CN106035337B - A kind of water-soluble granule and preparation method thereof of picloram salt - Google Patents
A kind of water-soluble granule and preparation method thereof of picloram salt Download PDFInfo
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- CN106035337B CN106035337B CN201610377261.4A CN201610377261A CN106035337B CN 106035337 B CN106035337 B CN 106035337B CN 201610377261 A CN201610377261 A CN 201610377261A CN 106035337 B CN106035337 B CN 106035337B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/12—Powders or granules
- A01N25/14—Powders or granules wettable
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of picloram salt raw medicine and its preparation method and application of water-soluble granule, which is directly reacted to obtain by solid picloram with solid basic material.Material keeps solid state in preparation process of the present invention, and product needs not move through crystallization process, simplifies synthesis step, improves yield, reduces energy consumption, three-waste free discharge, and no dust generates, and Safety and Environmental Protection is good, and environmental pollution is smaller.The picloram water-soluble granule of preparation reduces foaming characteristic by adjusting the selection and proportion of auxiliary material, improves disintegration rate and solubility, without precipitating in solution after dissolution, packs, transports compared with aqua, storing conveniently, at low cost, convenient for application.
Description
Technical field
The present invention relates to a kind of water-soluble granules and preparation method thereof of picloram salt, belong to pesticide chemical technology neck
Domain.
Background technique
Picloram is to report activity of weeding, the herbicide of Dao Hua company, U.S. exploitation by E.R.Laning in 1963.
Chlorine Fampridine acid category synthetic hormone type herbicide, it can be absorbed rapidly by plant stem-leaf and root, and in sensitive plant body, induction is planted
Object generates epinasty reaction, stagnates simultaneously necrosis rapidly so as to cause plant growth.The medicament lasting period is long, can be used for preventing and kill off herbage
Ground is annual and perennial broadleaf grass for example Rheum obtusifolia Linn, curled dock, creeping thistle, gentle thistle, honor fiber crops, pasture Ye Maomo, dandelion and
Herba stellariae mediae.There is fine selectivity simultaneously, most of broad leaf crops are all sensitive to this product in addition to crop in cruciferae, most of grass family
Crop is drug resistant.
In practical application, it usually needs picloram salt is made in picloram acid.Picloram salt is main
Dosage form has following a few classes: aqua, missible oil, aqueous emulsion, soluble powder, water dispersible granules.In these dosage forms, containing big in aqua
Amount water causes many inconvenience to packaging, transport and storage, while improving cost, and aqueous emulsion contains a large amount of organic solvents to environment
And human body has biggish damaging effect, although water dispersible granules are lower without solvent utilization rate, soluble powder is being used
When be easy to fugitive dust, have certain harm to human body, only soluble granula can just overcome the above shortcomings.At present, in the market
Product is mainly aqua, it is not yet found that picloram salt soluble granula.
Summary of the invention
The object of the present invention is to provide a kind of water-soluble granules and preparation method thereof of picloram salt；The water solubility grain
Agent disintegration is rapidly, solubility is high, foaming characteristic is low, functional；Preparation method is simple and easy to do.
Technical scheme is as follows:
A kind of water-soluble granule of picloram salt, by following mass percentage at being grouped as: picloram
Salt 5-95%, surfactant 2-5%, hard water resistance dose of 1-2%, water soluble filler surplus.
The water-soluble granule of above-mentioned picloram salt, it is preferred that consisting of, picloram salt 5-90%, surface are living
Property agent 5%, hard water resistance dose 1%, water soluble filler surplus；It is furthermore preferred that consisting of, picloram salt 80-90%, surface are living
Property agent 5%, hard water resistance dose 1%, water soluble filler surplus.
