobin, 50% kresoxim-methyl, 75% tribenuron-methyl, 75% isoxaflutole, 10% emamectin benzoate, 20% difenoconazole and the like, 38% pyraclostrobin boscalid and the like.
Preferably, the wetting agent comprises any one of or a combination of at least two of sodium dodecylbenzene sulfonate, sodium dodecyl sulfate, isooctyl sulfosuccinate sodium salt, isopropyl naphthalene sulfonate potassium salt, alkyl naphthalene sulfonate sodium salt, or alkyl naphthalene sulfonate potassium salt or alkyl sulfate salt.
Preferably, the dispersant comprises any one of or a combination of at least two of a sodium lignosulfonate salt, a calcium lignosulfonate salt, a sodium naphthalenesulfonate formaldehyde condensate, a sodium phenol formaldehyde condensate salt, a sodium polycarboxylate salt or a potassium polycarboxylate salt.
Preferably, the binder comprises any one of or a combination of at least two of polyvinylpyrrolidone, hydroxypropyl methylcellulose, dextrin, polyethylene glycol, fructose, xanthan gum, arabic gum, polyvinyl alcohol and gelatin; preferably polyvinylpyrrolidone and/or polyvinyl alcohol.
Preferably, the filler comprises any one or a combination of at least two of diatomite, bentonite, kaolin, light calcium carbonate, heavy calcium carbonate, white carbon black, potassium sulfate, anhydrous sodium sulfate or barium sulfate; preferably kaolin and/or barium sulphate.
In a preferred embodiment of the present invention, the spray drying in step (2) comprises pressure spray drying.
Preferably, the feeding pressure of the pressure spray drying is 0.1 to 0.5MPa, and for example, may be 0.1MPa, 0.2MPa, 0.3MPa, 0.4MPa, or 0.5 MPa.
Preferably, the feeding rate of the pressure spray drying is 5 to 15mL/min, and may be, for example, 5mL/min, 6mL/min, 8mL/min, 10mL/min, 12mL/min, 14mL/min, or 15 mL/min.
Specifically, the working parameters of the pressure spray drying include: the power of an induced draft fan is 10-20 KW (for example, 11KW, 13KW, 15KW, 16KW or 18KW and the like), the power of the induced draft fan is 5-20 KW (for example, 6KW, 8KW, 10KW, 15KW or 18KW and the like), the power of an electric heater is 10-50 KW (for example, 15KW, 20KW, 25KW, 30KW, 35KW, 40KW or 45KW and the like), the feeding speed of a peristaltic pump is 5-15 mL/min, the feeding pressure is 0.1-0.5MPa, the inlet air temperature is 100-150 ℃ (for example, 110 ℃, 120 ℃, 130 ℃, 135 ℃, 140 ℃ or 145 ℃ and the like), and the outlet air temperature is 40-60 ℃ (for example, 42 ℃, 45 ℃, 50 ℃, 55 ℃ or 58 ℃ and the like).
Preferably, the working time of the pressure spray drying is 1-2 h, for example, 1h, 1.2h, 1.4h, 1.5h, 1.6h, 1.8h or 2h, etc.
Preferably, the water content of the mother powder in the step (2) is 5-10%, for example, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, 10%, or the like.
Preferably, the amount of water used in step (3) is 1-5% by weight of the mother powder, and may be, for example, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, or the like.
Preferably, the boiling granulation is carried out in a fluid bed granulation dryer.
Preferably, the water inlet rate of the boiling granulation is 5 to 8mL/min, and may be, for example, 5mL/min, 5.5mL/min, 5.8mL/min, 6mL/min, 6.5mL/min, 7mL/min, 7.5mL/min or the like.
The air temperature of the boiling granulation is preferably 110 to 115 ℃, and may be, for example, 110 ℃, 111 ℃, 112 ℃, 113 ℃, 114 ℃, or 115 ℃.
Preferably, the air outlet temperature of the boiling granulation is 50 to 60 ℃, and may be, for example, 50 ℃, 52 ℃, 54 ℃, 55 ℃, 56 ℃, 58 ℃ or 60 ℃.
Specifically, the operating parameters of the boiling granulation may be: the power of an induced draft fan is 15KW, the power of an air blower is 10KW, the power of an electric heater is 30KW, the water inlet speed of a peristaltic pump is 5mL/min, the pressure of an atomizer is 0.3MPa, the air inlet temperature is 110 ℃, and the air outlet temperature is 50 ℃.
