CN108207947A - A kind of diquat dibromide soluble effervescent tablet and preparation method thereof - Google Patents

A kind of diquat dibromide soluble effervescent tablet and preparation method thereof Download PDF

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Publication number
CN108207947A
CN108207947A CN201711430030.6A CN201711430030A CN108207947A CN 108207947 A CN108207947 A CN 108207947A CN 201711430030 A CN201711430030 A CN 201711430030A CN 108207947 A CN108207947 A CN 108207947A
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China
Prior art keywords
acid
diquat dibromide
effervescent tablet
soluble effervescent
soluble
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CN201711430030.6A
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Chinese (zh)
Inventor
孙伯旺
孙晨
王明亮
周钰明
朱岭军
蒋叶豪
李瑶嘉
高志国
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Southeast University
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Southeast University
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Publication of CN108207947A publication Critical patent/CN108207947A/en
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/34Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Agronomy & Crop Science (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The present invention relates to a kind of diquat dibromide soluble effervescent tablet and preparation method thereof, diquat dibromide soluble effervescent tablet of the invention includes according to the component of mass percent meter:Diquat dibromide 1~40%, acid source 10~30%, source 5~30% of getting angry, surfactant 1~8%, binding agent 0.5~3%, free-flow agent 1~5%, surplus is filler material.The preparation method of the diquat dibromide soluble effervescent tablet of the present invention includes step 1, prepares the master batch of diquat dibromide;Step 2, the tabletting of diquat dibromide soluble effervescent tablet.Diquat dibromide soluble effervescent tablet of the present invention belongs to environmentally friendly novel agrochemical, the blank of this field herbicide products is filled up, and production technology is easy to be reliable, it is easy to use, both the voluntarily disintegration diffusion in paddy field can have directly been shed, can also put into sprayer and be sprayed on crop target after disintegration dispersion.

