CN1202714C - Niclosamide insecticide and molluscacide suspension and its prepn. process - Google Patents

Niclosamide insecticide and molluscacide suspension and its prepn. process Download PDF

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Publication number
CN1202714C
CN1202714C CN 02137938 CN02137938A CN1202714C CN 1202714 C CN1202714 C CN 1202714C CN 02137938 CN02137938 CN 02137938 CN 02137938 A CN02137938 A CN 02137938A CN 1202714 C CN1202714 C CN 1202714C
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Prior art keywords
niclosamidum
agent
suspending agent
suspension
molluscacide
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CN 02137938
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CN1389112A (en
Inventor
徐年凤
戴建荣
张瑶
梁幼生
韩顺宁
沈敏
熊建民
朱荫昌
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JIANGSU PROV INST OF AGRICULTURAL CHEMICALS
Jiangsu Institute of Parasitic Diseases
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JIANGSU PROV INST OF AGRICULTURAL CHEMICALS
Jiangsu Institute of Parasitic Diseases
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Abstract

The present invention relates to a suspending agent prepared from niclosamide as a chemical active substance and a quantity of added supplementary materials and a preparation method. The suspending agent is prepared from raw niclosamide, a wetting agent, a dispersing and suspending agent, an adhesion agent, a deicing agent, an antiseptic agent, a defoaming agent and water through uniformly mixing. The preparation method comprises: putting the materials in a barrel in prescribed proportion; opening a high-shear emulsifying machine to crush the materials to cause the materials to be uniformly mixed; milling the uniformly mixed materials by a sand mill for 1 to 2 times; inspecting the quality of the milled materials, and then packaging the qualified materials to obtain the suspending agent of the present invention. The present invention has the advantages of simple and feasible technology and low equipment investment, water is used as the dispersion system of continuous phases to save a large quantity of organic solvents, reduce cost and reduce the irritation caused by the organic solvents to operators and environmental pollution, three waste phenomena and dust nuisance phenomena are not generated in the process of preparation, and the preparation, the storage and the transportation are safe. The suspending agent is especially suitable for the preparation of agricultural chemical factories and is convenient for popularization and generalization.

