CN102726430B - Nicosulfuron soluble granule and preparation method thereof - Google Patents
Nicosulfuron soluble granule and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a nicosulfuron soluble granule and a preparation method of the nicosulfuron soluble granule. The nicosulfuron soluble granule is prepared from the following components in percentage by weight: 1%-70% of nicosulfuron, 0.5%-30% of alkali compound, and the balance of agricultural preparation auxiliary elements. The preparation method for the nicosulfuron soluble granule comprises the steps of preparing the raw materials; uniformly mixing ethanol with penetrating agent for later use; crushing and mixing the raw materials; squeezing, pelleting, drying and sieving the raw materials. Due to the nicosulfuron soluble granule, the difficulty that a soluble granule is difficult to prepare as the nicosulfuron is difficult to solve in water is overcome. Compared with a dispersible oil suspension, the content of active ingredients is increased; the dosage in a unit area is reduced; a large quantity of packaging materials, transportation cost and storage space can be saved, no organic solvent is used; and the production cost is greatly lowered. Moreover, the prepared soluble granule has good water solubility, and is beneficial to bringing pesticide effects into play.
Description
Technical field
The invention belongs to agriculture herbicide technology field, be specifically related to a kind of nicosulfuron soluble granula and preparation method thereof.
Background technology
Nicosulfuron (nicosulfuron) claims Yu Nongle again; Its chemical name is 2-(4,6-dimethoxypyridin-2-base carbamyl aminosulfonyl)-N, N-dimethyl nicotinamide.Nicosulfuron is systemic herbicide, can be weeds cauline leaf and root and absorb, in plant corpus, conduct subsequently, cause sensitive plant growth retardation, cauline leaf chlorisis, withered gradually, death in 20-25 days generally speaking, but under the lower situation of temperature, some perennial weed is needed the long time.In the dispenser good drug efficacy before the phase of 4 leaves behind the bud, the dispenser drug effect descended when seedling was big.This medical instrument has the preceding activity of weeding of bud, but active in low behind the bud.Applicable crops: corn, can prevent and kill off annual and perennial grassy weed, part broad leaved weed.Test shows that the strong weeds of susceptibility perception are had barnyard grass grass, green foxtail, wild oat, Amaranthus retroflexus; The medium weeds of susceptibility have Ben Shi knotweed, rule grass, kitchen garden, Monochoria vaginalis, Siberian cocklebur and piemarker, nutgrass flatsedge; The relatively poor weeds of susceptibility mainly contain lamb's-quarters, black nightshade, Commelina communis, summer cypress and weasel hemp nettle.
Because nicosulfuron itself is water insoluble and unstable decomposition easily in water, so be processed into formulation products such as can disperseing oil suspending agent, wetting powder, water dispersible granules usually, wherein mainly can disperse oil suspending agent based on the 40g/L nicosulfuron on the market.This formulation has that effective component content is low, using dosage is big, and the cost of transportation height contains a large amount of organic solvents and makes formulation cost relatively than problems such as height.Though wetting powder and water dispersible granules can address the above problem, but because of process equipment backward relatively, the research and development level is uneven, cause smashing fineness and prilling to be difficult to reach specification requirement, thereby influenced indexs such as disintegrative, suspensibility, reduced the performance of drug effect in use of this product.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of stable in properties, production process is simple, smooth, be difficult for the moisture absorption, nicosulfuron soluble granula that intensity is big and preparation method thereof.
The technical solution used in the present invention is: the nicosulfuron soluble granula, made by following components in weight percentage: nicosulfuron, 1%～70%, preferred 30%～70%; Alkali compounds, 0.5%～30%, preferred 5%～20%; The Agrotechnical formulation auxiliary element, surplus.
Described alkali compounds is the mixture of sodium carbonate, sodium bicarbonate, sodium hydroxide, one or more compositions of potassium hydroxide.
Nicosulfuron is white solid, 169～172 ° of C of fusing point, during 20 ° of C in the water solvability be 0.4g/L (pH5), be slightly soluble in water, by the nicosulfuron structural formula:
As can be known, group in the molecular structure
In the N-H key active, can with alkali compounds in basic group carry out acid-base neutralization reaction and generate water-soluble salt compounds, this compound can ionization go out ion in water, with the ionic species stable existence in water.
Described Agrotechnical formulation auxiliary element comprises wetting dispersing agent, bleeding agent and filler.
