CN109068629A

CN109068629A - Total preparation comprising plant growth regulator and oil and the method for making and using the preparation altogether

Info

Publication number: CN109068629A
Application number: CN201780020812.4A
Authority: CN
Inventors: R·布朗
Original assignee: Huntsman Corp Australia Pty Ltd
Current assignee: Indorama Ventures Oxides Australia Pty Ltd
Priority date: 2016-11-18
Filing date: 2017-10-12
Publication date: 2018-12-21
Also published as: EP3541183A4; JP2019535638A; WO2018090072A1; BR112018069842A2; AR110167A1; EP3541183A1; JP7015787B2; CA3017030A1; AU2017361105B2; AU2017361105A1; MX2018011686A

Abstract

A kind of agricultural preparation altogether, it includes: a effective amount of at least one plant growth regulator or at least one plant growth regulator and other bioactive ingredients, in the pulverised form of the average particle size with 1 to 12 micron range；At least one oil；At least one oil soluble surfactant dispersing agent；With at least one emulsifier, the wherein oil and one or more rheology modifiers and/or activator other by addition on demand, the ultimate density of at least one plant growth regulator or at least one plant growth regulator and other bioactive ingredients is optionally adjusted, so that the preparation altogether is substantially stable；And wherein the efficiency of the plant growth regulator is able to substantially maintain or improve；And one or more methods of the production preparation altogether.

Description

Comprising plant growth regulator and oily total preparation and make and use the total system The method of agent

Invention field

The present invention relates generally at least one plant growth regulator or at least one plant growth regulator and in addition Bioactive ingredients or their mixture and various oil total preparation, to form dispersion or oil based on agricultural oils Granular media.More particularly it relates to a kind of mixed containing plant growth regulator or plant growth regulator and herbicide The oil dispersion of object is closed, the oil dispersion is then used as defoliant.Hereinafter will relative to oil dispersion especially pair Cotton crop advantageously describes the present invention as the purposes of defoliant.It is, however, to be understood that the present invention is not limited only to the application.

Background of invention

The disleave of cotton crop is a kind of well determining practice commercially carried out for many years.Once disleave is drawn Hair, is mechanically just greatly facilitated to harvest cotton crop.It is most in chemicals used in the past, the practice Number realizes disleave by making plant be subjected to " biology suffer a shock ", and the biology shock leads to the freezing with chlorosis and as knot of leaf The plant burns of fruit.However, this handle the yield and quality for having adversely affected cotton crop.

Preferred practice is that pure disleave occurs, wherein only the leaf of plant is impacted and the rest part of plant is kept not It is undermined.Summarizing an example of this measure first is in U.S. Patent number 3,321,293 in 1967, and the patent describes Use the purine derivative of kinetin type, most preferably 6- anilino- purine.This compound is considered in a small amount of lower spy Not effectively any weeding seondary effect is not showed.

It has been subsequently found plant growth regulator, has especially delayed the effectiveness of those of specific nutrition growth characteristics, can have been used In the field of disleave.For example, thiadiazoles-urea derivative be used as plant growth regulator or with a kind of other plant growths The application that regulator combination is used as defoliant was described in U.S. Patent number 4,261,726 in 1981 by Schering AG first In.Based on this, in 1986, Schering AG was described in U.S. Patent number 4,613,354 by Thidiazuron and diuron group Share the defoliant composition being further improved.

The other improvement of the disleave efficiency of the basic mixture of Thidiazuron or the Thidiazuron combined with diuron is described in Such as in U.S. Patent number 6,274,535, improved wherein only being realized when these active constituents are combined with other insect disinfestation component Performance.

Not unexpectedly, seeking further efficiency or improvement always, so that modern agricultural chemicals meet For the needs of improved ecologicaI distribution, biopotency and/or economy.Thus, exploitation is preferably met in these requirements At least one and the benefit or the preparation and/or delivery system of advantage that continue to provide better than existing technologies there are corresponding need It wants.

Realize that a kind of Typical formulations layout strategy of this kind of requirement is combination or prepares agricultural chemicals altogether and/or specific match Auxiliary agent processed can be used alone in other ways.Primary logic is, meets one in the more effective way of above-mentioned requirements Kind, such as previously can be used as the agricultural chemicals of separated single delivery system application and/or the total preparation of specific formulation aid, A kind of preparation can be potentially served as to apply.This will lead to waste reduction, and labour input is reduced, reduced using complexity, and The benefit that may be cooperateed with about efficiency.

A kind of specific preparation type for being well suited for this delivery strategies is to disperse agricultural active solid in oil, Oil dispersed (hereinafter referred to as " OD ") concentrating agents or flowable (hereinafter referred to as " the OF ") concentrating agents of oily compatibility are formed, such as What the international trade association CropLife International for the agricultural synthesis company founded by 2001 was defined.In this feelings Key advantage under condition is, can usually apply in a usual manner as adjuvant as the oil or solvent of independent or independent spray oil It is included in composition itself.

The field of such preparation particularly disleave.For example, being discussed in U.S. Patent number 4,613,354 A possibility that mixture of preparation Thidiazuron or Thidiazuron and diuron, but the document also discloses that can include organic by addition The additive of solvent, wetting agent or oil improves the property and rate of the effect of given combination object.In multiple countries, it has been utilized This effect illustrated: not by changing specific defoliant composition via these components are added, and by for example may be used These components are applied to the pre- of pre-application and broadcast sowing mixture by commercially available spray oil form.Disleave is enhanced known to this measure Efficiency.

Although therefore will seem reasonably intuitively to go to attempt the total preparation of oil and defoliant with formed oil-based dispersions or OD, but well known by persons skilled in the art is that the nonaqueous dispersion of agrochemical active ingredient is notoriously difficult to stablize.It examines Considering has the associated main difficulty of the steady OD and OF preparation of system of viable commercial boundary of stability with exploitation, this Complicated preparation methodology and dedicated functional additive are generally required a bit.Therefore, it is typically selected for applying with successful formulation The relative simplicity of the most common delivery system of existing defoliant compares, develop this preparation it is not exclusively obvious and be also not with The process of intuition.This kind of common delivery system may include but be not limited to wettable powder, soluble powder, water dispersible Grain, water-soluble granular, dust, suspension concentrating agents, emulsifiable concentrating agents and lotion.

Due to commercial consideration will undoubtedly be extended to by developing the complexity of any OD or OF formulations Comparative traditional delivery methods, This unrealistic property of economy that will typically result in strength is asserted.For example, the business manufacture of OD preparation may be difficult and valuableness, together When special preparation component Cost comparisons' aqueous delivery system used in those may also be relatively high.Therefore, when assessment makes When being contemplated that benefit of the existing aqueous formulation being used in combination with oil base additive is used with OD or OF formulations Comparative, it would be possible to Only predict very little labour benefit, that is, need to handle a kind of product rather than two kinds.This leads to unrealistic property and even disadvantage Feel.

In addition, for most effective OD or OF preparation, the non-aqueous medium, preferably of significant concentration will be also preferably comprised Oil, wherein oil is bright relative to the remaining ingredient, the concentration of such as one or more emulsifying agents cosolvent for promoting preparation effectively to deliver It is aobvious higher.However, the oil, particularly mineral oil or base oil of high concentration are usually harmful to preparation stability, this is because its is low Polarity and the performance for influencing the function formulation aid such as dispersing agent and rheology modifier as a result.In addition, developing One of crucial predicament faced when OD preparation is that diluted surface-active is suitably stablized in permission in water before application Agent, particularly surfactant emulsifiers are often confrontation with stability.Which results in other unrealistic property, wherein developing Sufficiently stable OD preparation (promise by or close under allowable limit alloyd oil effective efficiency character) may be extremely difficult.

In fact, the present inventor makes thiadiazoles-urea plant growth regulator, such as Thidiazuron be suspended in desired richness Abnormal difficulty is suffered from terms of stablizing thiadiazoles-urea plant growth regulator, such as Thidiazuron when in oily carrier, wherein largely Wild effect often leads to the composition for being unsuitable for considering.Therefore, the present inventor attempts to prepare comprising plant growth regulator Available combination object.In addition, in the past, the mixture of Thidiazuron or Thidiazuron and diuron seems by inefficient application, and It has used more than amount needed for actually optimal efficiency, has generated waste.This has had not from the viewpoint of environment and economy The consequence of benefit.

Unexpectedly, inventor now discovered that a kind of method of the substantially stable and uniform preparation altogether of offer, described total The reduction of reactive compound amount needed for preparation has allowed the significant decrease and efficiency of total agricultural chemicals input, is especially used When in disleave application.It has been assumed that regardless of oil is the part applied as the total preparation for being diluted to spray liquid, or as independent Spray oil composition and another composition containing defoliant be applied in spray liquid jointly, the difference of disleave rate and efficiency It is different by very little.From above-mentioned this improved synergistic effect unpredictable in the prior art.This reduction is provided about reduction agriculture The advantages of with chemicals footprint.

The present invention attempts some in the shortcomings that overcoming or at least substantially improveing the prior art and shortcoming.

