CN115633680A - Granulation method of low-melting-point pesticide granules - Google Patents
Granulation method of low-melting-point pesticide granules Download PDFInfo
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- CN115633680A CN115633680A CN202211309830.3A CN202211309830A CN115633680A CN 115633680 A CN115633680 A CN 115633680A CN 202211309830 A CN202211309830 A CN 202211309830A CN 115633680 A CN115633680 A CN 115633680A
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- 239000008187 granular material Substances 0.000 title claims abstract description 99
- 238000005469 granulation Methods 0.000 title claims abstract description 99
- 230000003179 granulation Effects 0.000 title claims abstract description 99
- 238000000034 method Methods 0.000 title claims abstract description 57
- 239000000575 pesticide Substances 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 87
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002245 particle Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 238000002844 melting Methods 0.000 claims abstract description 15
- 230000008018 melting Effects 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000012216 screening Methods 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims abstract description 4
- 238000001125 extrusion Methods 0.000 claims description 14
- 239000004562 water dispersible granule Substances 0.000 claims description 10
- IUQJDHJVPLLKFL-UHFFFAOYSA-N 2-(2,4-dichlorophenoxy)acetate;dimethylazanium Chemical compound CNC.OC(=O)COC1=CC=C(Cl)C=C1Cl IUQJDHJVPLLKFL-UHFFFAOYSA-N 0.000 claims description 4
- CAWXEEYDBZRFPE-UHFFFAOYSA-N Hexazinone Chemical compound O=C1N(C)C(N(C)C)=NC(=O)N1C1CCCCC1 CAWXEEYDBZRFPE-UHFFFAOYSA-N 0.000 claims description 4
- 239000005869 Pyraclostrobin Substances 0.000 claims description 4
- YASYVMFAVPKPKE-UHFFFAOYSA-N acephate Chemical compound COP(=O)(SC)NC(C)=O YASYVMFAVPKPKE-UHFFFAOYSA-N 0.000 claims description 4
- ZEKANFGSDXODPD-UHFFFAOYSA-N glyphosate-isopropylammonium Chemical compound CC(C)N.OC(=O)CNCP(O)(O)=O ZEKANFGSDXODPD-UHFFFAOYSA-N 0.000 claims description 4
- VDCHTAFVUAPYGO-UHFFFAOYSA-N n-methylmethanamine;2-(phosphonomethylamino)acetic acid Chemical compound CNC.OC(=O)CNCP(O)(O)=O VDCHTAFVUAPYGO-UHFFFAOYSA-N 0.000 claims description 4
- HZRSNVGNWUDEFX-UHFFFAOYSA-N pyraclostrobin Chemical compound COC(=O)N(OC)C1=CC=CC=C1COC1=NN(C=2C=CC(Cl)=CC=2)C=C1 HZRSNVGNWUDEFX-UHFFFAOYSA-N 0.000 claims description 4
- PZBPKYOVPCNPJY-UHFFFAOYSA-N 1-[2-(allyloxy)-2-(2,4-dichlorophenyl)ethyl]imidazole Chemical compound ClC1=CC(Cl)=CC=C1C(OCC=C)CN1C=NC=C1 PZBPKYOVPCNPJY-UHFFFAOYSA-N 0.000 claims description 3
- 239000005795 Imazalil Substances 0.000 claims description 3
- RQVYBGPQFYCBGX-UHFFFAOYSA-N ametryn Chemical compound CCNC1=NC(NC(C)C)=NC(SC)=N1 RQVYBGPQFYCBGX-UHFFFAOYSA-N 0.000 claims description 3
- 229960002125 enilconazole Drugs 0.000 claims description 3
- LFULEKSKNZEWOE-UHFFFAOYSA-N propanil Chemical compound CCC(=O)NC1=CC=C(Cl)C(Cl)=C1 LFULEKSKNZEWOE-UHFFFAOYSA-N 0.000 claims description 3
- IROINLKCQGIITA-UHFFFAOYSA-N terbutryn Chemical compound CCNC1=NC(NC(C)(C)C)=NC(SC)=N1 IROINLKCQGIITA-UHFFFAOYSA-N 0.000 claims description 3
- HXMBBZAHRWCZOX-UHFFFAOYSA-N 2-(2,4-dichlorophenoxy)acetic acid;propan-2-amine Chemical compound CC(C)[NH3+].[O-]C(=O)COC1=CC=C(Cl)C=C1Cl HXMBBZAHRWCZOX-UHFFFAOYSA-N 0.000 claims description 2
- -1 diacyl-chlor Chemical compound 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000001704 evaporation Methods 0.000 abstract description 3
- 230000008020 evaporation Effects 0.000 abstract description 3
- 238000009835 boiling Methods 0.000 abstract description 2
- 238000001953 recrystallisation Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 33
- 239000000843 powder Substances 0.000 description 16
