CN109497061A - A kind of pendimethalin microcapsule suspending agent and preparation method thereof - Google Patents
A kind of pendimethalin microcapsule suspending agent and preparation method thereof Download PDFInfo
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- CN109497061A CN109497061A CN201811574105.2A CN201811574105A CN109497061A CN 109497061 A CN109497061 A CN 109497061A CN 201811574105 A CN201811574105 A CN 201811574105A CN 109497061 A CN109497061 A CN 109497061A
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- Prior art keywords
- pendimethalin
- capsule
- microcapsule suspending
- suspending agent
- prepared
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Classifications
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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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
- A01N33/18—Nitro compounds
-
- 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
-
- 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
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
Abstract
The invention discloses a kind of pendimethalin microcapsule suspending agents, including following weight percentage components: the pendimethalin pesticide micro-capsule of 14.2-85%, the dispersing agent of 1%-10%, the defoaming agent of 1%-2%, the antifreeze of 1%-8%, the preservative of 0.2%-5%, the thickener of 0.2%-5%, the salt of 2-10% and surplus water；Pendimethalin pesticide micro-capsule includes the component of following parts by weight: 1-50 parts of capsule-core and 4.2-35 part capsule material；Capsule-core is pendimethalin；Capsule material is to pass through the polyurethane that crosslinking curing obtains by isocyanates, polyurethane soft segment and chain extender；Pendimethalin microcapsule suspending agent disclosed by the invention makes that reaction process is steady, is easy to control using polyurethane soft segment as reaction raw materials, so as to facilitate the rate of release for adjusting pesticide micro-capsule.
Description
Technical field
The present invention relates to pesticide microcapsule technology field, more particularly to a kind of diformazan that can easily be accommodated rate of release
Penta clever microcapsule suspending agent and preparation method thereof.
Background technique
Pendimethalin (pendimethalin, Pendimethalin) belongs to phenyl amines herbicide, is that one kind is widely used in cotton
Flower, corn, rice, potato, soybean, peanut, tobacco and vegetable fields selective soil close herbicide, main dosage form is
Missible oil, there are following obvious shortcomings in use process: it is shorter using a large amount of organic solvent environmental protection coefficient differences, lasting period in preparation,
Missible oil is easy coloring and causes phytotoxicity etc..
In conjunction with pesticide microcapsules advantage, pendimethalin microcapsules can solve disadvantage mentioned above, the application effect of raising pendimethalin
Fruit, the common preparation method of pendimethalin microcapsule suspending agent is interfacial polymerization and situ aggregation method at present, but is made at this stage
The method of standby pendimethalin microcapsule suspending agent can not achieve the effect for facilitating and adjusting pendimethalin microcapsule suspending agent rate of release.Such as
Patent 201210217708.3, which is disclosed, to be prepared using Lauxite as wall material using situ aggregation method, patent 201610320446.1
It discloses and is prepared by monomeric diisocyanate and monomeric polycarboxylic amine, polyalcohol by interface polymerization reaction, patent
201710440274.6 disclose cyst material is generated by poly- allyl acetate and kayexalate reaction, patent
201180008250.4 the coloring effect of pendimethalin microcapsules is reduced in by addition organic salt；Above-mentioned technical proposal is prepared into
Arrived pendimethalin microcapsule suspending agent and improved its stability, but can not achieve adjust effective component delivery mode and
The effect of rate of release.Although in addition, as in patent CN98810827.5 by adjusting the type of diisocyanate in cyst wall and
The rate of release of the content adjustment acetamide-group herbicides effective component of capsule-core, but diisocyanate kind used in its method
More, actual production saves difficult, it is difficult to be promoted and be utilized.
Therefore it provides a kind of preparation method for the pendimethalin microcapsule suspending agent that can easily be accommodated rate of release, prepares pledge
Amount is stablized, and rate of release is controllable, constant superior pendimethalin microcapsule suspending agent in interface is that those skilled in the art need to solve
Certainly the problem of.
Summary of the invention
In view of this, the present invention provides a kind of pendimethalin microcapsule suspending agent and preparation method thereof, two be prepared
The clever microcapsule suspending agent quality of first penta is stablized, and rate of release is controllable, takes into account quick-release and slow releasing medicinal effect；And preparation method it is easy to operate,
Easily controllable, high production efficiency, preparation time are short.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of pendimethalin microcapsule suspending agent, which is characterized in that including following weight percentage components: 1%-50%
Pendimethalin, the capsule material of 4.2%-35%, the dispersing agent of 1%-10%, the defoaming agent of 0.2%-2%, 1%-8% it is freeze proof
Agent, the preservative of 0.2%-5%, the thickener of 0.2%-5%, the salt of 2-10% and surplus water；
The capsule material is to pass through the polyurethane that crosslinking curing obtains by isocyanates, polyurethane soft segment and chain extender, described
The weight ratio of isocyanates, polyurethane soft segment and chain extender is 2-10:2-20:0.2-5.
The beneficial effect of above-mentioned optimal technical scheme is: pendimethalin microcapsule suspending agent disclosed by the invention, wherein be with
Isocyanates, polyurethane soft segment and chain extender are reaction raw materials, and polyurethane capsule material is prepared by crosslinking, curing reaction, and
And using pendimethalin as capsule-core it is stable be rolled into pesticide micro-capsule, wherein making to react using polyurethane soft segment as reaction raw materials
Process is steady, is easy to control, so as to facilitate the rate of release for adjusting pesticide micro-capsule.
Preferably, the isocyanates includes aliphatic isocyanates or aromatic isocyanate.
Preferably, the isocyanates is aromatic isocyanate.
Preferably, the isocyanates includes methyl diphenylene diisocyanate, toluene di-isocyanate(TDI), naphthalene diisocyanate
One of ester, paraphenylene diisocyanate, dimethyl diphenyl diisocyanate or poly methylene poly phenyl poly isocyanate are more
Kind.
The beneficial effect of above-mentioned optimal technical scheme is: the isocyanates that the present invention uses can be with polyurethane soft segment and expansion
Chain agent cooperates, and is conducive to adjust cross-linking and curing reaction rate, to be conducive to adjust the structure for the polyurethane being prepared
And performance, and then realize the effect of conveniently regulating and controlling pesticide micro-capsule rate of release；The isocyanates that uses of the present invention can be with simultaneously
It cooperates with pendimethalin, realizes the effect for being rolled into pendimethalin micro-capsule that pendimethalin is stable.