Summary of the invention

According to the present invention, a kind of agricultural preparation altogether is provided, it includes:

I) a effective amount of at least one plant growth regulator or at least one plant growth regulator and other biology Active constituent, in the pulverised form of the average particle size with 1 to 12 micron range；

Ii) at least one oil；

Iii) at least one oil soluble surfactant dispersing agent；And

Iv) at least one emulsifier,

The wherein oil and one or more rheology modifiers and/or activator other by addition on demand, optionally to adjust Whole at least one plant growth regulator or at least one plant growth regulator and other bioactive ingredients it is final dense Degree, so that preparation is substantially stable altogether；And wherein the efficiency of plant growth regulator is able to substantially maintain or improve.

The form of total preparation of the invention can be selected from oil dispersed (" OD ") concentrating agents, oily compatibility flowable (" OF ") is concentrated Agent, Oil-based Suspension concentrating agents (" SC ") or oil base suspoemulsion (" SE ").When being used for disleave purpose, preparation is that oil base dispersion is dense altogether Contracting agent, i.e. OD preparation.

Term " effective quantity " mean to be sufficiently used for enhancing plant growth, yield and/or vigor and cannot cause to plant or The amount of the component of preparation altogether according to the present invention of phytotoxic any discernable symptom of crop.The visual plant of this amount or Included component in the type of crop, weather conditions and preparation altogether according to the present invention and change in a wide range.The amount can It is measured by the systemic field test in those skilled in the art's limit of power.

As it is used herein, term " plant growth regulator " includes with dosage-dependent manner in plant organ quantity Adjust the compound that aspect causes response.Plant organ quantity adjusts the enhancing or suppression for referring to plant organ growth or development System.Inhibit to be retardance or partial block completely.For example, plant organ quantity adjust can be related to branch inhibition or root formed Enhancing.Branch means the process that axillary bud or adventitious bud are grown, and results in nutrition branch, flower or inflorescence.Inhibition means permanent or temporary When check bud growth or inhibit root formation.Inhibit be complete (by influencing all axillary bud/adventitious buds) or partial (only influencing axillary bud/adventitious bud subset).

The example of plant growth regulator that can be used according to the invention includes but is not limited to: anti-auxin, and such as drop is solid Tri--iodo-benzoic acid of alkyd or 2,3,5-；Auxin, such as 4-CPA, 2,4-D, 2,4-DB, 2,4-DEP, 2,4- drop propionic acid, 2,4, 5- tears propionic acid, IAA, IBA, naphthalene acetamide, α-naphthylacetic acid, 1- naphthols, naphthyloxyacetic acid, cyclic potassium naphthenate, sodium naphthenate, 2,4,5-T； The basic element of cell division, such as 2iP, benzyladenine kinetin, zeatin；Defoliant, such as nitrolim, dimethipin, endothal, Ethephon (CEPHA),2-(chloroethyl) phosphonic acid, merphos, metoxuron, pentachlorophenol, Thidiazuron, De-Green；Ethylene inhibitor, such as tetraestrone (aviglycine) and 1- methyl cyclopropene；Ethylene evolution agent, such as ACC, ethylene silicon, ethephon (CEPHA),2-(chloroethyl) phosphonic acid and glyoxime；Growth inhibition Agent, such as abscisic acid, ancymidol, butralin, sevin, chlorphonium, chlorpropham, dikegulac, flumetralim, fluoridamid, Adjust phosphine, glyphosine, the phonetic propyl alcohol of benzene (isopyrimol), jasmonic, maleic acid hydrazide, first piperazine, the strong element of piperazine, jasmone, aniline Spirit, 2,3,5- tri--iodo-benzoic acids；Morphactin, such as chlorine fluorenes carboxylic acid, Chlorflurecol, two Chlorflurecols, Florencol；Growth retardant/tune Section agent, such as cycocel, daminozide, flurprimidol, mefluidide, paclobutrazol, cyproconazole, tetcyclacis, uniconazole P, ancymidol are anti-fall Ester and progexadione-CA；Growth stimulant, such as brassin lactones, chloropyuril, hymexazol, 2-amino-6-oxypurine Derivative, indolone derivatives, 3,4- disubstituted maleimides derivatives and condensed azatropylidene ketone derivatives.The term is also Including other active constituents, such as fluorine sulfanilamide (SN) grass, special gram grass, carvol, benzene cyanogen butyramide, benzene pyridazine, cloxyfonac, cyclopropionate acyl Amine, cycloheximide, love increase beautiful (epocholeone), 'Inshuzhi ', ethylene, pyridazine ketone acid, heptopargil, and chloroethene sulfinic acid is anti-fall Amine, Ka Tazan (karetazan), lead arsenate, methasulfocarb adjust naphthenic acid, than reaching agriculture, sintofen, triapenthenol and TrinexAN_SNacethyl. Plant growth regulator, plant stimulants derived from indolone described in such as WO 2005/107466；WO 2005/ 3,4- disubstituted maleimides derivative described in 107465；Condensed azatropylidene described in WO 2005/107471 Ketone derivatives；And 2-amino-6-oxypurine derivative described in WO 2005/107472 is also included in the term.

Term " plant " mentioned in this article or " crop " can be any plant or crop, especially agriculture of plantation or cultivation Crop, garden crop or afforestation crop, and it is highly preferred that vegetable lamb, including Transgenic cotton plants.

According to a preferred aspect of the present invention, plant growth regulator is Thidiazuron.In the particularly preferred of total preparation In embodiment, Thidiazuron with 1 to 500g/L or more preferable 1 to 250g/L or more preferable 1 to 200g/L or more preferable 1 to 150g/L or more preferable 1 to 120g/L or more preferable 1 to 100g/L or more preferable 1 to 80g/L or more preferable 1 to 50g/L, Or more preferable 1 to 30g/L or more preferable 1 to 20g/L or more preferable 50 to 100g/L or more preferable 50 to 150g/L, or more It is preferred that 100 to 150g/L or more preferable 100 to 200g/L or more preferable 150 to 250g/L concentration range exists.Optimal In the form of choosing, Thidiazuron exists with 60 to 120g/L concentration range, and most preferably, exists with the concentration of 100g/L.? In the case that plant growth regulator is not Thidiazuron, plant growth regulator with 1 to 500g/L or more preferable 1 to 200g/L, Or more preferable 1 to 120g/L, or exist even more preferably from 1 to 100g/L concentration range.

In another preferred form of the invention, preparation also includes that at least one other biology selected from the following is living altogether Property ingredient: fungicide, insecticide, herbicide, acaricide, nematicide, invertebrate poison, algicide, or kill harmful life Agent or their any mixture.In comprising Thidiazuron and one or more other bioactive ingredients listed above Any one or more combinations any preparation is when being included within the scope of the disclosure altogether, in a preferred shape of the invention In formula, preparation includes the Thidiazuron combined with fungicide altogether.In another preferred form, preparation includes and insecticide group altogether The Thidiazuron of conjunction.In another preferred form, preparation includes the Thidiazuron combined with acaricide altogether.In another preferred form In, preparation includes the Thidiazuron combined with nematicide altogether.In another preferred form, preparation includes and kills mollusk altogether The Thidiazuron of agent combination.In most preferred form of the invention, preparation includes the Thidiazuron with combinations of herbicides altogether.

In the particularly preferred embodiment of total preparation, bioactive ingredients in addition with 1 to 250g/L, or more preferably 1 to 100g/L or more preferable 1 to 80g/L or more preferable 1 to 60g/L or more preferable 1 to 50g/L or more preferable 1 to 30g/ L or more preferable 1 to 20g/L or more preferable 80 to 100g/L or more preferable 50 to 100g/L or more preferable 50 to 80g/L, or More preferable 30 to 50g/L or more preferable 20 to 30g/L concentration range exists.The concentration of other bioactive ingredients is optimal Choosing is respectively selected from 48,30 or 15g/L.In most preferred form, bioactive ingredients in addition exist with the concentration of 30g/L.

In the case where other bioactive ingredients are preferably at least a kind of herbicide, it can be selected from but be not construed as It is confined to: dinitraniline weedicide；Diphenyl ether herbicide；Aryloxyphenoxypropionate herbicide；And including Atrazine, the phonetic sulphur of cigarette Grand, azoles humulone, quinclorac, 2,4-D, quizalofop-ethyl, benfluralin, bentazone, prometryn, mesotrione, flumioxazin, different evil grass Pine, ethalfluralin, napropamide, diquat dibromide, S-metolachlor, ametryn, dimethenamid, fluazifop, ethoxy fluorine Careless ether, paraquat, topramezone, diuron, pentyl xanthate, alachlor, tembotrions, linuron, rimsulfuron, sethoxydim, Dissipate phosphorus, pendimethalin, pyrazon, cycloate, glyphosate, maleic acid hydrazide, halosulfuronmethyl, n-nonanoic acid, clethodim, metribuzin, sulfone Sulfometuron Methyl, terbacil, ethalfluralin, phenmedipham, clopyralid, the combination of clomazone and ethalfluralin, MCPB, gram Grass enemy, trefanocide or their any mixture.Including any kind of combination in Thidiazuron and herbicide listed above When any total preparation is included within the scope of the disclosure, in most preferred form, herbicide is diuron.

