CN109430268A - A kind of preparation method of low hexachlorobenzene content chlorothalonil suspending agent - Google Patents
A kind of preparation method of low hexachlorobenzene content chlorothalonil suspending agent Download PDFInfo
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- CN109430268A CN109430268A CN201811486048.2A CN201811486048A CN109430268A CN 109430268 A CN109430268 A CN 109430268A CN 201811486048 A CN201811486048 A CN 201811486048A CN 109430268 A CN109430268 A CN 109430268A
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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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/34—Nitriles
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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
- A01N25/02—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 containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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Abstract
The present invention relates to a kind of preparation method of low hexachlorobenzene content chlorothalonil suspending agent, the methods are as follows: mixes Bravo and part of auxiliary with water by formula ratio, mixed slurry is obtained after grinding；Ammonium hydroxide is added into mixed slurry, and is heated；Remaining auxiliary agent is added into the slurries by heat treatment, is then dispersed, obtains the Bravo suspending agent of low hexachlorobenzene content.The present invention prepare Bravo suspending agent during introduce basification, significantly reduce the content of hexachloro-benzene in Bravo suspending agent, hexachlorobenzene content < 10ppm, with good economic efficiency and application prospect in gained Bravo suspending agent.
Description
Technical field
The invention belongs to preparation technique of pesticide fields, and in particular to a kind of preparation of low hexachlorobenzene content chlorothalonil suspending agent
Method.
Background technique
Bravo is a kind of efficient, low toxicity, wide spectrum, and the protective fungicide of low-residual has the characteristics that non-interior suction, acts on
Mechanism is to have an effect with the glyceraldehyde 3-phosphate dehydrogenase in fungal cell, with the protein containing cysteine in the enzyme
It combines, to destroy the enzymatic activity, the metabolism of fungal cell is made to be damaged and lose vitality.
Bravo is widely used in agricultural and the fungal disease of forestry is prevented and treated, especially in vegetables, the industrial crops such as fruit
There are many upper application.There can be control efficiency to 52 kinds of diseases of 30 various crops according to Japanese data report Bravo.In addition,
Bravo also has important use in mould proof industrial circle, such as manufactures mildew resistant paint, mould proof wallpaper, electric appliance is mould proof, Pi Ping, timber
Deng it is mould proof.The production scale of Bravo at home constantly expands, it has also become one of excellent pesticide species of large-tonnage in the world.
Hexachloro-benzene contained in Bravo is a kind of noxious material, and there is extended residual, biology to raise product property, partly volatilize
Property and high toxicity, can result in the generation of a variety of diseases.Biological metabolism, light degradation and chemistry under natural environment drops in the substance
The effects of solution, has very strong resistivity, and natural degradation is extremely difficult.In recent years, with the continuous expansion of Bravo application field
Greatly and consumer environments consciousness increasingly reinforcement, market is to the indices of Bravo preparation, especially hexachlorobenzene content
It is required that being continuously improved.Therefore, efficient, low toxicity, safe and environment-friendly fungicide are the urgent needs for ensureing agricultural production.
Bravo suspending agent usually is prepared in such a way that raw material mixing is stirred, is sanded in the prior art.Such as
CN108669101A discloses a kind of Bravo suspending agent and preparation method thereof, the preparation method comprises the following steps: by soft water, Bravo, surface
Activating agent, ethylene glycol are added in agitated kettle, are uniformly mixed, obtain mixture A；Mixture A is put into sand mill, grinding
To granularity less than 2.5 microns, discharging obtains mixture B；Aluminium-magnesium silicate, xanthan gum, sodium benzoate, hair are added into mixture B
Golden bamboo extractive, is uniformly mixed, and obtains Bravo suspending agent.
CN108522506A discloses a kind of medicine fertilizer compatible type Bravo suspending agent and preparation method thereof, the preparation method comprises the following steps:
Dosage of each component is calculated with weight ratio according to the ratio, and is weighed, is mixed and stirred for uniformly；Water is added, is uniformly mixed, forms formula
Material is added pH adjusting agent for pH and is adjusted to 3-4；Suspending agent is made in formulation material wet grinding；Analytical control is measured, is packaged into
Library.