- 238000007796 conventional method Methods 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 239000011265 semifinished product Substances 0.000 description 8
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 5
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 5
- 235000011130 ammonium sulphate Nutrition 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 5
- 239000000080 wetting agent Substances 0.000 description 5
- 239000000498 cooling water Substances 0.000 description 4
- 239000003337 fertilizer Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000001413 cellular effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical class CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 235000019832 sodium triphosphate Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000005631 2,4-Dichlorophenoxyacetic acid Substances 0.000 description 1
- PUKLDDOGISCFCP-JSQCKWNTSA-N 21-Deoxycortisone Chemical compound C1CC2=CC(=O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@@](C(=O)C)(O)[C@@]1(C)CC2=O PUKLDDOGISCFCP-JSQCKWNTSA-N 0.000 description 1
- VTNQPKFIQCLBDU-UHFFFAOYSA-N Acetochlor Chemical compound CCOCN(C(=O)CCl)C1=C(C)C=CC=C1CC VTNQPKFIQCLBDU-UHFFFAOYSA-N 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- FCYKAQOGGFGCMD-UHFFFAOYSA-N Fulvic acid Natural products O1C2=CC(O)=C(O)C(C(O)=O)=C2C(=O)C2=C1CC(C)(O)OC2 FCYKAQOGGFGCMD-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- YZJQFZBOIZKCHF-UHFFFAOYSA-N azane;propan-2-amine Chemical compound N.CC(C)N YZJQFZBOIZKCHF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007791 dehumidification Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 125000002147 dimethylamino group Chemical class [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229940095100 fulvic acid Drugs 0.000 description 1
- 239000002509 fulvic acid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003090 pesticide formulation Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001007 puffing effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 239000004549 water soluble granule Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a granulation method of low-melting-point pesticide granules, which is characterized in that wet materials containing low-melting-point pesticide are granulated, the temperature is kept at 55-95 ℃ in the granulation process, and the discharging temperature is 45-85 ℃; cooling the granulated wet granules immediately by air cooling to cool and solidify the surfaces of the wet granules; and (4) drying the air-cooled particles in a fluidized bed, and then screening to obtain the granules. The invention adopts the high-temperature surface melting granulation with less water, improves the granulation rate during the initial production, ensures that the surface skeleton of the particles is rapidly formed due to the rapid evaporation of the surface moisture and the recrystallization of the melting material under the action of high temperature and cold air during the granulation, improves the strength of the wet particle material, reduces the surface viscosity of the material, ensures that the particles are not adhered and crushed after falling into a fluidized bed, cannot be crushed due to the stress of falling into the fluidized bed and the stress of drying boiling, improves the yield, reduces the rework, reduces the production difficulty and the cost of the product, and improves the economy of the product.
Description
Technical Field
The invention relates to a granulation method suitable for a pesticide with a low melting point, in particular to a granulation method for a low melting point pesticide granule with a melting point lower than 100 ℃, and belongs to the technical field of pesticide dosage form preparation.