When total preparation includes the combination of Thidiazuron and diuron, Thidiazuron is preferably deposited with 1 to 250g/L concentration range Or more preferable 1 to 200g/L or more preferable 1 to 100g/L or more preferable 1 to 80g/L or more preferable 1 to 50g/L, or more It is preferred that 1 to 30g/L or more preferable 1 to 20g/L, and most preferably, exist with the concentration of 60g/L；And diuron is preferably with 1 Concentration range presence to 250g/L or more preferable 1 to 100g/L or more preferable 1 to 80g/L or more preferable 1 to 60g/L, or More preferable 1 to 50g/L or more preferable 1 to 30g/L or more preferable 1 to 20g/L or more preferable 50 to 80g/L or more preferable 30 To 50g/L or more preferable 20 to 30g/L.The concentration of diuron is most preferably respectively selected from 48,30 or 15g/L.In most preferred shape In formula, diuron exists with the concentration of 30g/L.

It is present in total preparation of the invention in Thidiazuron itself or while combining with the diuron as bioactive ingredients In the case where, when compared with the existing defoliant used according to existing disleave practice, it has been found that preparation exhibits go out to crop altogether Unexpected collaboration disleave efficiency.

For the purpose of ensuring that with substantially stable form maintain dispersion concentration agent purpose, it is necessary to via for example crush or it is other Mode is finely divided by plant growth regulator and/or active constituent.In order to crush even more thin particle size range, machine can be used Device such as ball mill, vertical roll grinder, hammer-mill, roller press or high compression roller mill, vibrating mill, jet mill and analog. For the still thinner granularity of sometimes referred to as " extra-fine grinding ", profession grinding machine can be used.To at least one plant of the invention It is micro- that the crushing that growth regulator or at least one plant growth regulator and other bioactive ingredients carry out generates 1 to 12 The average particle size of the component of rice or more preferable 1 to 8 micron or even more preferably 1 to 6 micron range.It is of the invention most preferably In embodiment, it can be supplied via horizontal mill, such as by the Engineered Mills company of Illinois, Grayslake Grinding machine, crushed using wet grinding, to generate the total preparation with average particle size (d0.5) less than 5 microns, Middle grain size analysis is measured by micro- approximation method or using suitable grinding rule or Hegman rule.

At least one oil for forming the continuous phase of preparation altogether is preferably selected from paraffin oil, such as kerosene, for example, being purchased from The ExxonMobil Chemical company of Texas, SpringOne of D series；It is purchased from South Korea head Your SK company It is purchased from Caltex's12；It is purchased from Huntsman company1555 solvent of AG；Seed oil, such as methyl oleate and ethyl ester, methyl soyate and ethyl ester and they Corresponding fatty acid；Aromatic hydrocarbon, such as alkylbenzene and alkylnaphthalene are such as purchased from ExxonMobil Chemical company150；Polyalkylene glycol ethers；Fatty acid diesters；Fatty alkyl amide or diamides；Two alkylidene carbon Acid esters；Ketone；Alcohol；Or their any mixture.In most preferred form of the invention, at least one oil is selected from such as by corresponding viscous Spend any 2 or 3 class base oils of Index Definition.In preferred embodiments, at least one oily with 1 to 700g/L, or more preferably 100 to 700g/L or more preferable 100 to 450g/L or more preferable 100 to 300g/L or more preferable 1 to 450g/L, or it is more excellent Select 300 to 450g/L, or even further preferably, 450 to 700g/L concentration range come using.In the most preferred embodiment In, it is at least one oil with greater than 500g/L concentration come using.

Assist at least one oil soluble surfactant dispersing agent for making dispersion concentration agent be maintained at substantially stable form Addition be preferably selected from fatty acid-polyalkylene glycol condensation product, such as2510 dispersing agents；Or it is poly- Amine-fatty acid condensates, such as4850 dispersing agents or4890 dispersing agents； Random polyester condensation object, such as2520 dispersing agents；With the salt of polyolefin condensation product, such as2422 dispersing agents, the dispersing agent are the product of Huntsman company.It is highly preferred that at least one Kind dispersing agent is the condensation product of the reaction of polyalkylene glycol or polyalkylene glycol ethers and fatty acid, such as2510 dispersing agents, or random polyester condensation object, such as2520 dispersions Agent.Surfactant-dispersed agent with 1 to 70g/L or more preferable 1 to 40g/L or more preferable 40 to 70g/L or more preferable 1 to The concentration range of 15g/L come using.Term " condensation product " used herein refers in the retraction for eliminating water or small molecule Close the reaction product of reaction or the reaction product of addition reaction.

Total preparation of the invention further preferably includes at least one rheology modifier, to overcome finely divided plant growth regulating Agent itself or with when active ingredient combinations or strong trend that dispersed phase is settled or consolidated as time goes by.Rheology modifier with 1 to 20g/L or more preferable 1 to 15g/L or more preferable 1 to 10g/L or more preferable 1 to 5g/L amount come using.If necessary If, at least one rheology modifier is preferably selected from both fumed silica, hydrophobic and hydrophilic variant, such as by EVONIK'sOne kind that series provides；Gelling clay, such as by's One kind that the hydrophobic member of series provides, and more specifically,38 (hectorite of hydrophobically modified is viscous Soil) orSD-1 (the bentonite organic derivative of hydrophobically modified)；Other fat of triglycerides or glycerol Acid esters；Rubber-type copolymer, it is such as commercially available especially containing one kind of styrene residue, such as styrene-butadiene copolymer From KRATON companyG1701；And copolymer, block or in other ways, such as polyester and/or poly- Amide.It is highly preferred that rheology modifier isSD-1, or even further preferably, SD-1 (the bentonite organic derivative of hydrophobically modified) andThe combination of 200 (hydrophilic fumed silicas),SD-1 with 1 to 20g/L amount come using or more preferable 1 to 15g/L or more preferable 1 to 10g/L；200 with 1 to 40g/L amount come using or more preferable 1 to 20g/L or more preferable 1 to 10g/L, or it is more excellent It selects 1 to 5g/L.

Using rheology modifier, preparation also may include at least one second activator to generate optimality altogether Energy.The second activator include gelling clay in the case where, it may be desired to addition include water, methanol, ethyl alcohol, propene carbonate or it Any mixture polar solvent.In addition, preparation can further preferably comprise at least altogether using rheology modifier A kind of second activator is to promote the rheology modified performance being highly improved.

Preparation is such as purchased from preferably also comprising at least one inert solid fillers, including but not limited to titanium dioxide altogether The TIONA 625 and the inactive phyllosilicate of one or more rheologies of CRISTAL Global, can also act as helping to stablize The activator of preparation altogether.

Because total preparation of the invention exists as the continuous phase in one or more oil, the selection of emulsifier some It is dominated by the type for the one or more oil for being used as continuous phase.In general, with low hydrophobic-lipophobic balance (" HLB ") Emulsifier is most suitable.10 are usually less than for HLB needed for most of oily phases used in the present invention altogether preparation.This cream Agent is preferably selected from one or more alkoxy fatty alcohols, and one or more Isosorbide Dinitrates are corresponding with its a kind of or more Kind ethoxylate, the fatty acid of one or more ethoxylations, the castor oil of one or more ethoxylations, alkyl benzene sulphonate Calcium and ammonium and alkylammonium salt, one or more salts of alkyl sulfosuccinates salt, one or more ethylene oxide-propylene oxide blocks The alkyl phenol of copolymer, the alkylamine of one or more ethoxylations and one or more ethoxylations or any of theirs mix Close object.

When total preparation include Thidiazuron or combined with diuron Thidiazuron when, at least one emulsifier be most preferably selected from Under group: castor oil ethoxylate, especially3201 emulsifiers,3512 emulsifications Agent；Alcohol ethoxylate, especially12A3N, 12A4N, 13A7,13A9,17A2 and TDA-6；Alcohol alkoxylates, such as5429,5459 and 5500；Fatty acid ethoxylate, such asOF6；Isosorbide Dinitrate ethoxylate, such asT85；Sulfosuccinate/ester, Such as3665 emulsifiers, the person are purchased from Huntsman company；And the amine of dodecyl benzene sulfonic acid And calcium salt, such as it is purchased from INNOSPEC companyThe product of EVM series.Most preferred emulsifier includes 12 Any or any group of the calcium salt of alkyl benzene sulphonate, at least one alcohol alkoxylates and Isosorbide Dinitrate ethoxylate It closes, in an amount of from 1 to 300g/L or more preferable 1 to 250g/L or more preferable 1 to 175g/L or more preferable 1 to 150g/L, or more It is preferred that 175 to 250g/L or more preferable 150 to 175g/L or more preferable 100 to 150g/L or more preferable 1 to 100g/L.

Because total preparation of the invention exists as the continuous phase in one or more oil, (it can also be such as by one or more The presence of emulsifier promotes to be diluted in water), so the present invention can be also comprising helping to make the pre- aqueous dispersion dimension broadcasted sowing It is held in water soluble surfactant active's dispersing agent of substantially stable form.If necessary, at least one soluble surface is living Property agent dispersing agent is preferably selected from but is not limited to the sodium or ammonium salt of alkylnaphthalene sulfonate formaldehyde condensation products, such as2020；Sodium, calcium and the ammonium salt of lignosulfonic acid；The sodium or ammonium salt of copolymer, such as2700；Sulfonate/ester of isopropylbenzene or dimethylbenzene, is such as purchased from INNOSPEC company The product of ELTESOL SC or SX series.