Description

Niclosamidum insecticide and molluscacide suspension and preparation method thereof
Technical field
The present invention relates to that a kind of to contain niclosamidum be chemically reactive substance and add suspending agent and the preparation method that some auxiliary materials are formed.
Background technology
At present but the formulation developed at home of niclosamidum only has 25% the missible oil and the wet-milling of 70% ethanolamine salt, and its use pollutes environment.Up to the present the niclosamidum suspending agent does not also appear on the market.
Summary of the invention
The objective of the invention is to propose a kind of technology simple possible, equipment investment is few, environmental pollution is few niclosamidum insecticide and molluscacide suspension and preparation method thereof.
Technical solution of the present invention:
A kind of niclosamidum insecticide and molluscacide suspension, it is characterized in that it is mixed by dispersion suspending agent, tackifier, antifreezing agent, preservative, defoamer and the water of the formaldehyde condensation products of niclosamide active compound, wetting agent, alkyl naphthalene sulfonate or phenethyl phenol polyethenoxy ether condensation product makes, and the percentage by weight of its each composition is:
Niclosamidum 10-50%
Wetting agent 0.2-5%
The formaldehyde condensation products of alkyl naphthalene sulfonate or the condensation of phenethyl phenol polyethenoxy ether
Thing disperses suspending agent 0.5-10%
Preservative 0.1-2%
Antifreezing agent 1-8%
Tackifier 0.1-3%
Defoamer 0-5%
Water surplus
Wherein, the niclosamidum structural formula is:
Molecular formula is: C 13H 8Cl 2N 2O 4, chemical name is: 2 ', 3-two chloro-4 '-the nitro-salicylic acid anilid.
A kind of preparation method of niclosamidum insecticide and molluscacide suspension, it is characterized in that disperseing suspending agent, tackifier, antifreezing agent, preservative, defoamer and water to put into bucket the formaldehyde condensation products or the phenethyl phenol polyethenoxy ether condensation product of niclosamide active compound, wetting agent, alkyl naphthalene sulfonate in the ratio of claim 1, the unlatching high-shear emulsion machine is pulverized, it is mixed, with the above-mentioned material that mixes, grind 1-2 time through sand mill, can be packaged to be product of the present invention after quality examination is qualified.
Suspending agent is with water-soluble lower and fusing point is higher (general>60 ℃) solid pesticide adds suitable wetting agent, disperses components such as suspending agent, tackifier, antifreezing agent, preservative and water mostly, grinds through the sand mill wet method to form.The characteristics of this formulation have: (1) good drug efficacy, and the former medicine average grain diameter of dispersed solid 2-3 micron in the suspending agent, particle size range is little, is evenly distributed, thereby suspensibility and stability are improved; Strong adhesion behind the spreading, resistance of rainwater washing against, therefore, the longevity of residure is longer slightly.(2) production, safe in utilization, cost is low, and environmental pollution is few.Suspending agent is to be the dispersion of continuous phase with water, both can save a large amount of organic solvents, reduces cost, and can reduce organic solvent again to the behaviour person's of being stimulation with to the pollution of environment.Do not produce " three wastes " in the production, no dust from flying is produced, stores and transports all safer.
For the environment of protecting us to depend on for existence; to develop efficient environmentally safe new varieties of pesticides energetically on the one hand; to set about developing the little novel form of environmental pollution from formulation on the other hand; the characteristics that suspending agent had are just meeting these requirements; having overcome the shortcoming of wetting powder, is a main trend of formulations of pesticide development.
The present invention is according to the physicochemical property of niclosamidum, characteristics in conjunction with suspending agent, through development repeatedly, constantly adjust prescription, invented the niclosamidum suspending agent, this kind technology simple possible, equipment investment is few, and it is the dispersion of continuous phase with water, both saved a large amount of organic solvents, reduce cost, reduced organic solvent again, do not have " three wastes " in the production process and produce to operator's stimulation with to the pollution of environment, no dust from flying, therefore production, storing that we can say this formulation are all safer, are particularly suitable for the agricultural chemicals manufacturer production, are convenient to penetration and promotion.
Embodiment
Preparation method of the present invention is as follows:
The formaldehyde condensation products of niclosamide active compound, wetting agent, alkyl naphthalene sulfonate or dispersion suspending agent, tackifier, antifreezing agent, preservative, defoamer and the water of phenethyl phenol polyethenoxy ether condensation product are put into bucket, the unlatching high-shear emulsion machine is pulverized, it is mixed, and the percentage by weight of its each composition is:
Niclosamidum 10-50%
Wetting agent 0.2-5%