Preferably, the working time of the boiling granulation is 30-90 min, for example, 30min, 35min, 40min, 45min, 50min, 55min, 60min, 65min, 70min, 80min or 90 min.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) preparing raw materials for preparing a dry suspending agent, wherein the raw materials comprise 5-90% of raw pesticide, 1-10% of wetting agent, 10-30% of dispersing agent, 0.1-2% of adhesive and the balance of filler according to mass percentage;
mixing the preparation raw materials with water in a feeding kettle, and grinding by a wet method to obtain slurry with the solid content of 40-60% and the particle size D90 of 1-5 mu m;
(2) then, carrying out pressure spray drying on the slurry obtained in the step (1) to obtain mother powder, wherein the water content of the mother powder is 5-10%;
(3) and (3) mixing the mother powder obtained in the step (2) with water, wherein the amount of the water is 1-5% of the weight of the mother powder, and carrying out boiling granulation, drying and screening to obtain the dry suspending agent.
In a second aspect, the present invention provides the use of a method as described in the first aspect for the preparation of a dry suspension of a pesticide.
In a third aspect, the invention also provides a pesticide dry suspending agent prepared by the method in the first aspect.
In the invention, the particle size of the pesticide dry suspending agent prepared by the method is 10-30 meshes, the wetting time is less than or equal to 60s, the wear resistance index is more than or equal to 99%, and the dust is less than or equal to 30 mg; meets the index requirements of the water dispersible granule in national standard and enterprise standard.
The recitation of numerical ranges herein includes not only the above-recited values, but also any values between any of the above-recited numerical ranges not recited, and for brevity and clarity, is not intended to be exhaustive of the specific values encompassed within the range.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the invention provides a method for preparing a dry suspending agent by combining spray drying and boiling granulation, which comprises the steps of preparing slurry according to 40-60% of solid content, grinding the slurry to the particle size D90 of 1-5 mu m by a wet method, then carrying out spray drying to obtain mother powder, mixing the mother powder with 1-5% of an adhesive, carrying out boiling granulation, drying and screening to obtain the 10-30-mesh dry suspending agent, wherein the wetting time of the obtained dry suspending agent finished product is less than or equal to 60s, the wear resistance index is greater than or equal to 99%, and the dust content is less than or equal to 30 mg;
(2) the method provided by the invention solves the problem that the finished product prepared by spray granulation of the dry suspending agent has unqualified indexes such as wettability, wear resistance and dust, and the particle size of the obtained particles is between 10 and 30 meshes by a further boiling granulation mode, so that the indexes of wetting time, wear resistance, dust and the like of the dry suspending agent are qualified, and the indexes of the water dispersible granule meet the national standard.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a dry suspending agent by combining spray drying and boiling granulation provided by the invention.
Detailed Description
The technical solutions of the present invention are further described in the following embodiments with reference to the drawings, but the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The preparation method provided by the invention comprises the steps as shown in figure 1:
firstly, preparing raw materials: preparing a raw pesticide, a wetting agent, a dispersing agent, an adhesive and a filler in proportion, mixing the raw pesticide and water in a feeding kettle, and performing wet sanding to obtain slurry;
and spray-drying the obtained slurry to obtain master batches, mixing the master batches with water for boiling granulation, drying and screening after the boiling granulation is finished, and packaging after the detection is qualified to obtain the dry suspending agent.
Example 1
The embodiment provides a preparation method of a 75% tebuconazole-trifloxystrobin dry suspending agent, which specifically comprises the following steps:
(1) preparing raw materials of the dry suspending agent, wherein the mixture ratio of the raw materials is shown in table 1:
TABLE 1
Formulation composition Function(s) Feed proportioning
Tebuconazole original drug Active ingredient 50％
Trifloxystrobin technical Active ingredient 25％
Polycarboxylic acid sodium salt Dispersing agent 10％
Sulfonated succinic acid isooctyl ester sodium salt Wetting agent 3％
Polyvinylpyrrolidone Adhesive agent 0.2％
Barium sulfate Filler material Make up to 100%
(2) Preparing slurry according to 50% of solid content, adding 1000g of deionized water into a preparation kettle, and adding the following components under the stirring condition:
30g of sulfonated isooctyl succinate sodium salt, 100g of polycarboxylic acid sodium salt and 2g of polyvinylpyrrolidone are stirred until the sulfonated isooctyl succinate sodium salt, 100g of polycarboxylic acid sodium salt and 2g of polyvinylpyrrolidone are completely dissolved, 257.7g of 97% trifloxystrobin technical material and 515.5g of 97% tebuconazole technical material are added, and the kaolin is complemented to 1000 g;
cutting, and sanding until D90 is 3 μm to obtain slurry;
the slurry is subjected to pressure spray drying to collect mother powder with 6.5% of water, and then the mother powder is transferred into an FLP-3 multifunctional fluidized bed granulation dryer (Changzhou Lijian granulation drying equipment Co., Ltd.), and 4% of water is sprayed to be mixed with the mother powder for boiling granulation, drying and screening to obtain a sample.
