CN102365937B - Paraquat dichloride-containing water-soluble granular preparation and preparation method thereof - Google Patents
Paraquat dichloride-containing water-soluble granular preparation and preparation method thereof Download PDFInfo
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- CN102365937B CN102365937B CN201110281632.6A CN201110281632A CN102365937B CN 102365937 B CN102365937 B CN 102365937B CN 201110281632 A CN201110281632 A CN 201110281632A CN 102365937 B CN102365937 B CN 102365937B
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Abstract
The invention belongs to the pesticide field, and discloses a paraquat dichloride-containing water-soluble granular preparation and a preparation method thereof. The paraquat dichloride-containing water-soluble granular preparation comprises: by weight, 0.1 to 95% of paraquat dichloride, 1 to 30% of one or more surfactants, a triazole pyrimidone emetic of which weight is 0.18% of weight of the used paraquat dichloride, 0.001 to 0.1% of at least one bittering agent, 0.05% of at least one pigment, 0.1% of one or more stink agents, and 0 to 98% of a diluent. The paraquat dichloride-containing water-soluble granular preparation can prevent poisoning caused by contact with or intake of a conventional solvable enriched material or wettable powder in use, and poisoning caused by accidental or deliberate intake. The paraquat dichloride-containing water-soluble granular preparation still retains effects after being stored for a long time, and can effectively remove weeds growing in non-cultivated land, or mountain land, woodland, hillside land and the like.
Description
Technical field
The invention belongs to pesticide field, relate to water-soluble granular formulation containing paraquat dichloride and preparation method thereof.
Background technology
200 grams per liters and the 250 grams per liter paraquat aquas on market, sold at present, there is in actual use certain potential safety hazard, during as its dilution and skin contact, can absorb by skin, when spray atomization can by respiratory apparatus suck cause poisoning.And accidentally or intentionally taking in can be lethal, unless after taking in, carry out emergency treatment at once, but often because wrongly taking misuse, wait the injury causing and lose larger.
For solving its safety issue, there are many trials, have by the huge legendary turtle method of closing and solve, but safety issue can not solve eventually completely, also have can passivation paraquat activity by thinner clay etc. method, but because it loses removing activity, be restricted eventually, more have foreign patent report that it is mixed and make solid dosage forms and use together with other weed killer herbicide, but be also subject to the restriction of all factors, general effect is eventually undesirable.
Therefore, need preparation a kind of solution foregoing problems and there is excellent herbicidal effect, the preparation type that safety and cost are low.
Summary of the invention
The object of the invention is the above-mentioned defect for prior art, the water-soluble granular formulation containing paraquat dichloride is provided.
Another object of the present invention is to provide the preparation method of this water-soluble granular formulation.
Object of the present invention can be achieved through the following technical solutions:
A kind of water-soluble granular formulation that contains paraquat dichloride, comprise the active ingredient paraquat dichloride of following component: 0.1-95wt%, the surfactant of 1-30wt%, be equivalent to the emetic triazole pyrimidone of active ingredient paraquat dichloride 0.18wt%, the bitters of 0.001-0.1wt%, 0.05wt% pigment, the agent of 0.1wt% stink, 0-98wt% thinner; Wherein said surfactant is sulfonic compound, sulfuric acid based compound, anion surfactant and/or non-ionic surface active agent; Thinner is selected from any one or two kinds in ammonium chloride, potassium chloride, ammonium sulfate, ammonium nitrate and sodium sulphate.
Preferably 30～the 90wt% of content of wherein said active ingredient paraquat dichloride, further 50～75wt%.
Described surfactant is selected from one or more in following material: sodium salt or the calcium salt of alkylaryl sulfonates, di alkylaryl sulfonate, dialkyl group virtue sulfosuccinate, lignosulphonic acid sodium salt or sylvite or calcium salt, naphthalene sulfonic acid-formaldehyde condensation product, alkylated naphthalene sulfonic formaldehyde condensation compound, polyoxygenated ethylidene alkyl benzene sulphonate; Sodium salt or the calcium salt of alkyl sulfate, alkyl aryl sulfate, polyoxygenated ethylidene alkylsurfuric acid, polyoxygenated ethylidene alkylbenzene sulfuric acid; The sodium salt of polyoxyalkylene succinic acid or calcium salt; Sodium Benzoate, sodium carboxylate; Polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxygenated ethylidene alkyl phenyl polymer, SYNPERONIC PE/F68.
Described bitters is selected from least one material in benzene first DEXAMETHASONE SODIUM PHOSPHATE ammonium or saccharin benzylamine amide, and described pigment is selected from beautiful indigo plant, and described stink agent is selected from pyridine, one or more in n-butanol.