The scope of the present invention also extends to a kind of method for preparing total preparation of the invention, and the method includes following steps Suddenly, it wherein step c) and can d) carry out in any order or simultaneously:

A) by least one plant growth regulator or at least one plant growth regulator and other bioactivity at Divide and crush, to realize the average particle size of 1 to 12 micron range；

B) by stirring or high shear mixing, at least one plant growth regulator crushed at least one oil addition, Or at least one plant growth regulator and other bioactive ingredients, to generate oil dispersion；

C) at least one oil soluble surfactant dispersing agent is added to oil dispersion；

D) at least one emulsifier is added to oil dispersion；Optionally

E) with stirring, the temperature of oil dispersion is adjusted between about 60 DEG C and 70 DEG C；And optionally

F) oil and one or more rheology modifiers and/or activator other by addition on demand, to adjust dispersion At least one of plant growth regulator or at least one plant growth regulator and other bioactive ingredients it is final dense Degree, so that preparation is substantially stable altogether.

The scope of the present invention also extends to a kind of alternative for preparing total preparation of the invention, and the method includes following Step wherein step e) and can f) carry out in any order or simultaneously:

A) at least one rheology modifier and at least one oil are combined；

B) by stirring or high shear mixing, to the oil from step a) add at least one plant growth regulator or At least one plant growth regulator and other bioactive ingredients, to generate oil dispersion；

C) at least one activator is added, stablizes sexual behaviour further to generate the expectation of oil dispersion；

D) oil dispersion of step c) is crushed, with realize 1 to 12 micron range at least one plant growth regulator, Or the average particle size of at least one plant growth regulator and other bioactive ingredients；

E) at least one oil soluble surfactant dispersing agent is added to oil dispersion；

F) at least one emulsifier is added to oil dispersion；Optionally

G) with stirring, the temperature of oil dispersion is adjusted between about 60 DEG C and 70 DEG C；And optionally

H) oil and one or more other rheology modifiers and/or activator other by addition on demand, to adjust At least one of dispersion plant growth regulator or at least one plant growth regulator and other bioactive ingredients Ultimate density, so that preparation is substantially stable altogether.

The scope of the present invention extends to another preferred method for preparing total preparation of the invention, and the method includes following Step:

A) at least one oil soluble surfactant dispersing agent is added at least one oil；

B) by stirring or high shear mixing, at least one plant growth regulator or at least one plant are added to oil Growth regulator and other bioactive ingredients, to generate oil dispersion；

D) oil dispersion of step c) is crushed, with realize 1 to 12 micron range at least one plant growth regulator, Or the average particle size of at least one plant growth regulator and other bioactive ingredients；Optionally

F) by adding other oil, at least one emulsifier and one or more rheology modifiers and/or at least on demand A kind of others activator, to adjust at least one of dispersion plant growth regulator or at least one plant growth regulating The ultimate density of agent and other bioactive ingredients, so that preparation is substantially stable altogether.

In most preferred form, the present invention provides a kind of method for preparing substantially uniform stable total preparation, institute The method of stating includes the following steps, wherein step a) to d) step e) to g) before or after and carried out before step h):

A) at least one oil soluble surfactant dispersing agent is added to the first oil of at least one；

B) using stirring or high shear mixing, a effective amount of at least one plant growth regulator or extremely is added in the oil Few plant growth regulators and other bioactive ingredients, to generate oil dispersion；

D) oil dispersion of step c) is crushed, to generate substantially uniform first dispersion concentration agent, wherein at least one Plant growth regulators or at least one plant growth regulator and other bioactive ingredients have 1 to 12 micron of model The average particle size enclosed；

E) it by stirring or high shear mixing, disperses at least one rheology modifier at least one second oil, with Form the second substantially uniform dispersion concentration agent of gel form；

F) using continuously stirring or high shear mixing, at least one solvent is added to the second dispersion concentration agent and is improved with being formed Gel；

G) it by stirring or high shear mixing, disperses at least one oil soluble surfactant dispersing agent or emulsifier in In improved gel, to form the second substantially uniform dispersion concentration agent；

H) under low shear mixing, at least one other rheology modifiers are added to form premix to the gel of step g) Carrier；And

I) a certain amount of first dispersion concentration agent is added to obtain substantially uniform stabilization to a certain amount of premix carrier Total preparation.

It is worth noting that, once having added emulsifier, then occurs improved gel in step f).The improvements of gel It is, while it maintains similar rheology character, is easier to handle, having allows more preferably to mix in step (i) More low viscosity.The second stable dispersion concentration agent is thermodynamically also preferably formed, this helps to substantially avoid to abrasive material The unwanted seondary effect of pre-composition addition concentration emulsifier.

The scope of the present invention also extend to it is a kind of by the present invention altogether formulation application in the method for the crop for needing disleave, therefore It is expected that by least one plant growth regulator or at least one plant growth regulating combined with other bioactive ingredients The synergistic benefits that agent and at least one oil are prepared altogether can produce the benefit about improved formulation efficiency and biopotency.More specifically For, the inventor has discovered that when being used as defoliant, using total preparation of the invention in crop and especially cotton crop Disleave efficiency is set to be maintained or generate improvement.

It has been found that due to total preparation of the invention delivering or application improved, need with regard to itself or with other life The plant growth regulator of object active ingredient combinations is less.In addition, total preparation of the invention eliminates point such as carried out in the past Do not apply or mix the needs of at least one plant growth regulator and/or at least one active constituent, this from processing and it is easy-to-use It is advantageous from the point of view of property viewpoint.Combined due at least one plant growth regulator or with other bioactive ingredients to Therefore existing synergistic effect between few plant growth regulators and at least one oil, the present invention are produced and are substantially improved Disleave efficiency.

The scope of the present invention and discovery, which are not limited only to for oil-based dispersions to be total to preparation, to be used to take off such as cotton crop Leaf purpose.It is expected that synergistic effect shown by the composition is also transferred to more extensive and less specific pesticides Using.These include but is not limited to that application contains plant growth regulator, fungicide, Insecticides (tech) & Herbicides (tech), acaricide, kills The Oil-based Suspension of nematode agent, invertebrate poison, algicide or other pesticides or their any mixture is made altogether Agent

It is described below and only relates to specific embodiment of the invention, and be never intended to the scope of the present invention being defined in that A little specific embodiments.It is illustrative and not restrictive specifically, being described below.Need not necessarily depart from essence of the invention to institute The change and modification of published method can will be apparent to those skilled in the art.

Brief Description Of Drawings

In order to be understood that the present invention and actually come into force, Fig. 1 shows the knot of the flow assessment carried out to specific embodiment Fruit, it is described to go out to be attributed to the instable rheological charactristics of dispersion as the result is shown.This unstability has been associated with to by complete The other catastrophic wild effect that example of formulations shows altogether, and highlight it is provided by the present invention unexpectedly manage with That reduces these challenges does not need significantly improving for effect.

Detailed description of the invention

It include now Thidiazuron as plant growth regulator or Thidiazuron as plant growth regulator using Primary Reference Preparation is total to describe the present invention as the oil base of bioactive ingredients with diuron.It is expected that in oil-continuous phase it is insoluble its Its suspension formulation of solid-state plant growth regulator or bioactive ingredients in oil can find similar result.

When total preparation includes the Thidiazuron with regard to itself in oil, Thidiazuron is most preferably with 1 to 250g/L concentration model Presence or more preferable 1 to 200g/L or more preferable 1 to 100g/L or more preferable 1 to 80g/L or more preferable 1 to 50g/L are enclosed, Or more preferable 1 to 30g/L or more preferable 1 to 20g/L, and most preferably, exist with the concentration of 60g/L.

In most preferred form of the invention, at least one oil is the 3 class bases with the viscosity index (VI) between 110 and 120 Plinth oil, with 450 to 700g/L concentration range come using.

At least one oil soluble surfactant dispersing agent be most preferably polyalkylene glycol or polyalkylene glycol ethers and The condensation product of the reaction of fatty acid, such as2510 dispersing agents, or random polyester condensation object, such as2520 dispersing agents, the dispersing agent with 1 to 70g/L concentration range come using or more preferable 1 to 40g/L or more preferable 40 to 70g/L or more preferable 1 to 15g/L.

At least one emulsifier needed for total preparation comprising Thidiazuron or Thidiazuron and diuron is most preferably selected from following Group: Isosorbide Dinitrate ethoxylate, especially ECOTERIC^TMT85 fatty acid ethoxylate；Alcohol alkoxylates, Such as3201,5429,5459 and 5500 emulsifier；Alcohol ethoxylate, especially12A3N With13A7 fatty acid ethoxylate, the most of of the person are purchased from Huntsman company；And dodecane The amine and calcium salt of base benzene sulfonic acid, such asThe surfactant product of EVM series, and more preferably EVM 70/2E surfactant.Most preferred emulsifier is at least one or any calcium salt of dodecyl benzene sulfonic acid, at least one The combination of kind alcohol alkoxylates and Isosorbide Dinitrate ethoxylate, respective amount are 1 to 175g/L.

In the case where needing rheology modifier, the most preferably bentonite organic derivative of hydrophobically modified, i.e.,SD-1, or the bentonite organic derivative, i.e. of more preferably hydrophobically modifiedSD-1 and Hydrophilic fumed silica200 combination,SD-1 is made with 1 to 20g/L amount With or more preferable 1 to 15g/L or more preferable 1 to 10g/L；200 are most preferably made with 1 to 20g/L amount With.