Example 2
The embodiment provides a preparation method of a 75% pentoxazole and trifloxystrobin dry suspending agent, which specifically comprises the following steps:
(1) preparing raw materials for preparing the dry suspending agent, wherein the mixture ratio of the raw materials is shown in table 2:
TABLE 2
Formulation composition Function(s) Feed proportioning
Tebuconazole original drug Active ingredient 50％
Trifloxystrobin technical Active ingredient 25％
Polycarboxylic acid sodium salt Dispersing agent 10％
Sulfonated succinic acid isooctyl ester sodium salt Wetting agent 6％
Polyvinylpyrrolidone Adhesive agent 0.4％
Barium sulfate Carrier Make up to 100%
(2) Preparing slurry according to 50% of solid content, adding 1000g of deionized water into a preparation kettle, and adding the following components under the stirring condition:
60g of sulfonated isooctyl succinate sodium salt, 100g of polycarboxylic acid sodium salt and 4g of polyvinylpyrrolidone are stirred until the sulfonated isooctyl succinate sodium salt, 100g of polycarboxylic acid sodium salt and 4g of polyvinylpyrrolidone are completely dissolved, then 257.7g of 97% trifloxystrobin technical, 515.5g of 97% tebuconazole technical are added, and the kaolin is complemented to 1000 g;
cutting, and sanding until D90 is 3 μm to obtain slurry;
and (3) carrying out pressure spray drying on the slurry to collect mother powder with the water content of 9.5%, transferring the mother powder into an FLP-3 multifunctional fluidized bed granulation dryer, spraying 2.5% of water, mixing with the mother powder, carrying out secondary granulation, drying and screening to obtain a sample.
Example 3
The embodiment provides a preparation method of a 75% pentoxazole and trifloxystrobin dry suspending agent, which specifically comprises the following steps:
(1) preparing raw materials of the dry suspending agent, wherein the mixture ratio of the raw materials is shown in table 3:
TABLE 3
Figure BDA0002880717830000091
Figure BDA0002880717830000101
(2) Preparing slurry according to 50% solid content, adding 1000g of deionized water into a preparation kettle, and adding the following components under the stirring condition:
90g of sulfonated isooctyl succinate sodium salt, 100g of polycarboxylic acid sodium salt and 6g of polyvinylpyrrolidone are stirred until the sulfonated isooctyl succinate sodium salt, 100g of polycarboxylic acid sodium salt and 6g of polyvinylpyrrolidone are completely dissolved, then 257.7g of 97% trifloxystrobin technical product and 515.5g of 97% tebuconazole technical product are added, and the kaolin is complemented to 1000 g;
cutting, and sanding until D90 is 3 μm to obtain slurry;
and (3) carrying out pressure spray drying on the slurry to collect mother powder with the moisture content of 5.5%, transferring the mother powder into an FLP-3 multifunctional fluidized bed granulation dryer, spraying 4.5% of water, mixing with the mother powder, carrying out secondary granulation, drying and screening to obtain a sample.
Comparative example 1
The preparation method is different from the embodiment 1 in that after the slurry is subjected to pressure spray drying and collected, the water content of the mother powder is within 3 percent after boiling drying, and a dry suspending agent sample is obtained; namely, the granules are not transferred into a FLP-3 multifunctional fluidized bed granulation dryer for boiling granulation, and the rest steps are kept consistent with the steps in the example 1.
Comparative example 2
The difference from the embodiment 2 is that in the preparation method, after the slurry is subjected to pressure spray drying and collected, the water content of the mother powder is within 3 percent after boiling drying, and a dry suspending agent sample is obtained; namely, the mixture is not transferred into an FLP-3 multifunctional fluidized bed granulation dryer for boiling granulation, and the rest steps are kept consistent with the step 2.
Comparative example 3
The difference from the embodiment 3 is that in the preparation method, after the slurry is subjected to pressure spray drying and collected, the water content of the mother powder is within 3 percent after boiling drying, and a dry suspending agent sample is obtained; namely, the granules are not transferred into a FLP-3 multifunctional fluidized bed granulation dryer for boiling granulation, and the rest steps are kept consistent with the steps in the example 3.