The formaldehyde condensation products of alkyl naphthalene sulfonate or the condensation of phenethyl phenol polyethenoxy ether
Thing disperses suspending agent 0.5-10%
Preservative 0.1-2%
Antifreezing agent 1-8%
Tackifier 0.1-3%
Defoamer 0-5%
Water surplus
With the above-mentioned material that mixes, grind 1-2 time through sand mill, can pack after quality examination is qualified product.
Among the present invention, pesticide original medicine is a niclosamidum, and structural formula is
Molecular formula is C 13H 8Cl 2N 2O 4, chemical name is 2 ', 3-two chloro-4 '-the nitro-salicylic acid anilid.It is a kind of strong invertebrate poison, can kill spiral shell with 0.3g/l, and is used for water treatment, to disturb the human section of infection to schistosomiasis.This product is nontoxic to plant with field concentration.
Because former medicine water-soluble very little, need by means of wetting agent that the former medicine of solid is wetting, could be by levigate in water, and then make it to disperse and suspend.The used wetting agent of the present invention can adopt nekal, to methoxyl group fatty acyl amido benzene sulfonic acid sodium salt, polycarboxylate sodium salt, lignosulfonates, alkylbenzenesulfonate or sulphate etc.Sorbitol polyoxyethylene base ether etc.They may be used alone, can also be used in combination.
Suspending agent is unsettled heterogeneous system.Can keep the levigate degree of scatter of the former medicine particle of solid, prevent the cohesion caking, guarantee effect, must add and disperse suspending agent, it can form strong adsorption layer and protection barrier at the agricultural chemicals particle surface, stops cohesion.The used dispersion suspending agent of the present invention can adopt formaldehyde condensation products, phenethyl phenol polyethenoxy ether condensation product, alkylphenol-polyethenoxy base ether formaldehyde condensation products, alkyl benzene calcium sulfonate, phenethyl phenol polyethenoxy ether sodium sulfate salt and the phosphate of alkyl naphthalene sulfonate.They may be used alone, can also be used in combination.
Suitable viscosity is to guarantee suspending agent quality and the crucial factor of application effect.Tackifier as suspending agent are advisable with the big hydrophilic high molecular polymer of thixotropy.The used tackifier of the present invention can adopt polyvinyl alcohol, Sodium Polyacrylate, britesorb, sodium carboxymethylcellulose, polyvinylpyrrolidone, soluble starch, heteroglycan, xanthans, methylcellulose, gum Arabic, natural gum, gelatin, alginic acid etc.They may be used alone, can also be used in combination.
For preventing microorganism, must add preservative to the fermentation of some additive, the sex change that putrefaction produces.The used preservative of the present invention can adopt sodium salicylate, parabens, Sodium Benzoate, potassium sorbate etc.They may be used alone, can also be used in combination.
Suspending agent is medium with water, in low temp area production with use and all need consider antifreezely, uses and prevent effect otherwise can influence.The used antifreezing agent of the present invention can adopt sorbierite, propane diols, glycerine, ethylene glycol, urea etc.They may be used alone, can also be used in combination.
Owing to can produce a large amount of bubbles after containing surfactant, grinding in the material, normally need to add the defoamer froth breaking smoothly in order to make production.That the used defoamer of the present invention can adopt is silicone based, sulfonamides, higher aliphatic etc.They may be used alone, can also be used in combination.
The niclosamidum suspending agent novel pesticide that the present invention proposes is a kind of strong invertebrate poison, is used to the snail etc. of going out on be used on the health to go out spiral shell, agricultural.
Below described embodiment describe the solution of the present invention in detail, in these embodiments, except other had explanation, all marks and percentage were all by weight.
Example one
Former medicine niclosamidum 10.2g, phenethyl phenol polyethenoxy ether condensation product 3g, dibutyl sodium sulfonate 5g, aluminium-magnesium silicate 3g, ethylparaben 0.8g, glycerine 1.5g, silicone oil 0.8g and water 75.7g are mixed, entering sand mill grinds, fineness until suspension reaches requirement (2-3 μ), promptly gets 10% niclosamidum SC finished product.
Example two
Former medicine niclosamidum 23.1g, alkylphenol polyoxyethylene formaldehyde condensation products 2.5g, methyl fatty acyl amido benzene sulfonic acid sodium salt 6g, sodium carboxymethylcellulose 2g, sodium salicylate 1g, propane diols 2g, XBE2000 1.5g and water (mend to 100) are mixed, sending into sand mill grinds, fineness until suspending agent reaches requirement, promptly gets 25% (W/V) niclosamidum SC product.
Example three
Former medicine niclosamidum 45.02, sodium alkyl sulfonate 4, calcium lignosulfonate 4, polyvinyl alcohol 1.5, Sodium Benzoate 1, ethylene glycol 2, XBP2000 2 and water (mending to 100) are mixed, sending into sand mill grinds, fineness until suspension reaches requirement, promptly gets 45% niclosamidum SC finished product.
Example four