The second activator that further improvement performance can be needed to generate is most preferably selected from gelling clay, can also need to add packet Include the polar solvent of water, methanol, ethyl alcohol, propene carbonate or their any mixture.

Embodiment brief description

Typical oil powder preparation known in the art has composition described in following Table A.

Typical component needed for Table A-oil powder preparation:

* wherein the total amount of all components adds up to 100%.

Embodiment 1- comparing embodiment A

The following table 1 provides the embodiment of the typical commercial aqueous suspension concentrating agents (" SC ") containing Thidiazuron:

Table 1

Component	g/L
		Thidiazuron	500
One or more dispersing agents	10–50
		One or more wetting agents	10–20
Wetting agent	50–100
		Defoaming agent	1–10
Xanthan gum	0.1–0.5
		Biocide	0.05–0.25
Water	To volume (To volume)

This preparation will be prepared in a manner familiar to those skilled in the art.

Embodiment 2- comparing embodiment B

The following table 2 provides the embodiment of the commercially available aqueous suspension concentrating agents (" SC ") containing diuron and Thidiazuron:

Table 2

Component	g/L
		Diuron	60
Thidiazuron	120
		One or more dispersing agents	10–50
One or more wetting agents	10–20
		Wetting agent	50–100
Defoaming agent	1–10
		Xanthan gum	0.1–0.5
Biocide	0.05–0.25
		Water	To volume

The initial embodiment of total preparation embodiment 3- of the invention, and illustrate at the scene

The Oil-based Suspension for preparing diuron and Thidiazuron according to the present invention as follows is total to preparation:

Table 3

Firstly, via SILVERSON high-shear mixer, by by 10g38 (ELEMENTIS) points It dissipates in 86.66gIn, come prepare activation hydrophobically modified hectorite premix ' masterbatch '.With continuous Shearing adds 3.34g to gained homogeneous dispersionAG 1555, until obtaining uniform spawn. It is left unused.

It then, will be the desired amount of according to table 32510 dispersing agents, which are dissolved in, will allow 7% (weight Measure weight ratio) left and right Thidiazuron concentration it is a certain amount ofIn.Then it uses under high shear SILVERSON mixer disperses diuron and Thidiazuron technology pure (technical) in gained mixture.It is straight to continue this measure To the uniform mixture of acquisition.

Then this slurries are crushed to generate containing average particle size using horizontal mill (Engineered Mills company) (d0.5) concentrating agents of the component less than 5 μm.Grain size analysis is measured by micro- approximation method.

It is added to concentrating agents3201 emulsifiers,EVM 70/2E surfactant,The pre-prepared rheology modifier of 5459 emulsifiers and such as above-mentioned preparation, followed by surplusThen gained oil-based suspension is homogenized via down to moderate shear mixing.Then composition is observed To the satisfactory stability of displaying and dilution behavior.This is also the example for adding the methodology of rheology modifier after being pulverized.

The more high load variant of embodiment 4- embodiment 3, and illustrate at the scene

Table 4

It, will be the desired amount of according to table 42510 dispersing agents, which are dissolved in, will allow 12% (weight weight Than) left and right Thidiazuron concentration it is a certain amount ofIn.Then it is mixed under high shear using SILVERSON Device by diuron and Thidiazuron technology it is pure be scattered in gained mixture in.Continue this measure until obtaining uniform mixture.

Then this slurries are crushed using horizontal mill (Engineered Mills company).The process is related to concentrating agents It is slowly fed into so that in the milling apparatus of 500 to 1000RPM low rotation speed operation, wherein preload has grinding machine grinding chamber The glass of 1 to 1.6mm diameter of 60 to 80% total volume capacities or more preferably zirconium silica dioxide medium, and collet coolant Temperature is predetermined and is maintained at a temperature of 15 to 25 DEG C of external control.Rotation speed is slowly improved by 2000 to 2500RPM Continue 30 to 45 minutes periods, to generate the concentrating agents with substantially 5 μm of average particle sizes (d0.5), the granularity is by making With the approximation method measurement of 0 to 100 grinding rule or 8 to 0 Hegmans rule.Grain size analysis is measured additionally by micro- approximation method.

It is added to concentrating agents3201 emulsifiers andEVM 70/2E surfactant and Pre-prepared rheology modifier (described in embodiment 3), followed by surplusThen via in Etc. shear-mixeds gained oil-based suspension is homogenized.Then composition shows to show satisfactory stability and dilution row For.This is another embodiment for adding the methodology of rheology modifier after being pulverized.

The embodiment of embodiment 5- only Thidiazuron, and illustrate at the scene

The Oil-based Suspension for preparing Thidiazuron according to the present invention as follows is total to preparation:

Table 5

It, will be the desired amount of according to table 52510 dispersing agents, which are dissolved in, will allow 17 to 18% (weight Weight ratio) left and right Thidiazuron concentration it is a certain amount ofIn.Then SILVERSON is used under high shear Mixer by diuron and Thidiazuron technology it is pure be scattered in gained mixture in.Continue this mixing until obtaining uniform mixing Object.

Then this slurries are crushed using horizontal mill (Engineered Mills company).The process is related to concentrating agents It is slowly fed into so that in the milling apparatus of 500 to 1000RPM low rotation speed operation, wherein preload has grinding machine grinding chamber The glass of 1 to 1.6mm diameter of 60 to 80% total volume capacities or more preferably zirconium silica dioxide medium, and collet coolant Temperature is predetermined and is maintained at a temperature of 15 to 25 DEG C of external control.Rotation speed is slowly improved by 2000 to 2500RPM Continue 30 to 45 minutes periods, generates the concentrating agents with substantially 5 μm of average particle sizes (d0.5), the granularity is by using 0 To the approximation method measurement of 100 grinding rule or 8 to 0 Hegmans rule.In addition grain size analysis is measured by microscopy, wherein dispersing body display The weak active constituent crystal to moderate flocculates out.

It is added to concentrating agents3201 emulsifiers,EVM 70/2E surfactant and such as Pre-prepared rheology modifier described in embodiment 3, followed by surplusThen via down to medium Gained oil-based suspension is homogenized by shear-mixed.Then composition, which is observed, shows satisfactory stability and dilution row For.This is another embodiment for adding the methodology of rheology modifier after being pulverized.

Embodiment 6

The complete Oil-based Suspension that following preparation is used to prepare Thidiazuron according to the present invention is total to the abrasive material concentrating agents in preparation:

Table 6

It, will be the desired amount of according to table 64850 dispersing agents are dissolved in a certain amount of premixingIn SOLVESSO 150.Then use SILVERSON mixer by Thidiazuron technology under high shear It is pure to be scattered in gained mixture.Continue this measure until obtaining uniform mixture.

Embodiment 7

Table 7

It, will be the desired amount of according to table 72510 dispersing agents are dissolved in a certain amount of premixingIn SOLVESSO 150.Then use SILVERSON mixer by Thidiazuron technology under high shear It is pure to be scattered in gained mixture.Continue this measure until obtaining uniform mixture.

Embodiment 8

Table 8

It, will be the desired amount of according to table 82520 dispersing agents are dissolved in a certain amount of premixingIn SOLVESSO 150.Then use SILVERSON mixer by Thidiazuron technology under high shear It is pure to be scattered in gained mixture.Continue this measure until obtaining uniform mixture.

Embodiment 9

Table 9

It, will be the desired amount of according to table 94890 dispersing agents are dissolved in a certain amount of premixingIn SOLVESSO 150.Then use SILVERSON mixer by Thidiazuron technology under high shear It is pure to be scattered in gained mixture.Continue this measure until obtaining uniform mixture.

Embodiment 10

Table 10

According to table 10, to a certain amount ofIt adds the desired amount of3201、EVM70/2E and13A7.Then use SILVERSON mixer by thiophene benzene under high shear Grand technology is pure to be scattered in gained mixture.Continue this measure until obtaining uniform mixture.

Embodiment 11- compares rheologicai evaluation

The basic rheology inspection of embodiment 6 to 10 is passed through to these simple abrasive material concentrating agents progress analytic explanations Stablize associated abnormal difficulty with Thidiazuron.It is smart when the data highlight in the oil base carrier for being suspended in preferred concentration The dispersed phase opened is segmented there are inherent instability, and should usually assist that dispersion concentration agent is made to be maintained at substantially stable form Various Common surface activating agent dispersing agents there are unrelated.The present inventor has been inferred to observe in abrasive material concentrating agents this Latent instability is instable primary source in the complete preparation altogether comprising Thidiazuron and desired oil.

Flow assessment

40mm slab geomitry shape, 150 μm of gaps, 25 DEG C, 0.1- are used on Malvern Kinexus Pro rheometer 1.0s^-1The basic flow measurement (logarithmic table) of progress is shown in lower Fig. 1, shows embodiment 6,7 and the reality in lesser degree It applies total preparation exhibits described in example 10 and is attributed to the instable rheological charactristics of dispersion, such as about 1-100Pa's is low Shear viscosity.