The water-soluble granule of above-mentioned picloram salt, the surfactant are alkyl sulfate, alkylsulfonate, alkane
Base naphthalene sulfonate, alkylbenzene sulfonate, polycarboxylate, sulfuric acid, alkyl betaine, alkyl polyglycoside, Polyoxyethylene fatty
Amine, ethoxy castor oil, alkyl phenol polyoxyethylene ether, aliphatic amine polyoxyethylene ether, nonylphenol polyoxyethylene ether and ethylene oxide-
One or more of propylene oxide block copolymer；Preferably alkylbenzene sulfonate；More preferably alkyl betaine and
The mixture that alkyl polyglycoside is formed according to the mass ratio of 3:2.
Above-mentioned picloram water-soluble granula, described hard water resistance dose is EDTA, EDETATE SODIUM, Gan Luosu, EDTA tetra-
Sodium, citric acid or sodium tripolyphosphate；Preferably EDETATE SODIUM.
Above-mentioned picloram water-soluble granula, the water soluble filler are water-soluble inorganic salt, such as can be with are as follows:
Sulfate, nitrate, hydrochloride, carbonate, bicarbonate, phosphate, phosphoric acid hydrogen disalt, dihydric phosphate, borate and silicon
One or more of in hydrochlorate；Preferably sulfate.The cation of water-soluble inorganic salt can for sylvite, sodium salt or
Ammonium salt, each water-soluble inorganic salt effect is almost the same, preferably sylvite.
The water-soluble granule of above-mentioned picloram salt, preferably constitutes are as follows:
Picloram sylvite 90%, alkylnaphthalene sulfonate 2%, EDETATE SODIUM 1%, sodium sulphate surplus；Alternatively,
Picloram ammonium salt 80%, alkyl betaine 3%, alkyl polyglycoside 2%, EDETATE SODIUM 1%, sodium sulphate surplus；Or
Person,
Picloram dimethylamine salt 40%, alkyl betaine 3%, alkyl polyglycoside 2%, EDETATE SODIUM 1%, more than sodium sulphate
Amount；Alternatively,
Picloram isopropyl amine salt 5%, alkyl betaine 3%, alkyl polyglycoside 2%, EDETATE SODIUM 1%, sodium sulphate surplus；
Alternatively,
Picloram isopropanol amine salt 90%, alkyl betaine 3% and alkyl polyglycoside 2%, EDETATE SODIUM 1%, sodium sulphate
Surplus.
The water-soluble granule of above-mentioned picloram salt, picloram salt used can be commercially available or be voluntarily prepared.This hair
It is bright to provide a kind of preparation method of picloram salt: the following steps are included: by solid under the stirring condition of 60-100rpm
Picloram and alkaline matter mixing 10min~20min；Then heat to 50-70 DEG C, with the stirring rate of 30-50rpm into
Row stirring is reacted to complete.The alkaline matter is potassium hydroxide, potassium carbonate, saleratus, sodium hydroxide, sodium carbonate, carbonic acid
Hydrogen sodium, monomethyl amine, dimethylamine, trimethylamine, isopropylamine, isopropanolamine or ammonium hydrogen carbonate.Each alkaline matter it is basic at salt effect
Unanimously, preferably potassium carbonate or sodium bicarbonate.
It is the water-soluble granule of raw material preparation relative to the picloram salt prepared otherwise, with " admittedly method admittedly " system
Standby picloram salt be raw material prepared by water-soluble granule, when being dissolved in water, solution rate faster, more difficult
Bubble.
A kind of preparation method of the water-soluble granule of above-mentioned picloram salt of the invention, by picloram salt, table
Face activating agent, hard water resistance dose and water soluble filler are uniformly mixed, and are granulated, and drying can obtain picloram water-soluble granule.
In above-mentioned preparation method, it is granulated at 40-100 DEG C.
In above-mentioned preparation method, drying temperature is 60-90 DEG C.
Picloram water-soluble granule of the invention reduces foaming characteristic, mentions by adjusting the selection and proportion of auxiliary material
High disintegration rate and solubility overcome these defects without precipitating in solution after dissolution, and with aqua compared with packaging, transport,
Storage is convenient, at low cost, convenient for application.