Description

A kind of diquat dibromide soluble effervescent tablet and preparation method thereof
Technical field
The present invention relates to a kind of herbicides applied to farmland, and in particular to a kind of diquat dibromide soluble effervescent tablet and its Preparation method.
Background technology
The basic principle of effervescent table as agricultural chemical be in tablets containing acidic materials (acid source) and substance of getting angry (source of getting angry, The generally basic salt containing carbonate, such as ammonium hydrogen carbonate, sodium carbonate), acid source is neutralized with the source of getting angry after tablet meets water Reaction, releases carbon dioxide, and so as to reach foaming boiling, quickly disintegrated effect, effervescent table as agricultural chemical when in use can be with The voluntarily disintegration diffusion in paddy field is directly shed, can also put into sprayer and be sprayed on crop target after disintegration dispersion.
Diquat dibromide is generally used for conductibility and tags steriland herbicide, can be rapidly by green plants tissue resorption, with soil It is lost activity quickly after contact for the weedings such as before crop field, orchard, bare place, harvesting, is also used as potato and pachyrhizus Cauline leaf urge it is withered.
Diquat dibromide preparation in China's is aqua at present.Diquat dibromide is not particularly stable in water body, can be sent out in alkaline environment Raw degradation, and also side is not convenient in terms of storage and transport for diquat dibromide aqua.And soluble effervescent tablet have given configuration, Homeostasis, and transport and storage are all very convenient, are a kind of environmentally friendly agricultural chemical novel forms.
Chinese patent application CN201510284429 is disclosed " a kind of Herbicidal combinations ", and active ingredient includes diquat dibromide 1%~55%, Quizalotop-ethyl 1%~55%, pyraflufen-ethyl 1%~55%, further include surplus auxiliary agent, and auxiliary agent includes wetting agent, divides Powder, disintegrant, binding agent, filler, viscosity-controlling agent, antifreezing agent, oil base.Although the composition can solve herbicide it is single or Herbicidal spectrum narrow deficiency during dual use expands herbicide controlling spectrum, has many advantages, such as synergistic function, but also exists significantly not Foot:First, three kinds of component pesticides are more demanding to storage condition when existing simultaneously, it is easy to generate denaturation and go bad;Second is that three kinds Component pesticide is to all kinds of weeds drug effects difference, it is not easy to determine suitable component ratio.
Invention content
The shortcomings that the purpose of the present invention is to overcome diquat dibromide existing preparation, provides a kind of diquat dibromide soluble effervescent piece Agent and preparation method thereof, diquat dibromide soluble effervescent tablet of the invention belong to environmentally friendly novel agrochemical, fill up ability The blank of domain herbicide products.
According to a kind of diquat dibromide soluble effervescent tablet proposed by the present invention, which is characterized in that according to mass percent meter Component include:Diquat dibromide 1~40%, acid source 10~30%, source 5~30% of getting angry, surfactant 1~8%, binding agent 0.5~3%, free-flow agent 1~5%, surplus are filler material.
A kind of further preferred scheme of diquat dibromide soluble effervescent tablet proposed by the present invention is;
The acid source for maleic acid, citric acid, succinic acid, lactic acid, fumaric acid, tartaric acid, benzoic acid, adipic acid, oxalic acid, It is one or more in p-methyl benzenesulfonic acid, sulfamic acid, boric acid, amino acid, potassium dihydrogen phosphate, malonic acid, niacin or sorbic acid.
The source of getting angry is one or more in sodium bicarbonate, ammonium hydrogen carbonate, sodium carbonate or potassium carbonate.
The surfactant is dibutyl Cai sodium sulfonate, sodium lignin sulfonate, lauryl sodium sulfate, PO-EO blocks Polyethers, acrylate homopolymer sodium salt, dispersant N, maleic acid-acrylic acid copolymer sodium salt, phenolsulfonic acid condensation product sodium salt, naphthalene sulphur It is one or more in sour condensation product sodium salt or alkylphenol ethoxylate.
The binding agent is water soluble starch, sodium carboxymethyl starch, polyethylene glycol PEG4000 or polyethylene glycol PEG6000 In it is one or more.
The free-flow agent is one or more in white carbon, magnesium stearate or talcum powder.
The filler material is inert filler, using one or more in sucrose, glucose, sodium sulphate or ammonium sulfate.