Embodiment 8 shows to be markedly improved, and wherein initial measurement shows only lesser in surveyed range of shear rate The Viscosity readings of thixotropy and < < 1Pa.However, after 6 days, embodiment 8, which shows to show, identical goes opening for stabilization Begin, there is viscosity or shear viscosity close to 1Pa close to 1000 times of raising.

Embodiment 10 is unusual embodiment, further improved dispersion stabilization is highlighted, wherein showing shortage Thixotropy and the variation of time dependence rheology.However, this further improvement is unexpectedly being used to prepare complete group Close object in when do not show benefit, such as illustrated by embodiment 20, therefore highlight further unprecedented complexity.

Improvement of the embodiment 12- to embodiment 4

Table 12

It, will be the desired amount of according to table 1238 be added to it is a certain amount of Wherein The latter is equal to the amount for the Thidiazuron concentration for allowing 20% or so.Then (SILVERSON) makes gained suspend under high shear Liquid is subjected to the mixing of specific duration, is added dropwise followed by with continuous shear stress1555 solvent of AG with Generate rheological characteristic appropriate.Then shear rate is reduced, and adds required quality200 (EVONIK), Followed by the continuous shear stress specific duration.Then will2510 dispersing agents are dissolved in mixture It is pure followed by dispersion diuron and Thidiazuron technology to ensure uniformity.

Then this slurries are crushed using horizontal mill (Engineered Mills company).The process is related to concentrating agents It is slowly fed into so that in the milling apparatus of 500 to 1000RPM low rotation speed operation, wherein preload has grinding machine grinding chamber The glass of 1 to 1.6mm diameter of 60 to 80% total volume capacities or more preferably zirconium silica dioxide medium, and collet coolant Temperature is predetermined and is maintained at a temperature of 15 to 25 DEG C of external control.Rotation speed is slowly improved by 2000 to 2500RPM Continue 30 to 45 minutes periods, generates the concentrating agents with substantially 5 μm of average particle sizes (d0.5), the granularity is by using 0 To the approximation method measurement of 100 grinding rule or 8 to 0 Hegmans rule.Grain size analysis is measured additionally by micro- approximation method.

It is added to concentrating agents3201 emulsifiers andEVM 70/2E surfactant, connects Be surplusThen gained oil-based suspension is homogenized via low sheraing (aerial stirring).Combination Object shows to show satisfactory stability and dilution behavior.This is the methodology that rheology modifier is added before crushing Embodiment.

Improvement of the embodiment 13- to embodiment 5

Table 13

It, will be the desired amount of according to table 1338 are added to the amount for being equal to substantially 50% aggregate demandWith150(EXXON Chemical).Then under high shear (SILVERSON) So that gained suspension is subjected to the mixing of specific duration, is added dropwise followed by with continuous shear stressAG 1555 solvents are to generate rheological characteristic appropriate.Then shear rate is reduced, and adds required quality 200 (EVONIK), followed by the continuous shear stress specific duration.Then will2510 dispersing agents are molten Solution is to ensure uniformity in mixture, and followed by dispersing, Thidiazuron technology is pure.

It is added to concentrating agents3201 emulsifiers andEVM 70/2E surfactant, connects Be surplusThen gained oil-based suspension is homogenized via the aerial stirring of low sheraing.Composition It shows to show satisfactory stability and dilution behavior.This is the reality that the methodology of rheology modifier is added before crushing Apply example.

Embodiment 14

Table 14

Via SILVERSON high-shear mixer, by by 14.81gSD-1 (ELEMENTIS) points It dissipates in 80.25gIn come prepare premix " masterbatch " gel.With continuous shear stress, to gained homogeneous dispersion Add 4.94g150, until obtaining spawn.It is left unused.

By under high shear to 95.77g3 addition 4.23g200 until obtain Spawn premixes " masterbatch " gel to prepare.It is left unused.

It, will be the desired amount of according to upper table 142520 dispersing agents are dissolved in comprising surplus150 HesMixture in, the latter one be equal to by allow 20% or so thiophene The amount of the grand concentration of benzene.Then under high shear using SILVERSON mixer by Thidiazuron technology it is pure be scattered in gained mixture In.Continue this measure until obtaining uniform mixture.

It is added to concentrating agents3201 emulsifiers,EVM 70/2E surfactant,13A7 emulsifier and pre-prepared masterbatch gel, followed by surplusThen via low Shear-mixed come be homogenized gained oil-based suspension.Then composition shows to show satisfactory stability and further improvement Dilution behavior, this achieve desired commodity performance standards.This is the another of the methodology of addition rheology modifier after being pulverized One embodiment.

Further improvement of the embodiment 15- to embodiment 14

Table 15

Via SILVERSON high-shear mixer, by by 14.81gSD-1 (ELEMENTIS) points It dissipates in 83.19gIn come prepare premix " masterbatch " gel.With continuous shear stress, to gained homogeneous dispersion Add 2.00g150, until obtaining spawn.It is left unused.

By under high shear to 95.74g3 addition 4.23g200 until obtain Spawn premixes " masterbatch " gel to prepare another kind.It is left unused.

It, will be the desired amount of according to upper table 152520 dispersing agents are dissolved in comprising surplus150 HesMixture in, the latter one be equal to by allow 20% or so thiophene The amount of the grand concentration of benzene.Then under high shear using SILVERSON mixer by Thidiazuron technology it is pure be scattered in gained mixture In.Continue this measure until obtaining uniform mixture.

Further improvement of the embodiment 16- to embodiment 15

Table 16

Via SILVERSON high-shear mixer, by by 14.21gSD-1 (ELEMENTIS) points It dissipates in 76.39gIn come prepare premix " masterbatch " gel.With continuous shear stress, to gained homogeneous dispersion Add 9.40g150, until obtaining spawn.It is left unused.

By under high shear to 95.76g3 addition 4.24g200 until obtain Spawn premixes " masterbatch " gel to prepare another kind.It is left unused.

It, will be the desired amount of according to upper table 162520 dispersing agents are dissolved in comprising surplus150 HesMixture in, the latter one be equal to by allow 20% or so thiophene The amount of the grand concentration of benzene.Then under high shear using SILVERSON mixer by Thidiazuron technology it is pure be scattered in gained mixture In.Continue this measure until obtaining uniform mixture.

Then this slurries are crushed using horizontal mill (Engineered Mills company).The process is related to concentrating agents It is slowly fed into so that in the milling apparatus of 500 to 1000RPM low rotation speed operation, wherein preload has grinding machine grinding chamber The glass of 1 to 1.6mm diameter of 60 to 80% total volume capacities or more preferably zirconium silica dioxide medium, and collet coolant Temperature is predetermined and is maintained at a temperature of 15 to 25 DEG C of external control.Rotation speed is slowly improved by 2000 to 2500RPM Continue 30 to 45 minutes periods, generates the concentrating agents with substantially 5 μm of average particle sizes (d0.5), the granularity is by using 0 To the approximation method measurement of 100 grinding rule or 8 to 0 Hegmans rule.Grain size analysis is measured additionally by micro- approximation method.In addition by Microscopy measures grain size analysis, and wherein dispersion shows the weak active constituent crystal to moderate and flocculates.

With stirring, added to the desired amount of premix carrier3201 emulsifiers,EVM 70/2E surfactant,13A7 emulsifier, followed by being slowly added abrasive material concentrating agents and surplusContinue stirring until obtaining uniform suspension.This composition shows to show further improved Stablize sexual behaviour.This is another embodiment for adding the methodology of rheology modifier after being pulverized.

Further improvement of the embodiment 17- to embodiment 12

Table 17

Via SILVERSON high-shear mixer, by by 14.21gSD-1 (ELEMENTIS) points It dissipates in 200gIn prepare premix carrier.With continuous shear stress, 9.40g is added to gained homogeneous dispersion150, until obtaining gel-like consistency.Finally, adding 4.23g under low shear mixing200g is until obtain uniform but flowable gel.Mixture is left unused.

It, will be the desired amount of according to upper table 172520 dispersing agents are dissolved in comprising surplus150 HesMixture in, the latter one be equal to by allow 20% or so thiophene The amount of the grand concentration of benzene.Then institute is scattered in by diuron and Thidiazuron technology are pure using SILVERSON mixer under high shear It obtains in mixture.Continue this measure until obtaining uniform mixture.

Further improvement of the embodiment 18- to embodiment 16

Table 18

Via SILVERSON high-shear mixer, by by 14.21gSD-1 (ELEMENTIS) points It dissipates in 200gIn prepare premix carrier.With continuous shear stress, 9.40g is added to gained homogeneous dispersion150, until obtaining gel-like consistency.Finally, adding 4.24g under low shear mixing200g is until obtain uniform but flowable gel.Mixture is left unused.

It, will be the desired amount of according to upper table 182520 dispersing agents are dissolved in comprising surplus150 HesMixture in, the latter one be equal to by allow 20% or so thiophene The amount of the grand concentration of benzene.Then under high shear using SILVERSON mixer by Thidiazuron technology it is pure be scattered in gained mixture In.Continue this measure until obtaining uniform mixture.