Background
The granule is a common pesticide formulation, and the water-soluble granule and the water dispersible granule are both granules. Currently, the conventional granulation method of granules is: mixing the materials with water to obtain wet materials, feeding the wet materials into a granulator, granulating in the granulator, directly dropping the obtained granules into a fluidized bed for drying after cooling by adopting cold water, and then screening to obtain granules. In the granulation method, the water content of the wet material is generally between 15 and 25 percent, the water content is large, the granulation is generally carried out by extrusion granulation, the water solubility is enhanced due to overhigh temperature during the granulation, the water solubility of the material is changed due to extrusion in the granulation process, the material is changed into thin paste and cannot be granulated, and therefore the granulation is generally carried out at the low temperature of between 20 and 30 ℃. The wet material surface particles produced by low-temperature granulation are sticky and have poor strength because the moisture is not evaporated, and the materials are easy to stick or break after directly falling into a fluidized bed, so that the granulation rate is low, the appearance is poor, more powder and block materials are produced after screening, the reworking treatment is required, and the manufacturing cost is high.
When the original pesticide has the characteristics of easy water absorption and low melting point, the wet materials are more easily sticky and thinned in the granulation process, the strength of particles flowing into a fluidized bed is poorer, and the particles are more easily sticky and broken, so the granulation difficulty is higher, the granulation rate of the obtained particles is lower, the rework rate is higher, and the market competitiveness is low.
CN 107417426A discloses a method for producing a cellular instant granular compound fertilizer and a device thereof, wherein nitrogen, phosphorus and potassium macroelement fertilizers are fully mixed with medium and trace element raw materials and organic fertilizers such as fulvic acid according to a certain proportion, the raw materials are fully mixed according to a formula, and are subjected to extrusion granulation and continuous extrusion puffing granulation by a stainless steel screw controlled by a jacket to be cooled, cooling and shaping by a belt type quench cooler, dehydration by a vibrating fluidized bed dryer, cooling by the belt type quench, granule shaping by a blade type granulator, and screening by a plane rotary screen to obtain a cellular instant granular compound fertilizer product. The temperature of the air flow of a quench cooler used in the patent is less than or equal to 20 ℃, the material is melted by adopting a screw extrusion granulator to extrude and heat the material, the material is completely melted, and the material is rapidly cooled by a cooling section to cause rapid evaporation of water to form a honeycomb shape; the difficulty of temperature control by adopting extrusion heating is high, the phenomenon of overhigh or overlow temperature is easy to occur, and the product is not suitable for temperature sensitive products; the extrusion heating is adopted, the temperature rise is slow in the initial stage, the granulation is poor, more unqualified materials are produced, and the material reworking frequency is high.
Disclosure of Invention
Aiming at the defects of the conventional granulation method for preparing granules from low-melting-point raw pesticide, the invention provides the granulation method for the low-melting-point pesticide granules, which improves the granulation temperature and the cooling mode, so that the strength of the granules obtained from the low-melting-point raw material is improved, the obtained granules are not adhered and broken after falling into a fluidized bed, the granulation rate is high, the rework rate is low, and the production difficulty and the production cost of the product are reduced.
Aiming at the specific low melting point of the low-melting-point pesticide, the invention improves the granulation method, improves the granulation rate and reduces the rework rate. The low-melting-point pesticide refers to a pesticide with a melting point lower than 100 ℃, and comprises 2,4-D dimethylamine salt, 2,4-D isopropylamine salt, acephate, glyphosate dimethylamine salt, glyphosate isopropylamine salt, ametryn, hexazinone, acetochlor, terbutryn, propanil, imazalil, pyraclostrobin and the like.
The low-melting-point pesticide is easy to melt after being heated and is easy to solidify after being rapidly cooled because of low melting point. According to the characteristics, the granulation is carried out at a higher temperature in the granulation process, and the granulation temperature is effectively controlled to be stable, so that the surface of wet granules obtained by granulation is molten and the inside of the wet granules is solid. The granulated wet granules are immediately cooled by cold air, and after the granulation is carried out by the cold air, the materials melted on the surfaces of the granules are rapidly cooled and solidified, so that the outer surfaces of the granules become firm and are not adhered, and the strength of the wet granules is improved.
