CN105145567B - pretilachlor aqueous emulsion and preparation method thereof - Google Patents

Abstract

The invention provides a kind of pretilachlor aqueous emulsion and preparation method thereof.Described pretilachlor aqueous emulsion includes：Pretilachlor 20% ~ 60%, emulsifying agent 1% ~ 5%, structure thixotropic agent 0.1% ~ 0.5%, PH conditioning agents 0.1% ~ 1%, antifreeze 1% ~ 5%, water 30% ~ 70%.Invention also improves current aqueous emulsion product processing technology, the energy consumption in process can be greatly reduced.

Description

Pretilachlor aqueous emulsion and preparation method thereof

Technical field

The present invention relates to formulations of pesticide manufacture field, and in particular to the improvement of a kind of pesticide emulsion in water and its processing technology.

Background technology

Pretilachlor（Pretilachlor）, CAS 51218-45-2, the chloro- N- of chemical name 2-（1- methyl -2- methoxies Ethyl）-N-（2-ethyl-6- aminomethyl phenyls）Acetamide.Physicochemical property：Sterling is colourless liquid, b.p.135 DEG C/0.1Pa, phase To density 1.076（20℃.）, vapour pressure 0.133 × 10^{- 3}Pa.It is soluble in most of organic solvents, 20 DEG C of volumes in water Solubility is 50mg/L, distribution coefficient（N-octyl alcohol/water）12020. normal temperature storages 2 years are stable.Hydrolysising half-life is at 20 DEG C 20 ~ 50d. of half-life period in 200d (pH=1 ~ 9), 14d (Ph=13), soil

Pretilachlor is selective preemergence herbicide, cell division inhibitor.Weeds are absorbed by middle hypocotyl and plumule Medicament, interferencing protein synthesis, also has indirect influence to the photosynthesis and respiration of weeds.Typically by soil treatment, The weeds such as rice terrace barnyard grass, Monochoria vaginalis, difformed galingale herb, needle spikesedge herb are prevented and kill off, it is poor to perennial weeds preventive effect.

Progressively adjustment with the requirement of national environmental protection laws and regulations more and more sternly with industrial policy, in the market third Careless amine product is just from traditional missible oil formulation to aqueous emulsion agent transition, in current general aqueous emulsion processing technology In, conventional method is that emulsifying agent etc. is added into oil phase, and the composition such as thickener, stabilizer, antifreezing agent adds aqueous phase, then cut in height Under conditions of cutting, aqueous phase material is slowly added into oil phase, by the continuously input of mechanical energy, lasting high speed is cut Cut, aqueous phase system is disperseed in oil-based system, emulsification makes system first complete water-in-oil system, with continuing for aqueous phase system Increase, the viscosity of system continues to increase, after critical size is reached, system is transformed into oil-in-water system by water-in-oil system, most The configuration process of aqueous emulsion product is completed eventually.But in current processing technology, whole processing process is required for lasting High speed shear, although product forms are environmentally friendly, machining process still huge energy consumption, and in machining process, greatly Partial mechanical energy is not stayed in system finally, but is lost in the way of heat energy in environment.Cause the energy unnecessary Waste.

The content of the invention

Therefore, the present invention, which provides one kind, need not use high-speed shearing equipment, it is only necessary to be stirred using normal conventional Complete the preparation method of processing.

The technical scheme is that, a kind of pretilachlor aqueous emulsion, describing pretilachlor aqueous emulsion includes：Pretilachlor 20% ~ 60%, emulsifying agent 1% ~ 5%, structure thixotropic agent 0.1% ~ 0.5%, PH conditioning agents 0.1% ~ 1%, antifreeze 1% ~ 5%, water 30% ~ 70%.

Further, according to actual needs, minimal amount of bactericide may be also included in this aqueous emulsion product.

According to pretilachlor aqueous emulsion of the present invention, the emulsifying agent described is modified rosin base polyoxyethylene ether phosphorus Acid esters triethanolamine salt and castor oil polyoxyethylene ether phosphate mixture.

According to pretilachlor aqueous emulsion of the present invention, the structure thixotropic agent is the cross linked polyacrylate of different polymerization degree Resin.

According to pretilachlor aqueous emulsion of the present invention, described PH conditioning agents are triethanolamine.

According to pretilachlor aqueous emulsion of the present invention, described antifreeze is glycerine.

Present invention also offers a kind of improvement processing technology of pretilachlor aqueous emulsion, the technique is carried out as follows：

1）The emulsifying agent of 1 ~ 5 part of addition in 20 ~ 60 parts of pretilachlor active compound, forms oil phase；

2）In 30 ~ 70 parts of water, 0.1 ~ 0.5 part of structure thixotropic agent, slightly dispersed with stirring are added, aqueous phase is formed；

3）In the case of stirring at low speed or without stirring, oil phase is added in aqueous phase, oil phase automatic quick expansion in aqueous phase Emulsification is dissipated, emulsion is formed；

4）After oil phase spreads completely in aqueous phase, PH conditioning agent triethanolamines are added, stirring at low speed is quiet after 3 ~ 5 minutes Put more than 30 minutes, the viscosity of system rises to 200 ~ 500 mPa.s automatically, forms stable emulsion dispersion system.

It is an advantage of the current invention that compared to existing general aqueous emulsion processing formula, it is necessary to add oil phase using aqueous phase Method, be required for carrying out high speed shear to system using powerful mechanized clipping equipment in whole process making body System is scattered, emulsification, and the emulsion dispersion for making oil phase uniform particle in system by the technique of phase inversion is formed and stablized relatively into water System.For existing common processes, a 5000M³Aqueous emulsion process equipment, at least need configuration one 25 ~ 30 kilowatts When high-speed shearing machine, and all must be turned on during the entire process of Product processing, the mechanical energy one that shearing equipment is produced Point by the energy required for itself phase inversion of system absorption system, and the overwhelming majority all becomes invalid heat energy and lost, right The small active compound of some thermal capacity or thermally sensitive active compound must also install the heat sinks such as freezing additional on cutting kettle, virtually More increase the consume of the energy.And in present inventor, by the rational allocation of emulsifier proportion, you can make pretilachlor in water Disperse automatically without external energy input, and form stable emulsion, a 5000M³Aqueous emulsion process equipment, only The normal agitation of one 5 ~ 7.5 kilowatt hour of configuration is needed, is stirred 5 ~ 10 minutes in the last regulation acid-base value of product.

It is another advantage of the present invention that compared to existing general aqueous emulsion processing formula.Because the original of pretilachlor Medicine proportion is 1.076, and proportion is more great than the ratio of water, and the pretilachlor missible oil particle disperseed in system under gravity can be slow Sedimentation, causes concentration difference above and below system generation, and precipitation gathers integral particle and equally can also change the internal stress of system Structure, causes system to be demulsified in placement process and product is become unqualified, and in order to solve because caused by density difference The problem of flocculation is assembled or suspended in particle precipitation, xanthans, Arabic gum or carboxymethyl cellulose etc. are added generally in aqueous phase Aqueous colloidal makes the viscosity of aqueous phase become big, and resistance when making the particle move in aqueous phase becomes greatly, so that during the sedimentation of particle Between it is elongated, reach extension shelf life of products purpose.But the aqueous colloidals such as xanthans, Arabic gum or carboxymethyl cellulose exist The viscosity of aqueous phase is set to become big, metering is inaccurate product pellet sedimentation also brings along product packaging while slack-off when, is packed when using The drawbacks of residual becomes big is toppled in container.Xanthans, Arabic gum or carboxymethyl cellulose isocolloid are microorganism secretion simultaneously Material or natural glucide, it can be decomposed in aqueous phase by microorganisms such as bacteriums as sugar source, cause product putting Viscosity is tapered into during putting, and rise gas, and a certain amount of anti-corrosion must also be added in the problems such as product packaging is deformed, therefore system Agent.The structure thixotropic agent that the present invention is used is the CP of different polymerization degree, and the product is fully synthetic macromolecule Product, small with addition, thickening efficiency is high, and thixotroping flow is short, do not have unnecessary carbon source on molecular structure, will not be by microorganism Many advantages, such as corrosion.When the characteristics of maximum of this thickener is that PH is adjusted to 6 ~ 7 by product in aqueous phase, system becomes at once Into clear, colorless jelly, do not change the color of system script, and the thixotroping flow of system is very short, and system is viscous when static Degree is up to 300 ~ 500mPa.s, but as long as a slight agitation, the viscosity of system can drop to 20 ~ below 30mPa.s at once.It is static 300 ~ 500 mPa.s can be returned to again in 50 ~ 10 minutes afterwards, infinitely can be repeated without losing its viscosity.Both production can be solved The problem of product are precipitated or flocculated in placement process, can also solve product and topple over the problem of residual is big in application.

Embodiment

Embodiment 1

Pretilachlor active compound（96%）	31.5%
		APRO-5020	1.2%
PRZ-59	2.4%
		CARBPOL 934	0.2%
CARBPOL 941	0.1%
		Triethanolamine	0.3%
Glycerine	5.0%
		Deionized water	Supply 100%

1.2 grams of emulsifying agent APRO-5020 and 2.4 grams of emulsifying agent PRZ-59 are added in 31.5 grams of pretilachlor active compounds, formed Oil phase.0.2 gram of CARBPOL 934 and 0.1 gram of CARBPOL 941 and 5 grams of glycerine are added in 59.3 grams of deionized waters, used Glass bar is stirred, and soaks it, forms aqueous phase.Oil phase is slowly added in aqueous phase, its thermoplastic polymer is treated, emulsification forms uniform breast Shape liquid.PH conditioning agent triethanolamines are added, with glass bar mild agitation one minute, 3 ~ 5 minutes is stood, treats that system viscosity rises to 300mpa.s or so, that is, complete configuration.

Embodiment 2

Pretilachlor active compound（96%）	52.5%
		APRO-5020	2.2%
PRZ-59	2.8%
		CARBPOL 934	0.1%
CARBPOL 978	0.1%
		Preservative Kathon CG(Methylchloroisothiazolinone/Methylisothiazolinone combination)	0.1%
Triethanolamine	0.2%
		Glycerine	5.0%
Deionized water	Supply 100%

2.2 grams of emulsifying agent APRO-5020 and 2.8 grams of emulsifying agent PRZ-59 are added in 52.5 grams of pretilachlor active compounds, shape Into oil phase.By 0.1 gram of CARBPOL 934 and 0.1 gram of CARBPOL 978 and 0.1 gram of Preservative Kathon CG(Methylchloroisothiazolinone/Methylisothiazolinone combination) and 5 grams of antifreezing agents the third three Alcohol is added in 37 grams of deionized waters, is stirred with glass bar, is soaked it, forms aqueous phase.Oil phase is slowly added in aqueous phase, it is treated Thermoplastic polymer, emulsification forms uniform emulsion.PH conditioning agent triethanolamines are added, with glass bar mild agitation one minute, 3 are stood ~ 5 minutes, treat that system viscosity rises to 500mpa.s or so, that is, complete configuration.

The normal temperature performance indications of two above example：

Example

Apparent condition

Content

PH

Foam volume

Grain D90

Topple over residual

Index request

It is light yellow to milky

5~8

≤25ml

≤3.0um

≤5.0%

30%EW

Milky thick liquid

30.1

6.5

18 milliliters

0.98

1.2%

50%EW

Milky thick liquid

50.2

6.3

25 milliliters

1.03

1.8%

± ± 2 DEG C, 14 days of the thermodynamic stability index 54 of two above example：

Example

Apparent condition

Content

PH

Foam volume

Grain D90

Topple over residual

Index request

It is light yellow to milky

Degraded≤5.0%

5~8

≤25ml

≤3.0um

≤5.0%

30%EW

Milky thick liquid

29.8

6.8

15 milliliters

1.10

1.4%

50%EW

Milky thick liquid

49.7

6.4

23 milliliters

1.13

2.0%

Pretilachlor aqueous emulsion after heat storage 14 days, is analyzed into all technical, its indices under conditions of 54 ± 2 DEG C Still in claimed range, it is seen that aqueous emulsion is stable under reservoir condition.

0 ± 1 DEG C, 7 days of the cold storage stability indicator of two above example：

Example

Apparent condition

Content

PH

Foam volume

Grain D90

Topple over residual

Index request

It is light yellow to milky

Degraded≤5.0%

5~8

≤25ml

≤3.0um

≤5.0%

30%EW

Milky thick liquid

30.0

6.5

19 milliliters

0.99

1.5%

50%EW

Milky thick liquid

50.2

6.4

23 milliliters

1.07

2.1%

After pretilachlor aqueous emulsion is refrigerated 7 days under conditions of 0 ± 1 DEG C, all technical is analyzed, its indices is still In claimed range, it is seen that aqueous emulsion is also stable under refrigerated conditions.

Claims (5)

1. a kind of pretilachlor aqueous emulsion, it is characterised in that in mass ratio：Including pretilachlor 20% ~ 60%, emulsifying agent 1% ~ 5%, structure Thixotropic agent 0.1% ~ 0.5%, PH conditioning agents 0.1% ~ 1%, antifreeze 1% ~ 5%, water complements to 100%；

The emulsifying agent described is modified rosin base polyoxyethylene groups ether phosphate triethanolamine salt and castor oil polyoxyethylene ether Phosphate mixture；

The structure thixotropic agent is the CP of different polymerization degree.

2. a kind of pretilachlor aqueous emulsion according to claim 1, it is characterised in that also including a small amount of bactericide.

3. a kind of pretilachlor aqueous emulsion according to claim 1, it is characterised in that described PH conditioning agents are three ethanol Amine.

4. a kind of pretilachlor aqueous emulsion according to claim 1, it is characterised in that described antifreeze is glycerine.

5. the preparation method of pretilachlor aqueous emulsion, it is characterised in that carry out according to the following steps：

1）The emulsifying agent of 1 ~ 5 part of addition in 20 ~ 60 parts of pretilachlor active compound, forms oil phase；

2）In 30 ~ 70 parts of water, 0.1 ~ 0.5 part of structure thixotropic agent, slightly dispersed with stirring are added, aqueous phase is formed；

3）In the case of stirring at low speed or without stirring, oil phase is added in aqueous phase, oil phase automatic quick diffusion breast in aqueous phase Change, form emulsion；

4）After oil phase spreads completely in aqueous phase, add pH adjusting agent triethanolamine and pH is adjusted to 6 ~ 7, stirring at low speed 3 ~ 5 After minute, more than 30 minutes are stood, the viscosity of system rises to 200 ~ 500 mPa.s automatically, forms stable Emulsified Dispersion System；

The emulsifying agent described is modified rosin base polyoxyethylene groups ether phosphate triethanolamine salt and castor oil polyoxyethylene ether Phosphate mixture；

The structure thixotropic agent is the CP of different polymerization degree.