Method for determining amount of surface-active agents, desorbed from surface of phases division of liquid-liquid in herbicidal dispersed systems

FIELD: agriculture.

SUBSTANCE: emulsion is diluted with water at least in five stages, at that reducing the concentration of surface-active agent in two times after each dilution. The interfacial tension is determined. Creation of the curve of surface tension at the liquid-liquid interface of the surface-active agent concentration is carried out. Emulsion is held at each stage to its full coagulation. The repeated definition of interfacial tension and the definition of the desired amount of surface-active agent on the shift of the isotherm on the horizontal axis is conducted.

EFFECT: invention enables to optimise the content of surface-active agent in formulations of herbicidal preparations.

9 ex, 3 tbl

 

The invention relates to the development of formulations of herbicides and allows to optimize the number of surfactants in the formulations mulgirigala concentrates herbicides.

It is known that the lack of surfactant in the preparative form affects the physico-chemical and performance characteristics of the working water emulsion that reduces the effectiveness of the herbicide drugs [Wmmenu. Chemical engineering fundamentals to the design and improvement of the herbicide preparative forms. - M.: Chemistry, 2006. 320 C.]. On the contrary, unreasonable increase in the content of surfactants in the preparations contributes to the deterioration of their Toxicological characteristics and reduced Biodegradability [Surfactant. The Handbook. Under. edit Art and Gamgebeli. - L.: Chemistry, 1979. - 376 C.]. Thus, the amount of surfactant in herbicide dispersed systems must be optimal, that is sufficient to form a monomolecular adsorption layer on the surface of partition phases herbicide emulsion.

There is a method of determining the thickness of the shell microcapsules based on the amount of surfactant deposited on the surface of the emulsion (prototype). The disadvantage of this method is the difficulty of determining the amount of surfactant at the interface liquid-liquid that contributes to a significant discrepancy between the results of e is sperimental and does not allow to optimize the content of surfactant [Art. Surfactants. - L.: Chemistry, 1981. - 304 S.].

The objective of the invention is the optimization of the content of surfactants in the formulations of herbicide drugs, increasing their herbicide activity.

The problem is solved as follows. The method for determining the number of surface-active substances desorbed from the surface of the partition phase liquid-liquid in herbicide dispersed systems, includes dilution of the emulsion with water at least five stages, while reducing the concentration of surfactant in twice after each dilution, the determination of interfacial tension stalagmometer method, the construction of the curve of surface tension on the boundary of the liquid-liquid surfactant concentration, keeping the emulsion at each stage to complete coagulation, then re-determine the interfacial tension and the magnitude of shift of the isotherms on the x-axis determines the desired amount of surfactant.

Example 1

Mix 20 g of polyoxyethylene isononylphenol (neonols AF 9-12), 75 g of 2-ethylhexanol ester of 2,4-dichlorophenoxyacetic acid (2,4-D) and 5 g of aromatic hydrocarbon solvent nefras And 150/330. 1 g of the obtained concentrate emuleret in 100 ml of water and determine the interfacial tension stalagmometer method, and the particle size of the dispersed phase of the emulsion by the method of optical microscopy is AI. Serially dilute the resulting emulsion with water, thereby reducing the concentration of surfactant in twice after each dilution. After five stages of dilution water to build the curve of the dependence of surface tension on the boundary of the liquid-liquid surfactant concentration. All of the emulsion is kept in the sump before the deposition of the maximum amount of coagulant, then re-determine the interfacial tension. As a result of shift of the isotherms on the x-axis to determine the number of surfactant (wt.%), desorbed from the interface.

Example 2

Similarly app.1. The difference is that the number of neonols AF 9-12 in concentrate amounts to 15 g, the number of nefras And 150/330 - 10,

Example 3

Similarly app.1. The difference is that the number of neonols AF 9-12 in concentrate is 10 g, the number of nefras And 150/330 - 15,

Example 4

Similarly app.1. The difference is that the number of neonols AF 9-12 in concentrate 17.5 g, the number of nefras And 150/330 - 7,5,

Example 5

Similarly app.1. The difference is that instead of neonols AF 9-12 take sintana DC-10, instead of 2-ethylhexanol ester 2,4-D use 2-ethylhexyloxy ever-methoxy-3,6-dichlorobenzoyl acid (dicamba), instead of nefras And 150/330 use nefras AR 120/220. The data in table 2.

Example 6

Similarly PR. The difference is that if estvo cintanya DC-10 17.5 g, the number of nefras AR 120/220 - 7,5,

Example 7

Similarly PR. The difference is that the number of cintanya DC-10 is 15 g, the number of nefras AR 120/220 - 10,

Example 8

Similarly PR. The difference is that the number of cintanya DC-10 22.5 g, the number of nefras AR 120/220 - 2,5,

Example 9 - prototype

Similarly app.1. The difference is that the amount of surfactant is determined in the aqueous and organic phases of the emulsion photocolorimetric method, which allows to determine the total amount of surfactants in two phases, but does not allow one to determine the amount of desorbed from the interface surfactant.

Example 10

Field trials of herbicide preparations carried out on wheat and barley. The soil of the experimental field is ashed soil with a humus content of 8%.

Predominant weeds - young broadleaf and perennial soboliferous: white pigweed, wild radish, amaranth, Daisy field, picolinic, mountaineers, thistles pink and yellow, the bindweed. The treatment is carried out at the tillering stage of wheat and barley using a handheld sprayer. Dose of 0.7 l/ha (op-4) and 0.1 l/ha (op-8), the water flow rate is 100 l/ha the Area of one plot of 10 m2, repeated 4 times. The efficiency of herbicides was evaluated by weight of weeds and crops at the experimental and ntalnyh plots (option without herbicide treatment). The results of the experiments are presented in table 3.

