Viscoelastic auxiliary agent, and composition, preparation method and application thereof (2023)

Multifunctional monomers can be polybasic acids, difunctional acid halides, acid anhydrides, poly(acid anhydrides) and mixtures thereof, and can be used in agricultural chemical compositions, but the preparation process of t...

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[0056] Example 1

[0057] The embodiment of the present invention discloses a droplet viscoelastic water-based polymer additive and a composition thereof. The preparation method specifically includes the following steps:

[0058] (1) Add 2.75g of methanesulfonic acid and 561g of dimer acid (HONGTAI) to the reaction kettle, and replace it with nitrogen 3 times, raise the temperature to 140-160℃, add 156g of diethylenetriamine dropwise, and add Enter nitrogen for dehydration, while controlling the dropping temperature to 140-160℃, and the dropping time for 2.5-3h. After the dropping, control the temperature to 160-165℃ for the maturation reaction. The maturation time is 4-6h. When the water is collected about 36g, test When the acid value is less than 2.5mgKOH/g, add 280g of oleic acid, control the temperature at 180-185℃, and add a little nitrogen for dehydration, the maturation time is 5-7h, when the collected water is about 18g, when the detected acid value is less than 1.8mgKOH/g , Finally, vacuumize at 80-85℃ to remove the volatile components to obtain A1.

[0059] (2) Add 189g of A1 obtained in step (1) to the reactor, and replace it with nitrogen 3 times, raise the temperature to 115-130℃, and pass in 13.9g of ethylene oxide and nitrogen to make the pressure 0.15-0.35 MPa, and aging at 115-130°C for 1-3h, after the pressure remains unchanged, the reaction ends. At 80-85°C, evacuating vacuum to remove volatile components to obtain modified polyethylene polyamine ethoxylate B1 intermediate.

[0060] (3) Add 1.5g of NaOH to the modified polyethylene polyamine ethoxylate B1 intermediate obtained in step (2), replace it with nitrogen again three times, raise the temperature to 100-135°C, remove the water within a certain period of time, and make the reaction kettle Material moisture<

[0061] 0.5%, then the temperature is raised to 100-160°C, 260g of ethylene oxide is introduced, the feeding temperature is controlled at 100-160°C, and the maximum pressure of the feeding is less than 0.35MPa; the feeding is completed. Curing between 120-160℃, when the curing pressure is close to 0.02MPa, nitrogen is introduced to keep the pressure at 0.15-0.25MPa. When the pressure in the reactor remains unchanged, the reaction ends; the maturation time is about 1-3h. At 120-135℃, vacuumize for 0.5-1h, cool down by 70-80℃, add neutralizing reagent, adjust pH to 5-7. Add 84.6g of oleic acid, 2g of p-toluenesulfonic acid, control the temperature at 180-185°C, and add a little nitrogen for dehydration, the maturation time is 5-7h, when the water is collected about 5g, the acid value is less than 0.9mgKOH/g; Product, marked as B1.

[0062] (4) Put 54g of B into a four-necked flask, add 45g of water at 70-80℃, add 7.5g of 50% sodium chloroacetate aqueous solution dropwise, and react for 6-8h at 70-80℃. After the reaction is over, The aqueous solution is removed to obtain a water-based polymer additive C1.

[0063] Weigh 30 g of the sample of Example C1, 20 g of silicone additive SP-408, and 50 g of sulfosuccinic acid bis(2-ethylhexyl) sodium salt system (using methyl oleate as the system). Fully mix and stir at 70°C for 30 minutes to obtain a viscoelastic aid composition with a transparent appearance. The sample is recorded as Example D1.

[0064] Example 2

[0065] The embodiment of the present invention discloses a droplet viscoelastic water-based polymer additive and a composition thereof. The preparation method specifically includes the following steps:

[0066] (1) Add 3.1g p-toluenesulfonic acid and 561g dimer acid (UNIDYME TM 14), and replace with nitrogen 3 times, raise the temperature to 140-160℃, add 347g of pentaethylene hexaamine dropwise, and dehydrate with a little nitrogen, while controlling the temperature of the dropping to 180-190°C, and the dropping time for 2.5- 3h, after dripping, control the temperature at 180-190℃ for maturation reaction, maturation time is 4-6h, when the collected water is about 36g, the acid value is less than 1.8mgKOH/g, add 216g oleic acid, control the temperature at 180-195℃, Dehydrate with a little nitrogen, and the maturation time is 5-7h. When the collected water is about 18g, and the acid value is less than 1.2mgKOH/g, the volatile components can be removed by vacuum at 80-85℃ to obtain A2.

[0067] (2) Add 113.5g of A2 obtained in step (1) to the reactor, and replace it with nitrogen 3 times, raise the temperature to 115-130℃, and pass in 27g of ethylene oxide and nitrogen to make the pressure at 0.15-0.35 MPa, and aging at 115-130°C for 1-3h, after the pressure remains unchanged, the reaction ends. At 80-85°C, evacuating to remove volatile components to obtain modified polyethylene polyamine ethoxylate B2 intermediate.

