CN102365937A - 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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- CN102365937A CN102365937A CN2011102816326A CN201110281632A CN102365937A CN 102365937 A CN102365937 A CN 102365937A CN 2011102816326 A CN2011102816326 A CN 2011102816326A CN 201110281632 A CN201110281632 A CN 201110281632A CN 102365937 A CN102365937 A CN 102365937A
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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 that contains the 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 certain potential safety hazard in actual use; Can pass through skin absorbs when contacting with skin like its dilution, can be when spray atomization through respiratory apparatus suction causing poisoning.And, take in and can cause death accidentally or intentionally, carry out emergency treatment only if take in the back, but often wait the injury and the loss that cause bigger at once because of wrongly taking to misapply.
For solving its safety issue, many trials are arranged, have through the huge legendary turtle method of closing and solve; But safety issue can not solve eventually fully; But also have the method for thinner, but be restricted because of it loses removing activity eventually, more have the foreign patent report to use and process it with solid dosage forms with other weed killer herbicide and use with passivation paraquats such as clay activity; But also receive the restriction of all factors, general effect is undesirable eventually.
Therefore, need to prepare a kind of solution foregoing problems and have excellent herbicidal effect, the preparation type that safety and cost are low.
Summary of the invention
The objective of the invention is above-mentioned defective, the water-soluble granular formulation that contains the paraquat dichloride is provided to prior art.
Another object of the present invention provides the preparation method of this water-soluble granular formulation.
The object of the invention can be realized through following technical scheme:
A kind of water-soluble granular formulation that contains the paraquat dichloride; The active ingredient paraquat dichloride that comprises following component: 0.1-95wt%, the surfactant of 1-30wt% is equivalent to the emetic triazole pyrimidone of active ingredient paraquat dichloride 0.18wt%; The bitters of 0.001-0.1wt%; The 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 the sodium sulphate.
Preferred 30～the 90wt% of content of wherein said active ingredient paraquat dichloride, further 50～75wt%.
Described surfactant is selected from one or more in the following material: the 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; The 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, alkyl carboxylic acid sodium; Polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxygenated ethylidene alkyl phenyl polymer, SYNPERONIC PE/F68.
Described bitters is selected from least a material in benzene first ground sodium ammonium or the saccharin benzylamine amide, and described pigment is selected from beautiful indigo plant, and described stink agent is selected from pyridine, one or more in the n-butanol.
Described water-soluble granular formulation is through each component is mixed; The gained mixture was mediated 5-30 minute with the water based on the 1-20% of mixture weight; Use Squeezinggranulator with the mixture forming particle of mediating, and these particles were processed at 54-100 ℃ of dry 5-120 minute.
A kind of described preparation method who contains the water-soluble granular formulation of paraquat dichloro compound comprises the steps:
1) each component is mixed, and under 23～28 ℃, mixture was mediated 5-30 minute with the water based on the 1-20% of mixture weight;
2) use Squeezinggranulator that the product of step 1) is formed particle;
3) in fluidized bed dryer under 54-100 ℃ with step 2) dry 5-120 minute of product.
The content of described active ingredient paraquat dichloride is 30～90wt%, preferred 50～75wt%; Described surfactant is selected from one or more in the following material: the 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; The 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, alkyl carboxylic acid sodium; Polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxygenated ethylidene alkyl phenyl polymer, SYNPERONIC PE/F68; Described bitters is selected from least a material in benzene first ground sodium ammonium or the saccharin benzylamine amide; Described pigment is selected from beautiful indigo plant; Described stink agent is selected from pyridine, one or more in the n-butanol.
Described step 3) preferably in fluidized bed dryer under 54-100 ℃ with step 2) dry 30-60 minute of product.
Described step 2) preferably using Squeezinggranulator is the particle of 0.8～1.2mm with the product formation particle diameter of step 1).
Beneficial effect of the present invention:
The present invention is an active ingredient with the paraquat dichloride, and it is prepared into water-soluble granular formulation, has reduced because of contacting or take in the poisoning that causes and having prevented danger accidental or that deliberately take in.Compare with other method that strengthens its safety, water-soluble granule of the present invention is to the excellent herbicidal effect that demonstrates on uncultivated area or mountain region, forest land, ground, pond etc.