The percentage by weight of described wetting dispersing agent in described nicosulfuron soluble granula is 1%～10%, preferred 5%～10%.
The percentage by weight of described bleeding agent in described nicosulfuron soluble granula is 0.5%～20%, preferred 0.5%～10%.
Described wetting dispersing agent is lignosulfonates (sodium salt or calcium salts); Negel; condensation compound of methyl naphthalene sulfonic acid and formaldehyde sulphate; how sulfonic formaldehyde condensation compound; methanonaphthalene sodium sulfonate dibutyl is sulfonic formaldehyde condensation compound how; N-methyl fatty acyl group sodium taurocholate; polycarboxylate; naphthalene sulfonate; the withered powder of tea; saponin; lignosulfite; fatty alcohol polyoxyethylene ether sulfate; lauryl sodium sulfate; neopelex; draw back powder; one or more mixture of Aerosol OT.
Described bleeding agent is one or more the mixture in fatty alcohol-polyoxyethylene ether, aerosol-OT salt, the Laurocapram.
Described filler is one or more mixture of sodium sulphate, sodium chloride, potassium chloride, potassium sulphate, urea, lactose, glucose, sodium nitrate, potassium nitrate, white carbon.
Material described above all can be buied by market.
The preparation method of described nicosulfuron soluble granula comprises the steps:
1, prepares raw material by following component and the percentage by weight in the nicosulfuron soluble granula thereof: nicosulfuron, 1%～70%, preferred 30%～70%; Alkali compounds, 0.5%～30%, preferred 5%～20%; Wetting dispersing agent 1%～10%, preferred 5%～10%; Bleeding agent 0.5%～20%, preferred 0.5%～10%; Filler, surplus.
2, ethanol and bleeding agent are mixed standby, in ethanol and the step 1 all the weight ratio of raw materials be: 1:10～20.
3, with the nicosulfuron in the step 1 after being crushed to 325 orders～400 orders, add wetting dispersing agent, alkali compounds and filler therein.
4, mixture is carried out agravic mixing, add the ethanol got ready in the step 2 and the mixture of bleeding agent with spray pattern in the mixed process.
5, extruder grain 40～50 ℃ of dryings, gets grain diameter and is 0.5～1 millimeter dried particles.
6, dried particles is after screening, and packing makes the nicosulfuron soluble granula; Again granulation after oversized particles or dust, dust-removing powder return agravic blender and virgin material mixes.
Pulverize the equipment that uses in the described step 3 and be airslide disintegrating mill.
Carry out the equipment that agravic mixing uses in the described step 4 and be the agravic blender of pears cutter formula.
Carry out the dry equipment that uses in the described step 5 and be fluid bed dryer.
The equipment that sieves use in the described step 6 is the electronic sieve that shakes.
The incorporation time of described step 4 is 5～10 minutes.
Ethanol replaces the effect of water in mediating granulation process, remove in dry link.Because containing the soda acid composition in the material simultaneously, add water meeting antedating response generating portion salt compounds, the disintegrative when influence is used.
Under the same recipe condition, the more little dispersion of active ingredient fineness is more good, more is conducive to soup and enters plant tissue, and the drug effect performance is more good.The fineness of wetting powder and water dispersible granules is generally at 20～40 microns, and soluble granula is dissolved in water fully, is ionic condition, and the easier absorption of plant shows that through a large amount of field trials nicosulfuron soluble granula drug effect is better than other formulation products.But the active constituent content of the outstanding agent formulation of routine dispersed oil is generally between 4%～8%, the mu consumption is between 50～100ml, and the mu consumption of the present invention's 70 nicosulfuron soluble granulas is 5～6g, can save a large amount of packing materials and cost of transportation and storage space by the improvement of formulation.But organic solvent accounts for 70%～80% greatly in the outstanding agent prescription of dispersed oil, is example with the methyl oleate, and current reference price is 10,000 yuan/ton, amounts to into the preparation cost and can save 7000～8000 yuan/ton.Be example with a medium-sized agricultural chemicals enterprise, suppose that it is 500 tons that the annual 40g/L of production nicosulfuron can disperse oil suspending agent, only organic solvent is annual just can save 350～4,000,000 yuan.
