CN102177906A - Herbicide effervescent tablets and preparation method thereof - Google Patents

Herbicide effervescent tablets and preparation method thereof Download PDF

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Publication number
CN102177906A
CN102177906A CN201110063285XA CN201110063285A CN102177906A CN 102177906 A CN102177906 A CN 102177906A CN 201110063285X A CN201110063285X A CN 201110063285XA CN 201110063285 A CN201110063285 A CN 201110063285A CN 102177906 A CN102177906 A CN 102177906A
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acid
effervescent
agricultural chemical
halosulfuronmethyl
sodium
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CN102177906B (en
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方峰
赖开平
叶一强
莫炳荣
黄科林
阮恒
王俊
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GUANGXI SANJING CHEMICAL TECHNOLOGY Co Ltd
Guangxi Research Institute of Chemical Industry
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GUANGXI SANJING CHEMICAL TECHNOLOGY Co Ltd
Guangxi Research Institute of Chemical Industry
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Abstract

The invention discloses herbicide effervescent tablets containing halosulfuronmethyl and pretilachlor and a preparation method thereof. The active ingredients of the herbicide effervescent tablets comprise 0.5 to 5 weight percent of halosulfuronmethyl, 10 to 25 percent of pretilachlor and the balance of an assistant. The effervescent tablets can be prepared by a direct dry-process tabletting method or a method of wet-process granulating first and then tabletting; the direct dry-process tabletting method comprises mechanically grinding the assistant, uniformly mixing with the assistant and directly tabletting the two raw material medicines; and the method of wet-process granulating first and then tabletting comprises drying the two raw material medicines and the ground assistant, mixing, adhering, granulating to prepare an acid soft material and an alkaline soft material and tabletting. The prepared effervescent tablets are new herbicide preparation products which are environment-friendly and convenient to use. The herbicide effervescent tablets can effectively prevent and control various weeds such as weed from broad leave family, grass family, cyperaceae family and the like in rice shooting fields and transplanting fields.

Description

A kind of effervescent table as agricultural chemical and preparation method thereof
Technical field
The present invention relates to a kind of effervescent table as agricultural chemical and preparation method thereof, be herbicidal composition of active ingredient and preparation method thereof with the halosulfuronmethyl and the third careless amine particularly, this composition pesticide can be applied to remove weeds such as multiple broad-leaved, grass family and sedge family in the paddy field.
Background technology
China's paddy rice acreage under cultivation reaches about 3,000,000 hectares, occupy the 2nd in the world, the weeds that the whole nation generally takes place have that barnyard grass grass, fescue, Herba Cyperi Glomerati, difformed galingale herb, weeds are buried, pondweed, Monochoria vaginalis etc., weeds in paddy field extent of injury area of (2-5 level) more than medium reaches 1546.7 ten thousand hectares, wherein serious harm (4-5 level) area is 3,800,000 hectares, account for 46.8% and 11.5% of paddy rice cultivated area respectively, the grain loss that China causes because of weeds endanger every year is above 20,000,000,000 kilograms.
Herbicides for use in paddy principal item is bensulfuron-methyl, pyrazosulfuron, butachlor, propisochlor, the agent of mefenacet list and mixture preparation thereof at present, and often is processed into formulations uses such as granule, fine granule, wetting powder, soluble powder, suspension emulsion, missible oil.Could spray or spread fertilizer over the fields after generally need converting the water dilution during use or being made into pesticide-clay mixture, troublesome poeration, labour intensity are big, and often there is because of medication metering the inaccurate or inhomogeneous paddy rice seedling that causes of dispenser be injured, hinder the growth of paddy rice, when especially using missible oil, the organic solvent in the composition not only influences the healthy contaminated environment of going back simultaneously of operator.
The effervescent tablet technology is to be applied in the medical pharmacy at first, to the phase earlier 1970s Japan begin the effervescent tablet technology is applied in the formulations of pesticide processing.China recent years also begins to have the research of this respect, also beginning on the market now has the pesticide effervescence sheet of several kinds to sell, as the 18% benzyl dichloro effervescent tablet weed killer herbicide that Red Sun Group Co.,Ltd. produces, the 20% pyrazosulfuron effervescent tablet that Anhui chemical research institute produces.But present effervescent tablet kind is single, and the kind that has also exists careless extremely spectrum narrow, and is dangerous to paddy rice, is not suitable for the shortcoming of using in southern rice district.