Preferably, the polyurethane soft segment includes polyether polyol, and the polyether polyol is ethylene oxide and epoxy third
Alkane has rule or statistic copolymer, the structural formula of the polyether polyol are as follows:
The R includes propylene glycol, ethylene glycol, bisphenol-A, glycerol, pentaerythrite or diaryl phenolic condensates；
The n is the integer of 0-100, and the m is the integer of 0-100, the integer of the sum of the n and m for 0-100, and institute
Stating n and the m not is simultaneously 0.
Preferably, the sum of the n and m for 10-50 integer.
Preferably, the sum of the n and m for 15-25 integer.
Preferably, the polyurethane soft segment includes the 210 (ring of series block polyethers of Jiangsu Zhongshang Chemical Co., Ltd.'s production
Ethylene Oxide polymer molecular weight M1000), block polyether 330 (M3000), block polyether 2802 (glycerol and epoxypropane polymer
) or block polyether 1618A (glycerol and propylene oxide, ethylene oxide block polymers M5000, ethylene oxide segment accounting M3000
6%), the polyurethane soft segment capsule material further includes polyglycol ether Series P EG200, PEG400 or PEG1000 of BASF production.
The beneficial effect of above-mentioned optimal technical scheme is: polyurethane soft segment disclosed by the invention can be with isocyanates and expansion
Chain agent cooperates, and is conducive to adjust cross-linking and curing reaction rate, to be conducive to adjust the structure for the polyurethane being prepared
And performance, and then realize the effect for facilitating and adjusting pesticide micro-capsule rate of release；Meanwhile the polyurethane soft segment that the present invention uses may be used also
To cooperate with pendimethalin, the effect for being rolled into pendimethalin micro-capsule that pendimethalin is stable is realized.
Preferably, the polyurethane soft segment includes polyester polyol, the structural formula of the polyester polyol are as follows:
The R1For C2-C6Carbon chain compound, the R2For C2H5, the n1 is the integer of 1-100.
Preferably, the n1 is the integer of 10-30.
Preferably, the polyurethane soft segment capsule material includes adipic acid system polyester-diol.
Preferably, the polyurethane soft segment capsule material includes PEA-1000, PEA-2000, PEA-3000, PBA-580, PBA-
1000, one or more of PBA-2000, PDA-1000, PDA-2000, PHA-1000, PHA-2000 or PHA-3000.
Wherein, PEA-1000, PEA-2000 and PEA-3000 are the polyethylene glycol adipate glycol of Yantai Hua Da chemistry
(PEA) class；PBA-580, PBA-1000, PBA-2000 are polybutylene glyool adipate (PBA) class；PDA-1000,PDA-
2000 be polyadipate diethylene glycol (DEG) esterdiol (PDA) class；PHA-1000, PHA-2000, PHA-3000 are polyadipate hexylene glycol
Esterdiol (PHA) class.
The beneficial effect of above-mentioned optimal technical scheme is: polyurethane soft segment disclosed by the invention can be with isocyanates and expansion
Chain agent cooperates, and is conducive to adjust cross-linking and curing reaction rate, to be conducive to adjust the structure for the polyurethane being prepared
And performance, and then realize the effect for facilitating and adjusting pesticide micro-capsule rate of release；Meanwhile the polyurethane soft segment that the present invention uses may be used also
To cooperate with pendimethalin, the effect for being rolled into pendimethalin micro-capsule that pendimethalin is stable is realized.
Preferably, including being diamine, the structural formula of the diamine is the chain extender
H2N-R3-NH2
The R3Including C1-C12Carbon chain compound；The R3It further include the copolymer of propylene oxide and ethylene oxide, institute
The structural formula for stating the copolymer of propylene oxide and ethylene oxide is
The n2 is the integer of 1-100, and the m2 is the integer of 1-100, the sum of the n2 and m2 for 2-100 integer.
Preferably, the sum of the n2 and m2 for 10-40 integer.
Preferably, the diamine includes the CAM- of the CAM-2070 of Yangzhou morning new material, Yangzhou morning new material
2005, the graceful JEFFAMINE D- of CAED-600, Hensel of the CAED-900 of Yangzhou morning new material, Yangzhou morning new material
230, the graceful XTJ-502 of the graceful XTJ-501 of the graceful XTJ-500 of graceful JEFFAMINE D-240 of Hensel, Hensel, Hensel, Hensel
Or one of graceful XTJ-510 of Hensel or a variety of.
The beneficial effect of above-mentioned optimal technical scheme is: chain extender disclosed by the invention can be with isocyanates and polyurethane
Soft segment cooperates, and is conducive to adjust cross-linking and curing reaction rate, to be conducive to adjust the structure for the polyurethane being prepared
And performance, and then realize the effect for facilitating and adjusting pesticide micro-capsule rate of release；Meanwhile the chain extender that uses of the present invention can also be with
Pendimethalin cooperates, and realizes the effect for being rolled into pendimethalin micro-capsule that pendimethalin is stable.
Preferably, the dispersing agent includes aliphatic alcohol polyether, organic silicon dispersing agent or sulphosuccinates.
Preferably, the structural formula of the aliphatic alcohol polyether is
The R4For C8-C20Carbon chain compound；The n3 value range is the integer of 1-20.
Preferably, the R4For C8-C14；The n3 value range is the integer of 2-14.
Preferably, the aliphatic alcohol polyether include AE0-5, AE0-6, AE0-7, AE0-8, AE0-9 that Nanjing is changed very much or
AE0-10。
Preferably, the structural formula of the organic silicon dispersing agent is
The R5It is H, CH3Or C4H4；The R6For H or CH3；The n4 is the integer of 1-20.
Preferably, the n4 is the integer of 5-12.
Preferably, the organic silicon dispersing agent includes RH-208, RH-209, RH-213 or RH-225 of Ningbo profit standing grain.
Preferably, the structural formula of the sulphosuccinates is
The M includes Na, K or NH4；The R7For aliphatic alcohol polyether, the R8For aliphatic alcohol polyether；The R7And R8Knot
Structure formula is
The n3 is that the 0 or n3 is 1-10 integer and R7And R8Middle n3 is unequal.
The beneficial effect of above-mentioned optimal technical scheme is: dispersing agent disclosed by the invention can be mutual with chain extender and water phase
Continuous phase is cooperatively formed, then is cooperated with dispersed phase, to be conducive to adjust cross-linking and curing reaction rate, and then is conducive to adjust
The structure and performance of the polyurethane being prepared are saved, realizes the effect for facilitating and adjusting pesticide micro-capsule rate of release.