Surfactant is that surface-active is big and be the compound of amphipathic compound, and existing hydrophilic radical has lipophilic group again in its molecule.The washability that it is characterized in that its excellence, 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 appear the effect of said agricultural chemical activity component.
Described its purity of active ingredient paraquat dichloride can be 1-100%, and can suitably select according to the supplier or the preparation type of paraquat.
Method for using:
During use,, be dissolved in the water of 30KG, stir gently after particle dissolves fully, to the processing of spraying of target weeds with water-soluble granule 30-100 of the present invention gram.
Embodiment
Use embodiment and comparative example to describe water-soluble granule of the present invention in detail below.Following examples only are to describe the present invention for example, should not be construed as the restriction to protection domain of the present invention." % " that occur in following examples all representes weight percentage.
Embodiment 1:
With 75% paraquat dichloride, 5% naphthalenesulfonic acid-formaldehyde condensate, 2% SYNPERONIC PE/F68 (molecular weight 1500-2000; Below identical), be equivalent to the triazole pyrimidone of paraquat dichloride quality 0.18%; 0.03% benzene first ground sodium 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% water based on this mixture weight are mixed together 5 minutes, next, using comminutor that the mixture of mediating is formed particle diameter is 0.8～1.2mm particle.Then, in the liquefied bed drier that particle is following dry 60 minutes in 55 ℃.The water-soluble granule of preparation thus is used for biologic test and physico-chemical test.During use it is mixed with behind 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% water based on this mixture weight are mixed together 20 minutes, next, using comminutor that the mixture of mediating is formed particle diameter is 0.8～1.2mm particle.Then, in the liquefied bed drier that particle is following dry 30 minutes in 80 ℃.The water-soluble granule of preparation thus is used for biologic test and physico-chemical test.During use it is mixed with behind the aqueous solution the weeds processing of spraying.
Embodiment 3:
With 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 ground sodium 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% water based on this mixture weight are mixed together 30 minutes, next, using comminutor that the mixture of mediating is formed particle diameter is 0.8～1.2mm particle.Then, in the liquefied bed drier that particle is following dry 40 minutes in 100 ℃.The water-soluble granule of preparation thus is used for biologic test and physico-chemical test.During use it is mixed with behind 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 ground sodium 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% water based on this mixture weight are mixed together 15 minutes, next, use comminutor the mixture forming particle of mediating.Then, in the liquefied bed drier that particle is following dry 35 minutes in 70 ℃.The water-soluble granule of preparation thus is used for biologic test and physico-chemical test.During use it is mixed with behind the aqueous solution the weeds processing of spraying.
Embodiment 5 biological activity determinations
In order to compare with embodiments of the invention, the paraquat aqua of commodities purchased 250 grams per liters and 88.8% ammonium glyphosate soluble granula are used for biologic test for the contrast medicament.During use it is mixed with behind 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 with the contrast medicine, its agrochemistry effect is checked in 1,3,7 and 15 day after handling respectively.
Treated length be the weeds of 30CM and with its result separately in following table 1.
Table 1
As implied above; When handling with reference amount and double amount, to compare with the paraquat aqua in the contrast agents, the water-soluble granule for 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, reproduction ratio is low after promptly 7 days, and shows more excellent initial effect.
2, the agrochemistry effect test after the 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.
According to the product of embodiment and comparative example 1 preparation respectively after preparation at once, storage 1,2,3,6 and measuring by embodiment 5 said biological activity determination methods afterwards in 12 months.Checked its agrochemistry effect at second day that handles according to table 2.
Table 2
As implied above, the water-soluble granule of embodiment is identical with the influence of comparative example's product to the influence of weeds after the long term storage, and difference is not obvious, and therefore, long term storage is no problem.
3, storage-stable test
Storage-stable for the product that confirms embodiment carries out under 0 ℃ and 54 ℃, and the result sees the following form 3.
Table 3
As implied above, even the not effective constituent decomposition of under 54 ℃ harsh conditions, preserving in the water-soluble granule of the present invention preparation after 32 weeks is lower than 1%, so composition is stable after long term storage.
4, industrial applicibility
Water-soluble granule of the present invention is through paraquat, surfactant and mixing diluents and kneading, by the mixture forming particle of mediating, and these particle dryings are processed.
Dangerous when it can prevent to use concentrated thing of conventional solubility or wettable powder because of contacting or take in the poisoning that causes, and can prevent that the poisoning that causes because of accidental or intentional absorption is dangerous.