Halosulfuronmethyl (Halosulfuron methyl), chemical name: 3-(4,6-dimethoxypyridin-2-yl)-1-(1-methyl-3-chloro-4-methoxy methyl acyl group pyrazoles-5-yl) sulfonylureas.CAS:100784-20-1。Halosulfuronmethyl belongs to sulfonylurea selectivity inner sucting herbicide, and can be used for the rice field and prevent and kill off broad leaved weed and sedge weed, but relatively poor to grassy weed effects such as barnyard grass grass, moleplant seeds.The third careless amine (pretilachlor), chemical name: 2-chloro-2,6 '-diethyl N-(the 2-third oxygen ethyl) acetanil, CAS:51218-49-6.The third careless amine belongs to acetamide-group herbicides, it is the weed killer herbicide that grassy weed is had greater activity, it is very effective to grassy weeds such as non-irrigated barnyard grass, rice barnyard grass, moleplant seed, lady's-grass, green foxtail, Paspalum distichum, eleusine indica, bent grass, is one of efficacious agents of preventing and treating at present paddy fields in south china barnyard grass grass, moleplant seed.There is obvious synergistic effect halosulfuronmethyl and the third careless amine back that is mixed to moleplant seed and barnyard grass grass, and in addition, the third careless amine and halosulfuronmethyl are mixed and then paddy rice are shown strong detoxication.Therefore halosulfuronmethyl is mixed into preparation with the third careless amine, not only can reduces production costs, enlarge herbicidal spectrum, improve preventive effect, and can improve safety coefficient, reduce the poisoning odds paddy rice.Yet there are no the mixture preparation and the effervescent tablet of the halosulfuronmethyl and the third careless amine.
After the different medicaments that kill the grass spectrum of two kinds of the halosulfuronmethyl and the third careless amine are mixed, it is wider, safer to paddy rice to kill the grass spectrum, not only can be used as the seedling throwing field weeding but also can be used as the weeding of transplanting rice field, applicable surface is wider, has solved the last two kinds of single agent of present production and has used the unfavorable problem of drug effect separately.The halosulfuronmethyl and the third careless amine mixture preparation are developed to effervescent tablet, new breakthrough is being arranged again aspect the formulation processing, this improves agricultural production efficiency to improving China's formulations of pesticide level of processing, promotes that level of agricultural production has great importance.
Open source literature has also been reported some relevant effervescent tablets.For example: Chinese patent application number: CN00107465.2 publication number: CN1283388 denomination of invention: a kind of effervescent table as agricultural chemical and method for making thereof, inventor: Luo Yanhong, Feng Juntao, Fan Hongmei, Chen Anliang, open emerging applicant: Nuisanceless Pesticide Research Service Center, Xibei Agroforestry Science and T, summary: effervescent table as agricultural chemical is made up of pesticide original medicine, acid source, carbon dioxide source, waterproofing agent, insecticides adjuvant.Make soft material during manufacturing earlier, compressing tablet gets effervescent table as agricultural chemical again, various Insecticidal and acaricidal agents, bactericide, weed killer herbicide, plant growth regulator can be made effervescent tablet.This tablet volume is little, transports and store very convenient, and the disintegration and become sprayable agricultural-chemical suspension liquid automatically in water of this tablet also can be shed use during use in the paddy field.Can be widely used in the agricultural production.Chinese patent application number: CN98119079.0 publication number: CN1247702 denomination of invention: effervescent pesticide for rice field; inventor: Wu Xiuhua; Chen Weilin; Zheng Caihua; Yi Xiucheng; Liu Zhonghua; the precious applicant of Shen state: Agricultural Chemical Preparation Engineering Technology Centre, Ministry of Che; summary: a kind of effervescent pesticide for rice field; by weed killer herbicide 2-[[[[(4.6-dimethoxypyridin-2-yl) amino] carbonyl] amino] the sulfonyl methyl] methyl benzoate; 3.7-dichloroquinoline-8-carboxylic acid and insecticide 1-(6-chloro-3-pyridylmethyl)-basic amine of N-Nitroimidazoline-2 and solid acid; carbonate mixes the back in proportion to be pulverized, and is reprocessed into graininess; spherical; sheet; column; shapes such as plate-like.In the paddy field of 4~5 centimetres of water conservations, evenly get final product in the input water during use by every mu of some grains.The conventional method that said preparation has thoroughly changed pesticidal preparations or spray or spread.
Yet there are no the mixture preparation of the halosulfuronmethyl and the third careless amine and the research of effervescent tablet aspect thereof.
Summary of the invention
The present invention is directed to the compounded preparation of pesticide that the prior art deficiency provides a kind of synergy, wide spectrum, has been difficult for producing resistance, and complex preparation is processed into a kind of effervescent tablet, once use in agricultural production is killing weeds in rice field harm, overcome peasant under the prior art condition weed killer herbicide has been mixed that soil spreads fertilizer over the fields and the shortcoming that takes a lot of trouble, require great effort, saved time and artificial.