The granulation method of the low-melting-point pesticide granules comprises the following steps:
(1) Feeding the wet material containing the low-melting-point pesticide into a granulator for extrusion granulation, wherein the temperature of the granulator is kept at 55-95 ℃ in the granulation process, and the discharging temperature is kept at 45-85 ℃;
(2) The wet granules from the discharge port are immediately cooled by cold air to ensure that the surfaces of the wet granules are cooled and solidified;
(3) And (4) drying the air-cooled particles in a fluidized bed, and then screening to obtain the granules.
Furthermore, the granules comprise water dispersible granules and water soluble granules, and low-melting-point granules such as 2,4-D dimethylamine salt soluble granules, 2,4-D isopropylamine ammonium salt soluble granules, acephate soluble granules, glyphosate dimethylamine salt soluble granules, glyphosate isopropylamine salt soluble granules, ametryn water dispersible granules, hexazinone water dispersible granules, diacyl-chlor water dispersible granules, terbutryn water dispersible granules, propanil water dispersible granules, imazalil water dispersible granules, pyraclostrobin water dispersible granules and the like can be prepared by the method.
Further, in the step (1), the granulator is a double-screw front extrusion granulator or a double-screw side extrusion granulator.
Further, in the step (1), the temperature of the granulator is controlled to be 55-95 ℃ all the time during granulation, and the discharging temperature is controlled to be 45-85 ℃. The temperature of the granulator can be controlled by circulating water, the circulating water is added outside the granulator, and the granulator is stably maintained at the temperature by heating with hot water. Because the materials are extruded to release heat and rise temperature in the granulating process, the granulating machine only needs to be heated by introducing hot water in the initial granulating stage, and the granulating temperature can be maintained by adopting self-extrusion heat in the normal production process. The temperature of hot water of the granulator is increased and controlled, so that the granulation temperature can be effectively controlled to be stable, the granulation rate in the initial production is improved, the interior of the obtained granules is in a solid state, and the pesticide on the surface of the granules is in a molten state.
Further, in the step (1), the composition of the wet material containing the low-melting-point pesticide generally comprises the low-melting-point pesticide, an auxiliary agent and water, wherein the auxiliary agent can be a dispersing agent, a wetting agent, a filler, a disintegrating agent and the like according to different formulations, and is selected according to a specific formula.
Further, in the step (1), the moisture content in the wet material containing the low-melting-point pesticide is 1.5-5wt%. The invention has the advantages that the water content of the wet material is low during granulation, the wet material is only subjected to surface melting during the granulation process by controlling the water content, the increase of the water solubility of the material does not influence the granulation rate of the granulation, meanwhile, the temperature-sensitive pesticide can be coated with the additives such as the dispersing agent, the wetting agent and the like during the melting process, the desorption of the additives is not caused, and the disintegration and the dispersion of the final granules are not influenced.
Further, in the step (2), cold air can be realized by an air cooler, the air cooler is arranged at a discharge port of the granulator, the wet granules are cooled by the cold air as soon as being discharged from the discharge port of the granulator, the cold air blown out by the air cooler is dehumidified, the temperature of the cold air is 10-30 ℃, and the water content of the cold air is lower than 50%. After air cooling, the outer surfaces of the particles entering the fluidized bed are firm, and the particles are not adhered.
Furthermore, in the step (2), the cooling speed of the cold air is high, the required time is less than or equal to 20s, preferably about 10s, and the cooling can be realized in the process that wet granules fall from the granulator to the fluidized bed without prolonging the granulation time.
Further, after the particles enter the fluidized bed, the particles are dried in the fluidized bed through hot air, and then are screened and packaged, wherein the processes are carried out by adopting the mode of the prior art. For example, the temperature of the hot drying air in the fluidized bed may be 45-75 ℃.