Performance analysis
Performing performance analysis on the samples provided in examples 1-3 and comparative examples 1-3; the sample data for examples 1-3 are shown in Table 4:
TABLE 4
Figure BDA0002880717830000111
The data for the samples of comparative examples 1-3 are shown in Table 5:
TABLE 5
Figure BDA0002880717830000121
As can be seen from Table 4, through the fluidized bed boiling granulation for the second time, the detection results of 3 groups of examples show that the indexes such as wetting time, dust, wear resistance and the like all accord with the water dispersion particle size standard; wherein the wetting time is 40-55 s, the dust content is 20-28 mg, and the wear resistance is 99.2-99.8%;
as can be seen from Table 5, the comparative examples 1 to 3 show that the wetting time is reduced with the increase of the amount of the wetting agent, but the wetting time is still more than 90s, and the index requirements are not met; with the increase of the dosage of the adhesive, although the dust amount is also reduced, when the dosage of the adhesive is 0.6 percent, the dust index is qualified; therefore, with the increase of the consumption of the wetting agent and the adhesive, the dust index meets the index, the expressed suspension rate is reduced, but the indexes such as wetting time, wear resistance and the like are not qualified; therefore, increasing the amount of binder can only improve the dust index, but not the wetting time and wear resistance index, and the wetting agent and binder can not be increased infinitely.
Comparative example 4
The difference from example 1 is that the slurry was collected by pressure spray drying, mixed with 4% water and mother powder, transferred to a ZLB80 rotary extrusion granulator (zhanggang ronghua mechanical manufacturing limited) for granulation, and subjected to fluidized drying to compare with the sample obtained in example 1, and the analysis results are shown in table 6:
TABLE 6
Figure BDA0002880717830000131
Figure BDA0002880717830000141
From the table, the indexes of wetting time, dust, wear resistance and the like of the 75% pentoxazole-trifloxystrobin water dispersible particle size rotary extrusion granulation mode are superior to those of the fluidized bed boiling granulation mode, but the extrusion granulation process has stronger compactness than that of the boiling granulation, the disintegration frequency is far greater than that of the boiling granulation mode, the field use can prolong the dispersion time, and the suspension rate is lower than that of the fluidized bed boiling granulation mode.
Therefore, the dry suspending agent is further fluidized bed fluidized granulation to increase the particle size and compactness of particles, so that unqualified indexes such as wetting time, wear resistance, dust and the like can be solved.
Example 4
The embodiment provides a preparation method of an 80% dimethomorph dry suspending agent, which specifically comprises the following steps:
preparing slurry according to 50% of solid content, adding 1000g of water into a preparation kettle, adding 40g of diisopropyl sodium naphthalene sulfonate, 50g of phenol formaldehyde condensate, 50g of naphthalene sulfonic acid formaldehyde condensate, 30g of sodium polyacrylate, 2g of polyvinylpyrrolidone and kaolin to complement to 1000g under the stirring condition, and cutting and sanding until D90 is 3 mu m to obtain the slurry;
carrying out pressure spray drying on the slurry to collect mother powder with the water content of 7.5%, transferring the mother powder into an FLP-3 multifunctional fluidized bed granulation dryer, spraying 3.5% of water to mix with the mother powder for secondary granulation, and screening to obtain 80% of dimethomorph dry suspending agent;
for comparison, this example also collects a sample of a portion of the base meal that was boiling dried to less than 3% moisture, but not boiling granulated.
Example 5
The embodiment provides a preparation method of a 90% chlorothalonil dry suspending agent, which specifically comprises the following steps:
preparing slurry according to 50% of solid content, adding 1000g of water into a preparation kettle, adding 20g of sodium diisopropyl naphthalenesulfonate and 70.9g of sodium polyacrylate under the stirring condition, stirring until the sodium diisopropyl naphthalenesulfonate and the sodium polyacrylate are completely dissolved, then adding 909.1g of 99% chlorothalonil, and cutting and sanding the mixture until the D90 is 3 microns to obtain the slurry;
carrying out pressure spray drying on the slurry to collect mother powder with the water content of 5.5%, transferring the mother powder into an FLP-3 multifunctional fluidized bed granulation dryer, spraying 4.5% of water to mix with the mother powder for secondary granulation, drying and screening to obtain 90% of chlorothalonil dry suspending agent;
for comparison, this example also collects a sample of a portion of the base meal that was boiling dried to less than 3% moisture, but not boiling granulated.