Purpose of the present invention: provide a kind of broad weed-killing spectrum, have the Herbicidal composition of notable synergistic effect, and be processed into the direct effervescent tablet that can throw in the field, the agent for removing grass in paddy field method of a kind of difference and traditional type is provided.
Technical scheme of the present invention is as follows:
Effervescent table as agricultural chemical of the present invention is formulated by active ingredient and auxiliary agent, one of active ingredient is halosulfuronmethyl (English name Halosulfuron methyl), chemical name: 3-(4,6-dimethoxypyridin-2-yl)-and 1-(1-methyl-3-chloro-4-methoxy methyl acyl group pyrazoles-5-yl) sulfonylureas, CAS:100784-20-1; Two of effective ingredient is the third careless amine (English name pretilachlor), chemical name: 2-chloro-2,6 '-diethyl N-(the 2-third oxygen ethyl) acetanil, CAS:51218-49-6.The ratio of the shared prescription gross weight of halosulfuronmethyl is 0.5%-5%, and the ratio of the shared prescription gross weight of the third careless amine is 10%-25%.
Described assistant packet contains solid acid, carbon dioxide source, wetting dispersing agent, binding agent, glidant, desiccant and filler, calculate according to total amount weight, the percentage by weight of its raw material composition the best is: halosulfuronmethyl 0.5%-5%, the third careless amine 10%-30%, solid acid 10%-30%, carbon dioxide source 10%-40%, wetting dispersing agent 1%-15%, glidant 0-5%, binding agent 0-20%, desiccant 0-10%, filler 0-60%.
Can adopt direct compressing dry granulation method or wet granulation again pressed disc method make the target effervescent table as agricultural chemical, that its external form can be is spherical, column, plate-like, sheet etc.
In the effervescent table as agricultural chemical of the present invention, solid acid can be one or several mixtures in maleic acid, citric acid, succinic acid, lactic acid, fumaric acid, tartaric acid, benzoic acid, adipic acid, oxalic acid, p-methyl benzenesulfonic acid, sulfamic acid, boric acid, amino acid, potassium dihydrogen phosphate, malonic acid, nicotinic acid, the sorbic acid.
In the effervescent tablet of the present invention, carbon dioxide source (effervesce source) can be: one or several mixtures of carbonate, subcarbonate or bicarbonate.
In the effervescent tablet of the present invention, wetting dispersing agent can be: lauryl sodium sulfate, neopelex (calcium), nekal, polysorbate, fatty alcohol-polyoxyethylene ether, sodium alkyl sulfate, alkyl polyoxyethylene ether sulfonate, sodium lignin sulfonate, calcium lignosulfonate, nekal (Nekal BX), di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate (NNO), the polycarboxylate sodium salt, one or several mixtures of dodecyl polyoxyethylene ether phosphate or sulfuric ester.
In the effervescent tablet of the present invention, glidant can be: dolomol (calcium), dodecane magnesium sulfate, PEG, hydrogenated vegetable oil, corn starch, Sodium Benzoate, one or several mixtures of polysorbate.
In the effervescent tablet of the present invention, binding agent can be one or more mixtures in lactose, methylcellulose, PVP(polyvinyl pyrrolidone), gelatin, gum Arabic, dextrin, polyvinyl alcohol, polyethylene glycol, sodium carboxymethylcellulose, xanthans, starch and derivative, dextrin, the lactose.
In the effervescent tablet of the present invention, desiccant can be: CaO, CaCl 2, B 2O 3, BaO, Al 2O 3, Na 2SO 4In one or more mixtures.
In the effervescent tablet of the present invention, filler can be one or more mixtures in kaolin, diatomite, clay, Emathlite, mica, bentonite, attapulgite, froth breaking stone, calcium carbonate, white carbon, the talcum powder.
In the effervescent tablet of the present invention,, can not need to comprise glidant, binding agent or desiccant in the prescription according to producing needs.
Of the present invention is the preparation method of the effervescent table as agricultural chemical of active ingredient with the halosulfuronmethyl and the third careless amine:
Can adopt direct compressing dry granulation method and wet granulation again pressed disc method be prepared.
Directly the compressing dry granulation method is: with filler the third careless amine is adsorbed, and mix the back with halosulfuronmethyl and adopt airslide disintegrating mill to be crushed to the 500-800 order, add at last through mechanical crushing to 300-500 purpose solid acid, carbon dioxide source, wetting dispersing agent, binding agent, glidant, desiccant and filler, mix after the tablet press machine film-making, be lower than 120 ℃ of oven dry, detect, pack and get product;
Wet granulation pressed disc method again is to carry out according to the following steps:
(I) accurately take by weighing the third careless amine, halosulfuronmethyl, wetting dispersing agent, glidant, desiccant and filler by prescription, mix, precomminution to 200 order adopts airslide disintegrating mill that it is crushed to 500 orders~800 orders then, gets mixture A;
(II) solid acid, carbonate powder are broken to 300~500 orders, independent packaging is standby;
(III) the mixture A equivalent with preparation in (I) is divided into two parts; add solid acid, the carbon dioxide source of pulverizing in (II) respectively by prescription then; mix; add the binding agent that quantitatively prepares in advance; insert in the granulator and granulate; be dried to moisture less than 2% at 40 ℃~50 ℃ then, behind the whole grain of 20 mesh sieves, make acid softwood particle and alkali grain softwood respectively.