According to a kind of preparation method of diquat dibromide soluble effervescent tablet proposed by the present invention, which is characterized in that specific step It is rapid as follows:
Step 1, the master batch of diquat dibromide is prepared:It is measured first, in accordance with mass percent, by diquat dibromide, the acid after precise Source, surfactant, inert filler are uniformly mixed in mixing machine, obtain mixture, the compound powder then is broken to grain Diameter is powder more than 150 mesh, and the powder is collected in another mixing machine later, adds in binding agent and mediates, is made through squeezing Grain obtains wet granular, then drying obtains the particle that moisture content is less than 1%, and finally by the pellet through sieves, grain size is 30 after taking sieve The master batch of~60 mesh diquat dibromide is for use;
Step 2, the tabletting of diquat dibromide soluble effervescent tablet:It is measured first, in accordance with mass percent, after accurately measuring The master batch of diquat dibromide prepared of above-mentioned steps 1, source of getting angry, free-flow agent be uniformly mixed in mixing machine, then in tablet press machine In be pressed into disk, the thickness of the disk is 3~15mm, a diameter of 5~40mm of the disk, the monolithic weight of the disk It measures as 0.5~20g.
Its remarkable advantage is the present invention compared with prior art:First, the diquat dibromide soluble effervescent tablet category of the present invention In environmentally friendly novel agrochemical, the blank of this field herbicide products is filled up.Second is that the solvable sex vesicle of diquat dibromide of the present invention Effervescent tablet has given configuration, homeostasis, and transport and storage are all very convenient, and safety is good.Third, the enemy of the present invention The production technology of careless fast soluble effervescent tablet is easy to be reliable and easy to use, both can directly shed and has voluntarily been disintegrated in paddy field Diffusion can also put into sprayer and be sprayed on crop target after disintegration dispersion.
Specific embodiment
The specific embodiment of the present invention is described in further detail with reference to embodiment.
Embodiment 1-9 is a kind of diquat dibromide soluble effervescent tablet proposed by the present invention, and component is according to quality percentage Than metering, table 1 is referred to;The specification of its component meets national pesticide standard.
Table 1:
Below by taking diquat dibromide soluble effervescent tablet a kind of disclosed in embodiment 1, embodiment 6 and embodiment 9 as an example, into one Step discloses a kind of preparation method of diquat dibromide soluble effervescent tablet proposed by the present invention.
Embodiment 10.It is as 1% diquat dibromide soluble effervescent tablet to prepare diquat dibromide content described in embodiment 1 Example, is as follows:
Step 1, the master batch of diquat dibromide is prepared:A kind of chemical group of diquat dibromide soluble effervescent tablet according to the present invention Into, according to mass percent component measure, accurately weigh first diquat dibromide 1kg, acid source be maleic acid 10kg and citric acid 10kg, surfactant are dibutyl Cai's sodium sulfonate 8kg, inert filler is sucrose 10kg and glucose 28.5kg, by it in mixed It is uniformly mixed in conjunction machine, obtains mixture, the compound powder is then broken to grain size as powders more than 150 mesh, later will The powder is collected in another mixing machine, is added in 5kg and is mediated dissolved with aqueous solution of the binding agent for 10% water soluble starch, Wet granular is obtained through extruder grain, then drying obtains the particle that moisture content is less than 1%, and finally the particle is sieved through vibrating screen Sieving, grain size is for use for the master batch of 30~60 mesh diquat dibromide after taking sieve;
Step 2, the tabletting of diquat dibromide soluble effervescent tablet:It is measured first, in accordance with mass percent, after accurately measuring The master batch 68kg of diquat dibromide for preparing of above-mentioned steps 1, the source of getting angry be sodium bicarbonate 30kg, free-flow agent be white carbon 2kg in It is uniformly mixed in mixing machine, shape is then routinely pressed into tablet press machine as circular tablet, the monolithic diameter of the tablet For 5mm, the single-sheet thickness of the tablet is 3mm, and the monolithic weight of the tablet is in 0.5g or so.