CN102630667B discloses a kind of Bravo suspending agent and preparation method thereof of resistance of rainwater washing against, preparation method
Are as follows: Bravo, wetting agent, dispersing agent, preservative, antifreezing agent, suspending agent, defoaming agent and water are weighed by formula metering requirement, is filled
Share in the benefit it is wet and after mixing evenly enter sand mill be sanded, after granularity less than 5 μm, pH between 6.0-9.0 after, discharging to modulate
Kettle, and the thickener and synergist measured is added, it modulates uniformly to get product.
In the above method, the concentration of hexachloro-benzene has obtained reducing to a certain degree with the dilution of dampening in suspending agent, but outstanding
It is certain when the content of water in floating agent, the drug effect of Bravo can be reduced if hypervolia.Enterprise generally passes through purchase at present
The concentration of hexachloro-benzene in the low Bravo raw material control suspending agent of hexachlorobenzene content, but this kind of expensive raw material price, economy effect
Benefit is poor, it is difficult to obtain large-scale promotion.If can be during Bravo be prepared into suspending agent, by preparation method
The content for reducing hexachloro-benzene in Bravo suspending agent is improved, then can bring good economic benefit.
Summary of the invention
In view of problems of the prior art, it is outstanding that the purpose of the present invention is to provide a kind of low hexachlorobenzene content chlorothalonils
The preparation method of floating agent, prepare Bravo suspending agent during introduce basification, significantly reduce Bravo suspension
The content of hexachloro-benzene in agent, with good economic efficiency and application prospect.
To achieve this purpose, the present invention adopts the following technical scheme:
The present invention provides a kind of preparation methods of low hexachlorobenzene content chlorothalonil suspending agent, and the method includes following steps
It is rapid:
(1) Bravo and part of auxiliary are mixed by formula ratio with water, mixed slurry is obtained after grinding；
(2) ammonium hydroxide is added in the mixed slurry obtained to step (1), and is heated；
(3) remaining auxiliary agent is added in the slurries to step (2) by heat treatment, is then dispersed, obtains hexachloro-benzene
The Bravo suspending agent of content < 10ppm.
The present invention prepare Bravo suspending agent during introduce basification the step of, under heating conditions,
Hexachloro-benzene and ammonium hydroxide reaction, part hexachloro-benzene in Bravo are decomposed, and hexachloro-benzene in Bravo suspending agent is thereby reduced
Content.Hexachlorobenzene content < 10ppm, meets state specified standards in Bravo suspending agent obtained, has and preferably answers
Use prospect.
In addition, thickener is generally added in the prior art before the milling, easily cause in sand grinding process to thickener structure
It destroys, mobility decline, thickener is added after the completion of grinding in the present invention, in the premise for the performance for not influencing thickener effect
Under, the structure of thickener is protected well.
The formula of Bravo suspending agent of the present invention as a preferred technical solution, are as follows: Bravo 35-60%, suspending
Floating agent 1-3%, dispersing agent 1-3%, wetting agent 0-5%, emulsifier 1-5%, thickener 0.1-2%, defoaming agent 0.5-3%, prevent
Freeze agent 2-5%, preservative 0-1%, surplus is water.But non-to be only limitted to this, the other similar Bravo suspending agent in this field is matched
Side is equally applicable to the present invention.
Method provided by the invention is suitable for the Bravo raw material of various hexachlorobenzene contents, but in order to protrude effect of the invention
Fruit, generally selection hexachlorobenzene content >=30ppm Bravo are prepared as raw material.
According to the present invention, the suspension aid is bentonite, white carbon black, disodium hydrogen phosphate, diammonium hydrogen phosphate or phosphoric acid hydrogen
At least one of dipotassium, such as can be in bentonite, white carbon black, disodium hydrogen phosphate, diammonium hydrogen phosphate or dipotassium hydrogen phosphate
Any one, typical but infinite combination are as follows: bentonite and white carbon black, disodium hydrogen phosphate and diammonium hydrogen phosphate, bentonite,
Diammonium hydrogen phosphate and dipotassium hydrogen phosphate etc..