(IV) is respectively with (III)) in two kinds of softwoods making, accurately measure the back in proportion and add in the mixer and stir compressing tablet after 15~20 minutes, be pressed into the effervescent tablet of regulatory specifications, be lower than 120 ℃ of oven dry, detect, pack and get product.
The characteristics of effervescent table as agricultural chemical of the present invention are: efficient, wide spectrum, and easy to use, accurate measurement, a drug just can effectively be prevented and kill off paddy field weed, to paddy rice height of seedling degree safety, low toxicity is good with the environment blending.
Effervescent table as agricultural chemical of the present invention is applied to can effectively prevent and treat the harm of weeds such as multiple broad-leaved, grass family and sedge family to paddy rice in rice seedling throwing field and the transplant field.
The present invention has following remarkable result:
Have lot of advantages after the mixture preparation of the halosulfuronmethyl and the third careless amine is processed into effervescent tablet, as: the user can directly throw effervescent tablet and execute in the rice field during (1) dispenser, need not reduce and measure the formality of making up a prescription with special medical instruments; (2) save time, improve work efficiency.Every mu of paddy rice only needs a few minutes spraying time, compares with conventional pesticide, has improved work efficiency greatly.(3) reduced the dust of agricultural chemicals in producing and using, reduced the injury of medicament human body.That product of the present invention has is easy to use, save time, and improves the advantage of aspect such as work efficiency, has met the present formulations of pesticide towards efficient, safety, low toxicity, development trend easy to use.
Significantly remedy single weed killer herbicide after halosulfuronmethyl and the third careless amine is mixed and kill the narrow shortcoming of grass spectrum, both can play remarkable synergistic effect after being mixed according to certain ratio in addition, and this is to improving herbicide effects, reducing the field using dosage and have positive role.Halosulfuronmethyl is effective to broad leaved weed and sedge weed, but relatively poor to grassy weed effects such as barnyard grass grass, moleplant seeds.The third careless amine has the weed killer herbicide of greater activity to grassy weed, it is very effective to grassy weeds such as non-irrigated barnyard grass, rice barnyard grass, moleplant seed, lady's-grass, green foxtail, Paspalum distichum, eleusine indica, bent grass, be one of efficacious agents of preventing and treating at present paddy fields in south china barnyard grass grass, moleplant seed, but to broad leaved weed and sedge weed preventive effect extreme difference.Therefore, halosulfuronmethyl is mixed into preparation with the third careless amine, not only can reduces production costs, enlarge herbicidal spectrum, improve preventive effect, and can improve safety coefficient, reduce the poisoning odds paddy rice.
Embodiment:
Following embodiment each component proportioning all is weight percentage.
Example 1
20% halosulfuronmethyl, the third careless amine effervescent tablet: former medicine and auxiliary agent selection and proportioning are as follows: halosulfuronmethyl 2%, the third careless amine 18%, citric acid 9%, sodium bicarbonate 12%, di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate 3%, sodium lignin sulfonate 4%, lactose 13%, talcum powder 8%, the filler white carbon complements to 100%.
To prepare 100 kilograms of samples, calculate each amounts of components, weighing respectively by above proportioning.By direct compressing dry granulation method preparation, method is as follows:
Accurately take by weighing earlier 30.15 kilograms of white carbons, with the white carbon absorption 18.75 kilograms 96% the third careless amine, take by weighing 2.1 kilogram of 95% halosulfuronmethyl again, 9 kilograms of citric acids, 12 kilograms of sodium bicarbonates, 3 kilograms of di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonates, 4 kilograms of sodium lignin sulfonates, 13 kilograms of lactose, 8 kilograms of talcum powder, then all materials are mixed after airslide disintegrating mill is crushed to the 500-800 order, mix after tablet press machine compressing tablet slabbing is lower than 100 ℃ of oven dry, heavily about 1 gram/sheet, packing after the assay was approved.
Use 100 grams, 20% halosulfuronmethyl, the third careless amine effervescent tablet for every mu, can effectively prevent and kill off the multiple broad-leaved of seedling throwing field, sedge family and grassy weed, total fresh weight preventive effect is greater than 98.2%.