The performance test results:The disintegration time of 1% diquat dibromide soluble effervescent tablet that step 2 obtains is 67s, pH value is 4.3 (1% aqueous solutions).Component percentages in the present embodiment 10 are mass percent.
Embodiment 11.It is as 20% diquat dibromide soluble effervescent tablet to prepare the diquat dibromide content described in embodiment 6 Example, is as follows:
Step 1, the master batch of diquat dibromide is prepared:A kind of chemical group of diquat dibromide soluble effervescent tablet according to the present invention Into, measured according to the component of mass percent, accurately weigh the active compound 20kg of diquat dibromide first, acid source is sulfamic acid 20kg, Surfactant is naphthalene sulfonic acid condensate sodium salt 1kg, inert filler is glucose 25.5kg, it is mixed in mixing machine It is even, mixture is obtained, the compound powder is then broken to grain size as powders more than 150 mesh, later collects the powder It is mediated in another mixing machine, adding in 5kg dissolved with aqueous solution of the binding agent for 10% sodium carboxymethyl starch, through extruder grain Wet granular is obtained, then drying obtains the particle that moisture content is less than 1%, finally the particle through vibrating screen is sieved, takes sieve Grain size is for use for the master batch of 30~60 mesh diquat dibromide afterwards;
Step 2, the tabletting of diquat dibromide soluble effervescent tablet:It is measured first, in accordance with mass percent, after accurately measuring Above-mentioned steps 1 prepare diquat dibromide master batch 67kg, the source of getting angry is sodium carbonate 15kg and potassium carbonate 15kg, free-flow agent are sliding Mountain flour 3kg is uniformly mixed in mixing machine, and shape is then routinely pressed into tablet press machine as circular tablet, the tablet The a diameter of 24mm of monolithic, the single-sheet thickness of the tablet is 8mm, and the monolithic weight of the tablet is in 12.5g or so.
The performance test results:The disintegration time of 20% diquat dibromide soluble effervescent tablet that step 2 obtains is 80s, pH value For 4.6 (1% aqueous solutions).Component percentages in the present embodiment 11 are mass percent.
Embodiment 12.It is as 40% diquat dibromide soluble effervescent tablet to prepare the diquat dibromide content described in embodiment 9 Example, is as follows:
Step 1, the master batch of diquat dibromide is prepared:A kind of chemical group of diquat dibromide soluble effervescent tablet according to the present invention Into being measured according to the component of mass percent, accurately weigh the active compound 40kg of diquat dibromide first, acid source is niacin 6kg and sorb Sour 6kg, surfactant are PO-EO block polyethers 1kg, inert filler is glucose 12kg and ammonium sulfate 16kg, by it in mixed It is uniformly mixed in conjunction machine, obtains mixture, the compound powder is then broken to grain size as powders more than 150 mesh, later will The powder is collected in another mixing machine, is added in 5kg and is pinched dissolved with aqueous solution of the binding agent for 10% sodium carboxymethyl starch It closes, wet granular is obtained through extruder grain, then drying obtains the particle that moisture content is less than 1%, finally by the particle through vibrating screen Sieving sieving, grain size is for use for the master batch of 30~60 mesh diquat dibromide after taking sieve;
Step 2, the tabletting of diquat dibromide soluble effervescent tablet:It is measured first, in accordance with mass percent, after accurately measuring The master batch 84kg of diquat dibromide for preparing of above-mentioned steps 1, the source of getting angry be potassium carbonate 15kg, free-flow agent is talcum powder 1kg in mixed It is uniformly mixed in conjunction machine, shape is then routinely pressed into tablet press machine as circular tablet, the monolithic of the tablet is a diameter of 40mm, the single-sheet thickness of the tablet is 15mm, and the monolithic weight of the tablet is in 20g or so.
The performance test results:The disintegration time of 40% diquat dibromide soluble effervescent tablet that step 2 obtains is 87s, pH value For 4.9 (1% aqueous solutions).Component percentages in the present embodiment 12 are mass percent.
Concrete application effect of the present invention is further disclosed directly below, and table 2 is respectively used to prevent and kill off mandarin orange for 10-12 of the embodiment of the present invention Orangery weeds are tested, total preventive effect result of investigation in 30 days by a definite date.
Table 2:
The present invention experiment proves that, achieve satisfied trial effect.