Specific embodiment
The present invention will be further elaborated combined with specific embodiments below, and following embodiments are merely illustrative, not
Restriction effect is played to the present invention.
In following embodiments, the raw material of use is all common commercially available product, is all available on the market unless otherwise specified.Its
In, picloram salt used in embodiment 1-12 is commercially available；Manufacturer is: it is limited that Feng Huagong share is moistened in Shandong Weifang
Company, content specification are 95%.
The preparation of 1 picloram sylvite water-soluble granule of embodiment
Water-soluble granule formula is (wt%): picloram sylvite 90%, alkylnaphthalene sulfonate 2%, EDETATE SODIUM 1%, sulphur
Sour sodium surplus.
The preparation method comprises the following steps: taking 200g picloram sylvite raw medicine (content 95.6%), surfactant alkylnaphthalene is added
Sodium sulphate 6.1g is added in sulfonate 4.2g, hard water resistance dose of EDETATE SODIUM 2.1g, and each component is uniformly mixed in kneader, is mixed
Conjunction is finished to be granulated at 50 DEG C, is dried under the conditions of 70 DEG C to get to 90% picloram sylvite water-soluble granule, gained is water-soluble
Property granula granulating rate it is high, 99% or more, full grains are smooth, good fluidity.
The preparation of 2 picloram sodium salt water-soluble granule of embodiment
Water-soluble granule formula be (wt%): picloram sodium salt 80%, lauryl sodium sulfate 3%, EDETATE SODIUM 1%,
Sodium nitrate surplus.
The preparation method comprises the following steps: taking 250g picloram sodium salt raw medicine (content 95.3%), surface-active is added according to the proportion
Agent lauryl sodium sulfate 8.9g, hard water resistance dose of EDETATE SODIUM 2.9g, water soluble filler sodium nitrate 36g are mediating each component
It is uniformly mixed in machine, mixing is finished to be granulated at 60 DEG C, and drying is under the conditions of 80 DEG C to get water-soluble to 80% picloram sodium salt
Property granula, gained water-soluble granule granulating rate is high, and 99% or more, full grains are smooth, good fluidity.
The preparation of 3 picloram ammonium salt water soluble granule preparation of embodiment
Water-soluble granule formula is (wt%): picloram ammonium salt 80%, alkylnaphthalene sulfonate 2%, alkylbenzene sulfonate
1%, EDETATE SODIUM 0.5%, ammonium chloride surplus.
The preparation method comprises the following steps: taking 200g picloram ammonium salt raw medicine (content 95.4%), surfactant alkylnaphthalene is added
Sulfonate 4.8g, alkylbenzene sulfonate 2.4g, hard water resistance dose of EDETATE SODIUM 1.2g, water soluble filler ammonium chloride 29.6g, by each group
It point is sufficiently mixed in kneader uniformly, mixing is finished to be granulated at 65 DEG C, is dried under the conditions of 90 DEG C to get to 80% ammonia chlorine pyrrole
Pyridine acid ammonium salt water-soluble granule, gained water-soluble granule granulating rate is high, and 99% or more, full grains are smooth, good fluidity.
The preparation of 4 picloram monomethyl amine water-soluble granula of embodiment
Water-soluble granule formula be (wt%): picloram monomethyl amine salt 60%, alkyl amine oxide 5%, EDETATE SODIUM 1%,
Sodium phosphate surplus.
The preparation method comprises the following steps: taking 280g picloram monomethyl amine salt raw medicine (content 95.8%), surfactant alkyl is added
Each component is sufficiently mixed uniformly by amine oxide 22.4g, hard water resistance dose of EDETATE SODIUM 4.4g, water soluble filler sodium phosphate 140.2g,
Mixing is finished and is granulated at 50 DEG C, is dried under the conditions of 75 DEG C to get to 60% picloram monomethyl amine water-soluble granula, institute
It is high to obtain water-soluble granule granulating rate, 99% or more, full grains are smooth, good fluidity.