Former medicine niclosamidum 50g, alkyl benzene calcium sulfonate 2g, formaldehyde condensation products 4g, the soluble starch 1.5g of alkyl naphthalene sulfonate, benzoic acid 0.5g, sorbierite 2g, S-29 #1g and water (mend to 100) mix, and send into sand mill and grind, and reach requirement until the fineness of suspension, promptly get 50% niclosamidum SC finished product.
Embodiment two is carried out the test of pesticide effectiveness, the results are shown in the effect experiment report of Jiangsu Prov. Bilharziasis Prevention and Control Inst..
Niclosamidum suspending agent molluscicidal effect laboratory report:
Schistosomiasis is still one of parasitosis of serious harm people ' s health, and killing oncomelania is the important channel of control schistosomiasis.Niclosamidum is the snail killing agent of the unique recommendation of present WHO, but that 50% bayluscid wetting powder also exists in using at the scene is poorly soluble, use problem such as inconvenience.For this reason, this research to niclosamidum former formulation done on the improved basis its molluscicidal effect to be estimated, existing the result is reported as follows:
Material and method
The preparation of 1 niclosamidum suspending agent
It is 25% niclosamidum suspending agent (by patented method) that niclosamidum is made content.
2 oncomelanias
Picking up from Nanjing dragon Tan has the spiral shell irrigation canals and ditches, removes positive oncomelania with colony's ease larva of a tapeworm or the cercaria of a schistosome method, behind indoor feeding 24h, choose energetic, the spiral shell one-tenth spiral shell that age, 7-8 revolved, random packet is used for laboratory molluscicidal effect test.
3 niclosamidum wetting powders
50% bayluscid wetting powder, Wujiang Lu Sen chemical industry Co., Ltd produced in 2000.
The spiral shell test is killed in 4 laboratories
Niclosamidum wetting powder and suspending agent, with the dechlorination running water be made into 1.0000,0.5000,0.2500,0.1250,0.0625,0.0313 and 7 concentration liquids of 0.0157mg/L stand-by.Niclosamidum soup 100ml with variable concentrations pours into respectively in the glassware, puts into 10 oncomelanias in each glassware, and the loam cake plastic gauze prevents that oncomelania from climbing out of liquid level.Soak oncomelania 24h and 48h in 25 ℃ of laboratories, all set up the clear water contrast for every group.After soaking oncomelania 24h and 48h, method is observed the oncomelania death condition routinely.
The 5 on-the-spot spiral shells that kill are tested
In May calendar year 2001, select snail river beach scene, Jiangpu, Nanjing to carry out the little scene of niclosamidum suspending agent and kill the spiral shell test.During test temperature 15-32 ℃, beach earth water content is average 25.72%, and the oncomelania natural mortality rate is 4.9%.With suspending agent (niclosamidum) 0.5g/m 2Carry out spraying molluscicide, water consumption is respectively 100 and 1000ml/m 2Random sampling is established frame and is detected whole oncomelanias in the frame behind spray medicine 3,7 and the 15d, presses hammering method and observes mortality of snails.During test and 50% bayluscid wetting powder 1.0g/m 2Carry out the spraying molluscicide check experiment.
The result
The laboratory is soaked with niclosamidum suspending agent 0.2500mg/L and is killed oncomelania 24h and 48h, and mortality of snails is 100%; Soak with niclosamidum wetting powder 0.5000mg/L that extremely oncomelania 24h and 48h molluscicidal effect are consistent.Niclosamidum suspending agent 24h soaks oncomelania LC extremely 95And LC 50Be respectively 0.1127mg/L and 0.0442mg/L, 48h soaks oncomelania LC extremely 95And LC 50Be respectively 0.1188mg/L and 0.0412mg/L; Niclosamidum wetting powder 24h soaks oncomelania LC extremely 95And LC 50Be respectively 0.2269mg/L and 0.0947mg/L, 48h soaks oncomelania LC extremely 95And LC 50Be respectively 0.2161mg/L and 0.0583mg/L; As seen the suspending agent molluscicidal effect is better than wetting powder.Detailed results sees Table 1.
Table 1 different dosage form niclosamidum molluscicidal effect
Formulation asynchronism(-nization) niclosamidum formulation variable concentrations (mg/L) killing snail rate (%) LC 50
(h) 1.0000 0.5000 0.2500 0.1250 0.0625 0.0313 0.0157 (mg/L)
Pulvis 24 100.00 100.00 100.00 70.00 20.00 00 0.0947
48 100.00 100.00 100.00 90.00 60.00 10.00 0 0.0583
Suspending agent 24 100.00 100.00 100.00 100.00 80.00 20.00 0 0.0442
48 100.00 100.00 100.00 100.00 90.00 20.00 0 0.0412
In May calendar year 2001, select scene, beach, river, Jiangpu, Nanjing to carry out the niclosamidum suspending agent and kill the spiral shell test.Use suspending agent 0.5g/m 2Carry out spraying molluscicide, water consumption 1000ml/m 2Behind spray medicine 3,7 and the 15d, mortality of snails is respectively 95.77%, 99.07% and 97.09%; The minimizing water consumption is 100ml/m 2Behind spray medicine 3,7 and the 15d, mortality of snails is respectively 71.43%, 98.00% and 83.33%; With niclosamidum wetting powder 1.0g/m 2Carry out spraying molluscicide, water consumption is 1000ml/m 2, behind spray medicine 3,7 and the 15d, mortality of snails is respectively 97.37%, 95.19% and 97.41%.The result shows, suspending agent 0.5g/m 2Molluscicidal effect and niclosamidum wetting powder 1.0g/m 2The molluscicidal effect unanimity; Reduce suspending agent and spray water consumption and can reach snail killing function preferably equally, and save a large amount of use costs, and these to be niclosamidum wetting powders be beyond one's reach.