Preferably, the defoaming agent includes organic silicon defoamer or polyether antifoam agent.
Preferably, the antifreeze includes one of ethylene glycol, propylene glycol, glycerine or urea or a variety of combinations
Object.
Preferably, the preservative includes in benzoic acid, benzoic acid sodium salt, sorbic acid, sorbic acid sylvite or sulphite
One or more compositions.
Preferably, the thickener includes one in xanthan gum, Arabic gum, aluminium-magnesium silicate, polyvinyl alcohol or white carbon black
Kind or a variety of compositions.
Preferably, the salt include sodium chloride, sodium nitrate, sodium sulphate, potassium chloride, potassium nitrate, ammonium sulfate, sodium citrate,
One of potassium citrate or sodium oxalate or a variety of mixtures.
The beneficial effect of above-mentioned optimal technical scheme is: can reduce preparation using metal salt compound disclosed by the invention
Coloring adherency in use process, improves pesticide efficacy, while playing synergistic function.
A kind of preparation method of such as above-mentioned pendimethalin microcapsule suspending agent, which is characterized in that use continuous reaction work
Skill or intermittent reaction technique are prepared；The continuous reaction technique is to prepare diformazan based on microchannel or tubular reactor
Penta clever microcapsules.
Preferably, following reaction step is specifically included:
(1) according to a kind of pendimethalin suspension as described above, weigh pendimethalin, isocyanates, polyurethane soft segment,
Chain extender, dispersing agent, defoaming agent, antifreeze, preservative, thickener, Yan Heshui, it is spare；
(2) it prepares dispersed phase: pendimethalin, isocyanates and polyurethane soft segment being uniformly mixed, dispersed phase is obtained；
(3) it prepares continuous phase: dispersing agent, chain extender and defoaming agent being added to the water, stirs evenly and is prepared into continuous phase；
(4) it prepares micro-capsule: the above-mentioned dispersed phase being prepared and continuous phase is respectively charged into stirred tank, then with injecting
Pump is injected in the channel of microreactor, carries out reaction and micro-capsule is prepared；
(5) prepare microcapsule suspending agent: antifreeze, preservative, thickener and salt system is added in the micro-capsule that Xiang Shangshu is prepared
For at microcapsule suspending agent.
(6) cleaning equipment.
The beneficial effect of above-mentioned optimal technical scheme is: preparation method integrated operation disclosed by the invention is simple, is prepared into
The pendimethalin microcapsule suspending agent quality arrived is stablized, and rate of release is controllable, takes into account quick-release and slow releasing medicinal effect；Wherein first by isocyanic acid
Ester, polyurethane soft segment and pendimethalin melting mixing, it is ensured that uniform, the stable dispersed phase of the property being prepared；It will divide
Powder, defoaming agent and water are uniformly mixed with continuous phase, are conducive to dispersed phase uniform and stable dispersion in continuous phase；It utilizes
Stirred tank injects pump and microreactor and dispersed phase and continuous phase mutual cooperation, and stable regulation pendimethalin micro-capsule may be implemented
The effect of molecular weight, structure to realize the effect of stable adjusting pendimethalin microcapsule suspending agent rate of release, and is prepared into
The pendimethalin microcapsule structure arrived is stablized, and drug safety is improved.
Preferably, it is then uniformly mixed in the step (2) first by material heating melting.
The beneficial effect of above-mentioned optimal technical scheme is: so that raw material is in liquid condition by heating melting, thus favorably
It is uniformly mixed between raw material, so as to which uniform, stable dispersed phase is prepared, and then is conducive to property is prepared equal
One, stable pendimethalin micro-capsule.
Preferably, reaction temperature is 50-70 DEG C in the step (4), reaction time 8-20min.
The beneficial effect of above-mentioned optimal technical scheme is: can protect under reaction temperature disclosed by the invention, reaction time
Card isocyanates, polyurethane soft segment and chain extender sufficiently react, and improve raw material availability, and can guarantee that reaction generates poly-
Urethane by pendimethalin capsule-core it is stable be rolled into an entirety, so as to improve the stable structure of pendimethalin pesticide micro-capsule
Property.
Preferably, the charging rate of dispersed phase and continuous phase ratio is 1:1-2:1 in the step (4).
Preferably, the charging rate of dispersed phase is 1-1000mL/min in the step (4)；The charging rate of continuous phase is
2-2000mL/min；Discharging speed is 3-3000mL/min.
The beneficial effect of above-mentioned optimal technical scheme is: dispersed phase charging rate disclosed by the invention, continuous phase charging speed
Degree, discharging speed cooperate, it is ensured that reaction raw materials sufficiently react in microreactor, to guarantee the polyurethane generated
Pendimethalin micro-capsule is stablized and wraps up integral, the structural stability of raising pendimethalin pesticide micro-capsule；And pass through control point
Stable regulation pendimethalin micro-capsule molecular weight, structure may be implemented in dephasing charging rate, continuous phase charging rate, discharging speed
Effect, thus realize the effect of stable adjusting pendimethalin microcapsule suspending agent rate of release,
It can be seen via above technical scheme that compared with prior art, the present disclosure provides a kind of pendimethalin is micro-
Capsule suspending agent and preparation method thereof, has the following beneficial effects:
1, the type of the invention by adjusting polyurethane soft segment, mass fraction, hydrophily and the permeability for changing capsule material are real
Now adjust the effect of rate of release；
2, the present invention introduces hydrophilic soft segment in pendimethalin microcapsule suspending agent, so that capsule after the sprinkling of suspension dilution agent
The hydrolysis of wall soft segment, capsule-core dissolve out rapidly through soft segment, reach quick-release effect；Oleophylic soft segment is introduced, capsule-core can be made from cyst wall sky
Gap dissolution, rate of release are slower；
3, the present invention introduces polyurethane soft segment in capsule material, increases cyst wall elasticity, avoids that polyureas capsule material is hard to be caused
The problem of cold storage rupture crystallization, improve the storage stability of microcapsule suspending agent；
4, the present invention adds alkaline metal salt in pendimethalin microcapsule suspending agent, can reduce in preparation use process
Coloring adherency, improves pesticide efficacy, while playing synergistic function；
5, the present invention prepares micro-capsule, simple process, different rate of release micro-capsule preparation switchings using continous way microreactor
It is convenient, do not generate waste water, energy conservation and environmental protection.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the rate of release comparison diagram of embodiment 1-5 provided by the invention and comparative example 1.