Example 2
10% halosulfuronmethyl, the third careless amine effervescent tablet: former medicine and auxiliary agent selection and proportioning are as follows: halosulfuronmethyl 1%, the third careless amine 9%, citric acid 9%, sodium bicarbonate 12%, di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate 3%, sodium lignin sulfonate 4%, lactose 13%, talcum powder 8%, the filler white carbon complements to 100%.
To prepare 100 kilograms of samples, calculate each amounts of components, weighing respectively by above proportioning.Press wet granulation pressed disc method preparation again, method is as follows:
(I) accurately take by weighing earlier 40.575 kilograms of white carbons, with the white carbon absorption 9.375 kilograms 96% the third careless amine, take by weighing 1.05 kilogram of 95% halosulfuronmethyl again, 3 kilograms of di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonates, 4 kilograms of sodium lignin sulfonates, 13 kilograms of lactose, 8 kilograms of talcum powder adopt common cracker that mixture is crushed to 200 orders, be crushed to 500~800 orders through airslide disintegrating mill then, get mixture A.
(II) 9 kilograms of citric acid powder are broken to 300~500 orders, 12 kilograms of sodium bicarbonates are crushed to 300~500 orders, package spare respectively.
(II I) is divided into two parts, 39.5 kilograms every part with 79 kilograms of mixture A equivalent of preparation in (I).In a mixture, add 9 kilograms of citric acids pulverizing in (II); mix the back and add 0.05% carboxymethylcellulose sodium solution, insert in the granulator and granulate, be dried to moisture less than 2% at 40 ℃~50 ℃ then; behind the whole grain of 20 mesh sieves, make acid softwood particle.In other a mixture, add 12 kilograms of sodium bicarbonates pulverizing in (II); mix the back and add 0.04% carboxymethylcellulose sodium solution, insert in the granulator and granulate, be dried to moisture less than 2% at 40 ℃~50 ℃ then; behind the whole grain of 20 mesh sieves, make alkaline softwood particle.
(IV) is respectively with (III)) in the acid softwood particle and the alkaline softwood particle that make, add by 48.5: 51.5 mass ratioes and to stir compressing tablet after 15~20 minutes in the mixer, be pressed into the effervescent tablet of regulatory specifications, be lower than 120 ℃ of oven dry, detect, pack and get product.
Use 200 grams, 10% halosulfuronmethyl, the third careless amine effervescent tablet for every mu, can effectively prevent and kill off the multiple broad-leaved of seedling throwing field, sedge family and grassy weed, total fresh weight preventive effect reaches 96.1%.
Example 3
25% halosulfuronmethyl, the third careless amine effervescent tablet: former medicine and auxiliary agent selection and proportioning are as follows: halosulfuronmethyl 2%, the third careless amine 23%, citric acid 9%, sodium bicarbonate 12%, di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate 3%, sodium lignin sulfonate 4%, lactose 10%, the filler white carbon complements to 100%.
Calculate each amounts of components, weighing respectively by above proportioning.By direct compressing dry granulation method preparation, detailed process is with embodiment 1.
Use 80 grams, 25% halosulfuronmethyl, the third careless amine effervescent tablet for every mu, can effectively prevent and kill off the multiple broad-leaved of seedling throwing field, sedge family and grassy weed, total fresh weight preventive effect reaches 96.8%.
Example 4
30% halosulfuronmethyl, the third careless amine effervescent tablet: former medicine and auxiliary agent selection and proportioning are as follows: halosulfuronmethyl 3%, the third careless amine 27%, citric acid 12%, sodium bicarbonate 15%, nekal 4%, sodium lignin sulfonate 5%, bentonite 5%, the filler white carbon complements to 100%.
Calculate each amounts of components, weighing respectively by above proportioning.By direct compressing dry granulation method preparation, detailed process is with embodiment 1.
Use 67 grams, 30% halosulfuronmethyl, the third careless amine effervescent tablet for every mu, can effectively prevent and kill off the multiple broad-leaved of seedling throwing field, sedge family and grassy weed, total fresh weight preventive effect reaches 92.5%.
Example 5
15% halosulfuronmethyl, the third careless amine effervescent tablet: former medicine and auxiliary agent selection and proportioning are as follows: halosulfuronmethyl 1%, the third careless amine 14%, citric acid 9%, sodium bicarbonate 12%, di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate 4%, lignosulfonates 5%, the filler white carbon complements to 100%.
Calculate each amounts of components, weighing respectively by above proportioning.Press wet granulation pressed disc method preparation again, detailed process is with embodiment 2.