Example 6
The embodiment provides a preparation method of 82.5% chlorothalonil dry suspending agent, which specifically comprises the following steps:
preparing slurry according to 50% solid content, adding 1000g of water into a preparation kettle, adding 20g of lauryl sodium sulfate, 40g of naphthalene sulfonic acid formaldehyde condensate, 30g of sodium polyacrylate and 2g of polyvinyl alcohol under the stirring condition, stirring until the materials are completely dissolved, then adding 833.3g of 99% chlorothalonil, complementing the barium sulfate to 1000g, starting shearing and sanding until D90 is 3 microns, and obtaining the slurry;
carrying out pressure spray drying on the slurry to collect mother powder with the water content of 9.0%, transferring the mother powder into an FLP-3 multifunctional fluidized bed granulation dryer, spraying 2.5% of water, mixing with the mother powder, carrying out secondary granulation, drying and screening to obtain 82.5% of chlorothalonil dry suspending agent;
for comparison, this example also collects a sample of a portion of the base meal that was boiling dried to less than 3% moisture, but not boiling granulated.
Example 7
The embodiment provides a preparation method of 25% azoxystrobin dry suspending agent, which specifically comprises the following steps:
preparing slurry according to 50% of solid content, adding 1000g of water into a preparation kettle, adding 60g of sodium dodecyl benzene sulfonate, 30g of naphthalene sulfonic acid formaldehyde condensate and 10g of polyvinylpyrrolidone under the stirring condition, stirring until the mixture is completely dissolved, adding 255.1g of 98% azoxystrobin and kaolin to complement to 1000g, starting shearing and sanding until D90 is 3 mu m, and obtaining the slurry;
the slurry is sprayed and dried under pressure, mother powder with the water content of 8.5 percent is collected and then transferred into an FLP-3 multifunctional fluidized bed granulation dryer, and then 3.0 percent of water is sprayed to be mixed with the mother powder for secondary granulation, drying and screening to obtain 82.5 percent of chlorothalonil dry suspending agent;
for comparison, this example also collects a sample of a portion of the base meal that was boiling dried to less than 3% moisture, but not boiling granulated.
Example 8
The embodiment provides a preparation method of a 50% kresoxim-methyl dry suspending agent, which specifically comprises the following steps:
preparing slurry according to 50% of solid content, adding 1000g of water into a preparation kettle, adding 25g of isooctyl sulfosuccinate sodium salt, 50g of polyacrylic acid sodium salt and 5g of polyvinylpyrrolidone under the stirring condition, stirring until the materials are completely dissolved, adding 510.2g of kresoxim-methyl, complementing light calcium to 1000g, starting shearing and sanding until D90 is 3 mu m, and obtaining the slurry;
carrying out pressure spray drying on the slurry to collect mother powder with the water content of 6.0%, transferring the mother powder into an FLP-3 multifunctional fluidized bed granulation dryer, spraying 4.5% of water, mixing with the mother powder, carrying out secondary granulation, drying and screening to obtain 50% of kresoxim-methyl dry suspending agent;
for comparison, this example also collects a sample of a portion of the base meal that was boiling dried to less than 3% moisture, but not boiling granulated.
Example 9
The embodiment provides a preparation method of a 75% tribenuron-methyl dry suspending agent, which specifically comprises the following steps:
preparation of 75% tribenuron-methyl dry suspending agent
Preparing slurry according to 50% solid content, adding 1000g of water into a preparation kettle, adding 30g of isopropyl naphthalene sulfonic acid sodium salt, 100g of sodium lignosulphonate, 40g of polyacrylic acid sodium salt and 2g of hydroxypropyl methyl cellulose under the stirring condition, stirring until the materials are completely dissolved, adding 773.2g of tribenuron-methyl and barium sulfate to complement to 1000g, and starting shearing and sanding until D90 is 3 mu m to obtain the slurry;
carrying out pressure spray drying on the slurry to collect mother powder with the water content of 10%, transferring the mother powder into an FLP-3 multifunctional fluidized bed granulation dryer, spraying 1% of water, mixing with the mother powder, carrying out secondary granulation, drying and screening to obtain 75% tribenuron-methyl dry suspending agent;
for comparison, this example also collects a sample of a portion of the base meal that was boiling dried to less than 3% moisture, but not boiling granulated.
Example 10
The embodiment provides a preparation method of 75% isoxaflutole dry suspending agent, which specifically comprises the following steps:
preparation of 75% isoxaflutole dry suspending agent
Preparing slurry according to 50% of solid content, adding 1000g of water into a preparation kettle, adding 40g of sodium dodecyl sulfate, 60g of sodium polyacrylate and 5g of Arabic gum under stirring, stirring until the sodium dodecyl sulfate, the sodium polyacrylate and the Arabic gum are completely dissolved, adding 765.3g of isoxaflutole and kaolin to complement to 1000g, and cutting and sanding until D90 is 3 microns to obtain the slurry;
carrying out pressure spray drying on the slurry to collect mother powder with the moisture content of 5.5%, transferring the mother powder into an FLP-3 multifunctional fluidized bed granulation dryer, spraying 5.0% of water, mixing with the mother powder, carrying out secondary granulation, drying and screening to obtain 75% of isoxaflutole dry suspending agent;
for comparison, this example also collects a sample of a portion of the base meal that was boiling dried to less than 3% moisture, but not boiling granulated.