In figure:
1, which represents embodiment 1,2, represents embodiment 2,3 and represents embodiment 3,4 and represent embodiment 4,5 and represent embodiment 5,6 generations
Table comparative example 1.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a kind of pendimethalin microcapsule suspending agents, including following weight percentage components:
The pendimethalin of 1%-50%, the capsule material of 4.2%-35%, the dispersing agent of 1%-10%, the defoaming agent of 0.2%-2%, 1%-
8% antifreeze, the preservative of 0.2%-5%, the thickener of 0.2%-5%, the salt of 2-10% and the water of surplus；
The capsule material is to pass through the polyurethane that crosslinking curing obtains by isocyanates, polyurethane soft segment and chain extender, described
The weight ratio of isocyanates, polyurethane soft segment and chain extender is 2-10:2-20:0.2-5.
For further optimisation technique scheme, the isocyanates includes aliphatic isocyanates or aromatic series isocyanic acid
Ester.
For further optimisation technique scheme, the isocyanates is aromatic isocyanate.
For further optimisation technique scheme, the isocyanates includes methyl diphenylene diisocyanate, toluene two
Isocyanates, naphthalene diisocyanate, paraphenylene diisocyanate, dimethyl diphenyl diisocyanate or polymethylene polyphenyl polyisocyanate
One of cyanate is a variety of.
For further optimisation technique scheme, the polyurethane soft segment includes polyether polyol, the polyether polyol
It is that ethylene oxide and propylene oxide have rule or statistic copolymer, the structural formula of the polyether polyol are as follows:
The R includes propylene glycol, ethylene glycol, bisphenol-A, glycerol, pentaerythrite or diaryl phenolic condensates；
The n is the integer of 0-100, and the m is the integer of 0-100, the integer of the sum of the n and m for 0-100, and institute
Stating n and the m not is simultaneously 0.
For further optimisation technique scheme, the sum of the n and m for 10-50 integer.
For further optimisation technique scheme, the sum of the n and m for 15-25 integer.
For further optimisation technique scheme, the polyurethane soft segment includes what Jiangsu Zhongshang Chemical Co., Ltd. produced
Series block polyethers 210 (epoxypropane polymer molecular weight M1000), block polyether 330 (M3000), block polyether 2802
(glycerol and epoxypropane polymer M3000) or block polyether 1618A (glycerol and propylene oxide, ethylene oxide block polymers
M5000, ethylene oxide segment accounting 6%), the polyurethane soft segment capsule material further includes the polyglycol ether series of BASF production
PEG200, PEG400 or PEG1000.
For further optimisation technique scheme, the polyurethane soft segment includes polyester polyol, the polyester polyol
Structural formula are as follows:
The R1For C2-C6Carbon chain compound, the R2For C2H5, the n1 is the integer of 1-100.
For further optimisation technique scheme, the n1 is the integer of 10-30.
For further optimisation technique scheme, the polyurethane soft segment capsule material includes adipic acid system polyester-diol.
For further optimisation technique scheme, the polyurethane soft segment capsule material include PEA-1000, PEA-2000,
PEA-3000, PBA-580, PBA-1000, PBA-2000, PDA-1000, PDA-2000, PHA-1000, PHA-2000 or PHA-
One or more of 3000.
Wherein, PEA-1000, PEA-2000 and PEA-3000 are the polyethylene glycol adipate glycol of Yantai Hua Da chemistry
(PEA) class；PBA-580, PBA-1000, PBA-2000 are polybutylene glyool adipate (PBA) class；PDA-1000,PDA-
2000 be polyadipate diethylene glycol (DEG) esterdiol (PDA) class；PHA-1000, PHA-2000, PHA-3000 are polyadipate hexylene glycol
Esterdiol (PHA) class.
For further optimisation technique scheme, including being diamine, the structural formula of the diamine is the chain extender
H2N-R3-NH2
The R3Including C1-C12Carbon chain compound；The R3It further include the copolymer of propylene oxide and ethylene oxide, institute
The structural formula for stating the copolymer of propylene oxide and ethylene oxide is
The n2 is the integer of 1-100, and the m2 is the integer of 1-100, the sum of the n2 and m2 for 2-100 integer.
For further optimisation technique scheme, the sum of the n2 and m2 for 10-40 integer.
For further optimisation technique scheme, the diamine includes the CAM-2070 of Yangzhou morning new material, Yangzhou
The CAM-2005 of morning new material, the CAED-900 of Yangzhou morning new material, CAED-600, the Hensel of Yangzhou morning new material are graceful
JEFFAMINE D-230, the graceful XTJ-501 of the graceful XTJ-500 of graceful JEFFAMINE D-240 of Hensel, Hensel, Hensel, henry
One of this graceful XTJ-502 or the graceful XTJ-510 of Hensel or a variety of.
For further optimisation technique scheme, the dispersing agent includes aliphatic alcohol polyether, organic silicon dispersing agent or amber
Amber acid ester sulfonates.
For further optimisation technique scheme, the structural formula of the aliphatic alcohol polyether is
The R4For C8-C20Carbon chain compound；The n3 value range is the integer of 1-20.
For further optimisation technique scheme, the R4For C8-C14；The n3 value range is the integer of 2-14.
For further optimisation technique scheme, the aliphatic alcohol polyether includes AE0-5, AE0-6, AE0- that Nanjing is changed very much
7, AE0-8, AE0-9 or AE0-10.
For further optimisation technique scheme, the structural formula of the organic silicon dispersing agent is
The R5It is H, CH3Or C4H4；The R6For H or CH3；The n4 is the integer of 1-20.
For further optimisation technique scheme, the n4 is the integer of 5-12.
For further optimisation technique scheme, the organic silicon dispersing agent includes RH-208, RH- of Ningbo profit standing grain
209, RH-213 or RH-225.
For further optimisation technique scheme, the structural formula of the sulphosuccinates is
The M includes Na, K or NH4；The R7For aliphatic alcohol polyether, the R8For aliphatic alcohol polyether；
The R7And R8Structural formula be
The n3 is that the 0 or n3 is 1-10 integer and R7And R8Middle n3 is unequal.
For further optimisation technique scheme, the defoaming agent includes organic silicon defoamer or polyether antifoam agent.
For further optimisation technique scheme, the antifreeze includes in ethylene glycol, propylene glycol, glycerine or urea
One or more compositions.