According to the present invention, the dispersing agent is sodium lignin sulfonate, formaldehyde condensate of sodium methylnaphthalene sulfonate MF, dodecane
Base sodium sulphate, modified polypropylene copolymer Agrlian 700, alkylnaphthalene sulfonate formaldehyde condensation products Morwet D425, alkylnaphthalene
The mixture M orwet D 500 of sulfonate and formaldehyde condensation product and its block copolymer, sodium polyphosphate or 2- naphthalenesulfonateformaldehyde formaldehyde are poly-
At least one of object sodium salt NNO is closed, such as can be sodium lignin sulfonate, formaldehyde condensate of sodium methylnaphthalene sulfonate MF, ten
Sodium dialkyl sulfate, modified polypropylene copolymer Agrlian 700, alkylnaphthalene sulfonate formaldehyde condensation products Morwet D425, alkane
The mixture M orwet D 500 of base naphthalenesulfonate formaldehyde condensation compound and its block copolymer, sodium polyphosphate or 2- naphthalene sulfonic acids first
Any one in aldehyde polymer sodium salt NNO, typical but non-limiting combination are as follows: sodium lignin sulfonate and methyl naphthalene sulfonic acid sodium
Formaldehyde condensation products MF, lauryl sodium sulfate and modified polypropylene copolymer Agrlian 700, the contracting of alkylnaphthalene sulfonate formaldehyde
The mixture M orwet D 500 of object Morwet D425 and alkylnaphthalene sulfonate formaldehyde condensation products and its block copolymer are closed, it is more
Polyphosphate sodium and 2- naphthalene sulfonic acid formaldehyde polymer sodium salt NNO etc..
According to the present invention, the wetting agent is nonylphenol polyoxyethylene ether, alkylnaphthalene sulfonate and anion wetting agent
Mixture M orwet EFW, phenethyl phenylpropyl phenol polyethenoxy ether, Berol 790A anionic surfactant or fatty alcohol
At least one of polyoxyethylene ether peregal series, such as can be nonylphenol polyoxyethylene ether, alkylnaphthalene sulfonate and yin
Mixture M orwet EFW, phenethyl phenylpropyl phenol polyethenoxy ether, the Berol 790A anionic surface of ion wetting agent are living
Property agent or fatty alcohol polyoxyethylene ether peregal series in any one, typical but non-limiting combination are as follows: nonyl phenol is poly-
Ethylene oxide ether and phenethyl phenylpropyl phenol polyethenoxy ether, Berol 790A anionic surfactant and aliphatic alcohol polyethenoxy
Ether peregal series etc..
According to the present invention, the emulsifier is alkyl phenol polyoxyethylene ether OP series, TWEEN Series, phenethyl phenol polyoxy second
At least one of alkene ether or neopelex, for example, can be alkyl phenol polyoxyethylene ether OP series, TWEEN Series,
Any one in phenethyl phenol polyethenoxy ether or neopelex, typical but non-limiting combination are as follows: alkyl
Phenol polyethenoxy ether OP series and phenethyl phenol polyethenoxy ether, TWEEN Series and neopelex, phenethyl phenol are poly-
Ethylene oxide ether and neopelex etc..
According to the present invention, the thickener is xanthan gum, carboxymethyl cellulose, polyacrylamide, aluminium-magnesium silicate or poly- second
At least one of enol, such as can be in xanthan gum, carboxymethyl cellulose, polyacrylamide, aluminium-magnesium silicate or polyvinyl alcohol
Any one, typical but non-limiting combination are as follows: xanthan gum and carboxymethyl cellulose, polyacrylamide and aluminium-magnesium silicate,
Polyvinyl alcohol, xanthan gum and polyacrylamide etc..
According to the present invention, the defoaming agent is tributyl phosphate, three iso-butyl ester of phosphoric acid, butanol, organosilicon, C8-C10 fat
At least one of alcohols or ester-ether type compound, for example, can be tributyl phosphate, three iso-butyl ester of phosphoric acid, butanol, organosilicon,
Any one in C8-C10 fatty alcohols or ester-ether type compound, typical but non-limiting combination are as follows: tributyl phosphate and
Three iso-butyl ester of phosphoric acid, butanol and organosilicon, C8-C10 fatty alcohols and ester-ether type compound etc..
According to the present invention, the antifreezing agent is at least one in ethylene glycol, propylene glycol, glycerine, polyethylene glycol or urea
Kind, such as can be any one in ethylene glycol, propylene glycol, glycerine, polyethylene glycol or urea, it is typical but non-limiting
Combination are as follows: ethylene glycol and propylene glycol, glycerine and polyethylene glycol, ethylene glycol and urea etc..