Use 150 grams, 15% halosulfuronmethyl, the third careless amine effervescent tablet for every mu, can effectively prevent and kill off the multiple broad-leaved of seedling throwing field, sedge family and grassy weed, total fresh weight preventive effect reaches 96.8%.
Example 6
20% halosulfuronmethyl, the third careless amine effervescent tablet: former medicine and auxiliary agent selection and proportioning are as follows: halosulfuronmethyl 2%, the third careless amine 18%, citric acid 9%, sodium bicarbonate 12%, di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate 5%, lignosulfonates 6%, lactose 13%, aluminium-magnesium silicate 5%, the filler white carbon complements to 100%.
Calculate each amounts of components, weighing respectively by above proportioning.Press wet granulation pressed disc method preparation again, detailed process is with embodiment 2.
Use 100 grams, 20% halosulfuronmethyl, the third careless amine effervescent tablet for every mu, can effectively prevent and kill off the multiple broad-leaved of seedling throwing field, sedge family and grassy weed, total fresh weight preventive effect reaches 91.1%.
The land for growing field crops effect
Test period: in April, 2010~May
Test site: 4 groups in Li Jian village, Xingning District Si Tang town, Nanning City
Trial crops: paddy rice, kind are Shanyougui 99
Test is handled: in rice transplanting dispenser after 6 days (April 18), application method: effervescent tablet directly evenly is thrown into Tanaka, the contrast medicament is 20% bensulfuron-methyl. butachlor wetting powder (Lianyungang, Jiangsu Province east aurification worker Co., Ltd), and according to the usage of routine: spread fertilizer over the fields after wetting powder and dried fine sand mixed.
Result of the test: 30 days investigation fresh weight preventive effects behind the medicine.The result shows: example 1~6 all can effectively be prevented and treated weeds in paddy field, and its control efficiency is not less than the control efficiency of commercially available prod 20% benzyl butachlor WP to weeds in paddy field, and each medicament sees Table 2 to the control efficiency of weeds.
The different weed killer herbicides of table 2. are to the control efficiency of weeds in paddy field
Figure BSA00000452193100081

Claims (11)

1. effervescent table as agricultural chemical, it is characterized in that: this effervescent table as agricultural chemical is formulated by pesticide active ingredient and auxiliary agent, pesticide active ingredient is the halosulfuronmethyl (Halosulfuron methyl) and the third careless amine (pretilachlor), wherein the weight percentage of halosulfuronmethyl is 0.5%-5%, the weight percentage 10%-25% of the third careless amine, all the other are auxiliary agents;
Described auxiliary agent comprises two kinds or two or more mixtures in solid acid, carbon dioxide source, wetting dispersing agent, glidant, binding agent, desiccant and the filler.
2. effervescent table as agricultural chemical as claimed in claim 1 is characterized in that: described solid acid is maleic acid, citric acid, succinic acid, lactic acid, fumaric acid, tartaric acid, benzoic acid, adipic acid, oxalic acid, p-methyl benzenesulfonic acid, sulfamic acid, boric acid, amino acid, KH 2PO 4, one or several mixtures in the malonic acid, nicotinic acid, sorbic acid, account for the 10%-30% of effervescent tablet weight content.
3. effervescent table as agricultural chemical as claimed in claim 1 is characterized in that: described carbon dioxide source is one or several mixtures in carbonate, subcarbonate or the bicarbonate, accounts for the 10%-40% of effervescent tablet weight content.
4. effervescent table as agricultural chemical as claimed in claim 1, it is characterized in that: described wetting dispersing agent is a lauryl sodium sulfate, neopelex (calcium), nekal, polysorbate, fatty alcohol-polyoxyethylene ether, sodium alkyl sulfate, alkyl polyoxyethylene ether sulfonate, sodium lignin sulfonate, calcium lignosulfonate, nekal (Nekal BX), di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate (NNO), the polycarboxylate sodium salt, one or several mixtures in dodecyl polyoxyethylene ether phosphate or the sulfuric ester account for the 1%-15% of effervescent tablet weight content.
5. effervescent table as agricultural chemical as claimed in claim 1, it is characterized in that: described glidant is one or several mixtures in dolomol (calcium), dodecane magnesium sulfate, PEG, hydrogenated vegetable oil, corn starch, Sodium Benzoate, the polysorbate, accounts for the 0-5% of effervescent tablet weight content.
6. effervescent table as agricultural chemical as claimed in claim 1, it is characterized in that: described binding agent is one or more mixtures in lactose, methylcellulose, PVP(polyvinyl pyrrolidone), gelatin, gum Arabic, dextrin, polyvinyl alcohol, polyethylene glycol, sodium carboxymethylcellulose, xanthans, starch and derivative, dextrin, the lactose, accounts for the 0-20% of effervescent tablet weight content.