Example 11
The embodiment provides a preparation method of a 10% emamectin benzoate dry suspending agent, which specifically comprises the following steps:
preparing slurry according to 50% of solid content, adding 1000g of water into a preparation kettle, adding 40g of dibutyl naphthalene sulfonic acid potassium salt, 80g of sodium lignosulfonate, 60g of naphthalene sulfonic acid formaldehyde condensate, 20g of polyacrylic acid sodium salt, 6g of fructose and 300g of kaolin under the stirring condition, stirring until the mixture is completely dispersed, adding 130g of emamectin benzoate and bentonite to complement to 1000g, and performing shearing and sanding until D90 is 3 mu m to obtain the slurry;
carrying out pressure spray drying on the slurry to collect mother powder with the water content of 6.5%, transferring the mother powder into an FLP-3 multifunctional fluidized bed granulation dryer, spraying 3.5% of water, mixing with the mother powder, carrying out secondary granulation, drying and screening to obtain 10% of emamectin benzoate dry suspending agent;
for comparison, this example also collects a sample of a portion of the base meal that was boiling dried to less than 3% moisture, but not boiling granulated.
Example 12
The embodiment provides a preparation method of 20% difenoconazole dry suspension, which comprises the following steps:
preparing slurry according to 50% of solid content, adding 1000g of water into a preparation kettle, adding 30g of sodium dodecyl benzene sulfonate, 100g of phenol formaldehyde condensate sodium salt, 100g of naphthalene sulfonic acid formaldehyde condensate sodium salt and 30g of polyacrylic acid sodium salt under the stirring condition, stirring until the mixture is completely dispersed, adding 204g of difenoconazole and 30g of light calcium to complement to 1000g, and starting shearing and sanding until D90 is 3 mu m to obtain the slurry;
carrying out pressure spray drying on the slurry to collect mother powder with the moisture content of 7.2%, transferring the mother powder into an FLP-3 multifunctional fluidized bed granulation dryer, spraying 4.3% of water, mixing with the mother powder, carrying out secondary granulation, drying and screening to obtain 20% of difenoconazole dry suspending agent;
for comparison, this example also collects a sample of a portion of the base meal that was boiling dried to less than 3% moisture, but not boiling granulated.
Example 13
The embodiment provides a preparation method of a 38% pyraclostrobin-boscalid dry suspending agent, which specifically comprises the following steps:
preparing slurry according to 50% solid content, adding 1000g of water into a preparation kettle, adding 40g of diisobutylnaphthalenesulfonate, 30g of phenol formaldehyde condensate, 80g of polyacrylic acid sodium salt and 2g of xanthan gum under stirring, and stirring until the materials are completely dissolved. Under the condition of stirring, adding 132g of 97% pyraclostrobin, 257.1g of 98% boscalid and barium sulfate to complement to 1000g, and carrying out shearing and sanding until D90 is 3 mu m to obtain slurry;
carrying out pressure spray drying on the slurry to collect mother powder with the moisture content of 6%, transferring the mother powder into an FLP-3 multifunctional fluidized bed granulation dryer, spraying 3% of water, mixing with the mother powder, carrying out secondary granulation, drying and screening to obtain 38% pyraclostrobin-boscalid dry suspending agent;
for comparison, this example also collects a sample of a portion of the base meal that was boiling dried to less than 3% moisture, but not boiling granulated.
The above products were tested separately and the results are detailed in table 7:
TABLE 7
Figure BDA0002880717830000191
Figure BDA0002880717830000201
Remarking: the wetting time is less than or equal to 60s, the wear resistance is more than or equal to 99 percent, and the dust is less than or equal to 30 mg.
As can be seen from the data in the table above, after the 10 dry suspending agents are subjected to primary drying by grinding pressure spray, fluidized bed boiling granulation is performed, after drying and screening, the particle size of the finished product is increased, the compactness is strong, and the wetting time, the dust and the wear resistance index meet the requirements.
The invention solves the problems that the finished product of the dry suspending agent spray granulation has unqualified indexes such as wettability, wear resistance, dust and the like, and the particle size of the obtained particles is between 10 and 30 meshes by a further boiling granulation mode, so that the indexes of wetting time, wear resistance, dust and the like of the dry suspending agent granulation are qualified, and the indexes of the water dispersible granule meet the national standard.