For further optimisation technique scheme, the preservative includes benzoic acid, benzoic acid sodium salt, sorbic acid, sorb
One of acid potassium salt or sulphite or a variety of compositions.
For further optimisation technique scheme, the thickener includes xanthan gum, Arabic gum, aluminium-magnesium silicate, poly- second
One of enol or white carbon black or a variety of compositions.
For further optimisation technique scheme, the salt includes sodium chloride, sodium nitrate, sodium sulphate, potassium chloride, nitric acid
One of potassium, ammonium sulfate, sodium citrate, potassium citrate or sodium oxalate or a variety of mixtures.
A kind of preparation method of such as above-mentioned pendimethalin microcapsule suspending agent, specifically includes following reaction step:
(1) according to a kind of pendimethalin suspension as above, pendimethalin, isocyanates, polyurethane soft segment, chain extension are weighed
Agent, dispersing agent, defoaming agent, antifreeze, preservative, thickener, Yan Heshui, it is spare；
(2) it prepares dispersed phase: first by pendimethalin, isocyanates and polyurethane soft segment heating melting, being then uniformly mixed,
Obtain dispersed phase；
(3) it prepares continuous phase: dispersing agent, chain extender and defoaming agent being added to the water, stirs evenly and is prepared into continuous phase；
(4) it prepares micro-capsule: the above-mentioned dispersed phase being prepared and continuous phase is respectively charged into stirred tank, then with injecting
Pump injects dispersed phase with 1-100mL/min charging rate into the logical of microreactor with 2-200mL/min charging rate, continuous phase
In road, while controlling that discharging speed is 3-300mL/min, reaction temperature is 50-70 DEG C, reaction time 8-20min, by anti-
Micro-capsule should be prepared；
(5) prepare microcapsule suspending agent: antifreeze, preservative, thickener and salt system is added in the micro-capsule that Xiang Shangshu is prepared
For at microcapsule suspending agent；
(6) cleaning equipment: after reaction, by microreactor temperature control at 50-60 DEG C, in time with inject pump to it is micro- instead
Device is answered to squeeze into recirculated water, until cleaning up.
Embodiment 1
The embodiment of the present invention 1 discloses a kind of preparation method of pendimethalin microcapsule suspending agent, specifically includes following reaction
Step:
(1) 50g pendimethalin, 4g toluene di-isocyanate(TDI), 10g polyurethane soft segment PEA-1000,1g Yangzhou are weighed respectively
CAM2070,0.5g organic silicon defoamer, 4g RH-208 dispersing agent, the 2g Kathon CG preservative of morning new material, 1g ethylene glycol are anti-
Freeze agent, 2g ammonium sulfate and 2g aluminium-magnesium silicate thickener, and the water of surplus is weighed based on 100g total amount, it is spare；
(2) dispersed phase is prepared: by above-mentioned load weighted pendimethalin, toluene di-isocyanate(TDI) and polyurethane soft segment PEA-
1000 mixed heating and meltings are simultaneously uniformly mixed, and dispersed phase is prepared；
(3) prepare continuous phase: by above-mentioned load weighted dispersing agent RH-208, Yangzhou morning new material CAM2070, disappear
Infusion and water are mixed evenly, and continuous phase is prepared；
(4) it prepares micro-capsule: the temperature of microreactor is set to 60 DEG C, by the above-mentioned dispersed phase being prepared and continuous phase
It is respectively charged into stirred tank, is injected dispersed phase with the speed of 1mL/min with the speed of 2mL/min, continuous phase using pump is injected
Enter to carry out reaction in the channel of microreactor that micro-capsule is prepared, and collected with beaker, control discharging speed is 3mL/min, is made
Micro-capsule reacts 8min in waveform microreactor channel, forms Microcapsules Size D90It is 7-8 μm；
(5) it prepares microcapsules: above-mentioned load weighted ammonium sulfate, Kathon CG anti-corrosion being added into the beaker of above-mentioned collection micro-capsule
Agent, ethylene glycol antifreeze and aluminium-magnesium silicate thickener, stir evenly and pendimethalin microcapsule suspending agent can be obtained；
(6) equipment is cleaned: after reaction, microreactor temperature being controlled at 60 DEG C, is pumped in time to micro- reaction with injecting
Device squeezes into recirculated water, until cleaning up.
Embodiment 2
The embodiment of the present invention 2 discloses a kind of preparation method of pendimethalin microcapsule suspending agent, specifically includes following reaction
Step:
(1) 1g pendimethalin, 2g naphthalene diisocyanate, 10g PBA-580,0.5g MOCA, 6g AEO-5 dispersion are weighed
Agent, 0.2g silicon defoaming agent, 5g glycerine antifreeze, 0.5g benzoic acid sodium salt preservative, 0.2g xanthan gum thickener and 10g chlorine
Change sodium, and weighs the water of surplus based on 100g total amount, it is spare；
(2) it prepares dispersed phase: above-mentioned load weighted pendimethalin, naphthalene diisocyanate, PBA-580 is uniformly mixed, make
It is standby to obtain dispersed phase；
(3) it prepares continuous phase: above-mentioned load weighted MOCA chain extender, AEO-5 dispersing agent, silicon defoaming agent is uniformly mixed,
Dispersed phase is prepared；
(4) it prepares micro-capsule: the temperature of microreactor will be set to 50 DEG C, by the above-mentioned dispersed phase being prepared and continuously
It is mutually respectively charged into stirred tank, is injected dispersed phase and continuous phase into microreactor with the speed of 100mL/min using pump is injected
Channel in carry out reaction micro-capsule be prepared, and collected with beaker, control discharging speed is 100mL/min, makes micro-capsule in wave
10min is reacted in shape microreactor channel forms Microcapsules Size D90It can be between 2-3 μm；
(5) it prepares microcapsules: above-mentioned load weighted benzoic acid sodium salt, the third three being added into the beaker of above-mentioned collection micro-capsule
Alcohol, xanthan gum and sodium chloride stir evenly and pendimethalin microcapsule suspending agent can be obtained；
(6) equipment is cleaned: after reaction, microreactor temperature being controlled at 50 DEG C, is pumped in time to micro- reaction with injecting
Device squeezes into recirculated water, until cleaning up.