Described water-soluble granular formulation is by each component is mixed; together with the water of gained mixture and the 1-20% based on mixture weight, mediate 5-30 minute; use Squeezinggranulator by the mixture forming particle of mediating, and these particles are made at 54-100 ℃ of dry 5-120 minute.
A preparation method for the described water-soluble granular formulation containing paraquat dichloro compound, comprises the steps:
1) each component is mixed, and together with the water of mixture and the 1-20% based on mixture weight, mediate 5-30 minute at 23～28 ℃;
2) use Squeezinggranulator by step 1) product form particle;
3) in fluidized bed dryer at 54-100 ℃ by step 2) the dry 5-120 minute of product.
The content of described active ingredient paraquat dichloride is 30～90wt%, preferably 50～75wt%; Described surfactant is selected from one or more in following material: sodium salt or the calcium salt of alkylaryl sulfonates, di alkylaryl sulfonate, dialkyl group virtue sulfosuccinate, lignosulphonic acid sodium salt or sylvite or calcium salt, naphthalene sulfonic acid-formaldehyde condensation product, alkylated naphthalene sulfonic formaldehyde condensation compound, polyoxygenated ethylidene alkyl benzene sulphonate; Sodium salt or the calcium salt of alkyl sulfate, alkyl aryl sulfate, polyoxygenated ethylidene alkylsurfuric acid, polyoxygenated ethylidene alkylbenzene sulfuric acid; The sodium salt of polyoxyalkylene succinic acid or calcium salt; Sodium Benzoate, sodium carboxylate; Polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxygenated ethylidene alkyl phenyl polymer, SYNPERONIC PE/F68; Described bitters is selected from least one material in benzene first DEXAMETHASONE SODIUM PHOSPHATE ammonium or saccharin benzylamine amide; Described pigment is selected from beautiful indigo plant; Described stink agent is selected from pyridine, one or more in n-butanol.
Described step 3) preferably in fluidized bed dryer at 54-100 ℃ by step 2) the dry 30-60 minute of product.
Described step 2) preferably use Squeezinggranulator by step 1) product to form particle diameter be 0.8～1.2mm particle.
Beneficial effect of the present invention:
The present invention, take paraquat dichloride as active ingredient, is prepared into water-soluble granular formulation, has reduced because of contact or has taken in cause poisoning and prevented the danger of accidentally or deliberately taking in.Compared with other method that strengthens its safety, water-soluble granule of the present invention to uncultivated area or mountain region, forest land, pond etc. demonstrate excellent herbicidal effect.
Surfactant is that surface-active is large and be the compound of amphipathic compound, and in its molecule, existing hydrophilic radical has again lipophilic group.It is characterized in that its excellent washability, dispersibility, emulsifying capacity, solubilising power, wetting power, sterilizing ability, foamability and diafiltration ability.It play a part moistening, break and decentralized compound so that paraquat can effectively show its activity.
Thinner plays water-soluble granule filler of the present invention.It has kept the shape of water-soluble granule and has supported to present the effect of described agricultural chemical activity component.
Described its purity of active ingredient paraquat dichloride can be 1-100%, and can suitably select according to the supplier of paraquat or preparation type.
Using method:
During use, with water-soluble granule 30-100 gram of the present invention, be dissolved in the water of 30KG, stir gently until after particle dissolves completely, to the processing of spraying of target weeds.
Embodiment
Use embodiment and comparative example to describe water-soluble granule of the present invention in detail below.Following examples are only to describe for example the present invention, should not be construed as limiting the scope of the invention." % " that in following examples, occur all represents weight percentage.
Embodiment 1:
By 75% paraquat dichloride, 5% naphthalenesulfonic acid-formaldehyde condensate, 2% SYNPERONIC PE/F68 (molecular weight 1500-2000, identical below), be equivalent to the triazole pyrimidone of paraquat dichloride quality 0.18%, 0.03% benzene first DEXAMETHASONE SODIUM PHOSPHATE ammonium, 0.05% beautiful indigo plant, 0.1% pyridine, residue complements to 100% with ammonium sulfate and sodium sulphate (mass ratio 1: 1) salt-mixture.Then, at room temperature this mixture and 5% the water based on this mixture weight are mixed together to 5 minutes, next, using comminutor that the mixture of kneading is formed to particle diameter is 0.8～1.2mm particle.Then, in liquefied bed drier, particle is dried to 60 minutes at 55 ℃.The water-soluble granule of preparation is thus used for to biologic test and physico-chemical test.During use, be mixed with after the aqueous solution the weeds processing of spraying.