According to the present invention, the preservative is Kathon CG, benzoic acid, sodium benzoate, formaldehyde, polyformaldehyde, sodium citrate, water
At least one of poplar acid sodium or D-sorbite, such as can be Kathon CG, benzoic acid, sodium benzoate, formaldehyde, polyformaldehyde, lemon
Any one in sour sodium, sodium salicylate or D-sorbite, typical but non-limiting combination are as follows: Kathon CG and benzoic acid, benzene first
Sour sodium and formaldehyde, polyformaldehyde and sodium citrate, sodium salicylate and D-sorbite etc..
According to the present invention, based on mass percentage, the additional amount of step (2) described ammonium hydroxide is the 0.02- of Bravo
0.1%, for example, can be 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09% or
Specific point value between 0.1% and above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list.
The additional amount of above-mentioned ammonium hydroxide be the key that it is of the invention, when insufficient (< 0.02%) is added in ammonium hydroxide, act on it is limited,
The content of hexachloro-benzene is still higher in Bravo；When excessive (being greater than 0.1%) is added in ammonium hydroxide, Bravo suspending agent can be reduced
Drug effect.
According to the present invention, the temperature of step (2) described heat treatment is 60-90 DEG C, such as can be 60 DEG C, 65 DEG C, 70
DEG C, 75 DEG C, 80 DEG C, 85 DEG C or the specific point value between 90 DEG C and above-mentioned numerical value, as space is limited and for concise consideration,
The present invention no longer exclusive list.
As the temperature of heat treatment too low (60 DEG C of <), the decomposition of hexachloro-benzene is difficult to effectively carry out；When heat treatment
When temperature excessively high (90 DEG C of >), the drug effect of Bravo suspending agent can be reduced.
According to the present invention, step (2) heat treatment time be 20-90min, such as can be 20min, 30min,
Specific point value between 40min, 50min, 60min, 70min, 80min or 90min and above-mentioned numerical value as space is limited and goes out
In concise consideration, the present invention no longer exclusive list.
According to the present invention, the part of auxiliary added in step (1) is suspension aid, dispersing agent, wetting agent, emulsifier and disappears
Infusion.
According to the present invention, the defoaming agent additional amount is the 35-45% of defoaming agent total amount, for example, can be 35%, 36%,
37%, the specific point value between 38%, 39%, 40%, 41%, 42%, 43%, 44% or 45% and above-mentioned numerical value, is limited to
Length and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the additional amount of water is the 60-70% of water inventory in step (1), for example, can be 60%, 61%,
62%, the specific point value between 63%, 64%, 65%, 66%, 67%, 68%, 69% or 70% and above-mentioned numerical value, is limited to
Length and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the partial size that material in mixed slurry is ground in step (1) is 0.5-5 μm, such as can be 0.5
μm, 1 μm, 1.5 μm, 2 μm, 2.5 μm, 3 μm, 3.5 μm, 4 μm, 4.5 μm or the specific point value between 5 μm and above-mentioned numerical value, limit
In length and for concise consideration, the present invention no longer exclusive list.
According to the present invention, step (1) grinding is preferably sanded.
According to the present invention, the remaining auxiliary agent being added in step (3) is thickener, antifreezing agent, preservative and defoaming agent.
According to the present invention, the thickener is added in the form of content is the solution of 0.1-5wt%.
According to the present invention, the defoaming agent additional amount is the 55-65% of defoaming agent total amount, for example, can be 55%, 56%,
57%, the specific point value between 58%, 59%, 60%, 61%, 62%, 63%, 64% or 65% and above-mentioned numerical value, is limited to
Length and for concise consideration, the present invention no longer exclusive list.
According to the present invention, described be dispersed in the high-speed shearing machine that revolving speed is 4000-12000r/min of step (3) carries out,
The revolving speed can be 4000r/min, 5000r/min, 6000r/min, 7000r/min, 8000r/min, 9000r/min,
Specific point value between 10000r/min, 11000r/min or 12000r/min and above-mentioned numerical value, as space is limited and for letter
Bright consideration, the present invention no longer exclusive list.
According to the present invention, the water of formula surplus is added in step (3) described dispersion process.