Embodiment 3:
The embodiment of the present invention 3 discloses a kind of preparation method of pendimethalin microcapsule suspending agent, specifically includes following reaction
Step:
(1) 45g pendimethalin, 10g methyl diphenylene diisocyanate, 1gPDA-1000,0.2g diamine are weighed respectively
XTJ-500,10g styryl phenol polyethenoxy ether dispersing agent, 2g polyether antifoam agent, 3g potassium nitrate, 2g sorbic acid sylvite anti-corrosion
Agent, 3g propylene glycol antifreeze and 2g aluminium-magnesium silicate thickener, and based on 100g total amount weigh surplus water, it is spare；
(2) it prepares dispersed phase: above-mentioned load weighted pendimethalin, methyl diphenylene diisocyanate and polypropylene glycol is added
Heat is melted and is uniformly mixed, and dispersed phase is prepared；
(3) continuous phase is prepared: by above-mentioned load weighted styryl phenol polyethenoxy ether dispersing agent, diamine XTJ-500
It is mixed evenly with water, continuous phase is prepared；
(4) it prepares micro-capsule: the temperature of microreactor is set to 70 DEG C, by the above-mentioned dispersed phase being prepared and continuous phase
It is respectively charged into stirred tank, is pumped dispersed phase with the speed of 200mL/min, continuous phase using injecting with the speed of 100mL/min
It injects to carry out reacting in the channel of microreactor and micro-capsule is prepared, and collected with beaker, control discharging speed is 300mL/
Min makes micro-capsule react 20min in waveform microreactor channel, forms Microcapsules Size D90It can be between 5--6 μm；
(5) it prepares microcapsules: above-mentioned load weighted potassium nitrate, sorbic acid sylvite being added into the beaker of above-mentioned collection micro-capsule
Preservative, propylene glycol antifreeze and aluminium-magnesium silicate thickener, stir evenly and pendimethalin microcapsule suspending agent can be obtained；
(6) equipment is cleaned: after reaction, microreactor temperature being controlled at 70 DEG C, is pumped in time to micro- reaction with injecting
Device squeezes into recirculated water, until cleaning up.
Embodiment 4
The embodiment of the present invention 4 discloses a kind of preparation method of pendimethalin microcapsule suspending agent, specifically includes following reaction
Step:
(1) 45g pendimethalin, 10g methyl diphenylene diisocyanate, 5g polypropylene glycol, 0.2g second two are weighed respectively
Amine, 10g styryl phenol polyethenoxy ether dispersing agent, 3g potassium chloride, 2g organic silicon defoamer, 2g sorbic acid sylvite preservative,
3g propylene glycol antifreeze and 2g aluminium-magnesium silicate thickener, and based on 100g total amount weigh surplus water, it is spare；
(2) it prepares dispersed phase: above-mentioned load weighted pendimethalin, methyl diphenylene diisocyanate and polypropylene glycol is added
Heat is melted and is uniformly mixed, and dispersed phase is prepared；
(3) continuous phase is prepared: by above-mentioned load weighted styryl phenol polyethenoxy ether dispersing agent, the naphthalene sulfonic acids of modification
Salt, ethylenediamine and water are mixed evenly, and continuous phase is prepared；
(4) it prepares micro-capsule: the temperature of microreactor is set to 70 DEG C, by the above-mentioned dispersed phase being prepared and continuous phase
It is respectively charged into stirred tank, is pumped dispersed phase with the speed of 200mL/min, continuous phase using injecting with the speed of 100mL/min
It injects to carry out reacting in the channel of microreactor and micro-capsule is prepared, and collected with beaker, control discharging speed is 300mL/
Min makes micro-capsule react 20min in waveform microreactor channel, forms Microcapsules Size D90It can be between 5--6 μm；
(5) it prepares microcapsules: above-mentioned load weighted potassium chloride, sorbic acid sylvite being added into the beaker of above-mentioned collection micro-capsule
Preservative, propylene glycol antifreeze and aluminium-magnesium silicate thickener, stir evenly and pendimethalin microcapsule suspending agent can be obtained；
(6) equipment is cleaned: after reaction, microreactor temperature being controlled at 70 DEG C, is pumped in time to micro- reaction with injecting
Device squeezes into recirculated water, until cleaning up.
Embodiment 5
The embodiment of the present invention 5 discloses a kind of preparation method of pendimethalin microcapsule suspending agent, specifically includes following reaction
Step:
(1) 45g pendimethalin, 10g methyl diphenylene diisocyanate, 10g polypropylene glycol, 0.2g second two are weighed respectively
Amine, 10g styryl phenol polyethenoxy ether dispersing agent, 3g sodium chloride, 1g organic silicon defoamer, 2g sorbic acid sylvite preservative,
3g propylene glycol antifreeze and 2g aluminium-magnesium silicate thickener, it is spare；
(2) it prepares dispersed phase: above-mentioned load weighted pendimethalin, methyl diphenylene diisocyanate and polypropylene glycol is added
Heat is melted and is uniformly mixed, and dispersed phase is prepared；
(3) continuous phase is prepared: by above-mentioned load weighted styryl phenol polyethenoxy ether dispersing agent, the naphthalene sulfonic acids of modification
Salt, ethylenediamine and water are mixed evenly, and continuous phase is prepared；
(4) it prepares micro-capsule: the temperature of microreactor is set to 70 DEG C, by the above-mentioned dispersed phase being prepared and continuous phase
It is respectively charged into stirred tank, is pumped dispersed phase with the speed of 2000mL/min, continuous phase using injecting with the speed of 1000mL/min
It spends react in the channel for injecting microreactor and micro-capsule is prepared, and collected with beaker, control discharging speed is
300mL/min makes micro-capsule react 20min in waveform microreactor channel, forms Microcapsules Size D90It can be between 5-6 μm；
(5) it prepares microcapsules: above-mentioned load weighted sodium chloride, sorbic acid sylvite being added into the beaker of above-mentioned collection micro-capsule
Preservative, propylene glycol antifreeze and aluminium-magnesium silicate thickener, stir evenly and pendimethalin microcapsule suspending agent can be obtained；
(6) equipment is cleaned: after reaction, microreactor temperature being controlled at 70 DEG C, is pumped in time to micro- reaction with injecting
Device squeezes into recirculated water, until cleaning up.