And water-soluble granule of the present invention keeps its effect after long term storage.So it can remove the weeds on uncultivated area or mountain region, forest land, ground, pond etc. effectively.And its acts on soon the same with the paraquat aqua is so only can remove weeds in 3 days after handling.
Although the present invention describes in detail with embodiment, obvious, the present invention can carry out various improvement and correction in the scope of present technique scheme.And it also is conspicuous that these improvement and correction fall into additional claims." embodiment consumption " described in table 1 and the table 2 is meant the consumption of the tablet that contains the paraquat dichloride for preparing among each embodiment.
Claims (10)
1. water-soluble granular formulation that contains the paraquat dichloride; It is characterized in that comprising the active ingredient paraquat dichloride of following component: 0.1-95wt%, the surfactant of 1-30wt% is equivalent to the emetic triazole pyrimidone of active ingredient paraquat dichloride 0.18wt%; The bitters of 0.001-0.1wt%; The 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 the sodium sulphate.
2. the water-soluble granular formulation that contains the paraquat dichloride according to claim 1, the content that it is characterized in that described active ingredient paraquat dichloride is 30～90wt%.
3. the water-soluble granular formulation that contains the paraquat dichloride according to claim 2, the content that it is characterized in that described active ingredient paraquat dichloride is 50～75wt%.
4. the water-soluble granular formulation that contains the paraquat dichloride according to claim 1 is characterized in that described surfactant is selected from one or more in the following material: the 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; The 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, alkyl carboxylic acid sodium; Polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxygenated ethylidene alkyl phenyl polymer, SYNPERONIC PE/F68.
5. the water-soluble granular formulation that contains the paraquat dichloride according to claim 1; It is characterized in that described bitters is selected from least a material in benzene first ground sodium ammonium or the saccharin benzylamine amide; Described pigment is selected from beautiful indigo plant; Described stink agent is selected from pyridine, one or more in the n-butanol.
6. according to the described water-soluble granular formulation that contains the paraquat dichloride of claim 1～5; It is characterized in that described water-soluble granular formulation is through each component is mixed; The gained mixture was mediated 5-30 minute with the water based on the 1-20% of mixture weight; Use Squeezinggranulator with the mixture forming particle of mediating, and these particles were processed at 54-100 ℃ of dry 5-120 minute.
7. described preparation method who contains the water-soluble granular formulation of paraquat dichloro compound of claim 1 is characterized in that comprising:
1) component described in the claim 1 is mixed, and under 23～28 ℃, mixture was mediated 5-30 minute with-20% water based on mixture weight;
2) use Squeezinggranulator that the product of step 1) is formed particle;
3) in fluidized bed dryer under 54-100 ℃ with step 2) dry 5-120 minute of product.
8. preparation method according to claim 7, the content that it is characterized in that described active ingredient paraquat dichloride is 30～90wt%, preferred 50～75wt%; Described surfactant is selected from one or more in the following material: the 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; The 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, alkyl carboxylic acid sodium; Polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxygenated ethylidene alkyl phenyl polymer, SYNPERONIC PE/F68; Described bitters is selected from least a material in benzene first ground sodium ammonium or the saccharin benzylamine amide; Described pigment is selected from beautiful indigo plant; Described stink agent is selected from pyridine, one or more in the n-butanol.
9. preparation method according to claim 7 is characterized in that described 3) in fluidized bed dryer under 54-100 ℃ with step 2) dry 30-60 minute of product.
10. preparation method according to claim 7 is characterized in that described step 2) to use Squeezinggranulator that the product of step 1) is formed particle diameter be the particle of 0.8～1.2mm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103734126A (en) * | 2013-12-27 | 2014-04-23 | 山东省农药科学研究院 | Water-soluble granule containing paraquat dichloride and preparation method of water-soluble granule |
| 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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| CN1376030A (en) * | 1999-09-22 | 2002-10-23 | 东部韩农化学株式会社 | Water-dispersible granule containing paraquat dichloride and its preparing method |
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| CN1376030A (en) * | 1999-09-22 | 2002-10-23 | 东部韩农化学株式会社 | Water-dispersible granule containing paraquat dichloride and its preparing method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103734126A (en) * | 2013-12-27 | 2014-04-23 | 山东省农药科学研究院 | Water-soluble granule containing paraquat dichloride and preparation method of water-soluble granule |
| 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. |