The preparation of 5 picloram dimethylamine salt water-soluble granule of embodiment
Water-soluble granule formula is (wt%): picloram dimethylamine salt 50%, polycarboxylate 3%, more than diammonium hydrogen phosphate
Amount.
The preparation method comprises the following steps: taking 250g picloram dimethylamine salt raw pesticide (content 96.2%), surfactant alkane is added
Each component is sufficiently mixed uniformly mixing by base amine oxide 14.4g, water soluble filler diammonium hydrogen phosphate 216.6g in kneader
It finishes and is granulated at 60 DEG C, dried under the conditions of 65 DEG C to get to 50% picloram dimethylamine salt water-soluble granule, gained water
Dissolubility granula granulating rate is high, and 99% or more, full grains are smooth, good fluidity.
The preparation of 6 picloram trimethylamine water-soluble granula of embodiment
Water-soluble granule formula is (wt%): picloram front three amine salt 5%, alkyglycosides 4%, tetra- sodium of EDTA
1.5%, potassium sulfate surplus.
The preparation method comprises the following steps: taking 20g picloram front three amine salt raw medicine (content 95.2%), surfactant alkane is added
Base polyglycosides 15.2g, hard water resistance dose of EDTA tetra- sodium 5.7g, water soluble filler potassium sulfate 339.9g, by each component in kneader
In be sufficiently mixed uniformly, mixing is finished and is granulated at 60 DEG C, is dried under the conditions of 80 DEG C to get to 5% picloram front three amine salt
Water-soluble granule, gained water-soluble granule granulating rate is high, and 99% or more, full grains are smooth, good fluidity.
The preparation of 7 picloram isopropyl amine salt water-soluble granule of embodiment
Water-soluble granule formula is (wt%): picloram isopropyl amine salt 70%, fatty alcohol polyoxyethylene ether 3%, casein
1%, sodium carbonate surplus.
The preparation method comprises the following steps: taking 200g picloram isopropyl amine salt raw medicine (content 96.1%), surfactant rouge is added
Fat alcohol polyoxyethylene ether 8.3g, hard water resistance dose of casein 2.7g, water soluble filler sodium carbonate 63.1g, by each component in kneader
In be sufficiently mixed uniformly, mixing is finished and is granulated at 70 DEG C, is dried under the conditions of 80 DEG C to get to 70% picloram isopropylamine
Water-soluble granula, gained water-soluble granule granulating rate is high, and 99% or more, full grains are smooth, good fluidity.
The preparation of 8 picloram isopropanolamine water-soluble granula of embodiment
Water-soluble granule formula is (wt%): picloram isopropanol amine salt 80%, nonylphenol polyoxyethylene ether 2%, nonyl
Phenol polyethenoxy ether 2%, citric acid 1%, sodium bicarbonate surplus.
The preparation method comprises the following steps: taking 320g picloram isopropanol amine salt raw medicine (content 96.1%), surfactant is added
Nonylphenol polyoxyethylene ether 7.7g, nonylphenol polyoxyethylene ether 7.7g, hard water resistance dose of citric acid 3.8g, water soluble filler bicarbonate
Each component is sufficiently mixed uniformly by sodium 45.2g in kneader, and mixing is finished to be granulated at 60 DEG C, is dried under the conditions of 80 DEG C, i.e.,
80% picloram isopropanolamine water-soluble granula is obtained, gained water-soluble granule granulating rate is high, and 99% or more, particle is full
It is full, smooth, good fluidity.
Embodiment 9
Water-soluble granule formula is (wt%): picloram ammonium salt 80%, alkyl betaine 3% and alkyl polyglycoside 2%,
EDETATE SODIUM 1%, sodium sulphate surplus.Preparation method is referring to embodiment 1.
