Multi-carboxyl chelating agent as well as preparation method and application thereof
A chelating agent and polycarboxyl technology, applied in the field of polycarboxyl chelating agents and their preparation, can solve the problems of poor solubility of large molecular weight chelating agents, reducing the use of chemicals, large metal complex flocs, etc., and reducing the use of chemicals. Use, good sedimentation, excellent solubility
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[0031] Concrete, a kind of preparation method of polycarboxylate chelating agent comprises the following steps:
[0032] (1) Add dipentaerythritol and propionyl chloride into a three-necked flask, wherein the molar ratio of dipentaerythritol and propionyl chloride is 1:(3-3.1). After the addition is complete, stir the reaction at 35-45°C for 2-4 hours, and cool to room temperature. Neutralize with sodium hydroxide solution, wherein the concentration of the sodium hydroxide solution is 3-6% (mass fraction). Wash with water, extract with an organic solvent, and distill off the solvent under reduced pressure to obtain viscous liquid intermediate Ⅰ.
[0033] (2) Add the viscous liquid intermediate I obtained in step (1) into a four-necked flask, and the added amount of the viscous liquid intermediate I is 0.025 mol. Then add the first solvent dimethyl sulfoxide (DMSO) into the four-neck flask, and the added amount is 100 mL. After all the powder is dissolved, add powdered sodiu...
Embodiment 1
[0038] Add dipentaerythritol and propionyl chloride into a three-necked flask at a molar ratio of 1:3. After the addition is complete, stir and react at 40°C for 3h, and cool to room temperature. Neutralize with 5% (mass fraction) sodium hydroxide solution, wash with water, extract with organic solvent, and distill off the solvent under reduced pressure to obtain viscous liquid intermediate I. Take 0.025mol of the viscous liquid intermediate I and add it to the four-necked flask, then add 100mL dimethyl sulfoxide (DMSO) into the four-necked flask, and after it is completely dissolved, add 4g of powdered sodium hydroxide and stir the reaction at 30°C 0.5h, then add 0.05mol sodium chloroacetate into the solution containing dimethyl sulfoxide and other solvents, raise the temperature to 80°C, and react for 6h, then filter the above solution with suction to obtain the solid product Intermediate II. Add 0.02mol of solid product Intermediate II to 21.93g of dimethylformamide (DMF), ...
Embodiment 2
[0040]Add dipentaerythritol and propionyl chloride into a three-necked flask at a molar ratio of 1:3.02. After the addition is complete, stir and react at 40°C for 3h, and cool to room temperature. Neutralize with 5% (mass fraction) sodium hydroxide solution, wash with water, extract with organic solvent, and distill off the solvent under reduced pressure to obtain viscous liquid intermediate I. Take 0.025mol of the viscous liquid intermediate I and add it to the four-necked flask, then add 100mL dimethyl sulfoxide (DMSO) into the four-necked flask, and after it is completely dissolved, add 4g of powdered sodium hydroxide and stir the reaction at 30°C 0.5h, then add 0.05mol sodium chloroacetate into the solution containing dimethyl sulfoxide and other solvents, raise the temperature to 80°C, and react for 6h, then filter the above solution with suction to obtain the solid product Intermediate II. Add 0.02mol of solid product Intermediate II to 21.93g of dimethylformamide (DMF)...
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