Compared with prior art, beneficial effect of the present invention is:
1, solved because of nicosulfuron itself and be insoluble in the difficult problem that shipwreck is made soluble granula;
2, the soluble granula good water solubility that makes is beneficial to the drug effect performance;
3, be compared to and disperse oil suspending agent, improved active constituent content, reduced a mu consumption, can save a large amount of packing materials and cost of transportation and storage space;
4, soluble granula does not with an organic solvent greatly reduce production cost;
5, adopt nicosulfuron and alkali compounds is directly pulverized, the mode of kneading, granulation is made soluble granula, water is being used link fast reaction generation salt compounds, more traditional method for making is saved a large amount of energy consumptions, and is easy to operation.
Embodiment
Specify the present invention below in conjunction with embodiment.Percentage in the following example is mass percent, and the treatment dosage of field efficacy is the nicosulfuron consumption.
Below be component and the weight thereof among each embodiment, and the weight of absolute ethyl alcohol.
Embodiment 1
Component and weight: purity is 95% the former medicine 31.6kg of nicosulfuron, alkali compounds sodium carbonate 5kg, wetting dispersing agent calcium lignosulfonate and lauryl sodium sulfate are respectively 5kg and 1.5kg, bleeding agent fatty alcohol-polyoxyethylene ether 10kg, filler sodium sulphate 46.9kg.
Absolute ethyl alcohol: 5kg.
Embodiment 2
Component and weight: purity is 95% the former medicine 42.1kg of nicosulfuron, alkali compounds sodium carbonate and sodium bicarbonate, be respectively 5kg and 2kg, wetting dispersing agent condensation compound of methyl naphthalene sulfonic acid and formaldehyde sulphate and neopelex, be respectively 8kg and 2kg, bleeding agent aerosol-OT salt 8kg, filler urea 34.9kg.
Absolute ethyl alcohol: 6kg.
Embodiment 3
Component and weight: purity is 95% the former medicine 52.7kg of nicosulfuron, alkali compounds sodium bicarbonate and sodium hydroxide, be respectively 8kg and 2kg, wetting dispersing agent methanonaphthalene sodium sulfonate dibutyl is sulfonic formaldehyde condensation compound and draw back powder how, be respectively 6kg and 1.5kg, bleeding agent Laurocapram 3kg, filler sodium chloride 26.8kg.
Absolute ethyl alcohol: 10kg.
Embodiment 4
Component and weight: purity is 95% the former medicine 62.5kg of nicosulfuron, alkali compounds sodium bicarbonate and potassium hydroxide, be respectively 10kg and 4kg, wetting dispersing agent polycarboxylate and Aerosol OT, be respectively 5kg and 2kg, bleeding agent Laurocapram and aerosol-OT salt are respectively 2kg and 5kg, filler glucose 9.5kg.
Absolute ethyl alcohol: 8kg.
Embodiment 5
Component and weight: purity is 95% the former medicine 73.7kg of nicosulfuron, and alkali compounds sodium carbonate and potassium hydroxide are respectively 10kg and 5kg, wetting dispersing agent naphthalene sulfonate and lauryl sodium sulfate, be respectively 3kg and 1.5kg, bleeding agent Laurocapram 5kg, filler potassium nitrate 1.8kg.
Absolute ethyl alcohol: 10kg.
The preparation process of the nicosulfuron soluble granula in above-described embodiment 1～5 is as follows:
(1) mix absolute ethyl alcohol and bleeding agent standby.
(2) nicosulfuron is carried out ultramicro grinding through airslide disintegrating mill, be crushed to 325 orders～400 orders.Add alkali compounds, wetting dispersing agent and filler in the material after pulverizing.
(3) said mixture is carried out agravic mixing in the agravic blender of pears cutter formula, add the absolute ethyl alcohol got ready in the step (1) and the mixture of bleeding agent with spray pattern in the mixed process, incorporation time is not lumpd to observe material loosening, not thinning, do not generate heat and be advisable, about 5～10 minutes of this process.
(4) carry out extruder grain after, dry down 40～50 ℃ of temperature through fluid bed dryer again, get grain diameter and be 0.5～1 millimeter dried particles.
(5) with above-mentioned dried particles after the electronic sieve screening of shaking, qualified granule packaging makes the nicosulfuron soluble granula; Again granulation after oversized particles or dust, dust-removing powder return the agravic blender of pears cutter formula and virgin material mixes.