The invention is illustrated by the above embodiments that various indexes such as wetting time, wear resistance, dust and the like obtained by the fluidized bed boiling granulation method after pressure spray drying meet the preparation requirements of the water dispersible granule, but the invention is not limited to the above embodiments.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (10)

1. A method for preparing a dry suspending agent by combining spray drying and boiling granulation, which is characterized by comprising the following steps:
(1) preparing a preparation raw material of a dry suspending agent, mixing the preparation raw material with water, and crushing to obtain slurry;
(2) then, spray drying the slurry obtained in the step (1) to obtain mother powder;
(3) and (3) mixing the mother powder obtained in the step (2) with water, and carrying out boiling granulation, drying and screening to obtain the dry suspending agent.
2. The method according to claim 1, wherein the mass ratio of the preparation raw material to the water in the step (1) is 1 (0.5-1.5);
preferably, the pulverization of step (1) comprises wet grinding;
preferably, the particle size D90 of the slurry in the step (1) is 1-5 μm;
preferably, the solid content of the slurry in the step (1) is 40-60%.
3. The method according to claim 1 or 2, wherein the preparation raw materials in the step (1) comprise, by mass, 5-90% of raw pesticide, 1-10% of wetting agent, 10-30% of dispersing agent and 0.1-2% of adhesive, and the balance filler;
preferably, the technical material comprises any one or a combination of at least two of dimethomorph, trifloxystrobin tebuconazole, chlorothalonil, azoxystrobin, kresoxim-methyl, tribenuron-methyl, isoxaflutole, emamectin benzoate, difenoconazole or pyraclostrobin boscalid.
4. The method of claim 3, wherein the wetting agent comprises any one or a combination of at least two of sodium dodecylbenzene sulfonate, sodium dodecyl sulfate, isooctyl sulfosuccinate sodium salt, isopropyl naphthalene sulfonate potassium salt, alkyl naphthalene sulfonate sodium salt, or alkyl naphthalene sulfonate potassium salt or alkyl sulfate salt;
preferably, the dispersant comprises any one of or a combination of at least two of sodium lignosulfonate, calcium lignosulfonate, naphthalene sulfonic acid formaldehyde condensate sodium salt, phenol formaldehyde condensate sodium salt, polycarboxylic acid sodium salt or polycarboxylic acid potassium salt;
preferably, the binder comprises any one of or a combination of at least two of polyvinylpyrrolidone, hydroxypropyl methylcellulose, dextrin, polyethylene glycol, fructose, xanthan gum, arabic gum, polyvinyl alcohol and gelatin; preferably polyvinylpyrrolidone and/or polyvinyl alcohol;
preferably, the filler comprises any one or a combination of at least two of diatomite, bentonite, kaolin, light calcium carbonate, heavy calcium carbonate, white carbon black, potassium sulfate, anhydrous sodium sulfate or barium sulfate; preferably kaolin and/or barium sulphate.
5. The method according to any one of claims 1 to 4, wherein the spray drying of step (2) comprises pressure spray drying;
preferably, the feed pressure for the pressure spray drying is from 0.1 to 0.5 MPa;
preferably, the feeding speed of the pressure spray drying is 5-15 mL/min;
preferably, the working time of the pressure spray drying is 1-2 h;
preferably, the water content of the mother powder in the step (2) is 5-10%.
6. A process according to any one of claims 1 to 5, wherein the amount of water used in step (3) is from 1 to 5% by weight of the masterbatch.
7. The method according to any one of claims 1 to 6, wherein the boiling granulation is carried out in a fluidized bed granulation dryer;
preferably, the water inlet speed of the boiling granulation is 5-8 mL/min;
preferably, the air inlet temperature of the boiling granulation is 110-115 ℃;
preferably, the air outlet temperature of the boiling granulation is 50-60 ℃;
preferably, the working time of the boiling granulation is 30-90 min.
8. A method according to any one of claims 1 to 7, characterized in that the method comprises the steps of:
(1) preparing raw materials for preparing a dry suspending agent, wherein the raw materials comprise 5-90% of raw pesticide, 1-10% of wetting agent, 10-30% of dispersing agent, 0.1-2% of adhesive and the balance of filler according to mass percentage;
mixing the preparation raw materials with water in a feeding kettle, and grinding by a wet method to obtain slurry with the solid content of 40-60% and the particle size D90 of 1-5 mu m;
(2) then, carrying out pressure spray drying on the slurry obtained in the step (1) to obtain mother powder, wherein the water content of the mother powder is 5-10%;
(3) and (3) mixing the mother powder obtained in the step (2) with water, wherein the amount of the water is 1-5% of the weight of the mother powder, and carrying out boiling granulation, drying and screening to obtain the dry suspending agent.
