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Macromolecule chelating agent and preparation method thereof

A technology of polymer chelating agent and epichlorohydrin, which is applied in the direction of flocculation/sedimentation water/sewage treatment, etc., to achieve the effect of expanding application fields, easy access to raw materials, easy operation and control

Inactive Publication Date: 2014-04-16
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the above-mentioned technical problems existing in existing polymer chelating agents, the present invention provides a water-soluble iminodiacetic acid-type polymer chelating agent for removing various metal ions and a preparation method thereof

Method used

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  • Macromolecule chelating agent and preparation method thereof
  • Macromolecule chelating agent and preparation method thereof
  • Macromolecule chelating agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) According to the volume ratio of absolute ethanol and epichlorohydrin as 10:1, first add 158mL of absolute ethanol to a 500mL three-necked bottle with a reflux condenser and a mechanical stirrer, and then add 17.1g of imino di Acetonitrile was stirred until dissolved, then 15.8mL of epichlorohydrin was added dropwise, and reacted at 40°C for 6h;

[0030] (2) Keep the temperature at 40°C, add 14.4mL of NaOH solution with a mass percentage concentration of 45% to the solution in step (1) dropwise within 2h, continue to react for 1h after the dropwise addition, and then add 6.7mL of 6mol / L hydrochloric acid and excess NaOH, filtered to remove NaCl, then added 22.4mL diallylamine to the filtrate and continued the reaction at 70°C for 4h, distilled off the solvent to obtain 41.7g light yellow waxy solid;

[0031] (3) Add the solid obtained in step (2) to 365 mL of NaOH solution with a mass percent concentration of 4.5%, heat up to 95°C for hydrolysis for 0.5 h, add 12 mL...

Embodiment 2

[0033] (1) According to the volume ratio of absolute ethanol and epichlorohydrin as 15:1, first add 237mL of absolute ethanol to a 500mL three-necked bottle with a reflux condenser and a mechanical stirrer, and then add 18.1g of imino di Acetonitrile was stirred until dissolved, then 15.8mL epichlorohydrin was added dropwise, and reacted at 50°C for 5h;

[0034] (2) Keep the temperature at 50°C, add 13.3mL NaOH solution with a mass percentage concentration of 48% to the solution in step (1) dropwise within 2h, continue to react for 1h after the dropwise addition, and then add 6.7mL of 6mol / L hydrochloric acid and excess NaOH, filtered to remove NaCl, then added 23.6mL diallylamine to the filtrate to continue the reaction at 60°C for 4.5h, distilled off the solvent to obtain 43.6g light yellow waxy solid;

[0035] (3) Add the solid obtained in step (2) to 345 mL of NaOH solution with a mass percent concentration of 5%, heat up to 95° C. for hydrolysis for 1 h, add 12.7 mL of 6m...

Embodiment 3

[0037] (1) According to the volume ratio of absolute ethanol and epichlorohydrin as 20:1, first add 316mL of absolute ethanol to a 500mL three-necked bottle with a reflux condenser and a mechanical stirrer, then add 19g of iminodiacetonitrile Stir until dissolved, then add 15.8mL of epichlorohydrin dropwise, and react at 60°C for 4h;

[0038] (2) Keep the temperature at 60°C, add 12.6mL of 50% NaOH solution dropwise to the solution in step (1) within 2h, continue to react for 1h after the dropwise addition, and then add 6.7mL of 6mol / L hydrochloric acid and excess NaOH, filtered to remove NaCl, then added 24.9mL diallylamine to the filtrate and continued the reaction at 70°C for 4h, distilled off the solvent to obtain 45.6g light yellow waxy solid;

[0039] (3) Add the solid obtained in step (2) to 364 mL of NaOH solution with a mass percent concentration of 5%, heat up to 95° C. for hydrolysis for 1 h, add 13.3 mL of 6 mol / L hydrochloric acid to neutralize excess NaOH after c...

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Abstract

The invention discloses a macromolecule chelating agent and a preparation method thereof. The method enables iminodiacetonitrile and epoxy chloropropane to perform ring-opening reaction in absolute ethyl alcohol so as to enable the iminodiacetonitrile and the epoxy chloropropane to be cohered in the same molecule, NaOH is added to enable adjacent -OH and CI in the molecule to remove HCI under alkaline condition so as to generate epoxy group in closed-ring mode, the epoxy group and diallylamine perform ring-opening reaction to enable the diallylamine to be connected in the molecule, -CN group is hydrolyzed under alkaline condition to obtain carboxyl-COO-, and finally the macromolecule chelating agent is obtained by adopting radical aqueous solution polymerization. Each structure unit in the molecule of the macromolecule chelating agent contains a strong chelating group -N (CH2COO-)2 which can form chelate containing a plurality of stable five-membered rings with a plurality of kinds of metal ions. The method is wide in application range and particularly suitable for being combined with an ultra-filtration method to separate and extract rare metals and precious metals, efficient separation and enrichment of heavy metals, advanced treatment of waste water of heavy metals and the like.

Description

technical field [0001] The invention relates to a polymer chelating agent and a preparation method thereof, belonging to the fields of fine chemical industry and water treatment. Background technique [0002] A chelating agent refers to an organic compound that can coordinate with a central ion with multiple coordination atoms in the molecule to form a ring-shaped coordination compound. Chelating agents are widely used in industrial production and scientific research. For example, chelating agents can be widely used as stabilizing and coagulating agents, acidity regulators, moisture retention agents, antioxidants, and nutritional enhancers in the food industry. In the printing and dyeing process, it is generally necessary to bleach the fabric with hydrogen peroxide, Cu 2+ , Fe 2+ , Mn 2+ , Ni 2+ The presence of such metal ions can catalyze and accelerate the decomposition of hydrogen peroxide. Therefore, a hydrogen peroxide stabilizer must be added. Usually, sodium sili...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F126/02C02F1/56
Inventor 刘立华曾荣今曹菁唐安平周智华
Owner HUNAN UNIV OF SCI & TECH
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