Embodiment 6
The embodiment of the present invention 6 discloses a kind of preparation method of pendimethalin microcapsule suspending agent, specifically includes following reaction
Step:
(1) 45g pendimethalin, 10g methyl diphenylene diisocyanate, 10g polypropylene glycol, 0.2g second two are weighed respectively
Amine, 1g styryl phenol polyethenoxy ether dispersing agent, 3g sodium chloride, 1g organic silicon defoamer, 5g sorbic acid sylvite preservative, 8g
Propylene glycol antifreeze and 5g white carbon black thickener, and based on 100g total amount weigh surplus water, it is spare；
(2) it prepares dispersed phase: above-mentioned load weighted pendimethalin, methyl diphenylene diisocyanate and polypropylene glycol is added
Heat is melted and is uniformly mixed, and dispersed phase is prepared；
(3) continuous phase is prepared: by above-mentioned load weighted styryl phenol polyethenoxy ether dispersing agent, the naphthalene sulfonic acids of modification
Salt, ethylenediamine and water are mixed evenly, and continuous phase is prepared；
(4) it prepares micro-capsule: the temperature of microreactor is set to 60 DEG C, by the above-mentioned dispersed phase being prepared and continuous phase
It is respectively charged into stirred tank, is pumped dispersed phase with the speed of 1000mL/min, continuous phase using injecting with the speed of 1000mL/min
It spends react in the channel for injecting microreactor and micro-capsule is prepared, and collected with beaker, control discharging speed is
2000mL/min makes micro-capsule react 20min in waveform microreactor channel, forms Microcapsules Size D90It can be between 5-6 μm；
(5) it prepares microcapsules: above-mentioned load weighted sodium chloride, sorbic acid sylvite being added into the beaker of above-mentioned collection micro-capsule
Preservative, propylene glycol antifreeze and white carbon black thickener, stir evenly and pendimethalin microcapsule suspending agent can be obtained；
(6) equipment is cleaned: after reaction, microreactor temperature being controlled at 60 DEG C, is pumped in time to micro- reaction with injecting
Device squeezes into recirculated water, until cleaning up.
Comparative example 1
(1) 45g pendimethalin, 10g methyl diphenylene diisocyanate, 0.2g ethylenediamine, 10g styrene are weighed respectively
Base phenol polyethenoxy ether dispersing agent, 3g modified naphthalene sulfonate, 2g sorbic acid sylvite preservative, 3g propylene glycol antifreeze and 2g silicon
Sour magnalium thickener, and based on 100g total amount weigh surplus water, it is spare；
(2) dispersed phase is prepared: simultaneously by above-mentioned load weighted pendimethalin and methyl diphenylene diisocyanate heating and melting
It is uniformly mixed, dispersed phase is prepared；
(3) continuous phase is prepared: by above-mentioned load weighted styryl phenol polyethenoxy ether dispersing agent, the naphthalene sulfonic acids of modification
Salt, ethylenediamine and water are mixed evenly, and continuous phase is prepared；
(4) it prepares micro-capsule: the temperature of microreactor is set to 70 DEG C, by the above-mentioned dispersed phase being prepared and continuous phase
It is respectively charged into stirred tank, is pumped dispersed phase with the speed of 200mL/min, continuous phase using injecting with the speed of 100mL/min
It injects to carry out reacting in the channel of microreactor and micro-capsule is prepared, and collected with beaker, control discharging speed is 300mL/
Min makes micro-capsule react 20min in waveform microreactor channel, forms Microcapsules Size D90It can be between 5--6 μm；
(5) prepare microcapsules: be added into the beaker of above-mentioned collection micro-capsule above-mentioned load weighted sorbic acid sylvite preservative,
Propylene glycol antifreeze and aluminium-magnesium silicate thickener, stir evenly and microcapsule suspending agent can be obtained；
(6) equipment is cleaned: after reaction, microreactor temperature being controlled at 70 DEG C, is pumped in time to micro- reaction with injecting
Device squeezes into recirculated water, until cleaning up.
One, the pendimethalin microcapsule suspending agent obtained to above-described embodiment 3 and comparative example 1 detects, and testing result is such as
Shown in the following table 1.
Table 1
Can obviously be learnt by the result in above-mentioned table 1: compared to comparative example 1, the embodiment of the present invention 3 is prepared micro-
Its stability test result of wafer is more preferable, and especially the effect when carrying out cold storage and frozen process experiment is more preferable；Analysis is due to this
Invention introduces soft segment in cyst material, increases capsule material elasticity, and in temperature change, cyst wall is different elastic with the state of capsule-core
Adjustment, avoids capsule-core crystal from being precipitated, and quality is more stable；1 cyst wall of comparative example is only segmented polyurethane, and cyst wall is hard, in low temperature
It follows the string and is easily broken, crystal is caused to be precipitated, cause to influence product stability.It can be seen that the present invention is preferred by formula
Pendimethalin microcapsule suspending agent obtained has excellent survey storage stability, has good practical value.
Two, rate of release is carried out to the above-mentioned pendimethalin microcapsule suspending agent being prepared and control efficiency detects.
(1) rate of release inspection is carried out to the pendimethalin microcapsule suspending agent that above-described embodiment 1-5 and comparative example 1 are prepared
It surveys.
The measuring method of rate of release: weighing effective component raw medicine and each 1g of sample, mixed with a certain amount of diatomite respectively
It closes, is added separately in two glass columns (H=50cm, D=4.5cm) equipped with diatomite (H=35cm) after mixing,
100ml deionized water is added respectively daily into pillar.The diatomite of surface layer 5cm height is excavated after 30d, remaining part, with
2cm is that unit successively takes out soil sample, and acetonitrile extraction is used after drying, is filtered, filtrate is taken, surveys effective component mass fraction, is drawn
Relational graph between diatomite depth and leaching is as shown in Figure 1.
(2) control efficiency detection is carried out to above-described embodiment 3-5, comparative example 1
Using 33% pendimethalin missible oil as control group, above-mentioned pendimethalin microcapsules is observed respectively under for examination concentration to cotton
Safe influence is spent, insecticide-applying way is using soil spraying treatment before rear seedling is broadcast, and the prevention and treatment of weeds is imitated in investigation in 30 days after administration
Fruit, as a result as shown in table 2 below.