As a preferred technical solution, the preparation method of low hexachlorobenzene content chlorothalonil suspending agent of the present invention include with
Lower step:
(1) Bravo and suspension aid, dispersing agent, wetting agent, emulsifier and defoaming agent are mixed by formula ratio with water, is ground
The partial size for being milled to material is 0.5-5 μm, obtains mixed slurry, wherein defoaming agent additional amount is the 35-45% of defoaming agent total amount,
The additional amount of water is the 60-70% of water inventory；
(2) ammonium hydroxide of Bravo quality 0.02-0.1% is added in the mixed slurry obtained to step (1), and in 60-90
20-90min is heated at DEG C；
(3) thickener, antifreezing agent, preservative and defoaming agent is added in the slurries to step (2) by heat treatment, then
Dispersed in the high-speed shearing machine that revolving speed is 4000-12000r/min, the water of formula surplus is added in dispersion process, obtains
The Bravo suspending agent of hexachlorobenzene content < 10ppm, wherein thickener is added in the form of content is the solution of 0.1-5wt%,
The defoaming agent additional amount is the 55-65% of defoaming agent total amount.
Compared with prior art, the present invention is at least had the advantages that
(1) present invention prepare Bravo suspending agent during introduce basification, it is outstanding to significantly reduce Bravo
The content of hexachloro-benzene in agent is floated, hexachlorobenzene content < 10ppm in gained Bravo suspending agent is a kind of efficient, less toxic, environment friend
The fungicide of good type.
(2) present invention has adjusted the addition sequence of thickener, protects the structure of thickener, it is made to play maximum effect
Fruit.
(3) the suspending agent even particle size that method provided by the invention obtains is conducive to the stable storage for improving suspending agent
Deposit with drug effect play, 1-2 can be stored for a long time, have easily flow, not bleed, it is not stratified, the features such as agglomeration, solve
It is the problem of bleed can occur after preparation stored, easy to use, it has a good application prospect.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.
Select the Bravo that hexachlorobenzene content is 35ppm as raw material in the present invention in each embodiment and comparative example.
Typical but non-limiting embodiment of the invention is as follows:
Embodiment 1
The preparation method for present embodiments providing a kind of low hexachlorobenzene content chlorothalonil suspending agent, by mass percentage
Meter, the Bravo suspending agent of the low hexachlorobenzene are made of following raw material: Bravo 40%, dipotassium hydrogen phosphate and bentonite 1%,
Neopelex 1%, fatty alcohol polyoxyethylene ether paregal O -10 2%, neopelex 3%, xanthan gum
0.2%, three iso-butyl ester of phosphoric acid 0.5%, Kathon CG 0.2%, propylene glycol 5%, surplus is water.
It is prepared in accordance with the following methods:
(1) formula ratio is pressed by Bravo and dipotassium hydrogen phosphate and bentonite, neopelex, fatty alcohol polyoxy second
Alkene ether paregal O -10, neopelex and three iso-butyl ester of phosphoric acid are mixed with water, and the partial size for being ground to material is 0.5-5
μm, obtain mixed slurry, wherein three iso-butyl ester of phosphoric acid additional amount is the 35% of its total amount, and the additional amount of water is water inventory
70%；
(2) ammonium hydroxide of Bravo quality 0.05% is added in the mixed slurry obtained to step (1), and is heated at 80 DEG C
45min；
(3) xanthan gum, three iso-butyl ester of phosphoric acid, Kathon CG and propylene glycol is added in the slurries to step (2) by heat treatment,
Then dispersed in the high-speed shearing machine that revolving speed is 10000r/min, the water of formula surplus is added in dispersion process, obtains
Bravo suspending agent, wherein xanthan gum is added in the form of content is the solution of 3wt%, and three iso-butyl ester of phosphoric acid additional amount is it
The 65% of total amount.
Embodiment 2
The preparation method for present embodiments providing a kind of low hexachlorobenzene content chlorothalonil suspending agent, by mass percentage
Meter, the Bravo suspending agent of the low hexachlorobenzene are made of following raw material: Bravo 40%, bentonite 1%, sodium lignin sulfonate
1%, the mixture M orwet EFW2.5% of alkylnaphthalene sulfonate and anion wetting agent, phenethyl phenol polyethenoxy ether
2.5%, polyacrylamide 0.2%, tributyl phosphate 0.5%, sodium benzoate 0.2%, propylene glycol 5%, surplus is water.