Then this slurries are crushed using horizontal mill (Engineered Mills company).The process is related to concentrating agents It is slowly fed into so that in the milling apparatus of 500 to 1000RPM low rotation speed operation, wherein preload has grinding machine grinding chamber The glass of 1 to 1.6mm diameter of 60 to 80% total volume capacities or more preferably zirconium silica dioxide medium, and collet coolant Temperature is predetermined and is maintained at a temperature of 15 to 25 DEG C of external control.Rotation speed is slowly improved by 2000 to 2500RPM Continue 30 to 45 minutes periods, generates the concentrating agents with substantially 5 μm of average particle sizes (d0.5), the granularity is by using 0 To the approximation method measurement of 100 grinding rule or 8 to 0 Hegmans rule.Grain size analysis is measured additionally by micro- approximation method.It will be this Concentrating agents briefly leaves unused.

With stirring, added to the desired amount of premix carrier3201 emulsifiers,EVM 70/2E surfactant,13A7 emulsifier.Then gained mixture is heated approximately at 60 DEG C to 70 DEG C, and And with continuously stirring, it is slowly added abrasive material concentrating agents, followed by surplusContinue to stir, simultaneously Keep composition cooling, obtains uniform suspension.This composition shows to show improved stable sexual behaviour.This is to crush Another embodiment of the methodology of rheology modifier is added afterwards.

The alternative solution of embodiment 19- embodiment 15-addition titanium dioxide

Table 19

Via SILVERSON high-shear mixer, by by 3.90gSD-1 (ELEMENTIS) points It dissipates in 47.83gIn prepare premix carrier, generate superfine suspension.With continuous shear stress, to gained Homogeneous dispersion adds 2.57g150, until obtaining gel-like consistency.Then it is added to mixture 27.41g3201、6.85gEVM70/2E and 10.28g13A7, followed by Mixed on low speed is to be homogenized.Finally, being slowly added 1.15g under low shear mixing200, until obtaining uniform Weak coagulation mixture.Mixture is left unused.

It, will be the desired amount of according to upper table 192520 dispersing agents are dissolved in comprising surplus150 HesMixture in, the latter one be equal to by allow 20% or so thiophene The amount of the grand concentration of benzene.Then it is under high shear dispersed the pure and mild TIONA 625 of Thidiazuron technology in using SILVERSON mixer In gained mixture.Continue this measure until obtaining uniform mixture.

It is slowly added abrasive material concentrating agents to the desired amount of premix carrier, followed by surplusAfter Continuous stirring is until obtain uniform suspension.This composition shows to show further improved stable sexual behaviour.This be Another embodiment of the methodology of rheology modifier is added after crushing.

The alternative solution-of embodiment 20- embodiment 16 does not need dispersing agent

Table 20

Via SILVERSON high-shear mixer, by by 14.21gSD-1 (ELEMENTIS) points It dissipates in 200gIn come prepare premix " carrier base-material ".With continuous shear stress, add to gained homogeneous dispersion Add 9.40g150, until obtaining gel-like consistency.Finally, adding 4.24g under low shear mixing200 until obtain uniform but flowable gel.Mixture is left unused.

It is according to upper table 20, half is the desired amount of3201、EVM70/2E and13A7 is added to comprising surplus150 HesMixture, Middle the latter is equal to the amount for the Thidiazuron concentration for allowing 15% or so.Then SILVERSON mixer is used under high shear By Thidiazuron technology it is pure be scattered in gained mixture in.Continue this measure until obtaining uniform mixture.

With stirring, added to the desired amount of prefabricated " carrier base-material " remaining3201 emulsifiers,EVM 70/2E surfactant,13A7 emulsifier, followed by be slowly added abrasive material concentrating agents and SurplusContinue stirring until obtaining uniform suspension.This composition shows to show into one Walk improved stable sexual behaviour.This is another embodiment for adding the methodology of rheology modifier after being pulverized.

The alternative solution of embodiment 21- embodiment 16

Table 21

It, will be the desired amount of according to upper table 212520 dispersing agents are dissolved in comprising surplus150 HesMixture in, the latter one be equal to by allow 15% or so thiophene The amount of the grand concentration of benzene.Then it is under high shear dispersed the pure and mild TIONA 625 of Thidiazuron technology in using SILVERSON mixer In gained mixture.Continue this measure until obtaining uniform mixture.

It is expected that will also be further improved the stability characteristic (quality) of embodiment 17 to the method and composition that embodiment 16 improves.

The alternative solution of embodiment 22- embodiment 16

Table 22

It, will be the desired amount of according to upper table 224890 dispersing agents are dissolved in comprising surplus150 HesMixture in, the latter one be equal to by allow 15% or so thiophene The amount of the grand concentration of benzene.Then under high shear using SILVERSON mixer by Thidiazuron technology it is pure be scattered in gained mixture In.Continue this measure until obtaining uniform mixture.

It is slowly added abrasive material concentrating agents to the desired amount of premix carrier, followed by surplusAfter Continuous stirring is until obtain uniform suspension.Although the dispersing characteristic of abrasive material concentrating agents (embodiment 10) is improved, this Composition shows to show significantly reduced stable sexual behaviour.This is the another of the methodology of addition rheology modifier after being pulverized A embodiment.

Embodiment 23- preparation stability

The crucial measurement that the stability of preparation is total to the above-mentioned Oil-based Suspension of Thidiazuron according to the present invention is extended In period, to the simple visual observation for storing sample at ambient room temperature.

Table 23

Embodiment 24.1

Table 24.1: average defoliation, place A

G ai/ha (per hectare active constituent grammes per square metre) ratio of a=Thidiazuron

The g ai/ha ratio of b=diuron

The g ai/ha ratio of c=oil

* DC-TRON is the spray of the one or more emulsifying agents containing 827g/L petroleum oil and between 80-100g/L Leaching oil.

Embodiment 24.2

Table 24.2: average defoliation, place B

The g ai/ha ratio of a=Thidiazuron

The g ai/ha ratio of b=diuron

The g ai/ha ratio of c=oil

As a result

Acquired results and its efficiency are as indicated above after using total preparation of the invention.In all cases, when with When being compared using the preparation of the prior art, as shown in foregoing embodiments 24.1 and 24.2, synergistic effect by disleave performance guarantor It stays or improves to show and show, and although total agricultural chemicals input decreases.

In upper table 24.1 and 24.2, work is cooperateed with when assessment Thidiazuron or Thidiazuron and diuron and oily total preparation Used time, technical staff must be appreciated that application rate.

In this particular example, it shows when to prepare system described in embodiment 3 to 5 in use, passing through to fixed-ratio Agent obtain synergistic effect shown by disleave performance, be equal to or be better than respectively with based on per hectare active constituent etc. With ratio application such as the preparation as Thidiazuron or Thidiazuron and diuron as described in Examples 1 and 2 and with typical ratios application Spray oil.There may be the enhancement effects by the way that Thidiazuron or Thidiazuron and diuron to be prepared to realization altogether with oil, therefore lead to Crossing the agricultural chemicals input being substantially reduced realizes substantially equivalent or better performance.Alternatively, the effect of enhancing can draw Hair is promoted and with oily prepare altogether improved using less preparation or Thidiazuron or Thidiazuron and diuron displaying Disleave efficiency.

Embodiment 24.1 shown in table 24.1 as above highlights raw with the usual plant combined with the spray oil of preparation Long regulator or plant growth regulator are compared with the mixture of herbicide, by oil with plant growth regulator itself or with plant The total preparation of the mixture of object growth regulator and herbicide obtains synergistic effect.

About the total preparation of oil and the plant growth regulator used with regard to itself, act synergistically by the processing in table 24.1 13 are best represented by, and wherein Thidiazuron is total to preparation or OD preparation as oil base to apply.The the 4th, 7 and 14 day after the treatment (DAT) when, when with the processing 2 that Thidiazuron is applied together with spray oil formulation is compared with common fashion, this processing is always Show statistically improved disleave.These results pass through the reduction in the total agricultural chemicals input upper 34.8% of per hectare To realize.In addition, processing 13 can be considered as total agrochemicals comparable with processing 3, per hectare is applied whereby in disleave aspect of performance Product input and bioactivity defoliant reduce by 37.5% and 25% respectively.

About the total preparation of oil and plant growth regulator and the mixture of herbicide, act synergistically by table 24.1 Reason 10 is best represented by.In 4,7 and 14DAT, when with use spray oil formulation and use the plant growth regulator being equal and remove When processing 4 in the table 24.1 of careless agent ratio is compared, this processing always show out improved disleave performance.These results have been led to It crosses and inputs upper 60% reduction in the total agricultural chemicals of per hectare to realize.

Embodiment 24.2 shown in table 24.2 as above highlight with using as shown in Examples 1 and 22 with spray oil group The traditional plant growth regulator or plant growth regulator of conjunction are compared with the mixture of herbicide, pass through oil and plant growth tune It saves agent or obtains synergistic effect with the total preparation of the mixture of plant growth regulator and herbicide.

About the total preparation of oil and plant growth regulator itself, act synergistically best by the processing 13 in table 24.2 again Ground indicates.After the treatment the 8th day (DAT) when, when compared with the processing 2 in table 24.2, this processing shows statistics Upper equivalent disleave.In 14DAT, when compared with processing 2, processing 13 shows statistically improved disleave performance.These As a result it is realized by inputting upper 34.8% reduction in the total agricultural chemicals of per hectare.Again, processing 13 can also be in disleave Aspect of performance is considered as 3 comparable with processing, and total agricultural chemicals input of per hectare application and bioactivity defoliant have divided whereby It Jiang Di by 37.5% and 25%.