Table 2
It can obviously be learnt by the result in above-mentioned table 2: under equally effective component dose, crop field test examples 4 > reality
Apply 3 > embodiment of example, 5 > 33% pendimethalin missible oil > comparative example 1.The drug effect for wherein introducing the embodiment 3,4,5 of soft segment is obviously excellent
In missible oil, illustrate that preventive effect, rate of release and laboratory fitting data one can be improved in pendimethalin microcapsules disclosed by the invention
It causes, is more matched with field crop growth cycle, weed control effect is better.And comparative example 1 is also micro-capsule but drug effect is worse than missible oil,
Analysis is that effective component, which releases, after rupture plays drug effect, but some effective component is difficult to release since softgel shell is hard
It puts or release concentration is lower than effective concentration, cause later period control efficiency poor.In embodiment 3-5, soft segment mass fraction is different, causes
Rate of release is different, and control efficiency is variant.Crop field drug effect proves the micro-capsule release speed that preparation method disclosed in embodiment 4 obtains
Rate is more matched with the cotton growth period, while can more effectively prevent the decomposition of effective component, illustrates the present invention in practical application
In advantageously, be greatly facilitated agricultural production.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (10)
1. a kind of pendimethalin microcapsule suspending agent, which is characterized in that including following weight percentage components: the two of 1%-50%
Penta spirit of first, the capsule material of 4.2%-35%, the dispersing agent of 1%-10%, the defoaming agent of 0.2%-2%, 1%-8% antifreeze,
The preservative of 0.2%-5%, the thickener of 0.2%-5%, the salt of 2-10% and the water of surplus；
The capsule material is to pass through the polyurethane that crosslinking curing obtains, the isocyanide by isocyanates, polyurethane soft segment and chain extender
The weight ratio of acid esters, polyurethane soft segment and chain extender is 2-10:2-20:0.2-5.
2. a kind of pendimethalin microcapsule suspending agent according to claim 1, which is characterized in that the isocyanates includes rouge
Fat race isocyanates or aromatic isocyanate.
3. a kind of pendimethalin microcapsule suspending agent according to claim 1, which is characterized in that the polyurethane soft segment includes
Polyether polyol, the polyether polyol are that ethylene oxide and propylene oxide have rule or statistic copolymer, the polyethers
The structural formula of polyalcohol are as follows:
The R includes propylene glycol, ethylene glycol, bisphenol-A, glycerol, pentaerythrite or diaryl phenolic condensates；
The n is the integer of 0-100, and the m is the integer of 0-100, the sum of the n and m for 0-100 integer, and the n and
The m is not 0 simultaneously.
4. a kind of pendimethalin microcapsule suspending agent according to claim 1, which is characterized in that the polyurethane soft segment includes
Polyester polyol, the structural formula of the polyester polyol are as follows:
The R1For C2-C6Carbon chain compound, the R2For C2H5, the n1 is the integer of 1-100.
5. a kind of pendimethalin microcapsule suspending agent according to claim 1, which is characterized in that the chain extender is including being two
The structural formula of first amine, the diamine is
H2N-R3-NH2
The R3Including C1-C12Carbon chain compound；The R3It further include the copolymer of propylene oxide and ethylene oxide, the ring
The structural formula of the copolymer of Ethylene Oxide and ethylene oxide is
The n2 is the integer of 1-100, and the m2 is the integer of 1-100, the sum of the n2 and m2 for 2-100 integer.
6. a kind of pendimethalin microcapsule suspending agent according to claim 1, which is characterized in that the dispersing agent includes fat
Alcohol polyethers, organic silicon dispersing agent or sulphosuccinates.
7. a kind of pendimethalin microcapsule suspending agent according to claim 1, which is characterized in that the salt include sodium chloride,
One of sodium nitrate, sodium sulphate, potassium chloride, potassium nitrate, ammonium sulfate, sodium citrate, potassium citrate or sodium oxalate are a variety of
Mixture.
8. a kind of preparation method of the pendimethalin microcapsule suspending agent as described in claim 1-8 any one, which is characterized in that
It is prepared using continuous reaction technique or intermittent reaction technique；The continuous reaction technique is based on microchannel or pipe
Formula reactor prepares pendimethalin microcapsules.
9. a kind of preparation method of pendimethalin microcapsule suspending agent according to claim 8, which is characterized in that specifically include
Following reaction step:
(1) a kind of pendimethalin suspension according to any one of claims 1 to 8, weigh pendimethalin, isocyanates,
Polyurethane soft segment, chain extender, dispersing agent, defoaming agent, antifreeze, preservative, thickener, Yan Heshui, it is spare；
(2) it prepares dispersed phase: pendimethalin, isocyanates and polyurethane soft segment being uniformly mixed, dispersed phase is obtained；
(3) it prepares continuous phase: dispersing agent, chain extender and defoaming agent being added to the water, stirs evenly and is prepared into continuous phase；
(4) it prepares micro-capsule: the above-mentioned dispersed phase being prepared and continuous phase is respectively charged into stirred tank, then pushed away with injecting pump
It injects in the channel of microreactor, carries out reaction and micro-capsule is prepared；
(5) prepare microcapsule suspending agent: the micro-capsule that Xiang Shangshu is prepared is added antifreeze, preservative, thickener and salt and is prepared into
Microcapsule suspending agent.
(6) cleaning equipment.
10. a kind of preparation method of pendimethalin microcapsule suspending agent according to claim 9, which is characterized in that the step
Suddenly reaction temperature is 50-70 DEG C in (4), reaction time 8-20min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114246182A (en) * | 2021-12-30 | 2022-03-29 | 江苏仁信作物保护技术有限公司 | Pendimethalin microcapsule suspending agent and production process thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102770023A (en) * | 2010-02-03 | 2012-11-07 | 联合磷业有限公司 | An improved formulation |
| CN105076129A (en) * | 2014-04-22 | 2015-11-25 | 广东华润涂料有限公司 | Insecticide microcapsules and preparation method thereof |
| CN108552170A (en) * | 2018-03-27 | 2018-09-21 | 江苏精禾界面科技有限公司 | A kind of Pendimethalin microcapsules and its high efficiency preparation method |
-
2018
- 2018-12-21 CN CN201811574105.2A patent/CN109497061A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102770023A (en) * | 2010-02-03 | 2012-11-07 | 联合磷业有限公司 | An improved formulation |
| CN105076129A (en) * | 2014-04-22 | 2015-11-25 | 广东华润涂料有限公司 | Insecticide microcapsules and preparation method thereof |
| CN108552170A (en) * | 2018-03-27 | 2018-09-21 | 江苏精禾界面科技有限公司 | A kind of Pendimethalin microcapsules and its high efficiency preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114246182A (en) * | 2021-12-30 | 2022-03-29 | 江苏仁信作物保护技术有限公司 | Pendimethalin microcapsule suspending agent and production process thereof |
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