The data in table 1 show that the optimal content of neonols AF 9-12 in herbicide drug based ester 2,4-D 17.5-20%. The thickness of the surfactant adsorption layer is 0,0069 μm for the value of 17.5% and no longer increases with the value of 20%. The area per surfactant molecule, is 1.74·10-7μm2if the value is 17.5% and almost the same is 1.75·10-7μm for option 20%. The data of table 2 show that the optimal content of cintanya DC-10 in the herbicide agent based on broadcast dicamba is 20-22,5%. The thickness of the surfactant adsorption layer is 0,0071 μm for the value of 20% or more is not incremented when the value of 22.5%. The area per surfactant molecule at 1.38·10-7μm2when set to 20% and does not change when the value of 22.5%.

Field trials of herbicide in wheat and barley (table 3) confirmed the advantage of the preparations containing the optimum amount of surfactant. Formulations according to examples No. 1 and No. 4 with the contents of neonols 20% and 17.5% showed higher herbicide activity in comparison with examples 2 and 3 (the content of neonols 15% and 10%). Formulations according to examples No. 5 and No. 8 content cintanya 20% and 22.5%) showed higher herbicide activity in comparison with sample No. 6 and No. 7 (contents of cintanya 17.5% and 15%). The increase in the wheat crop is barley in experiments # 1 and # 4 above, than in experiments # 2 and # 3, as in experiments # 5 and # 8 are higher than in No. 6 and No. 7.

Table 1
Calculation of parameters of the adsorption layer of neonols AF 9-12 in the emulsion herbicide-based drug ester of 2,4-D.
IndicesValue
The number of neonols in the product, wt.%1015of 17.520
The average particle size of the dispersed phase, mcm12521,5
Volume odnri particles, μm3904,7865,454,189to 1.767
The dose of the drug per 1 ha, ml700700700700
The amount of the drug on 1 cm2treatment area, µm37·1067·1067·106
The number of particles on 1 cm2, pieces77371,07·1051,67·106of 3.96·106
The surface area of one particle, μm2452,3978,5412,577,07
The total surface area of particles, μm23,5·1068,4·1062,1·1072,8·107
The amount of emulsion per 1 ha, l100100100100
The amount of emulsion on 1 cm2treatment area, µm3109109109109
The number of neonols, desorbed from the interface, wt.%0,002 0,0150,02
The amount of neonols given its density, μm31,92·104to 5.57·10414,42·10419,2·104
The thickness of the adsorption layer of neonols, mcm0,00550,00660,00690,0069
Weight desorbed of neonols, mcg0,020,0580,150,199
The weight of one mole of neonols, mcg748·106748·106748·106748·106
The number of moles of neonols0,267·10-100,775·10-102,0·10-102,66·10-10
The number of molecules of neonols1,607·1013of 4.66·101312,04·1013 16,01·1013
The area per molecule, μm2at 2,178·10-71,80·10-71,74·10-7a 1.75·10-7

Tandbperson 2
Calculation of parameters of the adsorption layer cintanya DC-10 in the emulsion herbicide preparation on the basis of the ether dicamba
IndicesValue
The number of cintanya in the product, wt.%15of 17.52022,5
The average particle size of the dispersed phase, mcm10721,5
The volume of one particle, μm3523,6179,64,189to 1.767
The dose of the drug per 1 ha, ml100 100100100
The amount of the drug on 1 cm2treatment area, µm3106106106106
The number of particles on 1 cm2, pieces19105568238720565931
The surface area of one particle, μm2314,2other 153.912,577,07
The total surface area of particles, μm26·105to 8.57·1053·1064·106
The amount of emulsion per 1 ha, l100100100100
The amount of emulsion on 1 cm2treatment area, µm3109109 109109
The number of cintanya, desorbed from the interface, wt.%3·10-45,6·10-42,2·10-32,95·10-3
Volume cintanya given its density, μm32,884·1035,384·1032,115·1042,837·104
The thickness of the adsorption layer cintanya, mcm0,0480,00620,007100071
The weight of the desorbed cintanya, mcg0,0030,00560,0220,0295
The weight of one mole of cintanya, mcg610·106610·106610·106610·106
The number of moles of cintanya0,049·10-100,091·10-10 0,361·10-100,483·10-10
The number of molecules of cintanya0,295·10130,548·10-72,173·10132,908·1013
The area per molecule, μm22,034·10-71,564·10-7to 1.38·10-7to 1.38·10-7

Table 3
Herbicide activity of drugs in field experiments
No. of experimentsInhibition of weedsThe grain yield
Young leafLong soboliferouskg/ha+ -
Wheat
1928420,9+2,5
2837919,5+1,1
3786519,2+0,8
4918620,7+2,2
5909621,3+2,9
6788020,0+1,6
7757819,8+1,4
8929621,4+3,0
Control18,4
The barley
1 8623,4+2,9
2827222,3+1,8
37570of 21.9+1,4
4908523,2+2,7
5889223,5+3,0
6788321,8+1,3
7748021,6+1,1
8899423,7+3,2
Control20,5

The method for determining the number of surface-active substances desorbed from the interface liquid-liquid herbicide dispersed systems, including the dilution of the emulsion with water in five stages, while reducing the concentration of surfactant in twice after each dilution, the determination of the interfacial tension, build-up curve of the surface tension at the boundary of liquid-liquid surfactant concentration, keeping the emulsion at each stage to its full coagulation, then re-determination of interfacial tension and determining the desired amount of surfactant largest shift isotherms on the x-axis.



 

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