Embodiment 2:
60% paraquat dichloride, 5% octyl group sodium naphthalene sulfonate, 2% SYNPERONIC PE/F68, be equivalent to the triazole pyrimidone of paraquat dichloride quality 0.18%, 0.03% saccharin benzylamine amide, 0.05% beautiful indigo plant, 0.1% n-butanol, residue complements to 100% with ammonium sulfate and sodium sulphate (mass ratio 1: 1) salt-mixture.Then, at room temperature this mixture and 10% the water based on this mixture weight are mixed together to 20 minutes, next, using comminutor that the mixture of kneading is formed to particle diameter is 0.8～1.2mm particle.Then, in liquefied bed drier, particle is dried to 30 minutes at 80 ℃.The water-soluble granule of preparation is thus used for to biologic test and physico-chemical test.During use, be mixed with after the aqueous solution the weeds processing of spraying.
Embodiment 3:
By 60% paraquat dichloride, 5% naphthalenesulfonic acid-formaldehyde condensate, 2% SYNPERONIC PE/F68, be equivalent to the triazole pyrimidone of paraquat dichloride quality 0.18%, 0.03% benzene first DEXAMETHASONE SODIUM PHOSPHATE ammonium, 0.05% beautiful indigo plant, 0.1% pyridine, residue complements to 100% with ammonium sulfate and sodium sulphate (mass ratio 1: 1) salt-mixture.Then, at room temperature this mixture and 15% the water based on this mixture weight are mixed together to 30 minutes, next, using comminutor that the mixture of kneading is formed to particle diameter is 0.8～1.2mm particle.Then, in liquefied bed drier, particle is dried to 40 minutes at 100 ℃.The water-soluble granule of preparation is thus used for to biologic test and physico-chemical test.During use, be mixed with after the aqueous solution the weeds processing of spraying.
Embodiment 4:
50% paraquat dichloride, 5% octyl group sodium naphthalene sulfonate, 2% oxirane propane copolymer, be equivalent to the triazole pyrimidone of paraquat dichloride quality 0.18%, 0.03% benzene first DEXAMETHASONE SODIUM PHOSPHATE ammonium, 0.05% beautiful indigo plant, 0.1% n-butanol, residue complements to 100% with ammonium sulfate and sodium sulphate (mass ratio 1: 1) salt-mixture.Then, at room temperature this mixture and 8% the water based on this mixture weight are mixed together to 15 minutes, next, use comminutor by the mixture forming particle of mediating.Then, in liquefied bed drier, particle is dried to 35 minutes at 70 ℃.The water-soluble granule of preparation is thus used for to biologic test and physico-chemical test.During use, be mixed with after the aqueous solution the weeds processing of spraying.
Embodiment 5 biological activity determinations
For with embodiments of the invention comparison, the paraquat aqua of commodities purchased 250 grams per liters and 88.8% soluble granule of glyhosate ammonium are for contrast medicament is for biologic test.During use, be mixed with after the aqueous solution the weeds processing of spraying.
1, to wasteland weeds agrochemistry effect test
Be diluted to aqueous solution post processing weeds with embodiment 1-4 and contrast medicine, after processing, within 1,3,7 and 15 day, check its agrochemistry effect respectively.
Treated length is the weeds of 30CM and its result is separated in following table 1.
Table 1
As implied above, when processing by reference amount and double amount, compared with paraquat aqua in contrast agents, the water-soluble granule of preparing according to each embodiment demonstrates excellent preventive effect, the soluble granula of the glyphosate of contrast agents 2 is compared, also demonstrate excellent effect continuity, after 7 days, reproduction ratio is low, and shows more excellent initial effect.
2, the agrochemistry effect test after long term storage
In order to check the reduction of this effect, measure the agrochemistry effect of the water-soluble granule of the storage scheduled time.
The product of preparing according to embodiment and comparative example 1 respectively after preparation at once, storage 1,2,3,6 and measuring by biological activity determination method described in embodiment 5 afterwards for 12 months.At second day that processes according to table 2, check its agrochemistry effect.
Table 2
As implied above, after long term storage, the water-soluble granule of embodiment is identical with the impact of comparative example's product on the impact of weeds, and difference is not obvious, and therefore, long term storage is no problem.
3, storage-stable test
In order to confirm the storage-stable of product of embodiment, at 0 ℃ and 54 ℃, carry out, the results are shown in following table 3.
Table 3
As implied above, though under the harsh conditions of 54 ℃ after storage 32 weeks the not effective constituent in the water-soluble granule prepared of the present invention decompose lower than 1%, so composition is stable after long term storage.
4, industrial applicibility
Water-soluble granule of the present invention is by paraquat, surfactant and mixing diluents kneading, by the mixture forming particle of mediating, and these particle dryings are made.
When can preventing from using the concentrated thing of conventional solubility or wettable powder, it because of contact or take in the poisoning danger causing, and can prevent because of accidentally or the poisoning danger that deliberately absorption causes.