It is prepared in accordance with the following methods:
(1) by formula ratio by Bravo and bentonite, sodium lignin sulfonate, alkylnaphthalene sulfonate and anion wetting agent
Mixture M orwet EFW, phenethyl phenol polyethenoxy ether, three iso-butyl ester of phosphoric acid are mixed with water, and the partial size for being ground to material is
0.5-5 μm, obtain mixed slurry, wherein three iso-butyl ester of phosphoric acid additional amount is the 45% of its total amount, and the additional amount of water is water inventory
60%；
(2) ammonium hydroxide of Bravo quality 0.1% is added in the mixed slurry obtained to step (1), and is heated at 60 DEG C
90min；
(3) be added polyacrylamide in the slurries to step (2) by heat treatment, tributyl phosphate, sodium benzoate and
Then propylene glycol is dispersed in the high-speed shearing machine that revolving speed is 12000r/min, formula surplus is added in dispersion process
Water obtains Bravo suspending agent, wherein polyacrylamide is added in the form of content is the solution of 1wt%, and tributyl phosphate adds
Enter 55% that amount is its total amount.
Embodiment 3
The preparation method for present embodiments providing a kind of low hexachlorobenzene content chlorothalonil suspending agent, by mass percentage
Meter, the Bravo suspending agent of the low hexachlorobenzene are made of following raw material: Bravo 50%, white carbon black 1%, alkylnaphthalene sulfonate
Formaldehyde condensation products Morwet D425 1%, alkyl phenol polyoxyethylene ether OP-7 2%, aluminium-magnesium silicate 0.5%, ethyl silicon oil
0.5%, propylene glycol 5%, polyformaldehyde 0.2%, surplus is water.
It is prepared in accordance with the following methods:
(1) formula ratio is pressed by Bravo and white carbon black, alkylnaphthalene sulfonate formaldehyde condensation products Morwet D425, alkyl phenol
Polyoxyethylene ether OP-7, ethyl silicon oil are mixed with water, and the partial size for being ground to material is 0.5-5 μm, obtain mixed slurry, wherein
Ethyl silicon oil additional amount is the 35% of its total amount, and the additional amount of water is the 65% of water inventory；
(2) ammonium hydroxide of Bravo quality 0.06% is added in the mixed slurry obtained to step (1), and is heated at 90 DEG C
20min；
(3) aluminium-magnesium silicate, ethyl silicon oil, propylene glycol and polyformaldehyde is added in the slurries to step (2) by heat treatment,
Then dispersed in the high-speed shearing machine that revolving speed is 6000r/min, the water of formula surplus is added in dispersion process, obtains hundred
The clear suspending agent of bacterium, wherein aluminium-magnesium silicate is added in the form of content is the solution of 0.5wt%, and ethyl silicon oil additional amount is that it is total
The 65% of amount.
Embodiment 4
The preparation method for present embodiments providing a kind of low hexachlorobenzene content chlorothalonil suspending agent, by mass percentage
Meter, the Bravo suspending agent of the low hexachlorobenzene are made of following raw material: Bravo 55%, disodium hydrogen phosphate 2%, alkylnaphthalene sulphur
The mixture M orwet D 500 1% of hydrochlorate formaldehyde condensation products and its block copolymer, fatty alcohol polyoxyethylene ether paregal O-
10 2%, neopelex 4%, carboxymethyl cellulose 0.2%, methyl-silicone oil 0.5%, sodium citrate 0.2%, the third three
Alcohol 5%, surplus are water.
It is prepared in accordance with the following methods:
(1) formula ratio is pressed by Bravo and disodium hydrogen phosphate, alkylnaphthalene sulfonate formaldehyde condensation products and its block copolymer
Mixture M orwet D 500, fatty alcohol polyoxyethylene ether paregal O -10, neopelex, methyl-silicone oil and water
Mixing, the partial size for being ground to material is 0.5-5 μm, obtains mixed slurry, wherein methyl-silicone oil additional amount is its total amount
45%, the additional amount of water is the 65% of water inventory；
(2) ammonium hydroxide of Bravo quality 0.08% is added in the mixed slurry obtained to step (1), and is heated at 75 DEG C
60min；
(3) to step (2) by heat treatment slurries in be added carboxymethyl cellulose, methyl-silicone oil, sodium citrate and
Then glycerine is dispersed in the high-speed shearing machine that revolving speed is 4000r/min, formula surplus is added in dispersion process
Water obtains Bravo suspending agent, wherein methylcellulose is added in the form of content is the solution of 5wt%, and methyl-silicone oil is added
Amount is the 55% of its total amount.
Embodiment 5
The preparation method for present embodiments providing a kind of low hexachlorobenzene content chlorothalonil suspending agent, by mass percentage
Meter, the Bravo suspending agent of the low hexachlorobenzene are made of following raw material: Bravo 60%, bentonite 2%, detergent alkylate sulphur
Sour sodium 1%, fatty alcohol polyoxyethylene ether paregal O -10 2%, neopelex 5%, carboxymethyl cellulose 0.2%,
Three iso-butyl ester of phosphoric acid 0.5%, Kathon CG 0.2%, propylene glycol 5%, surplus are water.
It is prepared in accordance with the following methods:
(1) formula ratio is pressed by Bravo and bentonite, neopelex, fatty alcohol polyoxyethylene ether paregal O-
10, neopelex, three iso-butyl ester of phosphoric acid are mixed with water, and the partial size for being ground to material is 0.5-5 μm, obtain mixing slurry
Material, wherein three iso-butyl ester of phosphoric acid additional amount is the 38% of its total amount, and the additional amount of water is the 60% of water inventory；
(2) ammonium hydroxide of Bravo quality 0.04% is added in the mixed slurry obtained to step (1), and is heated at 70 DEG C
65min；
(3) to step (2) by heat treatment slurries in be added carboxymethyl cellulose, three iso-butyl ester of phosphoric acid, Kathon CG and
Then propylene glycol is dispersed in the high-speed shearing machine that revolving speed is 9000r/min, formula surplus is added in dispersion process
Water obtains Bravo suspending agent, wherein carboxymethyl cellulose is added in the form of content is the solution of 2.5wt%, and tricresyl phosphate is different
Butyl ester additional amount is the 62% of its total amount.
Comparative example 1
Compared with Example 1, other than removing the operation of step (2), other steps and condition and the complete phase of embodiment 1
Together, i.e., remaining auxiliary agent is directly added into the mixed slurry obtained to step (1) to be dispersed.
Comparative example 2
Compared with Example 1, other than being added without ammonium hydroxide in step (2), other steps and condition and the complete phase of embodiment 1
Together, i.e., the operation only heated in step (2).
Comparative example 3
Compared with Example 1, in addition in step (2) without heating other than, other steps and condition and the complete phase of embodiment 1
Together, i.e., the operation for adding ammonium hydroxide is only carried out in step (2).
Performance test:
According to " pesticide suspension concentrate product standard writes specification " (HG/T 2467.5-2003) and " Bravo suspending agent "
(HG/T 18171-2017) standard examines the content of hexachloro-benzene in Bravo aqueous suspension agent obtained by 1-5 of the embodiment of the present invention
It surveys, testing result is as shown in table 1.
Table 1
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within of the invention
Within protection scope and the open scope.
Claims (11)
1. a kind of preparation method of low hexachlorobenzene content chlorothalonil suspending agent, which is characterized in that the described method comprises the following steps:
(1) Bravo and part of auxiliary are mixed by formula ratio with water, mixed slurry is obtained after grinding；
(2) ammonium hydroxide is added in the mixed slurry obtained to step (1), and is heated；
(3) remaining auxiliary agent is added in the slurries to step (2) by heat treatment, is then dispersed, obtains hexachlorobenzene content
The Bravo suspending agent of < 10ppm.
2. the method as described in claim 1, which is characterized in that based on mass percentage, the Bravo suspending agent is matched
Side are as follows: Bravo 35-60%, suspension aid 1-3%, dispersing agent 1-3%, wetting agent 0-5%, emulsifier 1-5%, thickener
0.1-2%, defoaming agent 0.5-3%, antifreezing agent 2-5%, preservative 0-1%, surplus are water.