Embodiment 10
Water-soluble granule formula is (wt%): picloram dimethylamine salt 40%, alkyl betaine 3% and alkyl polyglycoside
2%, EDETATE SODIUM 1%, sodium sulphate surplus.Preparation method is referring to embodiment 1.
Embodiment 11
Water-soluble granule formula is (wt%): picloram isopropyl amine salt 5%, alkyl betaine 3% and alkyl polyglycoside
2%, EDETATE SODIUM 1%, sodium sulphate surplus.Preparation method is referring to embodiment 1.
Embodiment 12
Water-soluble granule formula is (wt%): picloram isopropanol amine salt 90%, alkyl betaine 3% and alkyl polysaccharide
Glycosides 2%, EDETATE SODIUM 1%, sodium sulphate surplus.Preparation method is referring to embodiment 1.
Embodiment 13
(1) in the 1L kneader with heating device, by 400g picloram raw medicine (purity 95%) and 162g carbon
Potassium hydrogen phthalate (purity 99%) is put into together, is mixed 10-20 minutes under normal temperature and pressure conditions, under the speed of 60-100rpm,
50-70 DEG C is then heated to, control mixing speed is 30-50rpm, is continuesd to mix at this temperature and mixing speed, 1 hour left side
The right detection material extent of reaction shows that reaction system is changed into completely soluble ammonia by picloram raw medicine not soluble in water
Chloropyridine acid potassium salt raw medicine dries the picloram sylvite raw medicine of preparation at 80 DEG C, obtains dry product 458g, contains through analysis
Amount (content is mass content, similarly hereinafter) is 95.6%, yield 99.6%.
(2) water-soluble granule formula is (wt%): picloram sylvite 90% prepared by step 1, alkylnaphthalene sulfonate 2%,
EDETATE SODIUM 1%, sodium sulphate surplus.Preparation method is referring to embodiment 1.
Embodiment 14
The performance of 1 ~ 13 products obtained therefrom of embodiment is detected, test result is as shown in table 1:
The water-soluble granule the performance test results of 1 picloram salt of table
It is measured by embodiment 1-13 properties of product it can be seen that the water-soluble granule of picloram salt of the present invention blisters
Property is low, and solution rate is fast, and PH is more stable, has no water-insoluble.Wherein embodiment 1,9-12 be preferred embodiment, foaming characteristic with
Solution rate is significantly lower than embodiment 2-8.Compared with Example 1, foaming characteristic and solution rate are better than embodiment to embodiment 13
1。
Embodiment 15
Composition analyzed is carried out to the water-soluble granule of picloram salt prepared in the above embodiments in accordance with the following methods:
Medicament used in 1
Test medicine: 1 ~ 13 resulting product of the embodiment of the present invention.
Comparison medicament: 24% picloram aqua, registration number PD20097825, Sichuan Lear crop science Co., Ltd
Production.
2 experimental methods
2.1 experimental methods:
The application of weeds foliar spray method, using the manual backpack sprayer of Singapore Jacto HD400 type, per hectare converts medical fluid
600 liters.
2.2 each dosings are as shown in table 2.
2 dosing of table
。
2.3 application same day weather conditions
The application same day is partly cloudy, and 23.8 DEG C of temperature on average, relative humidity 60%, no Precipitation Process, 2-10 days after application, with more
Based on the gas of the skies, 22.4 DEG C -25.6 DEG C of temperature, relative humidity 54-76%.It is experimental field red soil, pH5.6 or so.
The observation of 2.4 preventive effects and calculation:
Drug effect calculation method
15 days investigation weeds strain numbers, calculation formula are as follows after medicine:
Strain number preventive effect=(blank area strain number-treatment region strain number)/blank area strain number × 100
And the significance of difference is analyzed with poor (DMRT) method of the new multipole of Deng Kenshi.
2.5 preventive effects, as shown in table 3；
Table 3
Note: -- representative has no preventive effect.