About the total preparation of oil and plant growth regulator and the mixture of herbicide, act synergistically by table 24.2 Reason 10 is best represented by.In 8DAT, when compared with processing 4, this processing shows the disleave performance slightly improved.? 14DAT, processing 10 are statistically more excellent.These results pass through the drop in the total agricultural chemicals input upper 60% of per hectare It is low to realize.

Without departing from the scope of the invention, it can make the present invention that there is further advantage and improvement.Although Show and describes the present invention to be envisioned for most realistic and preferred embodiment, but can be appreciated that can the scope of the present invention with Deviation is made in spirit, the deviation is not limited to details disclosed herein, but should meet the full scope of claim, To include any and all equivalent devices and equipment.Any discussion of the prior art shall in no way be construed to through specification It is to recognize that such prior art is well-known or is formed in this field the common general knowledge in part.

In the case where using term "comprising", " containing " or term " includes " in the present specification, the term should be explained To provide the feature, entirety, step or being related to the presence of component, but one or more other spies are not precluded the presence or addition of Sign, entirety, step, component or its grouping.

Claims

1. agricultural preparation altogether, it includes:

I) a effective amount of at least one plant growth regulator or at least one plant growth regulator and other bioactivity Ingredient, in the pulverised form of the average particle size with 1 to 12 micron range；

Ii) at least one oil；

Iii) at least one oil soluble surfactant dispersing agent；And

Iv) at least one emulsifier,

The wherein oil and one or more rheology modifiers and/or activator other by addition on demand, come optionally adjust to The ultimate density of few plant growth regulators or at least one plant growth regulator and other bioactive ingredients, So that the preparation altogether is substantially stable；And wherein the efficiency of the plant growth regulator is able to substantially maintain or change Into.

2. preparation altogether according to claim 1, wherein the form of the preparation altogether is selected from oil dispersed (OD) concentrating agents, oil mixes Flowable (OF) concentrating agents of dissolubility, Oil-based Suspension concentrating agents (SC) or oil base suspoemulsion (SE).

3. preparation altogether according to claim 2, wherein the plant growth regulator is Thidiazuron.

4. preparation altogether according to claim 3, wherein Thidiazuron exists with 1 to 500g/L concentration range.

5. preparation altogether according to claim 4, wherein Thidiazuron exists with 1 to 200g/L concentration range.

6. preparation altogether according to claim 5, wherein Thidiazuron exists with 1 to 120g/L concentration range.

7. preparation altogether according to claim 6, wherein Thidiazuron exists with the concentration of 100g/L.

8. preparation altogether according to claim 1, wherein at least one other bioactive ingredients are selected from antifungal Agent, Insecticides (tech) & Herbicides (tech), acaricide, nematicide, invertebrate poison, algicide or pesticides or their times What mixture.

9. preparation altogether according to claim 8, wherein the other bioactive ingredients are at least one herbicides.

10. preparation altogether according to claim 9, wherein the plant growth regulator is Thidiazuron and the herbicide It is diuron.

11. preparation altogether according to claim 10, wherein Thidiazuron exists with 1 to 250g/L concentration range, and opposes Grass is grand to be existed with 1 to 250g/L concentration range.

12. preparation altogether according to claim 11, wherein Thidiazuron exists with the concentration of 60g/L, and diuron with The concentration of 30g/L exists.

13. preparation altogether according to claim 1, wherein at least one oil is selected from least one paraffin oil, at least one Kind seed oil ester, at least one aromatic hydrocarbon, at least one polyalkylene glycol ethers, at least one fatty acid diesters, at least one Fatty alkyl amide or diamides, at least one two alkylene carbonates, at least one ketone or at least one alcohol or their times What mixture.

14. preparation altogether according to claim 13, wherein at least one oil is with the concentration greater than 5% w/v In the presence of.

15. preparation altogether according to claim 14, wherein at least one oil is to be greater than the dense of 25% w/v Degree exists.

16. preparation altogether according to claim 15, wherein at least one oil is to be greater than the dense of 50% w/v Degree exists.

17. preparation altogether according to claim 16, wherein at least one oil is to be greater than the dense of 55% w/v Degree exists.

18. preparation altogether according to claim 1, wherein the oil soluble surfactant dispersing agent includes polyalkylene two The condensation product of the reaction of alcohol or polyalkylene glycol ethers and fatty acid.

19. preparation altogether according to claim 1, wherein the oil soluble surfactant dispersing agent contracts comprising random polyester Close object.

20. preparation altogether according to claim 1, also includes at least one rheology modifier.

21. preparation altogether according to claim 1, wherein the plant growth regulator is crushed in horizontal mill.

22. preparation altogether according to claim 21, wherein the average particle size is in 1 to 8 micron range.

23. preparation altogether according to claim 22, wherein the average particle size is in 1 to 6 micron range.

24. preparation altogether according to claim 23, wherein the average particle size is about 5 microns.

25. prepare it is according to claim 1 altogether preparation method, the described method comprises the following steps, wherein step c) and D) it can carry out in any order or simultaneously:

B) by stirring or high shear mixing, at least one oil add the crushing at least one plant growth regulator, Or at least one plant growth regulator and other bioactive ingredients, to generate oil dispersion；

C) to oil dispersion addition at least one oil soluble surfactant dispersing agent；

D) to oil dispersion addition at least one emulsifier；Optionally

E) with stirring, the temperature of the oil dispersion is adjusted between about 60 DEG C and 70 DEG C；And optionally

F) oil and one or more rheology modifiers and/or activator other by addition on demand, to adjust the dispersion Described at least one plant growth regulator or at least one plant growth regulator and other bioactive ingredients most Final concentration, so that the preparation altogether is substantially stable.

26. the method for preparing total preparation substantially stable described in claim 20, the described method comprises the following steps, wherein It step e) and can f) carry out in any order or simultaneously:

A) at least one rheology modifier and at least one oil are combined；

B) by stirring or high shear mixing, to the oil addition described at least one containing at least one rheology modifier Plant growth regulators or at least one plant growth regulator and the other bioactive ingredients, to generate Oil dispersion；

C) the desired rheological behavior of the oil dispersion is generated via at least one activator is added；

D) oil dispersion of step c) is crushed, to realize at least one plant growth tune of 1 to 12 micron range Save the average particle size of agent or at least one plant growth regulator and other bioactive ingredients；

E) to oil dispersion addition at least one oil soluble surfactant dispersing agent；

F) to oil dispersion addition at least one emulsifier；Optionally

G) with stirring, the temperature of the oil dispersion is adjusted between about 60 DEG C and 70 DEG C；And optionally

H) oil and one or more other activators other by addition on demand, to adjust described in the dispersion at least The ultimate density of one plant growth regulators or at least one plant growth regulator and other bioactive ingredients, with Keep the preparation altogether substantially stable.

27. the method for preparing preparation altogether according to claim 1, the described method comprises the following steps:

A) at least one oil addition at least one oil soluble surfactant dispersing agent or at least one cream Agent；

B) by stirring or high shear mixing, to the oil addition at least one plant growth regulator or it is described at least One plant growth regulators and the other bioactive ingredients, to generate oil dispersion；

C) at least one activator is added, stablizes sexual behaviour further to generate the expectation of the oil dispersion；

D) oil dispersion of step c) is crushed, with realize 1 to 12 micron at least one plant growth regulator, Or the average particle size of at least one plant growth regulator and the other bioactive ingredients；Optionally

F) by adding other oil, at least one emulsifier and one or more rheology modifiers and/or at least one on demand Other activator, to adjust at least one plant growth regulator described in the dispersion or at least one plant The ultimate density of growth regulator and the other bioactive ingredients, so that the preparation altogether is substantially stable.

28. the method for preparing substantially uniform stable agricultural preparation altogether according to claim 1, the method includes Following steps, wherein step a) to d) step e) to g) before or after and carry out before the step h):

A) at least one the first oil addition at least one oil soluble surfactant dispersing agent or at least one cream Agent；

B) with stirring or high shear mixing, a effective amount of at least one plant growth regulating is added in first oil Agent or at least one plant growth regulator and the other bioactive ingredients, to generate oil dispersion；

D) oil dispersion of step c) is crushed, to generate containing described in the average particle size with 1 to 12 micron range At least one plant growth regulator or at least one plant growth regulator and other bioactive ingredients substantially The first even dispersion concentration agent；

E) it by stirring or high shear mixing, disperses at least one rheology modifier at least one second oil, to be formed The substantially uniform dispersion concentration agent of the second of gel form；

G) by stirring or high shear mixing, by least one oil soluble surfactant dispersing agent or at least one emulsifier point It dissipates in the improved gel, to form the second substantially uniform dispersion concentration agent；

I) described substantially equal to obtain to a certain amount of first dispersion concentration agent of a certain amount of premix carrier addition Uniform stable total preparation.

29. the method according to any one of claim 25 to 28 is detached from for realizing the leaf of plant, wherein utilizing basis Total preparation described in any one of claim 1 to 24 handles plant.

30. according to the method for claim 29, wherein the plant is vegetable lamb.

31. according to the method for claim 30, wherein the vegetable lamb is transgenosis.