9. Use of a method according to any one of claims 1 to 8 for the preparation of a dry suspension of a pesticide.
10. A dry pesticide suspension prepared by the method of any one of claims 1 to 8;
preferably, the particle size of the pesticide dry suspending agent is 10-30 meshes;
preferably, the wetting time of the pesticide dry suspending agent is less than or equal to 60 s;
preferably, the wear resistance index of the pesticide dry suspending agent is more than or equal to 99 percent;
preferably, the dust of the pesticide dry suspending agent is less than or equal to 30 mg.
CN202011633893.5A 2020-12-31 2020-12-31 Method for preparing dry suspending agent by combining spray drying and boiling granulation Pending CN114681937A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011633893.5A CN114681937A (en) 2020-12-31 2020-12-31 Method for preparing dry suspending agent by combining spray drying and boiling granulation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011633893.5A CN114681937A (en) 2020-12-31 2020-12-31 Method for preparing dry suspending agent by combining spray drying and boiling granulation

Publications (1)

Publication Number Publication Date
CN114681937A true CN114681937A (en) 2022-07-01

Family

ID=82134001

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011633893.5A Pending CN114681937A (en) 2020-12-31 2020-12-31 Method for preparing dry suspending agent by combining spray drying and boiling granulation

Country Status (1)

Country Link
CN (1) CN114681937A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114176088A (en) * 2021-12-03 2022-03-15 中化化工科学技术研究总院有限公司 Azoxystrobin dry suspending agent and preparation method thereof
CN116831279A (en) * 2023-08-08 2023-10-03 江苏苏盐井神股份有限公司 Hollow granulating sodium-reducing edible salt and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114176088A (en) * 2021-12-03 2022-03-15 中化化工科学技术研究总院有限公司 Azoxystrobin dry suspending agent and preparation method thereof
CN116831279A (en) * 2023-08-08 2023-10-03 江苏苏盐井神股份有限公司 Hollow granulating sodium-reducing edible salt and preparation method thereof

Similar Documents

Publication Publication Date Title
CN114681937A (en) Method for preparing dry suspending agent by combining spray drying and boiling granulation
CN101579746B (en) Preparation method of micron-sized superfine silver powder with shapes of pine cones, flowers or trees
CN104248990B (en) The preparation method of the composite mesoporous carrier of spherical attapulgite and loaded catalyst and its preparation method and application and ethyl acetate
CN104248991B (en) The preparation method of the composite mesoporous carrier of spherical montmorillonite and loaded catalyst and its preparation method and application and ethyl acetate
CN104248980B (en) The preparation method of spherical diatomite mesoporous composite material and loaded catalyst and its preparation method and application and ethyl acetate
CN111607036B (en) Lignin modified polycarboxylate dispersant, and preparation method and application thereof
WO2020151377A1 (en) Preparation method for pesticide dry flowable
CN107501448A (en) A kind of preparation method and application of nanoscale sulfonated polystyrene microballoon
CN104248987A (en) Spherical montmorillonite mesoporous composite material, supported catalyst and preparation method and application thereof and preparation method of ethyl acetate
CN112317759B (en) Preparation method of micro-nano silver powder
CN107804854A (en) The method that cupric silicate nanotube is prepared using low-grade attapulgite clay
CN111978595B (en) Environment-friendly silver-loaded antibacterial agent based on plant waste powder and preparation method thereof
CN106278273B (en) A kind of preparation method of superfine boron carbide mist projection granulating powder
CA2362761C (en) Pigment granulate for the colouring of building materials and processes for its manufacture
CN113548653B (en) Production process of pharmaceutic adjuvant anhydrous calcium hydrophosphate with direct-pressure function
CN107930644A (en) A kind of high-performance methanol synthesis catalyst and preparation method thereof
CN101300975A (en) Granulation method of pesticide dry suspending agent
JP2703686B2 (en) Process for producing improved dye granules
CN105622896B (en) A kind of water-based pigment colour paste hyper-dispersant and preparation method thereof
CN105294313B (en) Low-grade talc fertilizer anti-caking agent and preparation method and application thereof
CN116967461A (en) High-dispersion low-burning-loss superfine silver powder and preparation method thereof
CN116393713A (en) Preparation method of small-particle-size flake silver powder for fine line printing
JPS63260816A (en) Manufacture of fine grain calcium sulfate
CN1548460A (en) Dry hydroxyalkyl starch producing process
CN116492396B (en) Preparation method of bunge cherry seed formula particles

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination