CN105777973B - A kind of amphipathic copolymer dispersant, preparation method and application - Google Patents
A kind of amphipathic copolymer dispersant, preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of amphipathic copolymer dispersant, preparation method and application, first configure water-alcohol solution and add chain tra nsfer and polyvinyl alcohol preheating, add initiator, methacrylic acid, Isooctyl acrylate monomer and function monomer, 80~100% neutralization reagents of carboxyl molal quantity are added after reaction, then dealcoholysis is evaporated under reduced pressure, liquid dispersant is obtained after adjusting pH；The liquid dispersant is by being dried to obtain solid dispersion；The function monomer is hydroxy-ethyl acrylate, sodium vinyl sulfonate or both combination, and in mass, the composition of each monomer is：20~80 parts of methacrylic acid, 10~50 parts of Isooctyl acrylate monomer, 0~40 part of hydroxy-ethyl acrylate, 0~20 part of sodium vinyl sulfonate.Use water alcohol system in preparation method of the present invention, the solvent of distillation recovery can continue directly to use without processing, three-waste free discharge, reduce production cost.And dispersant effect prepared by the present invention is good, suspensibility is up to 98.5%.
Description
Technical field
The present invention relates to macromolecule dispersing agent, and in particular to a kind of amphipathic copolymer dispersant, preparation method and application.
Background technology
Polymeric dispersant is the product released in last century, because it has the spies such as longer strand and steric hindrance
Sign so that dispersant can form stable interaction with solid particle, strengthen the dispersion stabilization of solid particle.Therefore it is poly-
Compound dispersant is widely used in the fields such as pigment, dyestuff, water reducer, agricultural chemicals.Such as in pesticides application, for retaining ring
The active compound particle for protecting the formulations of pesticide (such as water dispersible granules) disperses and keeps stable in aqueous, and the requirement to dispersant should
There is hydrophilic radical, ensure there be good " similar compatibility ", it is necessary to increase lipophilic group to improve between dispersant and active compound again
The hydrophobicity of polymeric dispersant.The deficiency of traditional small molecule dispersant is：Adsorbed in solid particles surface insecure, it is easy to
From surface dissociation, solid particle is caused to reassemble or precipitate.And the polyacrylate dispersant for passing through hydrophobically modified passes through
Steric hindrance acts on can make stable system with effects such as electrostatic repulsions, have more preferable dispersion effect than small molecule dispersant.Should
When compound of birdsing of the same feather flock together is used as dispersant, molecular weight is relatively low, and typically thousands of between tens of thousands of, the size of molecular weight is divided dispersant
The ability of dissipating important role.
In recent years, Chinese patent CN201110055926, CN201210014503, CN201110440872,
CN201310702373, CN201310702373, CN201410479767 etc. should be mentioned that methacrylic acid-St is common
Polymers or the terpolymer that the third monomer is added on the basis of bipolymer, its preparation method is with emulsion polymerization, light
Based on the methods of triggering polymerization and catalytic polymerization；Chinese patent CN201110102271, CN200710025659 report are third
Olefin(e) acid-alkyl acrylate copolymer, polymerisation in solution is carried out as medium using emulsion polymerization, organic solvent.Foreign patent
US20030150578, US20046677399 report are methacrylic acid-St copolymer or acrylic acid-benzene second
Alkene bipolymer.
Styrene is as lipophile unit, wherein containing phenyl ring, can form pi-pi bond with the planes of molecules of dispersed particle,
So that dispersed particle can stable dispersion, thus in macromolecule dispersing agent, it is substantially irreplaceable.However, benzene
Ethene has stimulation and anesthetic effect to eye and upper respiratory tract mucosa.
Preparing the emulsion that macromolecule dispersing agent is prepared using emulsion polymerization needs demulsification to obtain solid dispersion, its
The more difficult control of technique；Polymerisation in solution is carried out using organic solvent as solvent, it is necessary to be recycled to solvent, thus add
Production cost.
The content of the invention
The defects of to overcome prior art, the invention provides a kind of amphipathic copolymer dispersant, preparation method and application.
To achieve the above object, the technical scheme is that：
A kind of preparation method of amphipathic copolymer dispersant, first prepare water-alcohol solution and add chain-transferring agent and polyethylene
Alcohol, heating, adds initiator, methacrylic acid, Isooctyl acrylate monomer and function monomer, and carboxyl molal quantity is added after reaction
80~100% neutralization reagents, dealcoholysis is then evaporated under reduced pressure, liquid dispersant is obtained after adjusting pH；The liquid dispersant passes through
It is dried to obtain solid dispersion；
The function monomer is hydroxy-ethyl acrylate, sodium vinyl sulfonate or both combination, and methacrylic acid, acrylic acid are different
The mass ratio of monooctyl ester, hydroxy-ethyl acrylate and sodium vinyl sulfonate is 20~80：10~50：0~40：0~20.
The present invention can prepare liquid dispersant and solid dispersion simultaneously, enrich product category, to meet different shapes
The needs of state dispersant.Use water-alcohol system in preparation method of the present invention, the solvent of distillation recovery without processing can directly after
Continuous use, three-waste free discharge, reduce production cost.And dispersant effect prepared by the present invention is good, suspensibility is reachable
98.5%.The present invention, which adds 80~100% neutralization reagents, can fully ensure that the water solubility of the amphipathic copolymer.The present invention adds
Enter polyvinyl alcohol and scattered protective effect is generated to reaction system.
Preferably, step is：
1) water and isopropanol are added in the reactor, then heat chain-transferring agent and polyvinyl alcohol, agitating and heating；
2) aqueous solution, methacrylic acid, Isooctyl acrylate monomer and the function monomer of initiator are added dropwise into step 1) solution,
Neutralization reagent is added after insulation reaction；
3) it is evaporated under reduced pressure out isopropanol water solution and obtains reaction mixture, liquid dispersant is obtained after adjusting pH；The liquid
Dispersant is by being dried to obtain solid dispersion.
The present invention is using the method that monomer and initiator is progressively added dropwise to better control over product in whole polymerization process
The degree of polymerization, and timely and effectively exclude heat of polymerization.
It is further preferred that heating-up temperature is to 80~90 DEG C in the step 1).
It is further preferred that the quality of the water and isopropanol is methacrylic acid, Isooctyl acrylate monomer and function monomer
2~4 times of gross mass, the mass fraction of isopropanol is 20~70% in water and isopropanol.
It is further preferred that the dosage of the chain-transferring agent is that methacrylic acid, Isooctyl acrylate monomer and function monomer are total
The 0.1~2% of quality, the chain-transferring agent are n- dodecyl mereaptan, mercaptoethanol or TGA, and the dosage of polyvinyl alcohol is first
The 0.2~2% of base acrylic acid, Isooctyl acrylate monomer and function monomer gross mass.
It is further preferred that the initiator is sodium peroxydisulfate, ammonium persulfate or potassium peroxydisulfate, initiator amount is methyl
The 2~8% of acrylic acid, Isooctyl acrylate monomer and function monomer gross mass.On the premise of guaranteeing complete initiated polymerization,
The use of initiator is reduced, reduces production cost.
It is further preferred that the neutralization reagent be sodium hydroxide, potassium hydroxide, ammoniacal liquor, one kind in triethanolamine or
Two kinds.
It is further preferred that time for adding is 1~4h, 2~4h of insulation reaction in the step 2).
It is further preferred that step 3) the regulation pH to 7~8.
Preferably, the solid content of the liquid dispersant is 30~40%；The drying mode is spray drying.By spray
The dried product of mist has good fineness, dispersiveness, mobility and dissolubility.
It is further preferred that the preparation method of the liquid dispersant is, fitted to obtaining adding in solution after by regulation pH
The water of amount, that is, obtain the liquid dispersant that solid content is 30~40%.
A kind of amphipathic copolymer liquid dispersant is made using above-mentioned preparation method.
A kind of amphipathic copolymer solid dispersion is made using above-mentioned preparation method.
Preferably, the average relative molecular mass of the solid dispersion of the amphipathic copolymer dispersant is 2000~20000,
Molecular weight distributing index PDI is less than 2.7.
A kind of application of above-mentioned amphipathic copolymer liquid dispersant in processing inorganic particle and pesticidal preparations.
A kind of application of above-mentioned amphipathic copolymer solid dispersion in processing inorganic particle and pesticidal preparations.
Compared with prior art, beneficial effects of the present invention are：
1) amphipathic copolymer dispersant of the invention has good water solubility, there is good dispersiveness, suspensibility highest
Up to 98.5%；
2) amphipathic copolymer dispersant preparation technology of the invention is simple, it is easy, with short production cycle, distillation recovery to operate
Solvent can be continuing with, three-waste free discharge, be produced suitable for industrial scale.
Brief description of the drawings
Fig. 1 is that polymethylacrylic acid-Isooctyl acrylate monomer-hydroxyethylacrylate copolymer prepared by embodiment 4 disperses
The infrared spectrum of agent；
Fig. 2 is polymethylacrylic acid-Isooctyl acrylate monomer-hydroxy-ethyl acrylate-vinyl sulfonic acid prepared by embodiment 8
The infrared spectrum of sodium quadripolymer dispersant.
Embodiment
With reference to specific embodiment and accompanying drawing, the invention will be further described.
Embodiment 1：
1) synthesis of the different monooctyl ester-hydroxyethylacrylate copolymer of methacrylic acid-acrylic acid
With stirring, thermometer, reflux condensing tube 500mL four-hole boiling flask in add 220g45% isopropanols it is water-soluble
Liquid, 0.17g lauryl mercaptans and 0.80g polyvinyl alcohol are added, is heated to flowing back, reflux temperature is 82 DEG C；By 59.8g metering systems
Acid, 10.6g Isooctyl acrylate monomers, 17.6g hydroxy-ethyl acrylates are well mixed and mix monomer are made, by 3.52g sodium peroxydisulfates
It is dissolved in 84.0g deionized waters, initiator solution is made after well mixed, at a reflux temperature, is added dropwise into four-hole boiling flask
State mix monomer and initiator solution, time for adding 2h.Charging is further continued for reacting 2.5h after terminating, and after insulation terminates, is added dropwise
122.0g20% sodium hydroxide solutions, and be evaporated under reduced pressure out solvent and obtain isopropanol and water mixed liquid, after dealcoholysis terminates, adjust body
The pH value of system is 7~8, and it is 35% to add suitable quantity of water to adjust to solid content, and discharging obtains product liquid.Gained destination scatter agent is molten
Liquid obtains white powder product 1 by spray drying.
2) dispersant determines to the dispersiveness of inorganic mineral
Have to 100ml in plug graduated cylinder and add the dispersant that in 0.4g (being accurate to 0.0001g) above-described embodiment 1 prepared by (1)
With 50ml deionizations, add 1.0g (being accurate to 0.0001g) after dispersant dissolving and treat scattered solid particle titanium dioxide
(TiO2), then plus deionized water is to 100ml, turns upside down 30 times, is every time the 1-2 seconds.Tool plug graduated cylinder is vertically disposed in 30
In DEG C water bath with thermostatic control, half an hour is stood, tool plug graduated cylinder is taken out after half an hour, upper strata 90ml suspension is extracted out with suction pipe is vacuumized,
Completed in 15s.It is m that remaining 10ml suspension is transferred to the quality weighed1Desiccation culture ware in, and use deionized water
Rinse measurer plug graduated cylinder, it is ensured that the precipitum in graduated cylinder is transferred completely into culture dish, and culture dish is put into air dry oven
105 DEG C of drying, weigh m2, calculate the mass M of insoluble matter, M=m2-m1, its suspensibility according to the following formula：
In formula, 1.4000g is polymer and TiO in tool plug graduated cylinder2The quality of particle.
By aforesaid operations step, suspensibility of the prepared polymeric dispersant to tio_2 suspension in embodiment 1
For 98.36%.
Embodiment 2：
With stirring, thermometer, reflux condensing tube 500mL four-hole boiling flask in add the isopropanol waters of 220g 50%
Solution, 0.17g lauryl mercaptans and 0.80g polyvinyl alcohol are added, is heated to flowing back, reflux temperature is 82 DEG C；By 52.8g methyl-props
Olefin(e) acid, 15.8g Isooctyl acrylate monomers, 19.4g hydroxy-ethyl acrylates are well mixed and mix monomer are made, by 3.60g persulfuric acid
Sodium is dissolved in 84.0g deionized waters, and initiator solution is made after well mixed, at a reflux temperature, is added dropwise into four-hole boiling flask
Above-mentioned mix monomer and initiator solution, time for adding 2h.Charging is further continued for reacting 2.5h after terminating, after insulation terminates, drop
Add the sodium hydroxide solutions of 107.7g 20%, and be evaporated under reduced pressure out solvent and obtain isopropanol and water mixed liquid, after dealcoholysis terminates, adjust
The pH value of section system is 7~8, and it is 35% to add suitable quantity of water to adjust to solid content, and discharging obtains product liquid.By gained destination scatter
Agent solution obtains white powder product 2 by spray drying.
By 2) operating procedure in embodiment 1, prepared polymeric dispersant is to tio_2 suspension in embodiment 2
Suspensibility is 98.42%.
Embodiment 3：
With stirring, thermometer, reflux condensing tube 500mL four-hole boiling flask in add 220g55% isopropanols it is water-soluble
Liquid, 0.80g polyvinyl alcohol is added, is heated to flowing back, reflux temperature is 82 DEG C；By 48.8g methacrylic acids, 22.0g acrylic acid
Different monooctyl ester, 17.6g hydroxy-ethyl acrylates are well mixed and mix monomer are made, and 4.22g sodium peroxydisulfates are dissolved in into 84.0g ionized waters
In, initiator solution is made after well mixed, at a reflux temperature, above-mentioned mix monomer and initiator are added dropwise into four-hole boiling flask
Solution, time for adding 2h.Charging is further continued for reacting 2.5h after terminating, and after insulation terminates, it is molten that 99.8g20% sodium hydroxides are added dropwise
Liquid, and be evaporated under reduced pressure out solvent and obtain isopropanol and water mixed liquid, after dealcoholysis terminates, the pH value of regulation system is 7~8, is added suitable
It is 35% that amount water, which is adjusted to solid content, and discharging obtains product liquid.Gained destination scatter agent solution is obtained by spray drying
White powder product 3.
By 2) operating procedure in embodiment 1, prepared polymeric dispersant is to tio_2 suspension in embodiment 3
Suspensibility is 97.25%.
Embodiment 4：
With stirring, thermometer, reflux condensing tube 500mL four-hole boiling flask in add 220g55% isopropanols it is water-soluble
Liquid, 0.17g lauryl mercaptans and 0.80g polyvinyl alcohol are added, is heated to flowing back, reflux temperature is 82 DEG C；By 43.3g metering systems
Acid, 26.4g Isooctyl acrylate monomers, 18.5g hydroxy-ethyl acrylates are well mixed and mix monomer are made, by 3.52g sodium peroxydisulfates
It is dissolved in 84.0g ionized waters, initiator solution is made after well mixed, at a reflux temperature, is added dropwise into four-hole boiling flask above-mentioned
Mix monomer and initiator solution, time for adding 2h.Charging is further continued for reacting 2.5h after terminating, and after insulation terminates, is added dropwise
89.6g20% sodium hydroxide solutions, and be evaporated under reduced pressure out solvent and obtain isopropanol and water mixed liquid, after dealcoholysis terminates, adjust body
The pH value of system is 7~8, and it is 35% to add suitable quantity of water to adjust to solid content, and discharging obtains product liquid.Gained destination scatter agent is molten
Liquid obtains white powder product 4 by spray drying.
By 2) operating procedure in embodiment 1, prepared polymeric dispersant is to tio_2 suspension in embodiment 4
Suspensibility is 97.84%.
By the polymeric dispersant that embodiment 4 synthesizes KBr tablettings, with Japanese Shimadzu IRAffinity-1 type infrared spectrums
Instrument determines its infrared spectrum, as shown in Figure 1.We can obtain from Fig. 1,3439cm-1For hydroxy-ethyl acrylate in polymer
In-OH characteristic absorption peak, 2961cm-1It is-CH3Asymmetric stretching vibration peak, 2931cm-1It is-CH2Asymmetric stretch shake
Dynamic peak, 1732cm-1For the characteristic absorption peak of-C=O in ester, 1562cm-1And 1401cm-1For-COO-Characteristic absorption peak,
1274cm-1And 1160cm-1For the characteristic absorption peak of-C-O-C in ester, in addition in 1640cm-1The characteristic peak containing double bond is had no,
Illustrate that polymerisation is complete.As a result show that the different monooctyl ester-propylene of methacrylic acid-acrylic acid is successfully prepared by polymerisation
Sour hydroxyl ethyl ester terpolymer.
Embodiment 5：
With stirring, thermometer, reflux condensing tube 500mL four-hole boiling flask in add 220g40% isopropanols it is water-soluble
Liquid, 0.17g lauryl mercaptans are added, are heated to flowing back, reflux temperature is 82 DEG C；By 56.8g methacrylic acids, 10.6g acrylic acid
Different monooctyl ester, 12.1g hydroxy-ethyl acrylates, 8.5g sodium vinyl sulfonates are well mixed and mix monomer are made, by 3.52g persulfuric acid
Sodium is dissolved in 84.0g deionized waters, and initiator solution is made after well mixed, at a reflux temperature, is added dropwise into four-hole boiling flask
Above-mentioned mix monomer and initiator solution, time for adding 2h.Charging is further continued for reacting 2.5h after terminating, after insulation terminates, drop
Add 120.0g20% sodium hydroxide solutions, and be evaporated under reduced pressure out solvent and obtain isopropanol and water mixed liquid, after dealcoholysis terminates, regulation
The pH value of system is 7~8, and it is 35% to add suitable quantity of water to adjust to solid content, and discharging obtains product liquid.By gained destination scatter agent
Solution obtains white powder product 5 by spray drying.
By 2) operating procedure in embodiment 1, prepared polymeric dispersant is to tio_2 suspension in embodiment 6
Suspensibility is 96.14%.
Embodiment 6：
With stirring, thermometer, reflux condensing tube 500mL four-hole boiling flask in add the isopropanol waters of 220g 50%
Solution, 0.10g TGAs are added, are heated to flowing back, reflux temperature is 82 DEG C；By 50.8g methacrylic acids, 15.8g propylene
The different monooctyl ester of acid, 13.9g hydroxy-ethyl acrylates, 7.5g sodium vinyl sulfonates are well mixed and mix monomer are made, by 3.64g over cures
Sour sodium is dissolved in 84.0g deionized waters, and initiator solution is made after well mixed, at a reflux temperature, is dripped into four-hole boiling flask
Plus stating mix monomer and initiator solution, time for adding 2h.Charging is further continued for reacting 2.5h after terminating, after insulation terminates,
The sodium hydroxide solutions of 105.7g 20% are added dropwise, and is evaporated under reduced pressure out solvent and obtains isopropanol and water mixed liquid, after dealcoholysis terminates,
The pH value of regulation system is 7~8, and it is 35% to add suitable quantity of water to adjust to solid content, and discharging obtains product liquid.By gained target point
Dispersant solution obtains white powder product 6 by spray drying.
By 2) operating procedure in embodiment 1, prepared polymeric dispersant is to tio_2 suspension in embodiment 6
Suspensibility is 97.22%.
Embodiment 7：
With stirring, thermometer, reflux condensing tube 500mL four-hole boiling flask in add 220g55% isopropanols it is water-soluble
Liquid, 0.80g polyvinyl alcohol is added, is heated to flowing back, reflux temperature is 82 DEG C；By 46.8g methacrylic acids, 22.0g acrylic acid
Different monooctyl ester, 12.2g hydroxy-ethyl acrylates, 7.0g sodium vinyl sulfonates are well mixed and mix monomer are made, by 4.35g persulfuric acid
Sodium is dissolved in 84.0g ionized waters, and initiator solution is made after well mixed, at a reflux temperature, is added dropwise into four-hole boiling flask
State mix monomer and initiator solution, time for adding 2h.Charging is further continued for reacting 2.5h after terminating, and after insulation terminates, is added dropwise
97.0g20% sodium hydroxide solutions, and be evaporated under reduced pressure out solvent and obtain isopropanol and water mixed liquid, after dealcoholysis terminates, adjust body
The pH value of system is 7~8, and it is 35% to add suitable quantity of water to adjust to solid content, and discharging obtains product liquid.Gained destination scatter agent is molten
Liquid obtains white powder product 7 by spray drying.
By 2) operating procedure in embodiment 1, prepared polymeric dispersant is to tio_2 suspension in embodiment 7
Suspensibility is 96.35%.
Embodiment 8：
With stirring, thermometer, reflux condensing tube 500mL four-hole boiling flask in add 220g60% isopropanols it is water-soluble
Liquid, 0.17g TGAs and 0.40g polyvinyl alcohol are added, is heated to flowing back, reflux temperature is 82 DEG C；By 41.3g metering systems
Acid, 26.4g Isooctyl acrylate monomers, 14.3g hydroxy-ethyl acrylates, 6.0g sodium vinyl sulfonates are well mixed and mixing list are made
Body, 3.52g sodium peroxydisulfates are dissolved in 84.0g ionized waters, initiator solution is made after well mixed, at a reflux temperature, to
Above-mentioned mix monomer and initiator solution, time for adding 2h are added dropwise in four-hole boiling flask.Charging is further continued for reacting 2.5h after terminating,
After insulation terminates, 87.0g20% sodium hydroxide solutions are added dropwise, and is evaporated under reduced pressure out solvent and obtains isopropanol and water mixed liquid, take off
After alcohol terminates, the pH value of regulation system is 7~8, and it is 35% to add suitable quantity of water to adjust to solid content, and discharging obtains product liquid.Will
Gained destination scatter agent solution obtains white powder product 8 by spray drying.
By 2) operating procedure in embodiment 1, prepared polymeric dispersant is to tio_2 suspension in embodiment 8
Suspensibility is 97.03%.
The polymeric dispersant that embodiment 8 the is synthesized KBr tablettings of solid after purification, with Japanese Shimadzu
Its infrared spectrum of IRAffinity-1 types determination of infrared spectroscopy, as shown in Figure 2.We can obtain from Fig. 2,3428cm-1
For the characteristic absorption peak of-OH in hydroxy-ethyl acrylate in polymer, 2962cm-1It is-CH3Asymmetric stretching vibration peak,
2932cm-1It is-CH2Asymmetric stretching vibration peak, 1734cm-1For the characteristic absorption peak of-C=O in ester, 1401cm-1For-COO-
Characteristic absorption peak, 1274cm-1And 1160cm-1For the characteristic absorption peak of-C-O-C in ester, 1048cm-1Sulfonic feature is inhaled
Peak is received, in addition in 1640cm-1The characteristic peak containing double bond is had no, illustrates that polymerisation is complete.As a result show to pass through polymerisation
Different monooctyl ester-hydroxy-ethyl acrylate-sodium vinyl sulfonate the quadripolymer of methacrylic acid-acrylic acid is successfully prepared.
Embodiment 9：
With stirring, thermometer, reflux condensing tube 500mL four-hole boiling flask in add 220g55% isopropanols it is water-soluble
Liquid, 0.17g lauryl mercaptans and 0.80g polyvinyl alcohol are added, is heated to flowing back, reflux temperature is 82 DEG C；By 43.9g metering systems
Acid, 27.1g Isooctyl acrylate monomers, 17.0g sodium vinyl sulfonates are well mixed and mix monomer are made, by 3.52g sodium peroxydisulfates
It is dissolved in 84.0g ionized waters, initiator solution is made after well mixed, at a reflux temperature, is added dropwise into four-hole boiling flask above-mentioned
Mix monomer and initiator solution, time for adding 2h.Charging is further continued for reacting 2h after terminating, and after insulation terminates, is added dropwise
89.6g20% sodium hydroxide solutions, and be evaporated under reduced pressure out solvent and obtain isopropanol and water mixed liquid, after dealcoholysis terminates, adjust body
The pH value of system is 7~8, and it is 35% to add suitable quantity of water to adjust to solid content, and discharging obtains product liquid.Gained destination scatter agent is molten
Liquid obtains white powder product 10 by spray drying.
By 2) operating procedure in embodiment 1, prepared polymeric dispersant is to tio_2 suspension in embodiment 9
Suspensibility is 96.22%.
Embodiment 10：
Application of the amphipathic copolymer dispersant of the present invention in 40% difenoconazole suspending agent
Formula composition：Difenoconazole (active compound content 96%, Shandong Dongtai Agrochemical Co., Ltd) 41.7g, the present invention point
Powder (above-described embodiment 3, embodiment 4, embodiment 7, embodiment 8, embodiment 9 prepare liquid dispersant) 2.5g, wetting agent
3013 (Shandong De Shijia Science and Technology Ltd.s)：1.5, ethylene glycol (Tianjin Fu Yu Fine Chemical Co., Ltd)：4.0g, magnesium silicate
Aluminium (material in Suzhou)：1.0, xanthans (2%)：3.0g, running water：Complement to 100g.By above-mentioned adding according to agricultural chemicals suspension agent
Work method is ground, and discharging obtains 40% difenoconazole suspending agent.
Method of testing：Suspensibility is carried out by GB/T14825-2006；Store experiment method：The sample of development is packaged in peace
Train in bottle, carry out heat storage 14 days in (54 ± 2) DEG C constant temperature oven according to HG/T2467.2-2003 methods, suspensibility is surveyed after heat storage
Determined according to above-mentioned suspensibility method of testing.
Table 1 is suspensibility of the inventive dispersant to 40% difenoconazole suspending agent
Embodiment 11：
Application of the amphipathic copolymer dispersant of the present invention in 80% ametryn water dispersible granules
Processing method：By 83.3g ametryns (96%), 6.0g inventive dispersants (above-described embodiment 3, embodiment 4, reality
Apply example 7, embodiment 8, embodiment 9 and prepare solid powder dispersant) and the control dispersant TERSPERSE2700 (U.S.
HUNTSMAN companies, commercial polymers dispersant), 2.0g sodium olefin sulfonates, 4.0g sodium polyphosphates, starch complements to
100g.It is granulated according to the processing method of pesticide water dispersible granules, then 50 DEG C of drying 3h, sieve in constant temperature blast drying oven
Get 80% ametryn water dispersible granules product.
Method of testing is the same as the method for testing in embodiment 7.
Go out from the table below, amphipathic copolymer dispersant prepared by the present invention has very in 80% ametryn water dispersible granules
Good dispersion effect, reach equivalent effect with the TERSPERSE2700 of foreign countries.