7. effervescent table as agricultural chemical as claimed in claim 1 is characterized in that: described desiccant is: CaO, CaCl 2, B 2O 3, BaO, Al 2O 3, Na 2SO 4In one or more mixtures, account for the 0-10% of effervescent tablet weight content.
8. the effervescent table as agricultural chemical that contains the halosulfuronmethyl and the third careless amine as claimed in claim 1, it is characterized in that: described filler is one or more mixtures in kaolin, diatomite, clay, Emathlite, mica, bentonite, attapulgite, froth breaking stone, calcium carbonate, white carbon, the talcum powder, accounts for the 0-60% of effervescent tablet weight content.
9. the preparation method of effervescent table as agricultural chemical as claimed in claim 1, it is characterized in that: described effervescent table as agricultural chemical adopts direct compressing dry granulation method to make, its technical process is as follows: at first with filler the third careless amine is adsorbed, and mix the back with halosulfuronmethyl and adopt airslide disintegrating mill to be crushed to 500~800 orders, add at last through mechanical crushing to 300~500 purpose solid acids, carbon dioxide source, wetting dispersing agent, binding agent, glidant, desiccant and filler, mix after the tablet press machine film-making, make the tablet of regulatory specifications, be lower than 120 ℃ of oven dry, get product.
10. the preparation method of effervescent table as agricultural chemical as claimed in claim 1 is characterized in that: described effervescent table as agricultural chemical adopt wet granulation again pressed disc method make, its technical process comprises the steps:
(I) the third careless amine, halosulfuronmethyl, wetting dispersing agent, glidant, desiccant and filler are carried out weighing after, mix, precomminution to 200 order adopts airslide disintegrating mill that it is crushed to 500 orders~800 orders then, mixture A;
(II) solid acid, carbon dioxide source are crushed to 300~500 orders, independent packaging is standby;
(II I) is divided into two parts with (I) mixture A equivalent, add solid acid, the carbonate that (II) pulverized respectively by prescription then, mix, add the binding agent that quantitatively prepares in advance, insert in the granulator and granulate, be dried to moisture less than 2% at 40 ℃~50 ℃ then, behind the whole grain of 20 mesh sieves, make acid softwood particle and alkali grain softwood respectively;
(IV) is respectively with (III)) two kinds of softwoods making, accurately measure the back in proportion and add in the mixer and stir compressing tablet after 15~20 minutes, be pressed into the tablet of regulatory specifications, be lower than 120 ℃ of oven dry, detect, pack and get product.
11. effervescent table as agricultural chemical as claimed in claim 1 is in the purposes of control rice seedling throwing field and transplant field broad-leaved, grass family and sedge weed.
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CN102524279A (en) * 2011-12-22 2012-07-04 广东中迅农科股份有限公司 Pyrazosulfuron effervescent tablet and preparation method thereof
CN102823622A (en) * 2012-09-24 2012-12-19 发事达(南通)化工有限公司 Glyphosate soluble effervescent tablet and preparation method thereof
CN103190425A (en) * 2013-03-28 2013-07-10 济南科赛基农化工有限公司 Effervescent tablet herbicide and preparation method thereof
CN104970035A (en) * 2015-06-17 2015-10-14 广东中迅农科股份有限公司 Weeding composition containing penoxsulam, halosulfuron methyl and pretilachlor
CN105165826A (en) * 2015-08-13 2015-12-23 广东中迅农科股份有限公司 Pesticide effervescent granules and preparation method thereof
CN106490029A (en) * 2016-10-31 2017-03-15 郑州思辩科技有限公司 A kind of effervescent tablet of preventing and treating rice grub and preparation method thereof
CN106818818A (en) * 2015-12-03 2017-06-13 江苏龙灯化学有限公司 A kind of Herbicidal combinations
CN107517968A (en) * 2017-08-04 2017-12-29 安徽圣丰生化有限公司 A kind of herbicidal composition containing pretilachlor, penoxsuam and halosulfuronmethyl
CN107788042A (en) * 2017-11-01 2018-03-13 昭平县科学技术实验场 A kind of herbal pesticide effervescent tablet
CN107788034A (en) * 2017-11-01 2018-03-13 昭平县科学技术实验场 A kind of plant pesticide effervescent tablet
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CN107853321A (en) * 2017-11-01 2018-03-30 昭平县科学技术实验场 A kind of Recompounded pesticide effervescent tablet