The invention has the following beneficial effects:
1. the invention adopts the high-temperature surface melting granulation with less water, improves the granulation rate during the initial production, ensures that the surface skeleton of the particles is rapidly formed due to the rapid evaporation of the surface moisture and the recrystallization of the melting material under the action of high temperature and cold air during the granulation, improves the strength of the wet particle material, reduces the surface viscosity of the material, ensures that the particles are not adhered and crushed after falling into a fluidized bed, cannot be crushed due to the stress of falling into the fluidized bed and the stress of drying boiling, improves the yield, reduces the rework, reduces the production difficulty and the cost of the product, and improves the economy of the product.
2. When the granulation process is carried out, the granules are only externally melted, the solid materials in the granules are compacted and are in a compact state, the strength of the finished granules is high, the granules are not easily abraded and broken in the transportation and storage processes, and the attractiveness of the product is improved.
3. The granulator of the invention uses hot water to maintain the granulation temperature, and only when the consumption of the hot water is large in the initial granulation stage, the granulation temperature can be maintained by the material self-heating after the granulation is started, the steam consumption is reduced, the granulator does not need cold water for cooling, the power cost is reduced, and the product economy is improved.
4. The invention solves the problem of low granulation rate through water quantity control and surface melting granulation, solves the problems of low strength and adhesion of the granules by combining cold air cooling, reduces the breakage of the granules falling into a fluidized bed, and greatly improves the granulation rate.
5. The wet granules have low water content, short drying time in the fluidized bed and low energy consumption, reduces tail gas emission, reduces the manufacturing cost and improves the environmental protection efficiency.
6. The invention solves the problem of low granulation rate of the low-melting-point raw medicines such as dimethylamine salt, isopropylamine salt and the like, the obtained granules have high granulation rate, the granulation rate is more than 99 percent, the rework rate is low, the material rework frequency is reduced, the appearance of the granules is smooth, the appearance of finished granules is optimized, the look and feel of customers are improved, and the product competitiveness is improved.
Drawings
FIG. 1 is a schematic view showing the connection of the apparatus for granulation according to the present invention.
In the figure, 1, a mixer, 2, a granulation distributor, 3, a granulator, 4, a vibrated fluidized bed, 5 and a sieving machine.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments, but the scope of the present invention is not limited thereto. Unless otherwise specified, the raw materials used in the following examples are all commercially available products.
In the following examples, unless otherwise specified, the concentrations are mass percent concentrations.
In the following examples, the disintegration time of the obtained granules was evaluated according to the following test method, with a time standard of 60s, as follows: adding 100ml of standard hardness D water into a 100ml measuring cylinder with a plug, placing the measuring cylinder in a water bath constant temperature of 25 ℃, accurately weighing 2.0-2.1g of sample, pouring the sample into the measuring cylinder, rapidly pressing a stopwatch, turning the measuring cylinder up and down at 2 s/time until the sample is completely disintegrated, and recording the time.
Example 1
97.5 percent of TC 987.7kg of 2,4-D dimethylamine salt, 12.3kg of sodium tripolyphosphate and 50kg of deionized water are put into a mixer to be mixed for 10min, the materials are transferred into a granulating distributor and enter a granulator through uniform feeding, the granulator is preheated to 70-90 ℃ by circulating hot water, the temperature of the granulator is kept at 70-90 ℃ all the time in the granulating process, the materials are extruded into granules, the granules are discharged from a discharge port after being granulated, the discharge temperature is 60-80 ℃, granules discharged from the discharge port are immediately cooled by dehumidifying cold air at 15-20 ℃, the granules are cooled by cold air while falling, the surfaces of the granules are instantaneously hardened after being cooled by the cold air, the granules cooled by the cold air fall into a vibrating fluidized bed and are dried by hot air at 50-60 ℃, semi-finished products are screened and packaged to produce finished products, 995kg of finished products, 2kg of powder, 3.1kg of block materials, the granulation rate is 99.5%, the balance of total materials is 100.1%, and the disintegration time is 24s.