Table 2 is suspensibility of the inventive dispersant to 80% ametryn water dispersible granules
Above-mentioned although the embodiment of the present invention is described with reference to accompanying drawing, not to invention protection domain
Limitation, one of ordinary skill in the art should be understood that on the basis of technical scheme those skilled in the art are not required to
Pay various modifications that creative work can make or deformation is still within the scope of the present invention.
Claims (10)
1. a kind of preparation method of amphipathic copolymer dispersant, it is characterized in that, first prepare water-alcohol solution and add chain-transferring agent and
Polyvinyl alcohol, heating, adds initiator, methacrylic acid, Isooctyl acrylate monomer and function monomer, and carboxyl is added after reaction and is rubbed
80~100% neutralization reagents of your number, dealcoholysis is then evaporated under reduced pressure, liquid dispersant is obtained after adjusting pH；The liquid dispersion
Agent is by being dried to obtain solid dispersion；
The function monomer is hydroxy-ethyl acrylate, sodium vinyl sulfonate or both combination, and methacrylic acid, acrylic acid are different pungent
The mass ratio of ester, hydroxy-ethyl acrylate and sodium vinyl sulfonate is 20~80：10~50：0~40：0~20.
2. a kind of preparation method of amphipathic copolymer dispersant as claimed in claim 1, it is characterized in that, step is：
1) water and isopropanol are added in the reactor, then add chain-transferring agent and polyvinyl alcohol, agitating and heating；
2) aqueous solution, methacrylic acid, Isooctyl acrylate monomer and the function monomer of initiator, insulation are added dropwise into step 1) solution
Neutralization reagent is added after reaction；
3) it is evaporated under reduced pressure out isopropanol water solution and obtains reaction mixture, liquid dispersant is obtained after adjusting pH；The liquid dispersion
Agent is by being dried to obtain solid dispersion.
3. a kind of preparation method of amphipathic copolymer dispersant as claimed in claim 2, it is characterized in that, the water and isopropanol
Quality be methacrylic acid, 2~4 times of Isooctyl acrylate monomer and function monomer gross mass, isopropanol in water and isopropanol
Mass fraction is 20~70%.
4. a kind of preparation method of amphipathic copolymer dispersant as claimed in claim 2, it is characterized in that, the chain-transferring agent
Dosage is the 0.1~2% of methacrylic acid, Isooctyl acrylate monomer and function monomer gross mass, and the chain-transferring agent is positive 12
Mercaptan, mercaptoethanol or TGA, the dosage of polyvinyl alcohol is methacrylic acid, Isooctyl acrylate monomer and the total matter of function monomer
The 0.2~2% of amount；
Or, the initiator is sodium peroxydisulfate, ammonium persulfate or potassium peroxydisulfate, initiator amount is methacrylic acid, acrylic acid
The 2~8% of different monooctyl ester and function monomer gross mass；The neutralization reagent is sodium hydroxide, potassium hydroxide, ammoniacal liquor, triethanolamine
One or both of.
5. a kind of preparation method of amphipathic copolymer dispersant as claimed in claim 2, it is characterized in that, the step 3) regulation
PH to 7~8.
6. a kind of preparation method of amphipathic copolymer dispersant as claimed in claim 1, it is characterized in that, the liquid dispersant
Solid content be 30~40%；The drying mode is spray drying.
7. a kind of amphipathic copolymer liquid dispersant is made using any described preparation methods of claim 1-6.
8. a kind of amphipathic copolymer solid dispersion is made using any described preparation methods of claim 1-6.
9. a kind of amphipathic copolymer solid dispersion as claimed in claim 8, it is characterized in that, the amphipathic copolymer solid point
The average relative molecular mass of powder is 2000~20000, and molecular weight distributing index PDI is less than 2.7.
10. a kind of amphipathic copolymer liquid dispersant as claimed in claim 7 is in processing inorganic particle and pesticidal preparations
Using；
Or, a kind of amphipathic copolymer solid dispersion as claimed in claim 8 or 9 is in processing inorganic particle and pesticidal preparations
Application.
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