It is seen from the above data that the embodiment of the present invention prepares each medicament according to 1200 grams/ha of dosages of effective component
Field broadleaf weeds can be effectively prevented and kill off, preventive effect is better than control group medicament.In addition, by the preferred of auxiliary material, it is resulting water-soluble
Property granula shows significant synergistic effect, and herbicidal effect is further promoted.
Claims (2)
1. a kind of water-soluble granule of picloram salt, which is characterized in that by following mass percentage at being grouped as: ammonia
Chloropyridine acid potassium salt 90%, alkylnaphthalene sulfonate 2%, EDETATE SODIUM 1%, sodium sulphate surplus.
2. a kind of preparation method of the water-soluble granule of picloram salt, which comprises the following steps:
(1) in the 1L kneader with heating device, by the picloram raw medicine and 162g purity 99% of 400g purity 95%
Saleratus put into together, under normal temperature and pressure conditions, be mixed 10-20 minutes under the speed of 60-100rpm, then
It is warming up to 50-70 DEG C, control mixing speed is 30-50rpm, is continuesd to mix at this temperature and mixing speed, is examined within 1 hour or so
Material reaction degree is surveyed, display reaction system is changed into completely soluble ammonia chlorine pyrrole by picloram raw medicine not soluble in water
Pyridine acid potassium salt raw medicine dries the picloram sylvite raw medicine of preparation at 80 DEG C, obtains dry product 458g, as ammonia chloropyridine
Acid potassium salt raw medicine；
(2) 200g picloram sylvite raw medicine is taken, surfactant alkylnaphthalene sulfonate 4.2g, hard water resistance dose of EDTA bis- is added
Sodium sulphate 6.1g is added in sodium 2.1g, each component is uniformly mixed in kneader, mixing is finished to be granulated at 50 DEG C, 70 DEG C of items
It dries under part to get to 90% picloram sylvite water-soluble granule.
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| CN112608272A (en) * | 2020-12-25 | 2021-04-06 | 山东埃森化学有限公司 | Preparation method of picloram potassium salt bulk drug |
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|---|---|---|---|---|
| CN102715174A (en) * | 2012-06-28 | 2012-10-10 | 永农生物科学有限公司 | Compound pesticide composition containing picloram or salts thereof, preparation and application |
| CN104478925A (en) * | 2014-12-18 | 2015-04-01 | 山东潍坊润丰化工股份有限公司 | Preparation method of glyphosate potassium salt, glyphosate potassium salt water-soluble granule and preparation method of glyphosate potassium salt water-soluble granule |
| CN105175324A (en) * | 2015-08-14 | 2015-12-23 | 山东潍坊润丰化工股份有限公司 | Clopyralid salt active compound, preparation method for water-soluble granules of clopyralid salt active compound and applications |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102715174A (en) * | 2012-06-28 | 2012-10-10 | 永农生物科学有限公司 | Compound pesticide composition containing picloram or salts thereof, preparation and application |
| CN104478925A (en) * | 2014-12-18 | 2015-04-01 | 山东潍坊润丰化工股份有限公司 | Preparation method of glyphosate potassium salt, glyphosate potassium salt water-soluble granule and preparation method of glyphosate potassium salt water-soluble granule |
| CN105175324A (en) * | 2015-08-14 | 2015-12-23 | 山东潍坊润丰化工股份有限公司 | Clopyralid salt active compound, preparation method for water-soluble granules of clopyralid salt active compound and applications |
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Address after: 250100 Shandong Ji'nan high tech Zone comprehensive free trade zone, 1 north section of three Xing Road, Ji'nan No. 2, R & D platform area, 901 Applicant after: Run Bo bio tech ltd, Shandong Address before: 250000 A601, 6 / F, Ji'nan hi tech Innovation Service Center, 750 Shun Hua Road, Ji'nan hi tech Zone, Shandong. Applicant before: Run Bo bio tech ltd, Shandong |
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