According to the above feeding amount, the conventional method is adopted for granulation, and the method comprises the following steps: the granulator is cooled by cooling water, the temperature of the cooling water is not higher than 10 ℃, the granulation temperature is generally controlled below 45 ℃, and granules from the granulator are not cooled by cold air and fall into a fluidized bed to be dried under the same conditions. 860.5kg of finished product, 84kg of powder, 54.9kg of lump material, 86.1 percent of granulation rate, 99.94 percent of total material balance and 54s of disintegration time.
Example 2
97.5 percent TC 994.9kg of acephate, 5.1kg of citric acid and 30kg of deionized water are put into a mixer to be mixed for 15min, the materials are transferred into a granulating distributor and enter a granulator through uniform feeding, the granulator is preheated to 80-90 ℃ by circulating hot water, the temperature of the granulator is kept at 80-90 ℃ all the time in the granulating process, the materials are extruded into granules, the materials are discharged from a discharge port after being granulated, the discharge temperature is 75-85 ℃, granules discharged from the discharge port are cooled by dehumidification cold air at 10-20 ℃ in the falling process, the surfaces of the granules are cooled and hardened, the granules cooled by the cold air then fall into a vibrating fluidized bed and are dried by hot air at 45-65 ℃, semi-finished products are screened and packaged to produce 998kg of finished products, no powder, 1.98kg of lump materials, the granulation rate is 99.8 percent, the total material balance is 100.0 percent, and the disintegration time is 28s.
The above feed amount was measured, and the granulation was performed by the conventional method in the same manner as in example 1. 792.2kg of finished product, 113.5kg of powder, 92.8kg of lump material, 79.3 percent of granulation rate, 99.85 percent of total material balance and 48s of disintegration time.
Example 3
95% TC 842.1kg of glyphosate dimethylamine salt, 100kg of synergist, 57.9kg of ammonium sulfate and 15kg of deionized water are put into a mixer to be mixed for 30min, the materials are transferred into a granulating distributor and enter a granulator through uniform feeding, the granulator is preheated to 75-85 ℃ by circulating hot water, the temperature of the granulator is kept at 75-85 ℃ all the time in the granulating process, the materials are extruded into granules, the materials are discharged from a discharge port after being granulated, the discharge temperature is 65-75 ℃, granules discharged from the discharge port are cooled by dehumidifying cold air at 15-25 ℃ in the falling process, the surfaces of the granules are cooled and hardened, the granules cooled by the cold air then fall into a vibrating fluidized bed and are dried by hot air at 50-60 ℃, semi-finished products are screened and packaged to obtain finished products, the finished products are 996.5kg, 1.4kg of powder material, 2.1kg of lump material, the granulation rate is 99.65%, the total material balance is 100%, and the disintegration time is 26s.
The granulation was carried out by the conventional method according to the above-mentioned feed amount, and the method was the same as in example 1. 855.7kg of finished product, 28.6kg of powder, 116.1kg of lump material, 85.54 percent of granulation rate, 100.04 percent of total material balance and 60s of disintegration time.
Example 4
2, 97 percent of TC 876.3kg of 4-D isopropylamine salt, 15kg of sodium tripolyphosphate, 15kg of polyvinylpyrrolidone, 93.7kg of ammonium sulfate and 40kg of deionized water are put into a mixer to be mixed for 25min, the materials are transferred into a granulating distributor and then uniformly fed into a granulator, the granulator is preheated to 75-95 ℃ by circulating hot water, the temperature of the granulator is kept at 75-95 ℃ all the time in the granulating process, the materials are extruded into granules, the granules are discharged from a discharge port after being granulated, the discharge temperature is 65-85 ℃, the granules discharged from the discharge port are cooled by dehumidifying cold air at 20-30 ℃ in the falling process, the surfaces of the granules are instantly hardened, the granules cooled by the cold air fall into a vibrating fluidized bed, and then are dried by hot air at 65-75 ℃, and semi-finished products are packaged by screening, the finished products are 997.3kg, 1.1kg of powder, 1.4kg of block materials, the granulation rate is 99.75 percent, the total material balance is 99.98 percent, and the disintegration time is 32s.