And water-soluble granule of the present invention keeps its effect after long term storage.So, the weeds that it can remove uncultivated area or mountain region, forest land, pond etc. effectively.And its acts on soon the same with paraquat aqua, so only can remove weeds in 3 days after processing.
Although the present invention have been described in detail by embodiment, apparent, the present invention can carry out various improvement and correction in the scope of the technical program.And it is also apparent that these improvement and correction fall into additional claims." embodiment consumption " described in table 1 and table 2 refers to the consumption of the tablet that contains paraquat dichloride of preparing in each embodiment.
Claims (7)
1. a water-soluble granular formulation that contains paraquat dichloride, it is characterized in that comprising the active ingredient paraquat dichloride of following component: 50 ~ 75wt%, the surfactant of 1-30wt%, be equivalent to the emetic triazole pyrimidone of active ingredient paraquat dichloride 0.18wt%, the bitters of 0.001-0.1wt%, 0.05 wt % pigment, 0.1 wt % stink agent, 0-98 wt % thinner; In the described water-soluble granular formulation that contains paraquat dichloride, each component sum is 100%; Wherein said surfactant is more than one in alkylaryl sulfonates, naphthalene sulfonic acid-formaldehyde condensation product, SYNPERONIC PE/F68; Thinner is selected from any one or two kinds in ammonium chloride, potassium chloride, ammonium sulfate, ammonium nitrate and sodium sulphate.
2. the water-soluble granular formulation that contains paraquat dichloride according to claim 1, it is characterized in that described bitters is selected from least one material in benzene first DEXAMETHASONE SODIUM PHOSPHATE ammonium or saccharin benzylamine amide, described pigment is selected from beautiful indigo plant, described stink agent is selected from pyridine, one or more in n-butanol.
3. according to the water-soluble granular formulation that contains paraquat dichloride described in any one in claim 1 ~ 2; it is characterized in that described water-soluble granular formulation is by each component is mixed; together with the water of gained mixture and the 1-20% based on mixture weight, mediate 5-30 minute; use Squeezinggranulator by the mixture forming particle of mediating, and these particles are made at 54-100 ℃ of dry 5-120 minute.
4. a preparation method for the water-soluble granular formulation containing paraquat dichloro compound claimed in claim 1, is characterized in that comprising:
1) component described in claim 1 is mixed, and together with the water of mixture and the 1-20% based on mixture weight, mediate 5-30 minute at 23 ~ 28 ℃;
2) use Squeezinggranulator that the product of step 1) is formed to particle;
3) in fluidized bed dryer at 54-100 ℃ by step 2) the dry 5-120 minute of product.
5. preparation method according to claim 4, is characterized in that described bitters is selected from least one material in benzene first DEXAMETHASONE SODIUM PHOSPHATE ammonium or saccharin benzylamine amide; Described pigment is selected from beautiful indigo plant; Described stink agent is selected from pyridine, one or more in n-butanol.
6. preparation method according to claim 4, is characterized in that described 3) in fluidized bed dryer at 54-100 ℃ by step 2) the dry 30-60 minute of product.
7. preparation method according to claim 4, is characterized in that described step 2) use Squeezinggranulator that the product of step 1) is formed to the particle that particle diameter is 0.8 ~ 1.2mm.
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| CN102578099A (en) * | 2012-01-18 | 2012-07-18 | 南京华洲药业有限公司 | Water-soluble granule formulation containing paraquat dichloride and preparation method of water-soluble granule formulation |
| CN103734126B (en) * | 2013-12-27 | 2016-03-30 | 山东省农药科学研究院 | Containing the water-soluble granular formulation and preparation method thereof of paraquat dichloride |
| CN104872133A (en) * | 2015-03-28 | 2015-09-02 | 济南天邦化工有限公司 | Paraquat-fluoroglycofen ethyl water-soluble granule and preparation method thereof |
| CN105613504A (en) * | 2016-02-24 | 2016-06-01 | 苏州佳辉化工有限公司 | Water-soluble granule preparation containing paraquat and preparation method of water-soluble granule preparation |
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Effective date of registration: 20161125 Address after: 210047 Nanjing Chemical Industrial Park, Jiangsu aromatic South Road, No. 168 Patentee after: Nanjing Red Sun Biological Chemical Co., Ltd. Address before: Dongfeng Road, Xi Zhen Gaochun County of Nanjing City, Jiangsu province 211303, No. 8 Patentee before: Nanjing Redsun Co., Ltd. |
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Effective date of registration: 20180522 Address after: 210047 No. 168 aromatics South Road, Nanjing chemical industry park, Jiangsu Co-patentee after: Nanjing Redsun Co., Ltd. Patentee after: Nanjing Red Sun Biological Chemical Co., Ltd. Address before: No. 168 aromatics South Road, chemical industrial park Patentee before: Nanjing Red Sun Biological Chemical Co., Ltd. |