3. method according to claim 2, which is characterized in that the suspension aid is bentonite, white carbon black, phosphoric acid hydrogen two
At least one of sodium, diammonium hydrogen phosphate or dipotassium hydrogen phosphate；
Preferably, the dispersing agent is sodium lignin sulfonate, formaldehyde condensate of sodium methylnaphthalene sulfonate MF, dodecyl sulphate
Sodium, modified polypropylene copolymer Agrlian 700, alkylnaphthalene sulfonate formaldehyde condensation products Morwet D425, alkylnaphthalene sulfonate
The mixture M orwet D 500 of formaldehyde condensation products and its block copolymer, sodium polyphosphate or 2- naphthalene sulfonic acid formaldehyde polymer sodium
At least one of salt NNO；
Preferably, the wetting agent is the mixture of nonylphenol polyoxyethylene ether, alkylnaphthalene sulfonate and anion wetting agent
Morwet EFW, phenethyl phenylpropyl phenol polyethenoxy ether, Berol 790A anionic surfactant or fatty alcohol polyoxy second
At least one of alkene ether peregal series；
Preferably, the emulsifier is alkyl phenol polyoxyethylene ether OP series, TWEEN Series, phenethyl phenol polyethenoxy ether or ten
At least one of dialkyl benzene sulfonic acids sodium；
Preferably, the thickener is in xanthan gum, carboxymethyl cellulose, polyacrylamide, aluminium-magnesium silicate or polyvinyl alcohol
It is at least one；
Preferably, the defoaming agent is tributyl phosphate, three iso-butyl ester of phosphoric acid, butanol, organosilicon, C8-C10 fatty alcohols or ester
At least one of ether type compound；
Preferably, the antifreezing agent is at least one of ethylene glycol, propylene glycol, glycerine, polyethylene glycol or urea；
Preferably, the preservative be Kathon CG, benzoic acid, sodium benzoate, formaldehyde, polyformaldehyde, sodium citrate, sodium salicylate or
At least one of D-sorbite.
4. the method as described in claim 1, which is characterized in that the part of auxiliary added in step (1) is suspension aid, dispersion
Agent, wetting agent, emulsifier and defoaming agent；
Preferably, the defoaming agent additional amount is the 35-45% of defoaming agent total amount.
5. the method as described in claim 1, which is characterized in that the additional amount of water is the 60-70% of water inventory in step (1).
6. the method as described in claim 1, which is characterized in that the partial size for being ground to material in mixed slurry in step (1) is
0.5-5μm；
Preferably, step (1) is described is ground to be sanded.
7. the method as described in claim 1, which is characterized in that based on mass percentage, the addition of step (2) described ammonium hydroxide
Amount is the 0.02-0.1% of Bravo.
8. the method as described in claim 1, which is characterized in that the temperature of step (2) described heat treatment is 60-90 DEG C；
Preferably, the time of step (2) heat treatment is 20-90min.
9. the method as described in claim 1, which is characterized in that the remaining auxiliary agent being added in step (3) is thickener, antifreeze
Agent, preservative and defoaming agent；
Preferably, the thickener is added in the form of content is the solution of 0.1-5wt%；
Preferably, the defoaming agent additional amount is the 55-65% of defoaming agent total amount.
10. the method as described in claim 1, which is characterized in that step (3) revolving speed that is dispersed in is 4000-12000r/
It is carried out in the high-speed shearing machine of min；
Preferably, the water of formula surplus is added in step (3) described dispersion process.
11. such as the described in any item methods of claim 1-10, which is characterized in that the described method comprises the following steps:
(1) Bravo and suspension aid, dispersing agent, wetting agent, emulsifier and defoaming agent are mixed by formula ratio with water, is ground to
The partial size of material is 0.5-5 μm, obtains mixed slurry, wherein defoaming agent additional amount is the 35-45% of defoaming agent total amount, water
Additional amount is the 60-70% of water inventory；
(2) ammonium hydroxide of Bravo quality 0.02-0.1% is added in the mixed slurry obtained to step (1), and at 60-90 DEG C
Heat 20-90min；
(3) thickener, antifreezing agent, preservative and defoaming agent is added in the slurries to step (2) by heat treatment, then
Dispersed in the high-speed shearing machine that revolving speed is 4000-12000r/min, the water of formula surplus is added in dispersion process, obtains chlordene
The Bravo suspending agent of benzene content < 10ppm, wherein thickener is added in the form of content is the solution of 0.1-5wt%, described
Defoaming agent additional amount is the 55-65% of defoaming agent total amount.
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