CN108184838A (en) * 2018-01-11 2018-06-22 广西贺州市正丰现代农业股份有限公司 A kind of effervescent table as agricultural chemical
CN108402066A (en) * 2018-06-04 2018-08-17 山东耘歌生物科技有限公司 A kind of effervescent formulation and its preparation process containing furans sulphur humulone, pyraclonil and piperazine pyrazosulfuron
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CN117426267A (en) * 2023-12-21 2024-01-23 山东科赛基农生物工程有限公司 Rice production whole-course health management method and application thereof

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CN102524279A (en) * 2011-12-22 2012-07-04 广东中迅农科股份有限公司 Pyrazosulfuron effervescent tablet and preparation method thereof
CN102823622A (en) * 2012-09-24 2012-12-19 发事达(南通)化工有限公司 Glyphosate soluble effervescent tablet and preparation method thereof
CN102823622B (en) * 2012-09-24 2013-12-11 发事达(南通)化工有限公司 Glyphosate soluble effervescent tablet and preparation method thereof
CN103190425A (en) * 2013-03-28 2013-07-10 济南科赛基农化工有限公司 Effervescent tablet herbicide and preparation method thereof
CN104970035A (en) * 2015-06-17 2015-10-14 广东中迅农科股份有限公司 Weeding composition containing penoxsulam, halosulfuron methyl and pretilachlor
CN105165826A (en) * 2015-08-13 2015-12-23 广东中迅农科股份有限公司 Pesticide effervescent granules and preparation method thereof
CN109819994A (en) * 2015-12-03 2019-05-31 江苏龙灯化学有限公司 A kind of Herbicidal combinations
CN106818818A (en) * 2015-12-03 2017-06-13 江苏龙灯化学有限公司 A kind of Herbicidal combinations
CN106490029A (en) * 2016-10-31 2017-03-15 郑州思辩科技有限公司 A kind of effervescent tablet of preventing and treating rice grub and preparation method thereof
CN107517968A (en) * 2017-08-04 2017-12-29 安徽圣丰生化有限公司 A kind of herbicidal composition containing pretilachlor, penoxsuam and halosulfuronmethyl
CN107801726A (en) * 2017-10-24 2018-03-16 安徽丰乐农化有限责任公司 A kind of built herbicide for rice field
CN107788042A (en) * 2017-11-01 2018-03-13 昭平县科学技术实验场 A kind of herbal pesticide effervescent tablet
CN107788034A (en) * 2017-11-01 2018-03-13 昭平县科学技术实验场 A kind of plant pesticide effervescent tablet
CN107853321A (en) * 2017-11-01 2018-03-30 昭平县科学技术实验场 A kind of Recompounded pesticide effervescent tablet
CN108184838A (en) * 2018-01-11 2018-06-22 广西贺州市正丰现代农业股份有限公司 A kind of effervescent table as agricultural chemical
CN108402066A (en) * 2018-06-04 2018-08-17 山东耘歌生物科技有限公司 A kind of effervescent formulation and its preparation process containing furans sulphur humulone, pyraclonil and piperazine pyrazosulfuron
CN108432788A (en) * 2018-06-04 2018-08-24 山东耘歌生物科技有限公司 A kind of effervescent formulation containing pyrazosulfuron, mefenacet and furans sulphur humulone
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CN108477197A (en) * 2018-06-04 2018-09-04 山东耘歌生物科技有限公司 A kind of effervescent formulation containing Huan Wu Evil humulones, ethoxysulfuron and mefenacet
CN108605966A (en) * 2018-06-04 2018-10-02 山东耘歌生物科技有限公司 A kind of effervescent formulation and its preparation process containing furans sulphur humulone, mefenacet and piperazine pyrazosulfuron
CN108617678A (en) * 2018-06-04 2018-10-09 山东耘歌生物科技有限公司 A kind of effervescent formulation and preparation method thereof containing pyrazosulfuron, pretilachlor and three azole amides
CN108812653A (en) * 2018-06-04 2018-11-16 山东耘歌生物科技有限公司 It is a kind of to contain pyrazosulfuron, pretilachlor and effervescent formulation of furans sulphur humulone and preparation method thereof
CN108849877A (en) * 2018-06-04 2018-11-23 山东耘歌生物科技有限公司 It is a kind of to contain pyrazosulfuron, mefenacet and effervescent formulation of Huan Wu Evil humulone and preparation method thereof
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CN108575995A (en) * 2018-06-21 2018-09-28 河北省农林科学院植物保护研究所 A kind of bleeding agent and preparation method thereof being used cooperatively with insecticide
CN110057813A (en) * 2019-04-25 2019-07-26 沈阳溢源生物科技有限公司 The colour developing agent prescription and preparation method of instant capacity colorimetric method for determining available chlorine content
CN110772491A (en) * 2019-10-21 2020-02-11 徐州工程学院 Phellinus igniarius polysaccharide instant effervescent tablet and preparation method thereof
CN117426267A (en) * 2023-12-21 2024-01-23 山东科赛基农生物工程有限公司 Rice production whole-course health management method and application thereof

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