[0068] (3) Add 1.15g of KOH to the modified polyethylene polyamine ethoxylate B2 intermediate obtained in step (2), replace it with nitrogen again three times, raise the temperature to 100-135°C, and remove the water within a certain period of time to make the reaction kettle Material moisture<

[0069] 0.5%, then the temperature is raised to 100-160°C, 175g EO is introduced, the feeding temperature is controlled at 100-160°C, the maximum pressure of the feeding is less than 0.35MPa; the feeding is completed. Curing between 120-160℃, when the curing pressure is close to 0.02MPa, nitrogen gas is introduced to keep the pressure at 0.15-0.25MPa. When the pressure in the reactor remains unchanged, the reaction ends; the maturation time is about 1-3h. At 120-135℃, vacuumize for 0.5-1h, cool down by 70-80℃, add neutralizing reagent, adjust pH to 5-7. Add 84g of oleic acid, 3.52g of p-toluenesulfonic acid, control the temperature at 180-185℃, and add a little nitrogen for dehydration, the maturation time is 5-7h, when the collected water is about 5g, the acid value is less than 1.2mgKOH/g; Product, marked as B2.

[0070] (4) Add 80g of B2 to a four-necked flask, add 300g of water, add 10.8g of 37.5% hydrogen peroxide aqueous solution dropwise, and react at 70-80℃ for 6-8h. After the reaction, the aqueous solution is removed to obtain a High viscosity low viscosity droplet viscoelastic water-based polymer additive C2.

[0071] Weigh 35 g of sample C2, 15 g of silicone additive Silwet 77, and 50 g of sulfosuccinic acid bis(2-ethylhexyl) sodium salt system (using butanol as the system). Fully mix and stir at 70°C for 30 minutes to obtain a viscoelastic aid composition with a transparent appearance. The sample is recorded as Example D2.

[0072] Example 3

[0073] The embodiment of the present invention discloses a droplet viscoelastic water-based polymer additive and a composition thereof. The preparation method specifically includes the following steps:

[0074] (1) Add 7.5g p-toluenesulfonic acid and 561g dimer acid (UNIDYME TM 18), and replace with nitrogen 3 times, raise the temperature to 140-160℃, add 138g of diethylenetriamine dropwise, and add a little nitrogen for dehydration, while controlling the dropping temperature to 180-190°C, the dropping time is 2.5- 3h, after dripping, control the temperature at 180-190℃ for maturation reaction, maturation time is 4-6h, when collecting water about 35g, the acid value is less than 4mgKOH/g, add 228g coconut oleic acid, control the temperature at 180-195℃, Dehydrate with a little nitrogen, and the maturation time is 5-7h. When the collected water is about 11g, and the acid value is less than 0.8mgKOH/g, the volatile components can be removed by vacuum at 80-85℃ to obtain A3.

[0075] (2) Add 132g of A3 obtained in step (1) to the reaction kettle, and replace it with nitrogen 3 times, raise the temperature to 115-130℃, pass in 12gPO, pass in nitrogen to make the pressure at 0.15-0.35MPa, and at 115 After aging at -130°C for 1-3h, the reaction ends after the pressure remains unchanged. At 80-85°C, evacuating to remove volatile components to obtain modified polyethylene polyamine ethoxylate B3 intermediate.

[0076] (3) Add 1.2g KOH to the modified polyethylene polyamine ethoxylate B3 intermediate obtained in step (2), replace it with nitrogen again three times, raise the temperature to 100-135°C, and remove the water within a certain period of time to make the reaction kettle Material moisture<

[0077] 0.5%, then the temperature is raised to 100-160°C, 106g EO is introduced, the feeding temperature is controlled at 100-160°C, the maximum pressure of the feeding is less than 0.35MPa; the feeding is completed. Curing between 120-160℃, when the curing pressure is close to 0.02MPa, nitrogen gas is introduced to keep the pressure at 0.15-0.25MPa. When the pressure in the reactor remains unchanged, the reaction ends; the maturation time is about 1-3h. At 120-135℃, vacuumize for 0.5-1h, cool down 70-80℃, add neutralizing reagent, adjust pH to 5-7, add 43g oleic acid, 2.1g p-toluenesulfonic acid, control temperature at 180-185℃, Dehydrate with a little nitrogen, and the maturation time is 5-7h. When the collected water is about 2.7g and the acid value is less than 0.8mgKOH/g, the product is obtained, which is marked as B3.

[0078] (4) Add 117g of B3 to the four-necked flask, add 240g of water, drop 7.5g of 37.5% hydrogen peroxide aqueous solution, and react at 70-80℃ for 6-8h. After the reaction is over, the aqueous solution is removed to obtain a High viscosity low viscosity droplet viscoelastic water-based polymer additive C3.

[0079] Weigh 60 g of the sample of Example C3, 10 g of silicone additive SP-4078, and 30 g of sulfosuccinic acid bis(2-ethylhexyl) sodium salt system (using isooctyl alcohol as the system). Mix and stir well at 70°C for 30 minutes to obtain a viscoelastic auxiliary composition with a transparent appearance. The sample is recorded as Example D3.