The nicosulfuron soluble granula and the Comparative Examples 1:40g/L nicosulfuron that make in above-described embodiment 1～5 can be disperseed oil suspending agent, Comparative Examples 2:80% nicosulfuron wetting powder, and Comparative Examples 3:75 water dispersible granule of nicosulfuron carries out field efficacy relatively.Comparing data sees the following form 1 and table 2.
Table 1: 15 days field efficacy (%) behind each medicament medicine
Table 2: 30 days field efficacy (%) behind each medicament medicine
Data by table 1 and table 2 draw: under the Isodose, and the medicament that embodiment 1～5 makes, 15d weeds strain preventive effect all is better than the medicament of Comparative Examples 1～3 after the medication, and 30d weeds strain preventive effect is also significantly better than the medicament of Comparative Examples 1～3 after the medication.
Claims (5)
1. the nicosulfuron soluble granula is made by following components in weight percentage: nicosulfuron, 1%～70%, alkali compounds, 0.5%～30%, Agrotechnical formulation auxiliary element, surplus;
Described Agrotechnical formulation auxiliary element is wetting dispersing agent, bleeding agent and filler;
Described alkali compounds is the mixture of one or more compositions in sodium carbonate, sodium bicarbonate, sodium hydroxide or the potassium hydroxide.
2. nicosulfuron soluble granula according to claim 1 is characterized in that, the percentage by weight of described wetting dispersing agent in described nicosulfuron soluble granula is 1%～10%.
3. nicosulfuron soluble granula according to claim 1 is characterized in that, the percentage by weight of described bleeding agent in described nicosulfuron soluble granula is 0.5%～20%.
4. the preparation method of nicosulfuron soluble granula comprises the steps:
(1) prepares raw material by following component and the percentage by weight in the nicosulfuron soluble granula thereof: nicosulfuron, 1%～70%, alkali compounds, 0.5%～30%, wetting dispersing agent 1%～10%, bleeding agent 0.5%～20%, filler, surplus;
(2) ethanol and bleeding agent are mixed standby, in ethanol and the step (1) all the weight ratio of raw materials be: 1:10～20;
(3) with the former medicine of nicosulfuron in the step (1) after being crushed to 325 orders～400 orders, add wetting dispersing agent, alkali compounds and filler therein;
(4) mixture is carried out agravic mixing, add the ethanol got ready in the step (2) and the mixture of bleeding agent with spray pattern in the mixed process;
(5) extruder grain 40～50 ℃ of dryings, gets grain diameter and is 0.5～1 millimeter dried particles;
(6) dried particles is after screening, and packing makes the nicosulfuron soluble granula; Again granulation after oversized particles or dust, dust-removing powder return agravic blender and virgin material mixes;
Described alkali compounds is the mixture of one or more compositions in sodium carbonate, sodium bicarbonate, sodium hydroxide or the potassium hydroxide.
5. the preparation method of nicosulfuron soluble granula according to claim 4, the incorporation time of described step 4 is 5～10 minutes.
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| CN104412963A (en) * | 2013-08-29 | 2015-03-18 | 浙江新安化工集团股份有限公司 | Agricultural auxiliary agent, granules and preparation method of agricultural auxiliary agent and granules |
| CN118415181B (en) * | 2024-07-02 | 2024-09-13 | 安达市海纳贝尔化工有限公司 | Nicosulfuron granule and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1826893A (en) * | 2006-04-12 | 2006-09-06 | 周保东 | Water dispersible granule of nicosulfuron |
| CN101564044A (en) * | 2009-05-19 | 2009-10-28 | 美丰农化有限公司 | Soluble granule of glyhosate ammonium and preparation method |
| CN101632355A (en) * | 2009-08-31 | 2010-01-27 | 桂林集琦生化有限公司 | Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof |
| WO2011101966A1 (en) * | 2010-02-18 | 2011-08-25 | 全国農業協同組合連合会 | Herbicidal composition |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1826893A (en) * | 2006-04-12 | 2006-09-06 | 周保东 | Water dispersible granule of nicosulfuron |
| CN101564044A (en) * | 2009-05-19 | 2009-10-28 | 美丰农化有限公司 | Soluble granule of glyhosate ammonium and preparation method |
| CN101632355A (en) * | 2009-08-31 | 2010-01-27 | 桂林集琦生化有限公司 | Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof |
| WO2011101966A1 (en) * | 2010-02-18 | 2011-08-25 | 全国農業協同組合連合会 | Herbicidal composition |
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