The granulation was carried out by the conventional method according to the above feed amount, and the method was the same as in example 1. 848.4kg of finished product, 63.2kg of powder, 87.9kg of lump material, 84.88 percent of granulation rate, 99.95 percent of total material balance and 60s of disintegration time.
Example 5
95 percent of glyphosate isopropylamine salt TC 894.7kg, 90kg of synergist, 15.3kg of ammonium sulfate and 30kg of deionized water are put into a mixer to be mixed for 30min, the materials are transferred into a granulating distributor and enter a granulator through uniform feeding, the granulator is preheated to 60-80 ℃ by circulating hot water, the temperature of the granulator is kept at 60-80 ℃ all the time in the granulating process, the materials are extruded into granules, the granules are discharged from a discharge port after being granulated, the discharge temperature is 55-75 ℃, the granules discharged from the discharge port are cooled by 10-25 ℃ dehumidifying cold air in the falling process, the surfaces of the granules are cooled and hardened, the granules cooled by the cold air then fall into a vibrating fluidized bed and are dried by hot air at 55-65 ℃, and a semi-finished product is screened and packaged to obtain the finished product, wherein the finished product comprises 994.8kg of finished product, 2.2kg of lump material, 2.6kg of lump material, the granulation rate is 99.52%, the total material balance is 99.96%, and the disintegration time is 28s.
The granulation was carried out by the conventional method according to the above feed amount, and the method was the same as in example 1. 816.4kg of finished product, 73.5kg of powder, 107.6kg of lump material, 81.84 percent of granulation rate, 99.75 percent of total material balance and 56s of disintegration time.
Example 6
97 percent TC 773.20kg of hexazinone (with the fineness of 325 meshes), 90kg of dispersing agent, 25kg of wetting agent, 111.8kg of ammonium sulfate and 20kg of deionized water are put into a mixer to be mixed for 30min, the materials are transferred into a granulating distributor and then uniformly fed into a granulator, the granulator is preheated to 70-90 ℃ by circulating hot water, the temperature of the granulator is kept at 70-90 ℃ all the time in the granulating process, the materials are extruded into granules, the granules are discharged from a discharge port after being granulated, the discharge temperature is 75-85 ℃, the granules discharged from the discharge port are cooled by dehumidifying cold air at 20-30 ℃ in the falling process, the surfaces of the granules are cooled and hardened, the granules cooled by the cold air fall into a vibrating fluidized bed, and are dried by hot air at 55-65 ℃, and semi-finished products are screened and packaged to produce the finished products, wherein the finished products comprise 992.5kg of powder, 5.1kg of lump materials, the granulation rate is 99.24%, the total balance of the materials is 100.01%, and the disintegration time is 30s.
The granulation was carried out by the conventional method according to the above-mentioned feed amount, and the method was the same as in example 1. 843.4kg of finished product, 53.8kg of powder, 101.6kg of lump material, 84.44 percent of granulation rate, 99.88 percent of total material balance and 68 seconds of disintegration time.
Example 7
Pyraclostrobin (with fineness of 325 meshes) 98 percent of TC 204.08kg, dispersant 140kg, wetting agent 35kg, ammonium sulfate 250kg, talcum powder 370.92 kg and deionized water 50kg are put into a mixer to be mixed for 40min, the materials are transferred into a granulating distributor and enter a granulator through uniform feeding, the granulator is preheated to 55-65 ℃ by circulating hot water, the temperature of the granulator is kept to be 55-65 ℃ all the time in the granulating process, the materials are extruded into granules, the granules are discharged from a discharge port after being granulated, the discharge temperature is 45-55 ℃, the granules discharged from the discharge port are cooled by dehumidifying cold air at 15-25 ℃ in the falling process, the surfaces of the granules are cooled and hardened, the granules after being cooled by the cold air fall into a vibrating fluidized bed, and are dried by hot air at 45-55 ℃, semi-finished products are screened and packaged to obtain finished products, the finished products are 987.3kg, powder lot 3.7kg, lump material 9.2kg, the granulation rate is 98.71%, the total material balance is 100.02%, and the disintegration time is 28s.