Claims (7)

1, a kind of niclosamidum insecticide and molluscacide suspension, it is characterized in that it is mixed by dispersion suspending agent, tackifier, antifreezing agent, preservative, defoamer and the water of the formaldehyde condensation products of niclosamide active compound, wetting agent, alkyl naphthalene sulfonate or phenethyl phenol polyethenoxy ether condensation product makes, and the percentage by weight of its each composition is:
Niclosamidum 10-50%
Wetting agent 0.2-5%
The formaldehyde condensation products of alkyl naphthalene sulfonate or phenethyl phenol polyethenoxy ether condensation product disperse
Suspending agent 0.5-10%
Preservative 0.1-2%
Antifreezing agent 1-8%
Tackifier 0.1-3%
Defoamer 0-5%
Water surplus
Wherein, the niclosamidum structural formula is:
Figure C021379380002C1
Molecular formula is: C 13H 8Cl 2N 2O 4, chemical name is: 2 ', 3-two chloro-4 '-the nitro-salicylic acid anilid.
2, by the described niclosamidum insecticide and molluscacide suspension of claim 1, it is characterized in that described wetting agent adopt nekal, to methoxyl group fatty acyl amido benzene sulfonic acid sodium salt, polycarboxylate sodium salt, lignosulfonates, alkylbenzenesulfonate or sulphate or sorbitol polyoxyethylene base ether.
3,, it is characterized in that described tackifier adopt polyvinyl alcohol, Sodium Polyacrylate, britesorb, sodium carboxymethylcellulose, polyvinylpyrrolidone, soluble starch, heteroglycan, xanthans, methylcellulose, gum Arabic, natural gum, gelatin or alginic acid by the described niclosamidum insecticide and molluscacide suspension of claim 1.
4,, it is characterized in that described preservative adopts sodium salicylate, parabens, Sodium Benzoate or potassium sorbate by the described niclosamidum insecticide and molluscacide suspension of claim 1.
5,, it is characterized in that described antifreezing agent adopts sorbierite, propane diols, glycerine, ethylene glycol or urea by the described niclosamidum insecticide and molluscacide suspension of claim 1.
6,, it is characterized in that described defoamer adopts silicone based, sulfonamides or higher aliphatic by the described niclosamidum insecticide and molluscacide suspension of claim 1.
7, the preparation method of niclosamidum insecticide and molluscacide suspension as claimed in claim 1, it is characterized in that disperseing suspending agent, tackifier, antifreezing agent, preservative, defoamer and water to put into bucket the formaldehyde condensation products or the phenethyl phenol polyethenoxy ether condensation product of niclosamide active compound, wetting agent, alkyl naphthalene sulfonate in the ratio of claim 1, the unlatching high-shear emulsion machine is pulverized, it is mixed, with the above-mentioned material that mixes, grind 1-2 time through sand mill, can be packaged to be product of the present invention after quality examination is qualified.
CN 02137938 2002-07-11 2002-07-11 Niclosamide insecticide and molluscacide suspension and its prepn. process Expired - Fee Related CN1202714C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102047880A (en) * 2010-12-17 2011-05-11 江苏艾津农化有限责任公司 Niclosamide membrane spreading oil and preparation method and applications thereof

Families Citing this family (6)

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Publication number Priority date Publication date Assignee Title
CN1313438C (en) * 2004-12-24 2007-05-02 仲恺农业技术学院 Preparation method of snail killing agent crude medicine niclosamide
CN1985813B (en) * 2006-12-07 2010-10-06 江苏省血吸虫病防治研究所 Metronidazole ethanolamine spray as blood flukedisease preventing and treating medicine for farm cattle and its preparing method
CN100455194C (en) * 2007-01-25 2009-01-28 戴建荣 A compound suspension of molluscicidal drug niclosamide ethanolamine salt and its preparation method
CN103004763A (en) * 2013-01-21 2013-04-03 江苏省血吸虫病防治研究所 Ultra-low-capacity niclosamide spray for killing oncomelania and preparation method of spray
CN103583513A (en) * 2013-12-03 2014-02-19 四川省化学工业研究设计院 Suspending agent of chlorosalicylamide as snail control drug and preparation method thereof
CN103636609B (en) * 2013-12-19 2015-07-08 甘肃富民生态农业科技有限公司 Energy-saving production technology of metalaxyl suspending agent

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102047880A (en) * 2010-12-17 2011-05-11 江苏艾津农化有限责任公司 Niclosamide membrane spreading oil and preparation method and applications thereof
CN102047880B (en) * 2010-12-17 2013-03-27 江苏艾津农化有限责任公司 Niclosamide membrane spreading oil and preparation method and applications thereof

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