Claims (8)

1. a kind of diquat dibromide soluble effervescent tablet, which is characterized in that the component according to mass percent meter includes:Diquat dibromide 1 ~40%, acid source 10~30%, source 5~30% of getting angry, surfactant 1~8%, binding agent 0.5~3%, free-flow agent 1~ 5%, surplus is filler material.
2. a kind of diquat dibromide soluble effervescent tablet according to claim 1, which is characterized in that the acid source is Malaysia Acid, citric acid, succinic acid, lactic acid, fumaric acid, tartaric acid, benzoic acid, adipic acid, oxalic acid, p-methyl benzenesulfonic acid, sulfamic acid, boron It is one or more in acid, amino acid, potassium dihydrogen phosphate, malonic acid, niacin or sorbic acid.
3. a kind of diquat dibromide soluble effervescent tablet according to claim 2, which is characterized in that carbonic acid is in the source of getting angry It is one or more in hydrogen sodium, ammonium hydrogen carbonate, sodium carbonate or potassium carbonate.
4. a kind of diquat dibromide soluble effervescent tablet according to claim 3, which is characterized in that the surfactant is Dibutyl Cai sodium sulfonate, lauryl sodium sulfate, PO-EO block polyethers, acrylate homopolymer sodium salt, divides sodium lignin sulfonate Powder N, maleic acid-acrylic acid copolymer sodium salt, phenolsulfonic acid condensation product sodium salt, naphthalene sulfonic acid condensate sodium salt or alkyl phenol ethoxy It is one or more in based compound.
5. a kind of diquat dibromide soluble effervescent tablet according to claim 4, which is characterized in that the binding agent is water-soluble It is one or more in property starch, sodium carboxymethyl starch, polyethylene glycol PEG4000 or polyethylene glycol PEG6000.
6. a kind of diquat dibromide soluble effervescent tablet according to claim 5, which is characterized in that the free-flow agent is white It is one or more in carbon black, magnesium stearate or talcum powder.
7. a kind of diquat dibromide soluble effervescent tablet according to claim 6, which is characterized in that the filler material is inertia Filler is selected one or more in sucrose, glucose, sodium sulphate or ammonium sulfate.
8. according to a kind of preparation method of diquat dibromide soluble effervescent tablet of claim 1-7 any one of them, feature exists In being as follows:
Step 1, the master batch of diquat dibromide is prepared:Measured first, in accordance with mass percent, by after precise diquat dibromide, acid source, Surfactant, inert filler are uniformly mixed in mixing machine, obtain mixture, the compound powder then is broken to grain size is The powder is collected in another mixing machine by powders more than 150 mesh later, is added in binding agent and is mediated, is obtained through extruder grain The particle that moisture content is less than 1% is obtained to wet granular, then drying, finally by the pellet through sieves, grain size is 30~60 after taking sieve The master batch of mesh diquat dibromide is for use;
Step 2, the tabletting of diquat dibromide soluble effervescent tablet:It is measured first, in accordance with mass percent, it will be upper after accurate metering The master batch for stating the diquat dibromide of step 1 preparation, source of getting angry, free-flow agent are uniformly mixed in mixing machine, are then pressed in tablet press machine It is made disk, the thickness of the disk is 3~15mm, a diameter of 5~40mm of the disk, and the monolithic weight of the disk is 0.5~20g.
CN201711430030.6A 2017-11-21 2017-12-26 A kind of diquat dibromide soluble effervescent tablet and preparation method thereof Pending CN108207947A (en)

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CN2017111644881 2017-11-21

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109122683A (en) * 2018-09-21 2019-01-04 广州方中化工有限公司 The preparation of composite synergistic wetting agent and its application in the outstanding preparation of pymetrozine water
CN110506748A (en) * 2019-08-21 2019-11-29 中国农业科学院油料作物研究所 It is a kind of to urge withered desiccant applied to sesame

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102823589A (en) * 2012-09-24 2012-12-19 发事达(南通)化工有限公司 Pesticide water effervescent dispersible 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
CN102860302A (en) * 2012-09-24 2013-01-09 发事达(南通)化工有限公司 Brassinolide water-dispersible effervescent tablets and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102823589A (en) * 2012-09-24 2012-12-19 发事达(南通)化工有限公司 Pesticide water effervescent dispersible 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
CN102860302A (en) * 2012-09-24 2013-01-09 发事达(南通)化工有限公司 Brassinolide water-dispersible effervescent tablets and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109122683A (en) * 2018-09-21 2019-01-04 广州方中化工有限公司 The preparation of composite synergistic wetting agent and its application in the outstanding preparation of pymetrozine water
CN109122683B (en) * 2018-09-21 2021-03-09 广州方中化工有限公司 Preparation of composite synergistic wetting agent and application thereof in pymetrozine water suspension preparation
CN110506748A (en) * 2019-08-21 2019-11-29 中国农业科学院油料作物研究所 It is a kind of to urge withered desiccant applied to sesame

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