According to the above feeding amount, the conventional method is adopted for granulation, and the method comprises the following steps: cooling the granulator by cooling water, wherein the temperature of the cooling water is not higher than 10 ℃, the granulation temperature is generally controlled below 30 ℃, and granules from the granulator are not cooled by cold air and fall into a fluidized bed to be dried under the same conditions. 713.9kg of finished product, 122.1kg of powder, 158.9kg of block material, 71.76 percent of granulation rate, 99.49 percent of total material balance and 66s of disintegration time.
Example 8
97% TC 927.84kg of diacyl urea (with the fineness of 325 meshes), 50kg of dispersing agent, 15kg of wetting agent, 7.16kg of corn starch and 25kg of deionized water are put into a mixer to be mixed for 25min, the materials are transferred into a granulating distributor to be uniformly fed into a granulator, the granulator is preheated to 85-95 ℃ by circulating hot water, the temperature of the granulator is kept at 85-95 ℃ in the granulating process, the materials are extruded into granules, the granules are discharged from a discharge port after being granulated, the discharge temperature is 80-90 ℃, granules discharged from the discharge port are cooled by dehumidifying cold air at 20-30 ℃ in the falling process, the surfaces of the granules are cooled and hardened, the granules cooled by the cold air fall into a vibrating fluidized bed, and are dried by hot air at 55-65 ℃, semi-finished products are screened and packaged to produce the finished products, 972.9kg of finished products, 4.5kg of powder, 21.8kg of block materials, 97.37% of the granulating rate, the total material balance is 99.92%, and the disintegration time is 34s.
The granulation was carried out by the conventional method according to the above-mentioned feed amount, and the method was the same as in example 1. 752.3kg of finished product, 133.7kg of powder, 112.5kg of lump material, 75.34 percent of granulation rate, 99.85 percent of total material balance and 62s of disintegration time.
Claims (10)
1. A granulation method of low-melting-point pesticide granules is characterized by comprising the following steps:
(1) Feeding the wet material containing the low-melting-point pesticide into a granulator for extrusion granulation, wherein the temperature of the granulator is kept at 55-95 ℃ in the granulation process, and the discharging temperature is kept at 45-85 ℃;
(2) Cooling the wet granules from the discharge port by cold air immediately to cool and solidify the surfaces of the wet granules;
(3) And (4) drying the air-cooled particles in a fluidized bed, and then screening to obtain the granules.
2. The granulation method as set forth in claim 1, wherein: the low melting pesticide has a melting point of less than 100 ℃.
3. The granulation method according to claim 1 or 2, wherein: the low-melting-point pesticide comprises 2,4-D dimethylamine salt, 2,4-D isopropylamine salt, acephate, glyphosate dimethylamine salt, glyphosate isopropylamine salt, ametryn, hexazinone, diacyl-chlor, terbutryn, propanil, imazalil and pyraclostrobin.
4. The granulation method as set forth in claim 1, wherein: the granulator is a double-screw front extrusion granulator or a double-screw side extrusion granulator.
5. The granulation method as set forth in claim 1, wherein: in the step (1), the granulator is heated by circulating water.
6. The granulation method as set forth in claim 1, wherein: in the step (1), the moisture content in the wet material containing the low-melting-point pesticide is 1.5-5wt%.
7. The granulation method as set forth in claim 1, wherein: in the step (2), the cold air is dehumidified, the temperature of the cold air is 10-30 ℃, and the water content of the cold air is lower than 50%.
8. The granulation method as set forth in claim 1, wherein: in the step (2), air cooling and temperature reduction are carried out in the process that the granules are discharged from the granulator and fall between the granulator and the fluidized bed.
9. Granulation process according to claim 1, 7 or 8, characterized in that: the air cooling time is less than or equal to 20s, the outer surfaces of the particles entering the fluidized bed are firm after the air cooling, and the particles are not adhered.
10. The granulation method as set forth in claim 1, wherein: the granules comprise water dispersible granules and water soluble granules.
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